HIGH PERMEABILITY SOFT MAGNETIC ALLOY AND METHOD FOR THE PRODUCTION OF A HIGH PERMEABILITY SOFT MAGNETIC ALLOY

Abstract
A soft magnetic alloy is provided. The soft magnetic alloy consists essentially of 5 wt %≤Co≤25 wt %, 0.3 wt %≤V≤5.0 wt %, 0 wt %≤Cr≤3.0 wt %, 0 wt %≤Si≤3.0 wt %, 0 wt %≤Mn≤3.0 wt %, 0 wt %≤Al≤3.0 wt %, 0 wt %≤Ta≤0.5 wt %, 0 wt %≤Ni≤0.5 wt %, 0 wt %≤Mo≤0.5 wt %, 0 wt %≤Cu≤0.2 wt %, 0 wt %≤Nb≤0.25 wt % and up to 0.2 wt % impurities.
Description
BACKGROUND
1. Technical Field

The present invention relates to a soft magnetic alloy, in particular a high permeability soft magnetic alloy.


2. Related Art

Non-grain-oriented electrical steel with approx. 3 wt % silicon (SiFe) is the most common crystalline soft magnetic material used in laminated cores in electric machines. As the electric-powered vehicle sector progresses, more efficient materials that performance better than SiFe are needed. In addition to sufficiently high electrical resistance, this signifies that a higher level of induction in particular is desirable to provide high torques and/or compact components.


Even more efficient materials are desirable for use in sectors such as the automotive industry and electric-powered vehicles. Soft magnetic cobalt-iron (CoFe) alloys are also used in electric machines due to their extremely high saturation induction. Commercially available CoFe alloys typically have a composition of 49 wt % Fe, 49 wt % Co and 2% V. In compositions of this type both a saturation induction of approx. 2.35 T and a high electrical resistance of 0.4 μΩm are achieved. It is, however, also desirable to reduce the material and production costs of CoFe alloys resulting, for example, from the high Co content, additional manufacturing steps and scrap content.


SUMMARY

The object of the present invention is therefore to provide an FeCo alloy that has lower material costs and is easy to work in order to reduce the production costs of the alloy, up to and including laminated cores, and at the same time to achieve high power density.


According to the invention, a soft magnetic alloy, in particular a high permeability soft magnetic FeCo alloy, is provided that consists essentially of:



















  5 wt %
≤Co
  ≤25 wt %



0.3 wt %
≤V
 ≤5.0 wt %



  0 wt %
≤Cr
 ≤3.0 wt %



  0 wt %
≤Si
 ≤3.0 wt %



  0 wt %
≤Mn
 ≤3.0 wt %



  0 wt %
≤Al
 ≤3.0 wt %



  0 wt %
≤Ta
 ≤0.5 wt %



  0 wt %
≤Ni
 ≤0.5 wt %



  0 wt %
≤Mo
 ≤0.5 wt %



  0 wt %
≤Cu
 ≤0.2 wt %



  0 wt %
≤Nb
 ≤0.25 wt %



  0 wt %
≤Ti
 ≤0.05 wt %



  0 wt %
≤Ce
 ≤0.05 wt %



  0 wt %
≤Ca
 ≤0.05 wt %



  0 wt %
≤Mg
 ≤0.05 wt %



  0 wt %
≤C
 ≤0.02 wt %



  0 wt %
≤Zr
 ≤0.1 wt %



  0 wt %
≤O
≤0.025 wt %



  0 wt %
≤S
≤0.015 wt %










residual iron, wherein Cr+Si+Al+Mn≤3.0 wt %, and up to 0.2 wt % of other impurities. The alloy has a maximum permeability μmax≥5,000, preferably μmax≥10,000, preferably μmax≥12.000, preferably μmax≥17,000. Other impurities include, for example, B, P, N, W, Hf, Y, Re, Sc, Be and other lanthanides other than Ce. (wt % denotes weight percent)


Owing to the lower Co content, the raw material costs of the alloy according to the invention are less than those of an alloy based on 49 wt % Fe, 49 wt % Co, 2% V. The invention provides for an FeCo alloy with a maximum cobalt content of 25 percent by weight that offers better soft magnetic properties, in particular appreciably higher permeability, than other FeCo alloys with a maximum cobalt content of 25 percent by weight such as the existing commercially available FeCo alloys e.g. VACOFLUX 17, AFK 18 and HIPERCO 15. These existing commercially available alloys have a maximum permeability of less than 5000.


The alloy according to the invention has no significant adjustment in order and can therefore, unlike alloys with over 30 wt % Co, be cold rolled without first undergoing a quenching process. Quenching is a difficult process to control, particularly where large quantities of materials are concerned, as it is hard to achieve sufficiently fast cooling rates and ordering with the resulting embrittlement of the alloy may therefore take place. The lack of an order-disorder transition in the alloy according to the invention simplifies industrial-scale production.


Marked order-disorder transitions in alloys like that observed in CoFe alloys with a Co content greater than 30 wt % can be determined by means of differential scanning calorimetry (DSC) because they cause a peak in the DSC measurement. No such peak is observed in a DSC measurement carried out under the same conditions for the alloy according to the invention.


At the same time, however, in addition to an appreciably higher permeability level never previously attained for this type of alloy, this new alloy offers both significantly lower hysteresis losses than previously known commercially available alloys with Co contents of between 10 and 30 wt % and higher saturation. The FeCo alloy according to the invention can also produced cost-effectively on an industrial scale.


Owing to its higher permeability, the alloy according to the invention can be used in applications such as rotors and stators in electric motors in order to reduce the size of the rotor or stator and thus of the electric motor, and/or to increase output. For example, it makes it possible to generate a higher torque at the same physical size and/or weight, a solution that would prove advantageous if used in electrically-powered or hybrid motor vehicles.


In addition to a maximum permeability μmax≥5,000, preferably μmax≥10,000, preferably μmax≥12.000, preferably μmax≥17,000, the alloy can also have an electrical resistance ρ≥0.25 μΩm, preferably ρ≥0.30 μΩm, and/or hysteresis losses PHys≤0.07 J/kg, preferably hysteresis losses PHys≤0.06 J/kg, preferably hysteresis losses PHys≤0.05 J/kg, at an amplitude of 1.5 T, and/or coercive field strength Hc of ≤0.7 A/cm, preferably a coercive field strength Hc of ≤0.6 A/cm, preferably a coercive field strength Hc of ≤0.5 A/cm, preferably Hc of ≤0.4 A/cm, preferably Hc of ≤0.3 A/cm, and/or an induction B≥1.90 T at 100 A/cm, preferably B≥1.95 T at 100 A/cm, preferably B≥2.00 T at 100 A/cm.


The hysteresis losses PHys are determined from the re-magnetisation losses P at an amplitude of induction of 1.5 T across the y-axis intercept in a plot P/f over the frequency f by linear regression. The linear regression is carried out using at least 8 measured values distributed approximately evenly over a frequency range of 50 Hz to 1 kHz (e.g. at 50, 100, 200, 300, 400, 500, 600, 700, 800, 900 and 1000 Hz).


In one embodiment, the alloy has a maximum permeability μmax≥μmax≥10,000, an electrical resistance ρ≥0.28 μΩm, hysteresis losses PHys≤0.055 J/kg at an amplitude of 1.5 T, a coercive field strength Hc of ≤0.5 A/cm and an induction B≥1.95 T at 100 A/cm. This combination of properties is particularly advantageous for use as or in a rotor or stator of an electric motor in order to reduce the size of the rotor or stator and thus of the electric motor, and/or to increase output, or to generate higher torque at the same weight.


The soft magnetic alloy can therefore be used in an electric machine, e.g. as or in a stator and/or rotor of an electric motor and/or generator, and/or in an transformer and/or in an electromagnetic actuator. It can be provided in the form of a sheet with a thickness of 0.5 mm to 0.05 mm, for example. A plurality of sheets made of the alloy can be stacked together to form a laminated core to be used as a stator or rotor.


The alloy according to the invention has an electrical resistance of at least 0.25 μΩm, preferably a minimum of 0.3 μΩm. Eddy current losses can be reduced to a lower level by selecting a slightly smaller strip thickness.


The composition of the soft magnetic alloy is set out in greater detail in further embodiments, with 10 wt %≤Co≤20 wt %, preferably 15 wt %≤Co≤20 wt % and 0.3 wt %≤V≤5.0 wt %, preferably 1.0 wt %≤V≤3.0 wt %, preferably 1.3 wt %≤V≤2.7 wt % and/or 0.1 wt %≤Cr+Si≤2.0 wt %, preferably 0.2 wt %≤Cr+Si≤1.0 wt %, preferably 0.25 wt %≤Cr+Si≤0.7 wt %.


In one embodiment, the sum is defined in greater detail, with 0.2 wt %≤Cr+Si+Al+Mn≤1.5 wt %, preferably 0.3 wt %≤Cr+Si+Al+Mn≤0.6 wt %.


The soft magnetic alloy may also contain silicon, with 0.1 wt %≤Si≤2.0 wt %, preferably 0.15 wt %≤Si≤1.0 wt %, preferably 0.2 wt %≤Si≤0.5 wt %.


Aluminium and silicon can be interchanged such that in one embodiment the total Si and Al (Si+Al) is 0 wt %≤(Si+Al)≤3.0 wt %.


The alloys according to the invention are almost carbon-free and contain at most 0.02 wt % carbon, preferably ≤0.01 wt % carbon. This maximum carbon content should be regarded as an unavoidable impurity.


In the alloys according to the invention calcium, beryllium and/or magnesium may be added in small amounts of up to 0.05 wt % only for deoxidation and desulphurisation. In order to achieve particularly good deoxidation, it is possible to add up to 0.05 wt % cerium or cerium Mischmetal.


According to the invention, the improved magnetic properties can be achieved by heat treatment geared to the composition as described below. It has been shown, in particular, that ascertaining the phase transition temperatures for the selected compositions and determining the heat treatment temperatures and cooling rate in relation to the phase transition temperatures thus ascertained leads to improved magnetic properties. The fact that the alloys according to the invention with a cobalt content of at most 25 percent by weight have no order-disorder transition so that the manufacturing process does not require quenching to avoid ordering and the resulting embrittlement, is also taken into account.


Conventionally, CoFe alloys are used in strip thicknesses ranging from 0.50 mm to a thin 0.050 mm. In processing the strip, the material is conventionally hot rolled and then cold rolled to its final thickness. During cooling after hot rolling an embrittling adjustment in order takes place at approx. 730° C. and to ensure sufficient cold rollability special intermediate annealing followed by quenching is therefore also required to suppress the adjustment in order. The alloy according to the invention does requires no quenching since it has no order-disorder transition. This simplifies production.


To achieve the magnetic properties, CoFe alloys are subjected to a final heat treatment also referred to as final magnetic annealing. The stock is heated to the annealing temperature, held at the annealing temperature for a certain length of time and then cooled at a defined speed. It is advantageous to carry out this final annealing at the highest possible temperatures and in a clean, dry hydrogen atmosphere since at high temperatures, firstly, the reduction of impurities by means of hydrogen is more efficient and, secondly, the grain structure becomes rougher and so soft magnetic properties such as coercive field strength and permeability improve. In practice, the annealing temperature in the CoFe system has an upper limit since a phase transition from the magnetic and ferritic BCC phase to the non-magnetic and austenitic FCC phase takes place at approx. 950° C. in the binary system. When elements are added to the alloy, a two-phase region in which both phases coexist occurs between the FCC phase and the BCC phase. The transition between the BCC phase and the mixed two-phase or BCC/FCC region occurs at a temperature TÜ1 and the transition between the two-phase region and the FCC phase occurs at a temperature TÜ2, where TÜ2>TÜ1. The position and size of the two-phase region also depends on the nature and scope of the alloy making process. If annealing takes place in the two-phase region or in the FCC region, remnants of the FCC phase may impair the magnetic properties after cooling and incomplete retransformation. Even if retransformation is complete, the additional grain boundaries created have an damaging effect since coercive field strength behaves inversely proportionately to grain diameter. Consequently, the known commercial available alloys with Co contents of approx. 20 wt % undergo final annealing at temperatures below the two-phase BCC+FCC region. As a result, the recommendation for AFK 18 is 3 h/850° C. and that for AFK 1 is 3 h/900° C., for example. The recommendation for VACOFLUX 17 is 10 h/850° C. At such low final annealing temperatures and owing to the relatively high magneto-crystalline anisotropy (K1 approx. 45,000 J/m3 at 17 wt % Co), the potential for particularly good soft magnetic properties in these FeCo alloys is limited.


With VACOFLUX 17 strip, for example, the maximum permeability that can be reached at a typical coercive field strength of 1 A/cm is approx. 4,000 and its application is therefore limited.


In contrast to these known final annealing processes, the composition according to the invention permits a heat treatment that produces better magnetic properties than the standard single-step annealing with furnace cooling used with FeCo alloys, irrespective of the temperature range in which the single-step annealing takes place. The additives are selected such that the lower limit of the two-phase region and the BCC/FCC phase transition are pushed upwards to allow annealing at high temperatures, e.g. above 925° C. in the BCC-only region. Annealing heat treatments at such high temperatures are not conceivable with the FeCo alloys known to date. Moreover, the width of the two-phase region, i.e. the difference between the lower transition temperature TÜ1 and the upper transition temperature TÜ2 is kept as narrow as possible owing to the composition according to the invention. As a result, the advantages of high final annealing, i.e. the removal of potential magnetically unfavourable textures, the cleaning effect in H2 and the growth of large grains, are maintained by final annealing above the two-phase region in conjunction with cooling through the two-phase region followed by a holding period or controlled cooling in the BCC-only region without the risk of magnetically damaging remnants of the FCC phase.


It has been found that compositions with a phase transition between the BCC-only region and the mixed BCC/FCC region exhibit appreciably improved magnetic properties at higher temperatures, e.g. above 925° C., and with a narrow two-phase region, e.g. of less than 45K. Compositions with this specific combination of phase diagram features are selected according to the invention and heat treated accordingly in order to guarantee a high permeability of greater than 5000 or greater than 10,000.


Vanadium was identified as one of the most effective elements in an Fe—Co alloy, increasing electrical resistance and at the same time pushing the two-phase region up to higher temperatures. With a lower Co content, vanadium is more efficient at increasing transition temperatures. With the Fe-17Co alloy, it is even possible to increase the transition temperatures above the value of the binary FeCo composition by adding approx. 2% vanadium.


In the Fe—Co system, from approx. 15% cobalt the BCC/FCC phase transformation takes place at temperatures lower than the Curie temperature. Since the FCC phase is paramagnetic, the magnetic phase transition is now determined by the BCC/FCC phase transformation rather than the Curie temperature. Sufficiently large amounts of vanadium push the BCC/FCC phase transformation over the Curie temperature Tc, making the paramagnetic BCC Ophase visible.


However, if the vanadium content is too high, the width of the mixed region is increased. These compositions have lower maximum permeability values even though the phase transition between the mixed BCC/FCC region and the BCC-only region takes place at higher temperatures. Consequently, it has been established that that the composition has an influence both on the temperatures at which the phase transitions take place and on the width of the mixed region, and should therefore be taken into account when selecting the composition. In order to achieve the highest permeability values, the heat treatment temperatures can be selected in relation to the temperatures at which the phase transitions for this composition take place.


It has thus been found that a more precise determination of the temperatures at which the phase transitions take place is advantageous for a certain composition wen optimising the production process. These temperatures can be determined by means of differential scanning calorimetry (DSC) measurements. The DSC measurement can be carried out with a sample mass of 50 mg and at a DSC heating rate of 10 Kelvin per minute, and the phase transition temperatures thus determined can be used when heating and cooling the sample to determine the temperatures for heat treatment.


Chromium and other elements can be added in order, for example, to improve electrical resistance or mechanical properties. Like most other elements, chromium reduces the two-phase region of the binary Fe-17Co alloy. As a result, the amount of element to be added in addition to vanadium is preferably selected such together with vanadium it produces an increase in the two-phase region as compared to the binary FeCo alloy. In addition, the impurities and elements that have a particularly strong stabilising affect on the austenite (e.g. nickel) must be kept as low as possible.


The following contents have proved preferable in achieving very good magnetic properties:


cobalt content of 5 wt %≤Co≤25 wt %, with contents of 10 wt %≤Co≤20 wt % being preferred and contents of 15 wt %≤Co≤20 wt % being very particularly preferred;


vanadium content of 0.3 wt %≤V≤5.0 wt %, with contents of 1.0 wt %≤V≤3.0 wt % being preferred, and the following sum: 0.2 wt %≤Cr+Si+Al+Mn≤3.0 wt %.


The alloys according to the invention are almost carbon-free and have at most 0.02 wt % carbon, preferably ≤0.01 wt % carbon. This maximum carbon content should be regarded as an unavoidable impurity.


Only small amounts of calcium, beryllium and/or magnesium up to 0.05 wt % can be added to the alloys according to the invention for deoxidation and desulphurisation.


To achieve particularly good deoxidation and desulphurisation up to 0.05 wt % Cer or misch metal can be added.


The composition according to the invention allows a further improvement. Cobalt has a higher diffusion coefficient in the paramagnetic BCC phase than in the ferromagnetic BCC phase. As a result, by separating the two-phase region and the Curie temperature Tc, vanadium allows a further temperature range with high self diffusion, thereby allowing a larger BCC grain structure and thus better soft magnetic properties due to heat treatment in this range or cooling through this range. In addition, the separation of two-phase region and Curie temperature Tc signifies that during cooling both the passage through the two-phase BCC/FCC region and the transition to the region of the BCC-only phase take place completely in the paramagnetic state. This also has a positive effect on the soft magnetic properties.


According to the invention, a method is provided for the production of a soft magnetic FeCo alloy, this method comprising the following. A preliminary product (precursor) is provided with a composition consisting substantially of:



















  5 wt %
≤Co
  ≤25 wt %



0.3 wt %
≤V
 ≤5.0 wt %



  0 wt %
≤Cr
 ≤3.0 wt %



  0 wt %
≤Si
 ≤3.0 wt %



  0 wt %
≤Mn
 ≤3.0 wt %



  0 wt %
≤Al
 ≤3.0 wt %



  0 wt %
≤Ta
 ≤0.5 wt %



  0 wt %
≤Ni
 ≤0.5 wt %



  0 wt %
≤Mo
 ≤0.5 wt %



  0 wt %
≤Cu
 ≤0.2 wt %



  0 wt %
≤Nb
 ≤0.25 wt %



  0 wt %
≤Ti
 ≤0.05 wt %



  0 wt %
≤Ce
 ≤0.05 wt %



  0 wt %
≤Ca
 ≤0.05 wt %



  0 wt %
≤Mg
 ≤0.05 wt %



  0 wt %
≤C
 ≤0.02 wt %



  0 wt %
≤Zr
 ≤0.1 wt %



  0 wt %
≤O
≤0.025 wt %



  0 wt %
≤S
≤0.015 wt %










residual iron, where Cr+Si+Al+Mn≤3.0 wt %, and up to 0.2 wt % of other impurities due to melting. The other impurities may, for example, be one or more of the elements B, P, N, W, Hf, Y, Re, Sc, Be or other lanthanides other than Ce. In some embodiments the preliminary product has a cold-rolled texture or a fibre texture.


The preliminary product or the parts manufactured from the preliminary product are heat treated. In one embodiment, the preliminary product is heat treated at a temperature T1 and then cooled down from T1 to room temperature.


In an alternative embodiment, the preliminary product is heat treated at a temperature T1, then cooled down to a temperature T2 that is above room temperature, and further heat treated at temperature T2, where T1>T2. The preliminary product is not cooled to room temperature until it has been heat treated at temperature T2.


The preliminary product has a phase transition from a BCC phase region to a mixed BCC/FCC region to a FCC phase region, as the temperature increases the phase transition between the BCC phase region and the mixed BCC/FCC region taking place at a first transition temperature TÜ1 and, as the temperature continues to increase, the transition between the mixed BCC/FCC region and the FCC phase region taking place at a second transition temperature TÜ2, where TÜ2>TÜ1. Temperature T1 is above TÜ2 and temperature T2 is below TÜ1.


The transition temperatures TÜ1 and TÜ2 are dependent on the composition of the preliminary product. The transition temperatures TÜ1 and TÜ2 can be determined by means of DSC measurements, the transition temperature TÜ1 being determined during heating and the transition temperature TÜ2 being determined during cooling. In one embodiment, at a sample mass of 50 mg and a DSC heating rate of 10 Kelvin per minute the transition temperature TÜ1 is above 900° C., preferably above 920° C., and preferably above 940° C.


In one embodiment, the solidus temperature of the preliminary product is taken into account when selecting temperatures T1 and T2. In one embodiment, 900° C.≤T1<Tm, preferably 930° C.≤T1<Tm, preferably 940° C.≤T1<Tm, preferably 960° C.≤T1<Tm, and 700° C.≤T2≤1050° C. and T2<T1, Tm being the solidus temperature.


In one embodiment, the difference TÜ2−TÜ1 is less than 45K, preferably less than 25K.


In one embodiment, the cooling rate over at least the temperature range from T1 to T2 is 10° C./h to 50,000° C./h, preferably 10° C./h to 900° C./h, preferably 20° C./h to 1000° C./h, preferably 20° C./h to 900° C./h, preferably 25° C./h to 500° C./h. This cooling rate can be used with both of the heat treatments described above.


In one embodiment, the difference TÜ2−TÜ1 is less than 45K, preferably less than 25K, T1 is above TÜ2 and T2 is below T, 940° C.≤T1<Tm, where 700° C.≤T2≤1050° C. and T2<T1, Tm being the solidus temperature, and the cooling rate is 10° C./h to 900° C./h at least over the temperature range T1 to T2. This combination of properties of the alloy, i.e. TÜ2 and TÜ1, can be used with the heat treatment temperatures T1 and T2 to achieve particularly high permeability rates.


In one embodiment, the preliminary product is heat treated at above TÜ2 for a period of over 30 minutes and then cooled to T2.


In one embodiment, the preliminary product is heat treated at T1 for a period t, where 15 minutes≤t1≤20 hours, and then cooled from T1 to T2. In one embodiment, the preliminary product is cooled from T1 to T2, heat treated at T2 for a period t2, where 30 minutes≤t2≤20 hours, and then cooled from T2 to room temperature.


In embodiments in which the preliminary product is cooled down from T1 to room temperature, the preliminary product may than be heated up from room temperature to T2 and heat treated at T2 according to one of the embodiments described here.


As the alloy has no order-disorder transition, no quenching is carried out over the temperature range from 800° C. to 600° C. The cooling rate from 800° C. to 600° C. may, for example, be between 100° C./h and 500° C./h. However, a slower cooling rate can, in principle, also be chosen. The aforementioned cooling rates can also quite easily be carried out until room temperature is reached.


The preliminary product can be cooled from T1 to room temperature at a rate of 10° C./h to 50,000° C./h, preferably from 10° C./h to 1000° C./h, preferably from 10° C./h to 900° C./h, preferably from 25° C./h to 900° C./h, preferably from 25° C./h to 500° C./h.


The cooling rate from T2 to room temperature has less influence on magnetic properties so the preliminary product can be cooled from T2 to room temperature at a rate of 10° C./h to 50,000° C./h, preferably 100° C./h to 1000° C./h.


In a further alternative embodiment, the preliminary product is cooled from T1 to room temperature at a cooling rate of 10° C./h to 900° C./h. In embodiments with slow cooling from T1 to room temperature, e.g. with a cooling rate of less than 500° C./h, preferably less than 200° C./h, a further heat treatment at temperature T2 can be dispensed with.


Following heat treatment, the soft magnetic alloy may have the following combinations of properties:


a maximum permeability μmax≥5,000, and/or an electrical resistance ρ≥0.25 μΩm, and/or hysteresis losses PHys≤0.07 J/kg at an amplitude of 1.5 T, a coercive field strength Hc of ≤0.7 A/cm and an induction B≥1.90 T at 100 A/cm, or


a maximum permeability μmax≥10,000, and/or an electrical resistance ρ≥0.25 μΩm, and/or hysteresis losses PHys≤0.06 J/kg at an amplitude of 1.5 T, and/or a coercive field strength Hc of ≤0.6 A/cm, preferably Hc≤0.5 A/cm and/or an induction B≥1.95 T at 100 A/cm, or


a maximum permeability μmax≥≥12.000, preferably μmax≥17,000 and/or an electrical resistance ρ≥0.30 μΩm, and/or hysteresis losses PHys≤0.05 J/kg at n amplitude of 1.5 T, and/or a coercive field strength Hc of ≤0.5 A/cm, preferably Hc≤0.4 A/cm, preferably Hc≤50.3 A/cm and/or an induction B≥2.00 T at 100 A/cm.


In certain embodiments the soft magnetic alloy has one of the following combinations of properties:


a maximum permeability μmax≥5,000, an electrical resistance ρ≥0.25 μΩm, hysteresis losses PHys≤0.07 J/kg at n amplitude of 1.5 T, a coercive field strength Hc of ≤0.7 A/cm and an induction B≥1.90 T at 100 A/cm, or


a maximum permeability μmax≥10,000, an electrical resistance ρ≥0.25 μΩm, hysteresis losses PHys≤0.06 J/kg at an amplitude of 1.5 T, a coercive field strength Hc of ≤0.6 A/cm and an induction B≥1.95 T at 100 A/cm, or


a maximum permeability μmax≥12.000, an electrical resistance ρ≥0.28 μΩm, hysteresis losses PHys≤0.05 J/kg at an amplitude of 1.5 T, a coercive field strength Hc of ≤0.5 A/cm and an induction B≥2.00 T at 100 A/cm,


a maximum permeability μmax≥17,000, an electrical resistance ρ≥0.30 μΩm, hysteresis losses PHys≤0.05 J/kg at an amplitude of 1.5 T, a coercive field strength Hc of ≤0.4 A/cm, preferably Hc of ≤0.3 A/cm and an induction B≥2.00 T at 100 A/cm.


In one embodiment, the maximum difference in coercive field strength Hc after heat treatment measured parallel to the direction of rolling, measured diagonally (45°) to the direction of rolling or measured perpendicular to the direction of rolling between two of these directions is at most 6%, preferably at most 3%. In other words, the maximum difference in coercive field strength Hc measured parallel to the direction of rolling and measured diagonally (45°) to the direction of rolling is at most 6%, preferably at most 3%, and/or the maximum difference in coercive field strength Hc measured parallel to the direction of rolling and measured perpendicular to the direction of rolling is at most 6%, preferably at most 3%, and/or the maximum difference in the coercive field strength Hc measured diagonally (45°) to the direction of rolling or measured perpendicular to the direction of rolling between these two directions is at most 6%, preferably at most 3%. In rotor and stator applications, this anisotropy, which is extremely low for soft magnetic FeCo alloys, leads to uniform properties along the periphery and there is therefore no need to rotate rotor and stator sheets by layer to provide sufficient isotropy of the magnetic properties in the laminated core.


The heat treatment may be carried out in a hydrogen-containing atmosphere or in an inert gas.


In one embodiment, heat treatment is carried out in a stationary furnace at T1 and in a stationary furnace or a continuous furnace at T2. In another embodiment, heat treatment is carried out in a continuous furnace at T1 and in a stationary furnace or a continuous furnace at T2.


Prior to heat treatment the preliminary product may have a cold-rolled texture or a fibre texture.


The preliminary product may be provided in the form of a strip. At least one strip may be manufactured from the strip by stamping, laser cutting or water jet cutting. In one embodiment, heat treatment is carried out on stamped, laser-cut, electrical discharge machined or water jet-cut laminations manufactured from the strip material.


In one embodiment, after heat treatment a plurality of sheets are stuck (adhered) together using insulating adhesive to form a laminated core, or surface oxidized to form an insulating layer and then stuck, or laser welded together to form a laminated core, or coated with an inorganic-organic hybrid coating and then processed further to form a laminated core.


In some embodiments, the preliminary product takes the form of a laminated core and the laminated core is heat treated according to one of the embodiments described here. The heat treatment can thus be carried out on stamp bundled cores (progressively stacked cores) or welded laminated cores manufactured from laminations.


The preliminary product can be produced as follows. A molten mass may, for example, be provided by vacuum induction melting, electroslag remelting or vacuum arc remelting, this molten mass consisting substantially of:



















  5 wt %
≤Co
  ≤25 wt %



0.3 wt %
≤V
 ≤5.0 wt %



  0 wt %
≤Cr
 ≤3.0 wt %



  0 wt %
≤Si
 ≤3.0 wt %



  0 wt %
≤Mn
 ≤3.0 wt %



  0 wt %
≤Al
 ≤3.0 wt %



  0 wt %
≤Ta
 ≤0.5 wt %



  0 wt %
≤Ni
 ≤0.5 wt %



  0 wt %
≤Mo
 ≤0.5 wt %



  0 wt %
≤Cu
 ≤0.2 wt %



  0 wt %
≤Nb
 ≤0.25 wt %



  0 wt %
≤Ti
 ≤0.05 wt %



  0 wt %
≤Ce
 ≤0.05 wt %



  0 wt %
≤Ca
 ≤0.05 wt %



  0 wt %
≤Mg
 ≤0.05 wt %



  0 wt %
≤C
 ≤0.02 wt %



  0 wt %
≤Zr
 ≤0.1 wt %



  0 wt %
≤O
≤0.025 wt %



  0 wt %
≤S
≤0.025 wt %










residual iron, where Cr+Si+Al+Mn≤3.0 wt %, and up to 0.2 wt % of other impurities.


Other impurities may be one or more of the other B, P, N, W, Hf, Y, Re, Sc, Be or other lanthanides other than Ce. The molten mass is solidified to form an ingot and the ingot is mechanically formed to form a preliminary product with final dimensions, this mechanical forming being carried out by means of hot rolling and/or forging and/or cold forming.


In one embodiment, the ingot is mechanically formed to form a slab with a thickness D1 by means of hot rolling at temperatures between 900° C. and 1300° C. and then mechanically formed to form a strip with a thickness D2 by means of cold rolling, where 1.0 mm≤D1≤5.0 mm and 0.05 mm≤D2≤1.0 mm, where D2<D1. The degree of cold working by cold rolling may be >40%, preferably >80%.


In one embodiment, the ingot is mechanically formed to form a billet by means of hot rolling at temperatures between 900° C. and 1300° C. and then mechanically formed to form a wire by means of cold drawing. The degree of cold working due to cold drawing may be >40%, preferably >80%.


Intermediate annealing may be carried out in a continuous furnace or a stationary furnace at an intermediate dimension in order to reduce work hardening and so to set the desired degree of cold working.


The Curie temperature of the alloy may be taken into account when selecting the temperatures T1 and/or T2. For example, TÜ1>Tc, where Tc is the Curie temperature and Tc≥900° C. In one embodiment, TÜ1>T2>Tc.


In compositions in which there is a separation of the two-phase region and the Curie temperature Tc, there is a further temperature range with higher self diffusion. This allows a larger BCC grain structure and thus better soft magnetic properties as a result of heat treatment in this region or cooling through this region. The separation of the two-phase region and the Curie temperature Tc also signifies that during cooling both the passage through the two-phase BCC/FCC region and the transition to the BCC-only phase region take place entirely in the paramagnetic state. The soft magnetic properties can be further improved by selecting temperature T2 so that TÜ1>T2>Tc.


In one embodiment, the average grain size after final annealing is at least 100 μm, preferably at least 200 μm, preferably at least 250 μm.


In one embodiment, the measured density of the annealed alloy is more than 0.10% lower than the density calculated using the rule of three from the average atomic weight of the metallic elements of the alloy, the average atomic weight of the metallic elements of the corresponding binary FeCo alloy and the measured density of this annealed binary FeCo-alloy.


Owing to the heat treatment, the sulphur content in the finished alloy may be lower than that in the molten mass. For example, the upper limit of the sulphur content in the molten mass may be 0.025 percent by weight, while in the finished soft magnetic alloy the upper limit is 0.015 percent by weight.


In one embodiment, the preliminary product is also coated with an oxide layer for electrical insulation. This embodiment may, for example, be used if the preliminary product is used in a laminated core. The laminations or the laminated core can be coated with an oxide layer. The preliminary product may be coated with a layer of magnesium methylate or preferably zirconium propylate that transforms into an insulating oxide layer during heat treatment. The preliminary product may be heated treated in an atmosphere containing oxygen or water vapour to form an electrically insulating layer.


In one embodiment, laminations stamped, laser-cut or electrical discharge machined from the preliminary product are also subjected to final annealing, after which the annealed single sheets are then stuck together by means of an insulating adhesive to form a laminated core, or the annealed single sheets are surface-oxidised to form an insulating layer and then stuck, welded or laser-welded together to form a laminated core, or the annealed single sheets are coated with an inorganic-organic hybrid coating such as Remisol C5, for example, and then further processed to form a laminated core.


The soft magnetic alloy according to any one of the preceding embodiments, which can be produced using any one of the methods described here, may be used in an electric machine, e.g. as or in a stator and/or rotor of an electric motor and/or a generator, and/or in a transformer and/or in an electromagnetic actuator.





BRIEF DESCRIPTION OF THE DRAWINGS

Embodiments of the invention are described in greater detail below with reference to the drawings and the following examples.



FIG. 1 shows a schematic illustration (not to scale) of three variants of the heat treatment according to the invention.



FIG. 2 shows a typical course of a DSC heating and cooling curve during phase transition using the example of batch 930423.



FIG. 3 shows an illustration of the first onset temperatures of the phase transition of the Fe-17Co—Cr—V alloys according to the invention with increasing V content in comparison to the binary Fe-17Co molten mass for heating (DSC) and cooling (DSC). The course of maximum permeability μmax is plotted against a second y-axis.



FIG. 4 shows coefficients of the induction value B after multi-linear regression.



FIG. 5 shows coefficients of electrical resistance after multi-linear regression.



FIG. 6 shows coercive field strength Hc of batch 930329 (Fe-17Co1.5V-0.5Cr) as a function of the reciprocal of the grain diameter d for various annealing processes.



FIG. 7 shows the transition temperatures TÜ1 and TÜ2 and the best coercive field strength Hc achieved for this Fe-17Co special molten mass with different V contents for various batches. The alloys also contain up to a total of 0.6 wt % of Cr and/or Si. The data for FIG. 7 including details of the corresponding annealing process are given in Table 29.



FIG. 8 shows maximum permeability and coercive field strength after step annealing in the first annealing step.



FIG. 9 shows maximum permeability and coercive field strength after step annealing in the second annealing step below the phase transition after a previous first annealing step of 4 h at 1000° C. above the phase transition.



FIG. 10 shows the coercive field strength Hc of batches 930329 (Fe-17Co-0.5Cr-1.5V) und 930330 (Fe-17Co-2.0V) dependent on the degree of cold working.



FIG. 11 shows (200) pole figures for batch 93/0330 (Fe-17Co-2V).

    • a) Cold formed: top left
    • b) After final annealing at 910° C. for 10 h: top centre
    • c) After final annealing at 1050° C. for 4 h: top right
    • d) After final annealing at 1050° C. for 4 h and 910° C. for 10 h: bottom



FIG. 12 shows the coercive field strength Hc of batch 930330 (Fe-17Co-2V) measured parallel to the direction of rolling (“longitudinally”), at 45° to the direction of rolling and perpendicular to the direction of rolling (“transversely”) for the specified annealing.



FIG. 13 shows the coercive field strength Hc of batch 930335 (Fe-23Co-2V) measured parallel to the direction of rolling (“longitudinally”), at 45° to the direction of rolling and perpendicular to the direction of rolling (“transversely”) for the specified annealing.



FIG. 14 shows new curves for batches 930329 (Fe-17Co-1.5V-0.5Cr), 930505 (Fe-17Co-1.4V-0.4Si) and 930330 (Fe-17Co-2V) according to the invention after optimum annealing in comparison to a typical SiFe alloy (TRAFOPERM N4) and a typical FeCo alloy.



FIG. 15 shows the permeability of batches 930329 (Fe-17Co-1.5V-0.5Cr), 930505 (Fe-17Co-1.4V-0.4Si) and 930330 (Fe-17Co-2V) according to the invention after optimum annealing in comparison to a typical SiFe alloy (TRAFOPERM N4) and typical FeCo alloys.



FIG. 16 shows losses of batches 930329 (Fe-17Co-1.5V-0.5Cr) and 930330 (Fe-17Co-2V) according to the invention after optimum annealing at an induction amplitude of 1.5 T in comparison to a typical SiFe alloy (TRAFOPERM N4) and FeCo alloys. In each case the sheet thickness was 0.35 mm.



FIG. 17 shows a diagram of maximum permeability as a function of the relative density difference Δρ for Fe-17Co-based alloys for the data in Table 25.





DETAILED DESCRIPTION OF EXAMPLE EMBODIMENTS

According to the invention, a soft magnetic alloy is provided that consists essentially of:



















  5 wt %
≤Co
  ≤25 wt %



0.3 wt %
≤V
 ≤5.0 wt %



  0 wt %
≤Cr
 ≤3.0 wt %



  0 wt %
≤Si
 ≤3.0 wt %



  0 wt %
≤Mn
 ≤3.0 wt %



  0 wt %
≤Al
 ≤3.0 wt %



  0 wt %
≤Ni
 ≤0.5 wt %



  0 wt %
≤Mo
 ≤0.5 wt %



  0 wt %
≤Ta
 ≤0.5 wt %



  0 wt %
≤Cu
 ≤0.2 wt %



  0 wt %
≤Nb
 ≤0.25 wt %



  0 wt %
≤Ti
 ≤0.05 wt %



  0 wt %
≤Ce
 ≤0.05 wt %



  0 wt %
≤Ca
 ≤0.05 wt %



  0 wt %
≤Mg
 ≤0.05 wt %



  0 wt %
≤C
 ≤0.02 wt %



  0 wt %
≤Zr
 ≤0.1 wt %



  0 wt %
≤O
≤0.025 wt %



  0 wt %
≤S
≤0.015 wt %












    • residual iron,





and up to 0.2 wt % of other impurities due to melting. The impurities may, for example, be one or more of the elements B, P, N, W, Hf, Y, Re, Sc, Be or other lanthanides other than Ce.


In order to increase electrical resistance, it is also possible, in addition to the alloy element vanadium, to add one or more of the group of Cr, Si, Al and Mn in an amount that satisfies the following sum:





0.05 wt %≤Cr+Si+Al+Mn≤3.0 wt %.


The alloy according to the present invention is preferably melted in vacuum induction furnaces, though it can also be processed using vacuum arc remelting or electroslag remelting. The molten mass first solidifies into an ingot from which the oxide skin is removed and then forged or hot rolled at temperatures between 900° C. and 1300° C. Alternatively, the removal of the oxide skin can also take place on bars that have previously been forged or hot rolled. The desired dimensions can be achieved by hot working strips, billets or bars. Surface oxides can be removed from hot rolled stock by blasting, grinding or stripping. Alternatively, however, the desired final dimensions can also be achieved by cold working strips, bars or wires. In the case of cold rolled strips, a grinding process can be integrated to remove embedded oxides caused by the hot rolling process. If cold working leads to excessive solidification, one or more intermediate annealing processes may be carried out at temperatures between 400° C. and 1300° C. for recovery and re-crystallisation. The thickness or diameter for the intermediate annealing should be selected such that cold working of preferably >40%, particularly preferably >80%, is achieved by the final thickness.


The last processing step is heat treatment at temperatures between 700° C. and the solidus temperature Tm (typically at most 1200° C.), which is also referred to as final magnetic annealing. Final annealing is preferably carried out in a clean, dry hydrogen atmosphere. Annealing in an insert gas or vacuum is also possible. FIG. 1 shows a schematic illustration of three variants of the heat treatment according to the invention in relation to the phase transitions and in particular to the FCC, FCC+BCC and BCC regions.


In variant 1, which is illustrated by the continuous line in FIG. 1, a first annealing step in the FCC region is followed immediately by a second annealing step in the BCC region. The second annealing step is optional and can be used to further improve soft magnetic properties, in particular permeability and hysteresis losses. In variant 2, which is illustrated by the broken line in FIG. 1, the first annealing step in the FCC region is followed by cooling to room temperature. The second annealing step in the BCC region takes place at a later stage. In variant 3, which is illustrated by the dotted line in FIG. 1, the annealing step in the FCC region is followed by controlled cooling to room temperature. This type of controlled cooling can also take place in variant 1 during cooling from the first step to the second step (not shown in FIG. 1).


According to the invention, annealing may therefore take place either in two steps or by controlled cooling from a temperature above the upper transition temperature. Controlled cooling signifies that there is a defined cooling rate for creating the optimum soft magnetic properties. In all cases, one of the annealing steps takes place in the FCC region. The annealing processes according to the invention may be carried out in either a continuous furnace or a stationary furnace.


During the annealing process according to the invention, the alloy is annealed at least once at a temperature above TÜ2 between 900° C. (if TÜ2>900° C., then above TÜ2) and Tm in the austenitic FCC region in order to produce a large grain, to exploit the cleaning effect of the hydrogen and to remove potential magnetically disadvantageous textures. This final annealing step above TÜ2 takes place either in a stationary annealing process or in a continuous furnace. Alternatively, this heat treatment step may also take place on the strip stock in a continuous furnace. The alloy is then cooled at a rate of 10 to 50,000° C. per hour, preferably at a rate of 20 to 1000° C. per hour, to room temperature or to a temperature between 700° C. and 1000° C. in the BCC region.


A second annealing step may comprise either heating up or maintaining the temperature at between 700° C. and 1000° C. (if TÜ1<1000° C., then below TÜ1) in the ferritic BCC region in order to remove any potential remnants of the FCC phase. Following completed final magnetic annealing, the alloy is then cooled from the annealing temperature at a rate of 10 to 50,000° C. per hour, preferably at a rate of 20 to 1000° C. per hour.


The alloys according to the invention exhibit a phase transition from a BCC phase region to a mixed BCC/FCC region and at a slightly higher temperature a further phase transition from the mixed BCC/FCC region to a FCC phase region, as the temperature increases the phase transition taking place at a first transition temperature TÜ1 between the BCC phase region and the mixed BCC/FCC region and, as the temperature continues to increase, the transition taking place at a second transition temperature TÜ2 between the mixed BCC/FCC region and the FCC phase region, as shown in FIG. 2.


The temperature at which the phase transitions from a BCC phase region to a mixed BCC/FCC region and from the mixed BCC/FCC region to an FCC phase region occur can be determined by means of DSC measurements. FIG. 2 shows the typical course of a DSC heating and cooling curve at phase transition using the example of batch 930423. FIG. 2 also shows the Curie temperature and the first onset temperatures of the phase transition.


The figures that follow show the results of DSC measurements carried out using a dynamic heat-flow differential scanning calorimeter from the company Netzsch. Two identical corundum (Al2O3) crucibles are placed in a furnace, one containing a real measuring sample, the other containing a reference calibration sample. Both crucibles are subjected to the same temperature programme, which may consist of a combination of heating, cooling or isothermal sections. The thermal flow difference is determined quantitatively by measuring the temperature difference at a defined heat conduction path between sample and reference. The various maxima and minima (peaks) determined by DSC measurement can be allocated to certain types of phase transformations on the basis of their curve shapes. The result is typical curve shapes that are material-specific but also dependent on the measurement conditions, in particular on the sample mass and the heating and cooling rates. To guarantee the comparability of the measurements, identical instrument heating and cooling rates and identical sample masses were used. The heating and cooling rates used in these tests were 10 K/min; the sample mass was 50 mg.


The transition temperatures TÜ1 and TÜ2 are determined by means of DSC measurement by heating a sample of a defined mass at a defined heating rate. In this measurement the transition temperatures are represented by the first onset. This parameter is defined in DIN 51005 (“Thermal analysis”) and is also referred to as the extrapolated peak onset temperature. It represents the onset of the phase transformation and is defined as the intersection point of the extrapolated baseline with the tangent through the linear part of an increasing or decreasing peak flank.


The advantage of this parameter is that it is independent of sample mass and heating and cooling rates. The width of the two-phase region is defined as the difference between the first onset temperatures:











T

1

st





onset




(


BCC
+
FCC


FCC

)







(

from





DSC





heating

)




-






T

1

st





onset




(


BCC
+
FCC


BCC

)


=


T


U
¨






2


-

T


U
¨






1









(

from





DSC





cooling

)








The influence of composition on the transition temperatures TÜ1 and TÜ2 is determined by means of DSC measurement.



FIG. 3 shows an illustration of the first onset temperatures of the phase transition of the Fe-17Co—Cr—V alloys as V content increases (circles) in comparison to the binary Fe-17Co alloy (squares) for heating (solid symbols) and cooling (hollow symbols). The compositions of the alloys are specified in Tables 1 to 4.


The peak Curie temperatures Te of heating (DSC) and cooling (DSC) are indicated by diamonds. For the special molten masses with lower V contents, Tc is the temperature of the phase transition. The highest measured maximum permeability μmax (triangle) is plotted on the secondary axis. The highest maximum permeabilities are achieved for V contents of between 1 and 3 wt %.



FIG. 3 shows that as the V content increases phase transitions TÜ2 and TÜ1 take place at higher temperatures and that the width of the two-phase BCC+FCC regions, i.e. (TÜ2−TÜ1), increases.


Final annealing is carried out to set the soft magnetic properties. In this test it was always carried out in a H2 protective atmosphere. The H2 quality used was always stets hydrogen 3.0 (or technical hydrogen) with a H2 percentage >99.9%, where H2O≤40 ppm-mol, O2≤10 ppm-mol, N2≤100 ppm-v.


The magnetic properties of the alloys were tested using strip stock manufactured from 5 kg heavy ingots. The alloys were melted in a vacuum and then poured into a flat mould at approx. 1500° C. Once the oxide skin had been milled off the individual ingots, they were hot rolled into 3.5 mm thick strips at a temperature of approx. 1000° C. to 1300° C. The resulting hot-rolled strips were then pickled to remove the oxide skin and cold rolled to a thickness of 0.35 mm. Sample rings were stamped and resistor strips were cut out of the strip in order to characterise the magnetic properties. The electrical resistance ρ was determined on the resistor strips. Maximum permeability μmax, coercive field strength Hc, inductions B at field strengths of 20, 25, 50, 90, 100 and 160 A/cm, remanence Br and hysteresis losses PHys were measured on the sample rings in the annealed state at room temperature. Hysteresis losses were determined by measuring the losses at an induction amplitude of 1.5 T for various frequencies. The axis intercept determined by linear regression in the plot P/f over f gives the hysteresis losses.


A disc was sawn off the ingots to analyse the elements. The results of the analysis appear in Tables 1 to 4. Table 1 shows the wet-chemical analysis of the metallic elements in order to determine the basic composition. Residual iron and other elements <0.01% are not indicated, the data being given in wt %. Table 2 shows the analysis by hot gas extraction of non-metal impurities in the batches from Table 1, the data being given in wt %. Table 3 shows the wet-chemical analysis of the metallic elements in order to fine-tune the basic composition and to limit the composition ranges and impurities. Residual iron and other elements <0.01% are not specified. Data is given in wt %. In batches 930502 and 930503 the feed material used was iron with a high level of impurities. Table 4 shows the analysis by hot gas extraction of non-metallic impurities in the batches from Table 3, the data being given in wt %.


Table 3 also shows the analysis of the metallic elements in two large melts. Residual iron and the P content of large melt 76/4988 is 0.003 wt %, the P content of large melt 76/5180 is 0.002 wt %, other elements <0.01% are not specified. Table 4 also shows the analysis by hot gas extraction of non-metallic impurities in the two large melts from Table 3, the data being given in wt %.



FIGS. 4 and 5 show a statistical evaluation of the influence of the main alloy elements cobalt, vanadium and chromium on induction values after optimum annealing and on electrical resistance using multi-linear regression.



FIG. 4 shows coefficients of the induction value B after multi-linear regression. The figures following the B values (e.g. B20) indicate the field strength in A/cm. The bars show the change in induction values with the addition of 1 wt %. Only those elements with a regression value greater than the regression error are shown.



FIG. 5 shows coefficients of electrical resistance after multi-linear regression. The bars indicate the change in electrical resistance with the addition of 1 wt % of the relevant element.


These figures indicate that vanadium reduces low inductions less strongly than chromium and that chromium increases electrical resistance more strongly than vanadium at the same decrease in saturation (B160). Co increases saturation (B160) but has less influence on low induction values and on electrical resistance.


Table 7 shows annealing variants according to the invention of batch 93/0330 with a strip thickness of 0.35 mm in comparison to annealing variants not according to the invention (see FIG. 1). The cooling rate is 150° C./h unless otherwise indicated. No demagnetisation was carried out prior to measuring.



FIG. 6 shows the coercive field strength Hc of batch 930329 (Fe-17Co1.5V-0.5Cr) as a function of the reciprocal grain diameter d for various annealing processes. Table 5 shows the average grain sizes d, coercive field strengths Hc and maximum permeabilities μmax after the specified annealing (see FIG. 4). The cooling rate was 150° C./h.


Table 6 shows DSC transition temperatures and Curie temperatures Tc. Temperatures are given in ° C. #NV signifies that no signal is discernible in the DSC measurement.


One of the reasons for the very good soft magnetic properties is the grain structure achieved in the FCC region after annealing, which is unusually large for Fe—Co alloys.


After a short period of annealing of 4 h at 1050° C. in batch 93/0330 (Fe-17Co-2V), for example, grain sizes of 354 to 447 μm were determined. Similarly large grains could only be achieved by annealing in the BCC range after annealing lasting several days. FIG. 6 shows the coercive field strength Hc compared to reciprocal grain size in batch 930329 by way of example. It shows a linear relationship.


Batch 930330 was tested by way of example to compare the aforementioned annealing variants. Table 8 shows the results after step annealing in the first annealing step (batch 93/0330) (see FIG. 6). The cooling rate is 150° C./h. As long as initial annealing takes place in the lower FCC region (in this case at 1050° C.), all annealing variants show very good soft magnetic properties that are substantially better than annealing in the BCC region alone. A second annealing step in the upper BCC range following the first annealing step in the FCC region improves the values still further.



FIG. 7 shows the transition temperatures TÜ1 and TÜ2 as a function of the best coercive field strength Hc achieved for the Fe-17Co special melts with different V contents. The labels indicate the V content. FIG. 7 shows that the V content is crucial in setting the soft magnetic properties. If the V content is too low, TÜ1 is not increased. If the V content is too high, the soft magnetic properties deteriorate because the two-phase region (TÜ2−TÜ1) is broadened by vanadium (see also FIG. 3 and Table 6). As a result, the minimum coercive field strength Hc occurs at approx. 1.4 to 2 wt % vanadium.


To find the optimum annealing temperature, samples are annealed at different annealing temperatures and then measured. If the number of annealing processes required is greater than the number of samples available, the same set of samples is generally annealed at different temperatures. This so-called “step annealing” starts at a low starting temperature and anneals at successively higher temperatures. Step annealing can be used to detect precipitation regions, recrystallization temperatures and phase transformations, for example, that have a direct influence on magnetic characteristics.



FIG. 8 shows maximum permeability and coercive field strength after step annealing in the first annealing step. Table 9 shows the results after the step annealing of batch 93/0330 below the phase transition following a first annealing step of 4 h at 1000° C. above the phase transition. The cooling rate is 150° C./h. An extended maximum can be identified at approx. 1000° C. The corresponding DSC measurement is also shown to provide a comparison with the phase position.



FIG. 9 shows maximum permeability and coercive field strength after step annealing in the second annealing step below the phase transition (circles) after a first annealing step for 4 h at 1000° C. above the phase transition (diamonds). No demagnetisation was carried out before measuring the static values. A maximum can be seen at 950° C. After the last annealing step in the step annealing process at 1000° C. the samples were annealed against for 10 h at 950° C. (triangles). This time the original values for step annealing at 950° C. were not achieved. Passing through the two-phase BCC+FCC region again impairs the soft magnetic properties.


The magnetic properties were measured for alloys of various compositions after various annealing processes. The results are given in Tables 10 to 24, giving values B20, B25, B50, B90, B100, B160 (T) Hc (A/cm), μmax, Br (T) and PHys 1.5 T (Ws/kg).


Table 10 shows the results after annealing a selection of batches at 850° C. for 4 h at a cooling rate of 150° C./h. These embodiments are not in accordance with the invention.


Table 11 shows the results after annealing a selection of batches for 10 h at 910° C. at a cooling rate of 150° C./h. No demagnetisation was carried out prior to measuring the static values. These embodiments are not in accordance with the invention.


Table 12 shows the results after annealing a selection of batches for 10 h at 910° C. and cooling to room temperature, followed by annealing for 70 h at 930° C. The cooling rate is 150° C./h. No demagnetisation was carried out prior to measuring the static values. These embodiments are not in accordance with the invention.


Table 13 shows the results after annealing a selection of batches for 4 h at 1000° C.


Cooling rate 150° C./h. No demagnetisation was carried out prior to measuring the static values.


Table 14 shows the results after annealing a selection of batches in the first annealing step for 4 h at 1000° C. with cooling to room temperature, following by a second annealing step for 10 h at 910° C. The cooling rate is 150° C./h. No demagnetisation was carried out prior to measuring the static values.


Table 15 shows the results after annealing all the Fe—Co—V—Cr batches for 4 h at 1050° C. Cooling rate 150° C./h. No demagnetisation was carried out prior to measuring the static values. The resistances of batches 930322 to 930339 were measured after annealing for 4 h at 850° C. In V-rich batches 930422 and 930423 TÜ2 was only just below 1050° C. Adjusted annealing steps are indicated in Table 18.


Table 16 shows the results after annealing all the Fe—Co—V—Cr batches in a first annealing step for 4 h at 1050° C. with cooling to room temperature, followed by a second annealing step for 10 h at 910° C. Cooling rate 150° C./h. Demagnetisation was carried out prior to measuring. In the batches marked in grey, TÜ1 is either not far enough above or too far above 910° C. Adjusted annealing steps are indicated in Table 17.


Table 17 shows the results after adjustment of the annealing processes on the batches in which the transition temperatures of the DSC measurement (Table 6) do not or only just coincide with annealing for 4 h at 1050° C.+10 h at 910° C. (Tables 15 and 16). The cooling rate is 150° C./h. When annealing was carried out for 4 h at 1050° C. no demagnetisation was carried out prior to measuring. In all other cases demagnetisation was carried out prior to measuring.


Table 18 shows the results after annealing of batch 930423 in various phase regions to clarify the influences of the ferromagnetic and paramagnetic BCC region on magnetic properties (see also FIG. 2). The cooling rate is 150° C./h. When annealing was carried out for 4 h at 1050° C. no demagnetisation was carried out prior to measuring. In all other cases demagnetisation was carried out prior to measuring.


Table 19 shows the results after annealing a selection of batches for 4 h at 1050° C. followed by slow cooling to room temperature at 50° C./h. No demagnetisation was carried out prior to measuring the static values.


Table 20 shows the results after annealing a selection of batches for 4 h at 1050° C. with slow cooling to room temperature at 50° C./h and a second annealing step for 10 h at 910° C. with furnace cooling at approx. 150° C./h. No demagnetisation was carried out prior to measuring the static values.


Table 21 shows the results after annealing a selection of batches for 4 h at 1100° C. The cooling rate is 150° C./h. No demagnetisation was carried out prior to measuring the static values except on batches 930422 and 930423.


Table 22 shows the results after annealing a selection of batches in a first annealing step for 4 h at 1100° C. and cooling to room temperature followed by a second annealing step for 10 h at 910° C. The cooling rate is 150° C./h. No demagnetisation was carried out prior to measuring the static values.


Table 23 shows the results after annealing a selection of batches for 4 h at 1150° C. The cooling rate is 150° C./h. No demagnetisation was carried out prior to measuring the static values except on batch 930442.


Table 24 shows the results after annealing a selection of batches in a first annealing step for 4 h at 1150° C. and cooling to room temperature followed by a second annealing step for 10 h at 910° C. The cooling rate is 150° C./h. No demagnetisation was carried out prior to measuring the static values.


Table 25 shows the data for maximum permeability and density for various Fe-17Co alloy compositions with various additives. Based on the binary alloy Fe-16.98Co, its measured density of 7.942 g/cm3 and its average atomic weight of 56.371 g/mol (calculated from the metallic alloy element contents analysed), the fictitious density of Fe-17Co alloys with added V, Cr, Mn, Si, Al and other metallic elements is calculated using their average atomic weights and compared with the measured density. For the alloy Fe-17.19Co-1.97V (batch 93/0330), for example, the average atomic weight is 56.281 g/mol. It is then possible, using the rule of three (7.942 g/cm3×56.281/56.371=7,929 g/cm3), to calculate the fictitious density that this alloy Fe-17.19Co-1.97V should have if its lattice constant were unchanged in relation to the binary Fe-16.98Co alloy. In reality, however, the density measured for this alloy, 7.909 g/cm3, is −0.26% lower than the fictitious density of 7.929 g/cm3. This signifies that the lattice constant of this alloy must be approx. 0.085% greater than that of the binar alloy.


Table 26 shows the data for selected batches and annealing processes that have both particularly high maximum permeabilities and low hysteresis losses at the same time as a very high level of induction B at 100 A/cm (B100).


Table 27 shows the data for the impurities C and S in ppm for selected batches and annealing processes. These impurities are effectively reduced by annealing at 1050° C. in hydrogen.


Table 28 shows magnetic values for the two large melts 76/4988 and 76/5180. The letters A and B refer to ingots A and B; the molten masses were poured into two moulds. The specific resistance of batch 76/4988 is 0.306μΩm; that of batch 76/5180 is 0.318μΩm.


Table 29 shows for various batches the transition temperatures TÜ1 and TÜ2 and the best coercive field strength Hc achieved for these Fe-17Co special melts with different V contents, including details of the annealing treatment. The alloys also contain up to a total of 0.6 wt % Cr and/or Si. FIG. 7 represents this data in graphic form.



FIGS. 8 and 9 show that the BCC/FCC phase transition present in the alloy 930330 according to the invention has a strong influence on maximum permeability and coercive field strength.


In the first annealing step (FIG. 8) the first onset of cooling (=TÜ1, lower limit two-phase region) coincides with the rise in μmax and μmax reaches its maximum value and Hc reaches its minimum value above the first onset of heating (=TÜ2, upper limit two-phase region). Magnetic characteristics deteriorate again at higher temperatures in the FCC region.


In the second annealing step (FIG. 9) μmax reaches its maximum value below TÜ1 and drops as it enters the two-phase region. If the two-phase region is exceeded and annealing is repeated below TÜ1 (here 950° C.), the maximum μmax value is no longer reached, presumably because this sample has passed through the mixed BCC+FCC region twice and this causes the formation of additional grain boundaries.


In summary, it can be said that the best magnetic properties are achieved if the first annealing step takes place at above TÜ2 and the second annealing step takes place at below TÜ1.


The influence of the degree of cold deformation on the magnetic properties is tested.



FIG. 10 shows the coercive field strength Hc for batches 930329 (Fe-17Co-0.5Cr-1.5V) and 930330 (Fe-17Co-2.0V) dependent on the degree of cold deformation. At “without intermediate annealing” the hot rolling thickness corresponds to a cold deformation of 0%; at “with intermediate annealing” the thickness of the intermediate annealing corresponds to a cold deformation of 0%.


Cold deformation (KV) on strip stock with a final thickness D2 is defined as the percentage reduction in thickness in relation to a non-cold-deformed starting thickness D1 since expansion during rolling can be disregarded. The non-cold-deformed starting thickness D1 may, for example, be achieved by hot rolling or by intermediate annealing (ZGL or int. anneal).






KV[%]=[(D1−D2)/D1]×100


In FIG. 10 the coercive field strength Hc shows by way of example that as cold deformation increases magnetic properties improve by up to approx. 90% cold deformation as a result of intermediate annealing at different D1 values (1.3 mm; 1.0 mm; 0.60 mm) and identical final thickness D2 values (0.35 mm).


Assuming a constant D1 of 3.5 mm (hot rolling thickness), cold deformation achieved by a high degree of rolling to 0.20 mm and 0.10 mm once again results in an increase in Hc, as indicated by the broken line. This can be explained by the fact that too many nucleation sites for grains occur at the highest degrees of cold deformation and the grains obstruct one another's growth during annealing. As a result, the alloy in batch 930329 (Fe-17Co-0.5Cr-1.5V) (in wt %) produced without intermediate annealing after final annealing for 4 h at T1=1000° C. and for 10 h at T2=910° C. has an average grain size of 0.25 mm at a final thickness of 0.35 mm; an average grain size of 0.21 mm at a final thickness of 0.20 mm; and an average grain size of 0.15 mm at a final thickness of 0.10 mm. There is therefore an optimum degree of cold deformation of approx. 90%.


In order to test whether texture formation is a significant factor for magnetic properties, the texture was determined by means of X-ray diffraction on sheets measuring 50 mm×45 mm.



FIG. 11 shows (200) pole figures from batch 93/0330 (Fe-17Co-2V). On the left-hand side is the result for an unannealed sheet with a rolling texture. In the centre is the result for a sheet annealed at 910° C. for 10 h that has only a very indistinct texture. On the right-hand side is the result for sheet annealed at 1050° C. for 4 h annealed that has no texture. At the bottom is the result for sheet annealed at 1050° C. for 4 h and at 910° C. for 10 h that has no texture.


Here the sample was subject to angle-dependent Cu-Kα=0.154059295 nm radiation and the diffracted intensity was measured with a 2 mm pinhole aperture. A Lynxexe semi-conductor strip detector with 2° angular range and energy-dispersive operation was used as the detector. As shown by the (200) pole figures, for example, a rolling texture is present in the unannealed, full hard state that dissolves completely after annealing in the FCC region for 4 h at 1050° C. in H2.


The lack of texture also corresponds to the measurements of the directional Hc. Five Hc strips with dimensions of 50 mm×10 mm were taken from various directions relative to the direction of rolling (longitudinally=0°, diagonal=45°, transversely=90°) and measured in a Förster coercimeter.



FIG. 12 shows the coercive field strength Hc for batch 930330 (Fe-17Co-2V) measured parallel to the direction of rolling (“longitudinally”), at 45° to the direction of rolling and perpendicular to the direction of rolling (“transversely”) for the annealing processes specified. Each point represents the mean value from a series of five measurements. The error bars represent standard deviation.



FIG. 13 shows the coercive field strength Hc for batch 930335 (Fe-23Co-2V) measured parallel to the direction of rolling (“longitudinally”), at 45° to the direction of rolling and perpendicular to the direction of rolling (“transversely”) for the annealing processes specified. Each point represents the mean value from a series of five measurements. The error bars represent standard deviation.


Following annealing for 4 h at 910° C., the mean values exhibit anisotropic behaviour, though this anisotropy is not significant if statistical errors are taken into account. However, this slight anisotropy corresponds to residual texture from the corresponding pole figure (top centre image in FIG. 11). Almost identical mean values are obtained in Hc after annealing for 4 h at 1050° C. and for 4 h at 1050° C.+10 h at 910° C. The annealing in the FCC region at 1050° C. completely removes any texture present and the subsequent second annealing step in the BCC region at 910° C. produces no new texture.


Below, the magnetic properties of the alloy according to the invention are compared with comparative alloys based on the example of batches 930329 (Fe-17Co-1.5V-0.5Cr) and 930330 (Fe-17Co-2.0V) according to the invention. The comparative alloys shown are TRAFOPERM N4 (Fe-2,5Si—Al—Mn), a typical electrical steel; three FeCo VACOFLUX 17 alloys (Fe-17Co-2Cr—Mo—V—Si); VACOFLUX 48 (Fe-49Co-1.9V) and a HYPOCORE special melt. The HYPOCORE special melt was melted according to the composition published by Carpenter Technologies (Fe-5Co-2.3Si-1Mn-0.3Cr—values in wt %).



FIG. 14 shows new curves for batches 930329 (Fe-17Co-1.5V-0.5Cr), 930505 (Fe-17Co-1.4V-0.4Si) and 930330 (Fe-17Co-2V) according to the invention after optimum annealing in comparison with a SiFe (TRAFOPERM N4) and FeCo comparative alloys.



FIG. 15 shows the permeabilities for batches 930329 (Fe-17Co-1.5V-0.5Cr), 930505 (Fe-17Co-1.4V-0.4Si) and 930330 (Fe-17Co-2V) according to the invention following optimum annealing in comparison with a SiFe (TRAFOPERM N4) and FeCo comparative alloys.



FIG. 16 shows losses for batches 930329 (Fe-17Co-1.5V-0.5Cr) and 930330 (Fe-17Co-2V) according to the invention following optimum annealing at an amplitude of 1.5 T in comparison with a SiFe (TRAFOPERM N4) and FeCo comparative alloys. The hysteresis losses (y-axis intercept) of 930329, 930330 and TRAFOPERM N4 are similar. The sheet thickness was 0.35 mm.



FIG. 17 shows maximum permeability as a function of the relative density difference Δρ for Fe-17Co-based alloys (see data in Table 25). High maximum permeabilities are obtained for alloys having a relative density difference of −0.10% to −0.35% and particularly high maximum permeabilities are obtained for alloys having a relative density difference of −0.20% to −0.35%. Ultimately, this relative density difference compared to the binary Fe-17Co-alloy signifies that the lattice constant of these alloys needs to be somewhat larger than that of the binary alloy. Owing to the larger inter-atomic distance in the crystal lattice, a larger lattice constant signifies lower activation energy for place change processes and so better diffusion. This also contributes to grain growth and so to lower coercive field strength and higher permeability.


In order to test the properties of the alloys according to the invention on a production scale, two large melts were carried out using the normal manufacturing process. 2.2 t of the desired composition were melted in a vacuum induction furnace and, once the exact composition had been set and analysed, poured into two round moulds with a diameter of 340 mm. After solidification and cooling, the round ingots were removed from the moulds and heated to a temperature of 1170° C. for hot rolling in a gas-fired rotary hearth furnace. The heated ingots were then hot rolled on a blooming roll to form slabs with a cross section of 231×96 mm2. These slabs were then ground on all sides to a dimension of 226×93 mm2 to remove the oxide skin.


Both slabs obtained from batch 76/4988 in this manner were rolled out on a hot rolling mill to form hot strip. To this end, the slabs were first heated at a temperature of 1130° C. and then, once sufficiently warmed through, rolled to form hot strip. The final thickness chosen for one of the strips was 2.6 mm. The final rolling temperature of this band was 900° C., the reeling temperature 828° C. The final thickness chosen for the other strip was 1.9 mm. The final rolling temperature of this strip was 871° C., the reeling temperature 718° C. Both hot strips were then blasted to remove the oxide skin. One part of the hot-rolled strip was intermediate annealed for 1 h at 750° C. in an H2 inert gas atmosphere. Another part of the hot-rolled strip was intermediately annealed for 1 h at 1050° C. in a H2 inert gas atmosphere. A remaining part of the hot-rolled strip did not undergo intermediate annealing. The strips were then rolled to their final thicknesses, oxides being removes from both sides of the strips at an intermediate thickness. Before the strip was hot rolled, sections with a thickness of 15 mm were also sawn off the slabs and made into a strip by hot rolling (to a thickness of 3.5 mm), pickling the hot strip thus obtained and then cold rolling in the pilot plant. The results obtained are also presented for the purposes of comparison.


In the case of batch 76/5180, a disc with a thickness of 15 mm was sawn off either end of the two slabs. These discs were preheated at 1200° C. and then hot rolled to form a strip with a thickness of 3.5 mm. The hot strips obtained in this manner were picked to remove oxides, then cold rolled to a thickness of 0.35 mm.


Stamped rings were produced from all the strips obtained in this way and then subjected to an annealing process. Table 28 shows the results obtained for the magnetic values. The specific resistance of batch 76/4988 is 0.306 μΩm; that of batch 76/5180 is 0.318 μΩm.


As is apparent from Table 28, better magnetic properties are measured for samples from the large melt than for the commercially available alloys with a Co content of below 30 percent by weight such as VACOFLUX 17. For a sample from the large melt 76/5180B, a maximum permeability of above 20,000 was measured. The alloy according to the invention is therefore suitable for the industrial-scale production of strip stock with improved magnetic properties.


The alloy according to the invention exhibits higher inductions than VACOFLUX 17 for all field strengths. At inductions above the inflection point, the new alloy lies between TRAFOPERM N4 and VACOFLUX 48. For both batches, the air flow-corrected induction B at a field strength of 400 A/cm close to magnetic saturation is 2.264 T (corresponding to a polarisation J of 2.214 T). In the operating range of typical electric motors and generators torque for the new alloy will therefore be higher than for VACOFLUX 17 and TRAFOPERM N4.


A comparison of 930329 and 930330 indicates that vanadium in conjunction with the heat treatment described above increases the rectangularity of the hysteresis loop to such an extent that, depending on the additive, maximum permeability is almost as high as that of VACOFLUX 48. This is surprising, not to say astounding, since the anisotropy constant K1 shows a zero crossing at approx. 50% Co that is not present at 17% Co. By contrast, at 17% Co the anisotropy constant K1 in the Fe—Co system is very high.


Very good soft magnetic properties are also apparent in the hysteresis losses, which are on a level comparable with those of TRAFOPERM N4. As frequency rises, TRAFOPERM N4 losses at identical strip thickness increase due to the higher electrical resistance, though less strongly than with the new alloy. It is, however, possible to compensate for this effect by selecting a somewhat smaller strip thickness with correspondingly lower eddy current losses.


In summary, a high permeability soft magnetic alloy is provided that offers both better soft magnetic properties, e.g. appreciably higher permeability and lower hysteresis losses, and higher saturation than existing, commercially available FeCo alloys. At the same time, however, this new alloy also offers significantly lower hysteresis losses than previously known commercially available alloys with Co contents between 10 and 30 wt % and, above all, an appreciably higher level of permeability never previously achieved for this type of alloy. The alloy according to the invention can also be produced cost effectively on an industrial scale.



















TABLE 1





Batch












93/
Co
Ni
Cr
Mn
V
Si
Al
Mo
Be
Cer

























0322
17.80
<0.01
0.01
<0.01
<0.01
<0.01
<0.01
2.50
<0.01



0323
16.98
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01



0324
23.20
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01



0325
17.05
<0.01
2.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01



0326
23.25
<0.01
2.03
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01



0327
17.14
<0.01
1.54
<0.01
0.50
<0.01
<0.01
<0.01
<0.01



0328
17.08
<0.01
1.04
<0.01
0.98
<0.01
<0.01
<0.01
<0.01



0329
17.12
<0.01
0.54
<0.01
1.46
<0.01
<0.01
<0.01
<0.01



0330
17.19
<0.01
<0.01
<0.01
1.97
<0.01
<0.01
<0.01
<0.01



0331
23.09
0.012
1.04
<0.01
0.99
<0.01
<0.01
<0.01
<0.01



0332
22.97
<0.01
1.04
<0.01
0.99
0.19
<0.01
<0.01
<0.01



0333
22.96
<0.01
1.03
<0.01
0.98
<0.01
0.18
<0.01
<0.01



0334
23.01
0.022
1.04
<0.01
0.98
<0.01
<0.01
<0.01
0.06



0335
22.93
<0.01
<0.01
<0.01
1.95
<0.01
<0.01
<0.01
<0.01



0336
23.07
<0.01
1.04
<0.01
0.98
<0.01
<0.01
<0.01
<0.01
<0.001












(used: 0.02)


0337
22.93
<0.01
1.03
<0.01
0.98
<0.01
<0.01
<0.01
<0.01
<0.001












(used: 0.01)


0338
23.07
<0.01
1.04
<0.01
0.98
<0.01
<0.01
<0.01
<0.01
<0.001












(used: 0.005)


0339
23.06
0.017
<0.01
<0.01
<0.01
<0.01
1.96
<0.01
<0.01





















TABLE 2





Batch 93/
C
S
O
N







0322
0.0050
0.0012
0.0016
0.0012


0323
0.0045
0.0010
0.0150
0.0011


0324
0.0038
0.0010
0.0130
0.0009


0325
0.0031
0.0011
0.0100
0.0011


0326
0.0032
0.0011
0.0085
0.0012


0327
0.0032
0.0011
0.0097
0.0011


0328
0.0029
0.0011
0.0100
0.0013


0329
0.0028
0.0012
0.0093
0.0013


0330
0.0024
0.0011
0.0092
0.0014


0331
0.0030
0.0011
0.0087
0.0011


0332
0.0022
0.0011
0.0068
0.0012


0333
0.0040
0.0011
0.0014
0.0011


0334
0.0036
0.0010
0.0022
0.0013


0335
0.0034
0.0010
0.0120
0.0016


0336
0.0040
0.0010
0.0088
0.0014


0337
0.0039
0.0010
0.0058
0.0012


0338
0.0036
0.0011
0.0082
0.0012


0339
0.0025
0.0009
0.0026
0.0010





























TABLE 3





Batch















93/
Co
V
Cr
Mn
Ni
Nb
Mo
Si
Al
Ta
Ti
Cer
Cu




























0420
17.03
2.26
<0.01
<0.01
0.011
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0421
20.01
2.29
<0.01
<0.01
0.012
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0422
16.98
3.01
<0.01
<0.01
0.010
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0423
17.04
3.49
<0.01
<0.01
0.011
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0424
9.94
1.47
0.50
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0425
13.97
1.49
0.50
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0426
20.03
1.48
0.50
<0.01
0.012
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0427
25.00
1.50
0.50
<0.01
0.015
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0428
16.95
1.48
0.50
<0.01
0.010
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0429
16.94
1.48
0.49
<0.01
0.010
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0430
17.04
1.50
0.50
<0.01
0.010
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0431
16.97
1.48
0.50
0.094
0.010
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0432
17.00
1.49
0.50
0.27
0.010
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0433
17.02
1.48
0.50
<0.01
0.12
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0434
16.99
1.45
0.50
<0.01
0.32
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0435
17.01
1.43
0.50
<0.01
<0.01
0.057
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0436
17.03
1.43
0.50
<0.01
<0.01
<0.01
0.30
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0437
17.02
1.47
0.50
<0.01
<0.01
<0.01
<0.01
0.055
<0.01
<0.01
<0.01
<0.01
<0.01


0438
16.95
1.47
0.50
<0.01
0.016
<0.01
<0.01
0.026
<0.01
0.086
<0.01
<0.01
<0.01


0439
17.00
1.49
0.50
<0.01
0.012
<0.01
<0.01
0.021
<0.01
<0.01
0.078
<0.01
<0.01


0440
17.02
1.50
0.50
<0.01
0.010
<0.01
<0.01
0.022
<0.01
<0.01
<0.01
0.006
<0.01














(used:














0.05)


0441
17.04
1.49
0.50
<0.01
0.010
<0.01
<0.01
0.022
<0.01
<0.01
<0.01
<0.01
0.11


0442
16.99
<0.01
<0.01
<0.01
0.010
<0.01
<0.01
0.019
1.97
<0.01
<0.01

<0.01


0443
17.05
4.02
<0.01
<0.01
0.011
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01


0502
16.96
1.66
0.32
0.04
0.025
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01

0.01


0503
16.97
1.68
0.32
0.04
0.024
<0.01
<0.01
<0.01
<0.01
<0.01
<0.01
<0.001
0.01














(used:














0.10)


0504
16.94
1.68
<0.01
<0.01
0.011
<0.01
<0.01
0.20
<0.01
<0.01
<0.01
<0.01
<0.01


0505
16.97
1.39
<0.01
<0.01
0.011
<0.01
<0.01
0.40
<0.01
<0.01
<0.01
<0.01
<0.01







Large melts:




















76/4988
16.81
2.29
0.013
0.024
0.028
<0.001
<0.001
0.016
<0.001
<0.001
<0.001
<0.001
0.005


76/5180
17.11
1.47
0.011
0.094
0.008
<0.001
<0.001
0.28
<0.001
<0.001
<0.001
<0.005
0.006




















TABLE 4





Batch 93/
C
S
O
N







0420
0.0034
0.0012
0.0130
0.0016


0421
0.0021
0.0012
0.0110
0.0014


0422
0.0021
0.0012
0.0110
0.0015


0423
0.0034
0.0012
0.0100
0.0014


0424
0.0028
0.0011
0.0110
0.0010


0425
0.0032
0.0012
0.0089
0.0012


0426
0.0020
0.0012
0.0081
0.0011


0427
0.0022
0.0011
0.0084
0.0010


0428
0.0026
0.0012
0.0086
0.0013


0429
0.0056
0.0012
0.0070
0.0012


0430
0.0170
0.0012
0.0048
0.0012


0431
0.0014
0.0013
0.0094
0.0013


0432
0.0019
0.0013
0.0096
0.0012


0433
0.0019
0.0012
0.0100
0.0012


0434
0.0017
0.0025
0.0110
0.0010


0435
0.0030
0.0032
0.0150
0.0007


0436
0.0022
0.0030
0.0110
0.0007


0437
0.0023
0.0017
0.0110
0.0006


0438
0.0027
0.0010
0.0093
0.0011


0439
0.0050
0.0010
0.0023
0.0006


0440
0.0022
0.0008
0.0050
0.0010


0441
0.0020
0.0009
0.0075
0.0008


0442
0.0027
0.0008
0.0017
0.0005


0443
0.0032
0.0009
0.0130
0.0070


0502
0.0038
0.0028
0.0120
0.0029


0503
0.0058
0.0022
0.0035
0.0028


0504
0.0025
0.0010
0.0092
0.0008


0505
0.0024
0.0010
0.0063
0.0008


Large melts






76/4988
0.0010
0.0042
0.0121
0.0023


76/5180
0.0021
0.0062
0.0073
0.0026






















TABLE 5






Strip

Average





Batch
thickness

grain
1/d
Hc


93/
mm
Annealing
size d mm
1/mm
A/cm
μmax





















0329
0.35
4 h 850° C.
0.075
13.33
1.035
3584


0329
0.35
10 h 910° C.
0.151
6.62
0.622
5090


0329
0.35
10 h 910° C. +
0.254
3.94
0.418
5737




70 h 930° C.


0329
0.35
4 h 1100° C.
0.214
4.67
0.524
7497


0329
0.35
4 h 1100° C. +
0.360
2.78
0.396
12084




10 h 910° C.


0329
0.35
4 h 1050° C.
0.302
3.31
0.501
7943


0329
0.35
4 h 1050° C. +
0.214
4.67
0.367
14291




10 h 910° C.


0329
0.35
4 h 1150° C.
0.254
3.94
0.473
7860


0325
0.35
4 h 1050° C.
0.197
5.08
1.004
3554


0328
0.35
4 h 1050° C.
0.278
3.60
0.625
5387


0330
0.35
4 h 1050° C.
0.401
2.49
0.353
11509


0329
0.35
4 h 1000° C. +
0.250
4.00
0.384
15658




10 h 910° C.


0329
0.20
4 h 1000° C. +
0.213
4.69
0.474
10978




10 h 910° C.


0329
0.10
4 h 1000° C. +
0.151
6.62
0.523
10965




10 h 910° C.























TABLE 6





Batch
1st onset
Peak
1st onset
Peak
Tc peak
Tc peak
Middle


93/
heating (TÜ2)
heating
cooling (TÜ1)
cooling
heating
cooling
Tc peak






















0322
928
938
908
897
#NV
#NV
#NV


0323
940
951
932
919
#NV
#NV
#NV


0324
950
964
944
928
#NV
#NV
#NV


0325
905
918
880
859
#NV
#NV
#NV


0326
921
937
884
862
#NV
#NV
#NV


0327
919
930
897
879
#NV
#NV
#NV


0328
934
943
914
898
#NV
#NV
#NV


0329
952
958
933
926
937
#NV
#NV


0330
980
987
958
951
943
931
937


0331
934
946
913
895
#NV
#NV
#NV


0332
931
945
910
893
#NV
#NV
#NV


0333
937
950
915
898
#NV
#NV
#NV


0334
933
945
912
895
#NV
#NV
#NV


0335
962
974
953
939
#NV
#NV
#NV


0336
933
947
912
895
#NV
#NV
#NV


0337
933
947
912
895
#NV
#NV
#NV


0338
934
947
913
895
#NV
#NV
#NV


0339
1070
1088
1020
1011
962
950
956


0420
988
995
964
958
941
933
937


0421
971
978
956
947
960
#NV
#NV


0422
1017
1026
979
974
940
931
936


0423
1037
1063
994
988
938
929
934


0424
993
997
952
947
886
878
882


0425
965
971
939
933
916
907
912


0426
949
958
935
923
#NV
#NV
#NV


0427
951
963
939
924
#NV
#NV
#NV


0428
951
960
934
923
936
#NV
#NV


0429
947
960
934
922
938
#NV
#NV


0430
944
952
932
917
938
#NV
#NV


0431
950
958
931
920
937
#NV
#NV


0432
946
953
925
912
935
#NV
#NV


0433
949
957
929
919
938
#NV
#NV


0434
944
952
921
911
937
#NV
#NV


0435
953
961
932
924
938
#NV
#NV


0436
952
959
931
922
935
#NV
#NV


0437
954
961
934
926
937
#NV
#NV


0438
955
962
934
926
938
#NV
#NV


0439
958
965
936
926
934
#NV
#NV


0440
954
961
934
925
936
#NV
#NV


0441
952
959
932
924
937
#NV
#NV


0442
#NV
#NV
(1065)
(1050)
924
916
920


0443
#NV
#NV
1012
1001
936
925
931


0502
960
968
941
930
939
#NV
#NV


0503
959
968
941
929
939
#NV
#NV


0504
975
982
956
949
939
929
934


0505
970
977
953
946
936
926
931


76/4988
989
995
962
957
939
929
934


76/5180
965
974
949
942
938
#NV
#NV



























TABLE 7






Annealing
B20
B25
B50
B90
B100
B160
Hc in

Br
PHys 1.5 T


Annealing
variant
in T
in T
in T
in T
in T
in T
A/cm
μmax
in T
Ws/kg


























4 h 1050° C.
1
1.813
1.84
1.933
2.025
2.043
2..21
0.296
19653
1.505
0.045


Cool. 50° C./h +


10 h, 910° C.


4 h 1050° C. +
1
1.814
1.84
1.931
2.024
2.042
2.12
0.340
17767
1.525
0.046


10 h 910° C.


10 h 1050° C.
1
1.760
1.788
1.888
1.990
2.010
2.102
0.316
14358
1.457
0.050


Cool. 30° C./h +


10 h 910° C.


4 h 1050° C. +
1
1.790
1.817
1.916
2.015
2.034
2.122
0.346
12584
1.378
0.049


10 h 910° C.


4 h 1050° C.
1
1.643
1.672
1.776
1.892
1.917
2.035
0.660
6010
1.392
0.075


Cooling zone +


10 h, 910° C.


4 h 1050° C.,
2
1.799
1.825
1.921
2.018
2.037
2.124
0.326
14586
1.542
0.043


10 h 910° C.


4 h 1050° C.,
2
1.795
1.820
1.915
2.012
2.032
2.119
0.341
13837
1.532
0.043


2 h 930° C.


4 h 1050° C.,
2
1.798
1.824
1.921
2.018
2.037
2.125
0.354
13105
1.517
0.044


2 h 910° C.


2 h 1050° C.,
2
1.798
1.824
1.919
2.016
2.036
2.123
0.380
12581
1.508
0.046


4 h 910° C.


10 h 1050° C.
2
1.749
1.776
1.877
1.982
2.003
2.098
0.293
12494
1.482
0.045


Cool., 50° C./h


to 930° C. 10 h


4 h 1050° C.,
2
1.790
1.817
1.914
2.012
2.031
2.119
0.413
9787
1.384
0.051


2 h 910° C.


4 h 1050° C.
3
1.812
1.839
1.932
2.025
2.043
2.122
0.305
14015
1.518
0.043


Cool. 50° C./h


4 h 1050° C.
3
1.812
1.838
1.929
2.021
2.04
2.119
0.347
12670
1.502
0.045


Cool. 150° C./h


10 h 1050° C.
3
1.756
1.783
1.885
1.986
2.007
2.095
0.342
10419
1.438
0.051


Cool. 30° C./h


4 h 1050° C.
3
1.791
1.819
1.917
2.016
2.036
2.124
0.359
10348
1.405
0.047


Cool. 150° C./h


10 h 910° C. +
Not acc. to
1.595
1.622
1.723
1.838
1.863
1.991
0.456
5415
1.271
0.072


70 h 930° C. +
invention


61 h 950° C.


10 h 910° C. +
Not acc. to
1.613
1.640
1.740
1.853
1.877
1.999
0.662
4868
1.148
0.072


70 h 930° C.
invention


10 h 910° C.
Not acc. to
1.615
1.642
1.74
1.848
1.873
1.989
0.684
4868
1.112
0.074



invention


4 h 1050° C.
Not acc. to
1.635
1.667
1.775
1.893
1.917
2.035
0.740
3769
0.969
0.095


Cooling zone
invention


4 h 850° C.
Not acc. to
1.648
1.677
1.776
1.883
1.906
2.019
1.052
3533
0.867
0.081



invention

























TABLE 8






B20
B25
B50
B90
B100
B160
Hc in

Br


Annealing
in T
in T
in T
in T
in T
in T
A/cm
μmax
in T
























10 h 910° C.
1.615
1.642
1.740
1.848
1.873
1.989
0.684
4868
1.112


10 h 910° C. + 70 h 930° C.
1.613
1.640
1.740
1.853
1.877
1.999
0.662
4868
1.148


10 h 910° C. + 70 h 930° C. +
1.595
1.622
1.723
1.838
1.863
1.991
0.456
5415
1.271


61 h 950° C.


10 h 910° C. + 70 h 930° C. +
1.596
1.623
1.722
1.838
1.863
1.990
0.473
5557
1.222


61 h 950° C. + 4 h 960° C.


10 h 910° C. + 70 h 930° C. +
1.713
1.742
1.842
1.948
1.969
2.070
0.544
8117
1.391


61 h 950° C. + 4 h 960° C. +


4 h 970° C.


10 h 910° C. + 70 h 930° C. +
1.783
1.811
1.909
2.011
2.030
2.119
0.414
10784
1.452


61 h 950° C. + 4 h 960° C. +


4 h 970° C. + 4 h 980° C.


10 h 910° C. + 70 h 930° C. +
1.792
1.822
1.923
2.025
2.045
2.131
0.358
11337
1.432


61 h 950° C. + 4 h 960° C. +


4 h 970° C. + 4 h 980° C. +


4 h 990° C.


10 h 910° C. + 70 h 930° C. +
1.779
1.808
1.911
2.015
2.035
2.117
0.315
11155
1.406


61 h 950° C. + 4 h 960° C. +


4 h 970° C. + 4 h 980° C. +


4 h 990° C. + 4 h 1000° C.


10 h 910° C. + 70 h 930° C. +
1.772
1.803
1.908
2.015
2.036
2.128
0.321
11227
1.397


61 h 950° C. + 4 h 960° C. +


4 h 970° C. + 4 h 980° C. +


4 h 990° C. + 4 h 1000° C. +


4 h 1010° C.


10 h 910° C. + 70 h 930° C. +
1.757
1.787
1.892
2.002
2.023
2.120
0.343
10375
1.387


61 h 950° C. + 4 h 960° C. +


4 h 970° C. + 4 h 980° C. +


4 h 990° C. + 4 h 1000° C. +


4 h 1010° C. + 4 h 1030° C.


10 h 910° C. + 70 h 930° C. +
1.703
1.734
1.844
1.962
1.986
2.095
0.371
8527
1.343


61 h 950° C. + 4 h 960° C. +


4 h 970° C. + 4 h 980° C. +


4 h 990° C. + 4 h 1000° C. +


4 h 1010° C. + 4 h 1030° C. +


4 h 1050° C.


























TABLE 9






B20
B25
B50
B90
B100
B160
Hc in

Br



Annealing
in T
in T
in T
in T
in T
in T
A/cm
μmax
in T
Demagnetised?

























4 h 1000° C.
1.801
1.828
1.923
2.019
2.038
2.123
0.407
10618
1.444
No


4 h 1000° C. + 4 h 900° C.
1.796
1.825
1.921
2.018
2.038
2.124
0.422
10593
1.324
No


4 h 1000° C. + 4 h 900° C. +
1.796
1.824
1.921
2.018
2.037
2.123
0.414
11436
1.359
No


4 h 910° C.


4 h 1000° C. + 4 h 900° C. +
1.795
1.822
1.918
2.015
2.034
2.119
0.406
12326
1.363
No


4 h 910° C. + 4 h 920° C.


4 h 1000° C. + 4 h 900° C. +
1.799
1.826
1.921
2.017
2.036
2.121
0.386
13961
1.410
No


4 h 910° C. + 4 h 920° C. +


4 h 930° C.


4 h 1000° C. + 4 h 900° C. +
1.791
1.818
1.916
2.013
2.031
2.119
0.387
15856
1.511
Yes


4 h 910° C. + 4 h 920° C. +


4 h 930° C. + 4 h 940° C.


4 h 1000° C. + 4 h 900° C. +
1.793
1.819
1.916
2.013
2.032
2.119
0.401
16609
1.550
Yes


4 h 910° C. + 4 h 920° C. +


4 h 930° C. + 4 h 940° C. +


4 h 950° C.


4 h 1000° C. + 4 h 900° C. +
1.794
1.820
1.916
2.012
2.031
2.117
0.427
15298
1.554
Yes


4 h 910° C. + 4 h 920° C. +


4 h 930° C. + 4 h 940° C. +


4 h 950° C. + 4 h 960° C.


4 h 1000° C. + 4 h 900° C. +
1.767
1.794
1.890
1.990
2.009
2.102
0.525
11053
1.497
Yes


4 h 910° C. + 4 h 920° C. +


4 h 930° C. + 4 h 940° C. +


4 h 950° C. + 4 h 960° C. +


4 h 970° C.


4 h 1000° C. + 4 h 900° C. +
1.787
1.815
1.917
2.017
2.036
2.123
0.433
9550
1.469
No


4 h 910° C. + 4 h 920° C. +


4 h 930° C. + 4 h 940° C. +


4 h 950° C. + 4 h 960° C. +


4 h 970° C. + 4 h 980° C.


4 h 1000° C. + 4 h 900° C. +
1.787
1.815
1.917
2.018
2.037
2.124
0.430
11789
1.463
Yes


4 h 910° C. + 4 h 920° C. +


4 h 930° C. + 4 h 940° C. +


4 h 950° C. + 4 h 960° C. +


4 h 970° C. + 4 h 980° C.


4 h 1000° C. + 4 h 900° C. +
1.782
1.811
1.910
2.011
2.031
2.119
0.431
12585
1.482
Yes


4 h 910° C. + 4 h 920° C. +


4 h 930° C. + 4 h 940° C. +


4 h 950° C. + 4 h 960° C. +


4 h 970° C. + 4 h 980° C. +


4 h 990° C.


4 h 1000° C. + 4 h 900° C. +
1.783
1.812
1.912
2.012
2.032
2.120
0.429
9965
1.485
No


4 h 910° C. + 4 h 920° C. +


4 h 930° C. + 4 h 940° C. +


4 h 950° C. + 4 h 960° C. +


4 h 970° C. + 4 h 980° C. +


4 h 990° C.


4 h 1000° C. + 4 h 900° C. +
1.778
1.807
1.907
2.009
2.028
2.117
0.433
11762
1.424
Yes


4 h 910° C. + 4 h 920° C. +


4 h 930° C. + 4 h 940° C. +


4 h 950° C. + 4 h 960° C. +


4 h 970° C. + 4 h 980° C. +


4 h 990° C. + 4 h 1000° C.


4 h 1000° C. + 4 h 900° C. +
1.779
1.807
1.908
2.009
2.029
2.118
0.437
9405
1.425
No


4 h 910° C. + 4 h 920° C. +


4 h 930° C. + 4 h 940° C. +


4 h 950° C. + 4 h 960° C. +


4 h 970° C. + 4 h 980° C. +


4 h 990° C. + 4 h 1000° C.


4 h 1000° C. + 4 h 900° C. +
1.775
1.804
1.905
2.007
2.026
2.116
0.460
11012
1.430
Yes


4 h 910° C. + 4 h 920° C. +


4 h 930° C. + 4 h 940° C. +


4 h 950° C. + 4 h 960° C. +


4 h 970° C. + 4 h 980° C. +


4 h 990° C. + 4 h 1000° C. +


10 h 950° C.



























TABLE 10





Batch






Hc


rho in
PHys 1.5 T


93/
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
μΩm
Ws/kg


























0322
1.676
1.709
1.815
1.924
1.947
2.056
1.465
3130
1.098
0.3081
0.107


0323
1.765
1.795
1.892
1.995
2.016
2.121
1.120
3815
1.015
0.1872
0.079


0324
1.800
1.836
1.949
2.059
2.082
2.189
1.451
2544
0.766
0.1570
0.093


0325
1.700
1.729
1.830
1.937
1.959
2.068
0.894
4195
0.919
0.3360
0.067


0326
1.715
1.753
1.873
1.992
2.016
2.133
1.144
2735
0.533
0.3739
0.074


0327
1.665
1.694
1.794
1.904
1.926
2.039
0.890
4059
0.908
0.3287
0.070


0328
1.656
1.686
1.787
1.895
1.918
2.031
0.928
3890
0.945
0.3154
0.076


0329
1.651
1.681
1.780
1.887
1.911
2.024
1.035
3584
0.876
0.3042
0.079


0330
1.648
1.677
1.776
1.883
1.906
2.019
1.052
3533
0.867
0.2859
0.081


0331
1.693
1.729
1.847
1.967
1.991
2.110
1.167
2639
0.551
0.3326
0.080


0332
1.681
1.719
1.837
1.956
1.980
2.098
1.229
2633
0.588
0.3580
0.083


0333
1.703
1.740
1.856
1.972
1.996
2.109
1.328
2788
0.756
0.3518
0.088


0334
1.788
1.822
1.929
2.035
2.055
2.151
0.968
3656
0.692
0.3475
0.069


0335
1.673
1.710
1.826
1.945
1.970
2.089
1.248
2643
0.658
0.2857
0.089


0336
1.696
1.733
1.850
1.969
1.992
2.109
1.198
2626
0.586
0.3396
0.081


0337
1.698
1.735
1.852
1.969
1.992
2.107
1.270
2563
0.578
0.3388
0.082


0338
1.696
1.734
1.852
1.970
1.994
2.110
1.241
2653
0.636
0.3334
0.084



























TABLE 11





Batch






Hc


rho in
PHys 1.5 T


93/
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
μΩm
Ws/kg


























0328
1.623
1.652
1.751
1.864
1.887
2.005
0.627
4902
1.022

0.067


0329
1.618
1.646
1.746
1.858
1.881
2.002
0.622
5090
1.129

0.069


0330
1.615
1.642
1.74
1.848
1.873
1.989
0.684
4868
1.112

0.074


0331
1.657
1.69
1.807
1.933
1.961
2.09
0.659
3795
0.502

0.074


0334
1.799
1.832
1.938
2.039
2.059
2.148
0.659
4556
0.81

0.059


0335
1.652
1.686
1.801
1.923
1.948
2.073
0.928
3059
0.587

0.082



























TABLE 12





Batch






Hc


Rho in
PHys 1.5 T


93/
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
μΩm
Ws/kg


























0328
1.771
1.802
1.911
2.017
2.036
2.126
0.473
6912
1.164

0.061


0329
1.598
1.624
1.725
1.842
1.868
1.997
0.418
5737
1.168

0.061


0330
1.613
1.64
1.74
1.853
1.877
1.999
0.662
4868
1.148

0.072


0331
1.658
1.693
1.811
1.941
1.967
2.098
1.265
2702
0.938

0.104


0334
1.787
1.820
1.931
2.038
2.060
2.155
1.289
3228
1.158

0.099


0335
1.652
1.688
1.809
1.943
1.972
2.116
0.978
3246
0.546

0.084



























TABLE 13





Batch






Hc


Rho in
PHys 1.5 T


93/
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
μΩm
Ws/kg


























0323
1.719
1.75
1.855
1.973
1.997
2.111
0.492
5433
1.003
0.189
0.071


0328
1.768
1.797
1.895
1.994
2.013
2.102
0.643
5392
1.212
0.317
0.065


0329
1.803
1.83
1.923
2.017
2.035
2.117
0.509
7929
1.377
0.310
0.055


0330
1.809
1.836
1.927
2.019
2.037
2.117
0.369
16218
1.498
0.291
0.046


0331
1.703
1.739
1.86
1.985
2.01
2.127
1.033
2980
0.967
0.335
0.091


0334
1.707
1.742
1.860
1.979
2.002
2.113
1.145
2994
0.958
0.350
0.091


0335
1.801
1.833
1.942
2.046
2.067
2.155
0.414
6043
1.168
0.289
0.064


0339
1.707
1.739
1.851
1.968
1.990
2.089
0.297
7651
0.869

0.051



























TABLE 14





Batch






Hc


Rho in
PHys 1.5 T


93/
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
μΩm
Ws/kg


























0323
1.72
1.748
1.853
1.971
1.995
2.11
0.402
7983
1.312
0.189
0.060


0328
1.777
1.805
1.902
2.001
2.02
2.108
0.415
11322
1.493
0.317
0.049


0329
1.808
1.834
1.927
2.02
2.038
2.12
0.383
13490
1.529
0.311
0.046


0330
1.807
1.834
1.927
2.02
2.039
2.119
0.353
14673
1.529
0.290
0.047


0331
1.701
1.734
1.854
1.982
2.008
2.129
0.926
4382
1.277
0.335
0.081


0334
1.705
1.738
1.855
1.975
1.999
2.113
0.998
4145
1.184
0.348
0.087


0335
1.802
1.834
1.941
2.047
2.066
2.156
0.401
5998
1.234
0.288
0.065



























TABLE 15





Batch






Hc


rho in
PHys 1.5 T


93/
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
μΩm
Ws/kg


























0322
1.691
1.722
1.828
1.942
1.965
2.077
0.731
4574
1.093

0.074


0323
1.713
1.742
1.852
1.972
1.997
2.114
0.456
5732
0.998

0.074


0324
1.757
1.79
1.908
2.036
2.063
2.186
0.713
4522
1.051

0.078


0325
1.680
1.710
1.816
1.929
1.952
2.063
1.004
3554
0.925

0.082


0326
1.695
1.732
1.858
1.988
2.014
2.136
1.336
2397
0.899

0.107


0327
1.674
1.705
1.813
1.929
1.953
2.068
0.826
4061
0.948

0.078


0328
1.767
1.796
1.893
1.993
2.012
2.103
0.625
5387
1.179

0.066


0329
1.809
1.836
1.928
2.021
2.039
2.12
0.501
7943
1.388

0.054


0330
1.812
1.838
1.929
2.021
2.040
2.119
0.347
12670
1.502

0.045


0331
1.707
1.743
1.863
1.986
2.012
2.125
0.969
3049
0.948

0.088


0332
1.700
1.734
1.854
1.977
2.002
2.115
0.974
2982
0.894

0.087


0333
1.677
1.712
1.833
1.960
1.986
2.109
0.921
3259
0.903

0.084


0334
1.704
1.740
1.857
1.976
2.000
2.112
1.071
3042
0.925

0.087


0335
1.809
1.840
1.947
2.051
2.070
2.159
0.480
5631
1.194

0.068


0336
1.701
1.735
1.855
1.979
2.004
2.120
0.931
3140
0.907

0.085


0337
1.703
1.737
1.857
1.983
2.007
2.125
0.950
3157
0.926

0.087


0338
1.707
1.743
1.860
1.982
2.006
2.121
1.058
2934
0.912

0.089


0339
1.674
1.716
1.849
1.971
1.993
2.094
0.623
3911
0.552

0.053


0420
1.792
1.817
1.910
2.001
2.019
2.101
0.393
11121
1.483
0.3000
0.049


0421
1.795
1.822
1.919
2.017
2.037
2.124
0.459
7856
1.387
0.3013
0.058


0422
1.749
1.774
1.866
1.960
1.978
2.064
0.472
9770
1.441
0.3289
0.052


0423
1.577
1.604
1.703
1.815
1.838
1.956
0.798
5361
1.287
0.3552
0.079


0424
1.728
1.752
1.840
1.934
1.953
2.039
0.352
13523
1.458
0.2683
0.045


0425
1.783
1.808
1.898
1.989
2.007
2.089
0.404
11119
1.464
0.2928
0.048


0426
1.783
1.812
1.913
2.017
2.037
2.129
0.562
5515
1.229
0.2993
0.064


0427
1.782
1.817
1.934
2.049
2.071
2.171
0.765
3805
1.013
0.3137
0.078


0428
1.764
1.790
1.885
1.981
2.001
2.089
0.580
6594
1.284
0.3004
0.059


0429
1.780
1.806
1.900
1.996
2.015
2.102
0.514
7120
1.276
0.3019
0.055


0430
1.777
1.804
1.898
1.993
2.012
2.097
0.637
5092
0.997
0.2999
0.061


0431
1.796
1.822
1.913
2.005
2.023
2.106
0.672
6160
1.263
0.3069
0.059


0432
1.795
1.821
1.910
1.997
2.015
2.099
0.746
5357
1.204
0.3149
0.064


0433
1.774
1.801
1.897
1.995
2.014
2.104
0.544
6782
1.291
0.3038
0.058


0434
1.746
1.775
1.873
1.976
1.998
2.094
0.683
5514
1.255
0.3057
0.066


0435
1.795
1.821
1.915
2.010
2.029
2.113
0.488
8261
1.437
0.3020
0.057


0436
1.769
1.798
1.896
1.995
2.015
2.105
0.500
6983
1.322
0.3128
0.059


0437
1.763
1.791
1.889
1.991
2.010
2.101
0.436
7917
1.336
0.3064
0.056


0438
1.804
1.830
1.924
2.016
2.034
2.116
0.470
8359
1.370
0.3065
0.054


0439
1.643
1.673
1.780
1.898
1.923
2.041
0.578
5351
1.228
0.3026
0.076


0440
1.800
1.828
1.921
2.016
2.035
2.117
0.391
10119
1.301
0.2996
0.052


0441
1.800
1.828
1.925
2.021
2.039
2.121
0.353
8636
1.260
0.3053
0.053


0442
1.654
1.684
1.791
1.903
1.926
2.026
0.243
8863
0.803
0.3464
0.050


0443
1.561
1.590
1.693
1.807
1.830
1.949
0.792
4639
1.133
0.3869
0.078


0502
1.742
1.770
1.871
1.974
1.996
2.092
0.615
7186
1.307
0.2999
0.063


0503
1.751
1.779
1.878
1.979
1.999
2.094
0.547
6764
1.157
0.3019
0.057


0504
1.772
1.801
1.899
1.998
2.018
2.109
0.394
10716
1.303
0.3059
0.055


0505
1.785
1.814
1.912
2.012
2.031
2.119
0.334
12009
1.264
0.3085
0.051


























TABLE 16





Batch






Hc


PHys 1.5 T


93/
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
Ws/kg

























0322
1.693
1.722
1.826
1.940
1.964
2.077
0.586
8599
1.373
0.061


0323
1.715
1.744
1.852
1.973
1.996
2.114
0.400
9047
1.272
0.062


0324
1.753
1.786
1.903
2.032
2.058
2.180
0.718
4769
1.126
0.079


0325
1.669
1.701
1.815
1.936
1.960
2.075
0.813
3928
0.961
0.082


0326
1.694
1.731
1.856
1.986
2.013
2.135
1.782
1959
0.886
0.131


0327
1.704
1.736
1.849
1.965
1.988
2.093
0.653
4605
1.034
0.075


0328
1.773
1.800
1.896
1.995
2.014
2.102
0.410
13856
1.488
0.050


0329
1.808
1.833
1.925
2.018
2.035
2.115
0.369
17227
1.528
0.046


0330
1.813
1.839
1.930
2.021
2.039
2.118
0.354
19591
1.514
0.046


0331
1.717
1.750
1.868
1.993
2.018
2.132
0.883
4899
1.281
0.079


0332
1.704
1.738
1.855
1.980
2.004
2.119
0.852
4964
1.267
0.076


0333
1.671
1.705
1.824
1.953
1.979
2.104
0.771
5067
1.240
0.073


0334
1.707
1.740
1.855
1.976
2.000
2.114
0.944
4607
1.187
0.080


0335
1.817
1.846
1.951
2.053
2.073
2.161
0.451
9277
1.273
0.064


0336
1.713
1.746
1.864
1.989
2.014
2.131
0.766
5201
1.271
0.073


0337
1.707
1.74
1.859
1.986
2.011
2.131
0.792
5153
1.275
0.074


0338
1.71
1.743
1.859
1.981
2.006
2.120
0.904
4893
1.239
0.078


0339
1.684
1.723
1.850
1.968
1.990
2.089
0.512
4711
0.596
0.052


0420
1.786
1.811
1.904
1.997
2.015
2.098
0.445
12018
1.506
0.058


0421
1.797
1.824
1.920
2.018
2.037
2.122
0.489
8162
1.433
0.066


0422
1.746
1.773
1.866
1.962
1.980
2.066
0.512
9799
1.423
0.062


0423
1.573
1.601
1.702
1.814
1.838
1.955
0.845
5155
1.282
0.092


0424
1.726
1.750
1.839
1.931
1.949
2.035
0.383
14713
1.504
0.053


0425
1.780
1.806
1.896
1.987
2.005
2.089
0.399
15271
1.553
0.053


0426
1.785
1.814
1.915
2.017
2.038
2.129
0.561
6785
1.415
0.067


0427
1.791
1.825
1.941
2.055
2.077
2.176
0.823
4271
1.173
0.083


0428
1.772
1.799
1.893
1.990
2.009
2.097
0.540
8640
1.450
0.061


0429
1.781
1.807
1.901
1.996
2.015
2.103
0.465
10832
1.486
0.056


0430
1.782
1.809
1.901
1.995
2.014
2.101
0.520
9229
1.463
0.057


0431
1.801
1.827
1.918
2.010
2.027
2.110
0.572
9119
1.503
0.060


0432
1.815
1.840
1.927
2.017
2.033
2.113
0.516
11109
1.491
0.050


0433
1.782
1.808
1.903
2.000
2.020
2.108
0.412
12767
1.478
0.050


0434
1.752
1.780
1.877
1.980
2.001
2.095
0.495
11386
1.467
0.054


0435
1.795
1.821
1.914
2.009
2.027
2.111
0.404
15751
1.542
0.049


0436
1.775
1.802
1.900
1.998
2.017
2.104
0.402
13814
1.480
0.049


0437
1.767
1.793
1.891
1.993
2.013
2.103
0.409
13273
1.488
0.053


0438
1.810
1.836
1.929
2.021
2.039
2.120
0.406
15090
1.547
0.047


0439
1.647
1.676
1.783
1.901
1.925
2.042
0.761
4766
1.319
0.087


0440
1.801
1.829
1.921
2.016
2.033
2.115
0.347
15730
1.499
0.047


0441
1.804
1.832
1.927
2.022
2.040
2.120
0.327
16232
1.493
0.048


0442
1.655
1.685
1.792
1.903
1.925
2.026
0.256
9205
0.784
0.050


0443
1.559
1.590
1.694
1.808
1.831
1.946
0.865
4148
1.143
0.097


0502
1.744
1.772
1.869
1.973
1.993
2.089
0.527
10468
1.423
0.056


0503
1.757
1.784
1.879
1.980
2.000
2.095
0.453
11708
1.408
0.050


0504
1.776
1.803
1.900
1.999
2.019
2.109
0.351
14009
1.396
0.051


0505
1.787
1.813
1.912
2.011
2.031
2.118
0.297
15480
1.362
0.047



























TABLE 17





Batch







Hc


PHys 1.5 T


93/
Annealing
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
Ws/kg


























0322
4 h 1000° C. +
1.724
1.754
1.859
1.969
1.991
2.097
0.768
4338
1.069
0.079



10 h 880° C.
1.729
1.759
1.862
1.972
1.995
2.102
0.737
5449
1.261
0.074


0323
4 h 1000° C. +
1.719
1.750
1.858
1.976
2.000
2.116
0.486
5242
0.913
0.079



10 h 880° C.
1.721
1.750
1.858
1.978
2.002
2.118
0.483
5573
0.968
0.075


0325
4 h 1000° C. +
1.684
1.716
1.824
1.938
1.962
2.073
0.999
3559
0.940
0.083



10 h 850° C.
1.687
1.716
1.823
1.939
1.963
2.075
0.903
4733
1.224
0.077


0326
4 h 1000° C. +
1.711
1.749
1.873
1.996
2.021
2.137
1.485
2412
0.911
0.110



10 h 850° C.
1.710
1.745
1.866
1.992
2.018
2.137
1.478
2945
1.010
0.102


0327
4 h 1000° C. +
1.688
1.719
1.827
1.941
1.964
2.072
0.830
4123
0.992
0.076



10 h 850° C.
1.689
1.720
1.828
1.942
1.965
2.073
0.890
4324
1.130
0.080


0328
4 h 1000° C. +
1.768
1.795
1.892
1.991
2.011
2.101
0.655
5130
1.160
0.068



10 h 880° C.
1.772
1.799
1.896
1.995
2.014
2.104
0.637
6179
1.368
0.067


0331
4 h 1000° C. +
1.716
1.753
1.873
1.995
2.019
2.132
1.053
3037
0.942
0.090



10 h 880° C.
1.717
1.752
1.870
1.992
2.016
2.130
1.192
3336
1.065
0.093


0332
4 h 1000° C. +
1.706
1.741
1.862
1.986
2.011
2.124
0.994
3212
0.950
0.088



10 h 880° C.
1.709
1.745
1.865
1.988
2.013
2.128
1.079
3460
1.153
0.095


0333
4 h 1000° C. +
1.691
1.726
1.843
1.964
1.989
2.105
1.147
3036
0.944
0.090



10 h 880° C.
1.683
1.718
1.837
1.961
1.986
2.107
1.089
3858
0.972
0.081


0334
4 h 1000° C. +
1.707
1.742
1.860
1.979
2.003
2.115
1.144
3075
0.928
0.090



10 h 880° C.
1.706
1.742
1.859
1.978
2.001
2.114
1.100
3581
1000
0.089


0336
4 h 1000° C. +
1.732
1.766
1.883
2.001
2.024
2.133
1.035
3128
0.893
0.085



10 h 880° C.
1.736
1.770
1.885
2.003
2.027
2.137
1.092
3634
1.125
0.088


0337
4 h 1000° C. +
1.707
1.741
1.861
1.985
2.010
2.127
1.027
3190
0.943
0.089



10 h 880° C.
1.704
1.738
1.857
1.982
2.007
2.123
1.095
3449
1.108
0.095


0338
4 h 1000° C. +
1.712
1.749
1.866
1.986
2.010
2.122
1.161
2888
0.919
0.092



10 h 880° C.
1.713
1.748
1.864
1.986
2.010
2.125
1.260
3421
1.057
0.094


0339
4 h 1100° C. +
1.686
1.722
1.841
1.961
1.983
2.085
0.587
5345
0.897
0.059



10 h 910° C. +
1.687
1.723
1.843
1.963
1.986
2.087
0.507
6186
0.952
0.058



4 h 1000° C.
1.692
1.726
1.841
1.960
1.983
2.086
0.438
6989
0.984
0.061


0420
4 h 1050° C. +
1.788
1.813
1.905
1.998
2.018
2.101
0.420
11185
1.479




10 h 910° C. +
1.789
1.816
1.907
2.000
2.017
2.098
0.444
11842
1.514
0.058



10 h 950° C.
1.794
1.820
1.912
2.004
2.023
2.102
0.433
14222
1.540
0.056


0421
4 h 1050° C. +
1.795
1.822
1.919
2.017
2.037
2.124
0.459
7856
1.387
0.058



10 h 910° C. +
1.797
1.824
1.920
2.018
2.037
2.122
0.489
8162
1.433




10 h 940° C.
1.798
1.825
1.921
2.018
2.037
2.121
0.467
11468
1.519
0.061


0422
4 h 1100° C. +
1.733
1.760
1.856
1.955
1.974
2.063
0.432
11411
1.408
0.053



10 h 960° C.
1.736
1.764
1.859
1.958
1.978
2.068
0.382
14880
1.448
0.048


0423
4 h 1100° C. +
1.635
1.662
1.760
1.867
1.888
1.993
0.653
6647
1.280
0.065



4 h 950° C.
1.634
1.661
1.760
1.868
1.891
1.998
0.621
7626
1.296
0.064


0424
4 h 1050° C. +
1.728
1.752
1.840
1.934
1.953
2.039
0.352
13523
1.458
0.045



10 h 910° C. +
1.726
1.750
1.839
1.931
1.949
2.035
0.383
14713
1.504




10 h 940° C.
1.716
1.743
1.836
1.930
1.948
2.033
0.329
12908
1.217
0.055


0425
4 h 1050° C. +
1.783
1.808
1.898
1.989
2.007
2.089
0.404
11119
1.464
0.048



10 h 910° C. +
1.780
1.806
1.896
1.987
2.005
2.089
0.399
15271
1.553




10 h 925° C.
1.781
1.807
1.897
1.988
2.006
2.088
0.361
18225
1.559
0.047


0432
4 h 1000° C. +
1.797
1.824
1.915
2.009
2.027
2.112
0.640
6876
1.329
0.059



10 h 900° C.
1.799
1.826
1.917
2.010
2.028
2.113
0.541
10118
1.509
0.058


0434
4 h 1000° C. +
1.739
1.767
1.868
1.973
1.995
2.094
0.675
5583
1.235
0.067



10 h 900° C.
1.737
1.765
1.865
1.971
1.992
2.092
0.617
7890
1.420
0.064


0443
60 h 980° C.
1.564
1.595
1.701
1.813
1.836
1.949
1.022
3991
1.245
0.108



























TABLE 18





Batch







Hc


PHys 1.5 T


93/
Annealing
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
Ws/kg


























0423
4 h 1050° C. +
1.577
1.604
1.703
1.815
1.838
1.956
0.798
5361
1.287
0.079



10 h 910° C.
1.573
1.601
1.702
1.814
1.838
1.955
0.845
5155
1.282
0.092


0423
4 h 1100° C. +
1.635
1.662
1.760
1.867
1.888
1.993
0.653
6647
1.280
0.065



4 h 950° C.
1.634
1.661
1.760
1.868
1.891
1.998
0.621
7626
1.296
0.064


0423
4 h 1100° C. +
1.639
1.666
1.764
1.871
1.893
1.998
0.630
6814
1.278
0.065



4 h 910° C. +
1.636
1.664
1.762
1.869
1.890
1.996
0.715
6508
1.241
0.071



4 h 950° C. +
1.635
1.662
1.761
1.870
1.892
1.998
0.616
7820
1.321
0.065



4 h 1030° C.
1.635
1.662
1.762
1.870
1.892
1.999
0.874
5103
1.303
0.076


0423
4 h 910° C.
1.597
1.625
1.723
1.831
1.853
1.964
0.777
4524
0.974
0.077


0423
20 h 910° C.
1.588
1.616
1.716
1.825
1.847
1.962
0.744
4412
1.016
0.074


0423
4 h 950° C.
1.576
1.604
1.703
1.816
1.839
1.959
0.593
4901
1.117
0.071


0423
20 h 950° C.
1.579
1.607
1.705
1.814
1.837
1.952
0.608
4782
1.193
0.080


























TABLE 19





Batch






Hc


PHys 1.5 T


93/
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
Ws/kg

























0325
1.691
1.721
1.829
1.945
1.968
2.079
0.804
4377
1.139
0.079


0328
1.77
1.798
1.898
1.999
2.019
2.108
0.530
6309
1.283
0.060


0330
1.812
1.839
1.932
2.025
2.043
2.122
0.305
14015
1.518
0.043


























TABLE 20





Batch






Hc


PHys 1.5 T


93/
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
Ws/kg

























0325
1.679
1.71
1.822
1.941
1.966
2.078
0.657
4347
1.054
0.078


0328
1.773
1.801
1.899
1.999
2.019
2.108
0.369
9970
1.417
0.050


0330
1.813
1.84
1.933
2.025
2.043
2.121
0.296
19653
1.505
0.045



























TABLE 21





Batch






Hc


Rho in
PHys 1.5 T


93/
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
μΩm
Ws/kg


























0322
1.674
1.705
1.813
1.929
1.953
2.069
0.694
4737
1.067
0.3155
0.071


0323
1.681
1.711
1.820
1.945
1.971
2.095
0.473
6562
1.154
0.1891
0.065


0324
1.747
1.781
1.903
2.034
2.061
2.185
0.655
4720
1.025
0.1572
0.078


0325
1.652
1.684
1.797
1.917
1.941
2.061
0.845
3729
0.878
0.3393
0.081


0326
1.685
1.724
1.852
1.984
2.012
2.136
1.283
2410
0.895
0.3731
0.108


0327
1.649
1.680
1.793
1.917
1.942
2.061
0.712
4155
0.909
0.3274
0.077


0328
1.726
1.754
1.854
1.958
1.980
2.077
0.685
4958
1.097
0.3171
0.069


0329
1.797
1.824
1.918
2.012
2.031
2.114
0.524
7497
1.347
0.3019
0.053


0330
1.786
1.814
1.910
2.009
2.028
2.117
0.382
10051
1.414
0.2904
0.051


0331
1.689
1.724
1.847
1.975
2.002
2.123
0.935
3003
0.884
0.3356
0.088


0332
1.679
1.715
1.838
1.968
1.995
2.115
0.907
3034
0.863
0.3624
0.089


0333
1.664
1.699
1.821
1.951
1.978
2.103
0.828
3402
0.869
0.3557
0.085


0334
1.718
1.754
1.872
1.992
2.016
2.126
0.979
2986
0.826
0.3533
0.083


0335
1.811
1.843
1.948
2.051
2.071
2.158
0.479
5484
1.141
0.2922
0.066


0336
1.687
1.723
1.845
1.972
1.998
2.117
0.877
3184
0.843
0.3372
0.086


0337
1.679
1.715
1.839
1.970
1.996
2.120
0.865
3245
0.882
0.3346
0.087


0338
1.703
1.739
1.858
1.979
2.004
2.119
0.999
2916
0.865
0.3356
0.088


0339
1.686
1.722
1.841
1.961
1.983
2.085
0.587
5345
0.897
0.3027
0.059


0422
1.733
1.760
1.856
1.955
1.974
2.063
0.432
11411
1.408

0.053


0423
1.635
1.662
1.760
1.867
1.888
1.993
0.653
6647
1.280

0.065


























TABLE 22





Batch






Hc


PHys 1.5 T


93/
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
Ws/kg

























0322
1.674
1.702
1.808
1.926
1.950
2.069
0.471
7929
1.376
0.056


0323
1.684
1.714
1.823
1.946
1.971
2.096
0.383
8883
1.353
0.058


0324
1.750
1.783
1.903
2.034
2.060
2.184
0.695
4542
1.113
0.080


0325
1.649
1.681
1.796
1.921
1.946
2.066
0.783
3975
0.968
0.085


0326
1.690
1.728
1.854
1.986
2.012
2.137
1.644
1987
0.915
0.131


0327
1.667
1.699
1.813
1.936
1.961
2.075
0.616
4476
0.992
0.080


0328
1.730
1.757
1.856
1.962
1.982
2.080
0.489
8729
1.393
0.054


0329
1.805
1.831
1.923
2.016
2.034
2.116
0.396
12084
1.520
0.047


0330
1.787
1.814
1.908
2.006
2.025
2.113
0.378
9892
1.457
0.054


0331
1.693
1.726
1.846
1.974
2.001
2.123
0.854
4279
1.237
0.080


0332
1.679
1.714
1.834
1.964
1.990
2.113
0.817
4486
1.233
0.080


0333
1.664
1.698
1.817
1.949
1.977
2.104
0.656
5334
1.274
0.071


0334
1.722
1.755
1.869
1.987
2.011
2.121
0.851
4767
1.253
0.078


0335
1.815
1.845
1.948
2.051
2.070
2.158
0.457
5600
1.258
0.064


0336
1.696
1.729
1.849
1.977
2.002
2.125
0.747
4965
1.228
0.075


0337
1.685
1.719
1.841
1.972
1.999
2.123
0.738
4623
1.226
0.078


0338
1.712
1.745
1.861
1.983
2.008
2.125
0.897
4543
1.246
0.081


0339
1.687
1.723
1.843
1.963
1.986
2.087
0.507
6186
0.952
0.058



























TABLE 23












Hc


Rho in
PHys 1.5 T


batch93/
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
μΩm
Ws/kg


























0323
1.678
1.708
1.818
1.943
1.97
2.095
0.397
6506
1.087
0.1929
0.069


0328
1.692
1.721
1.823
1.933
1.956
2.063
0.683
4863
1.088
0.3146
0.070


0329
1.778
1.806
1.902
1.999
2.018
2.106
0.473
7860
1.346
0.3022
0.053


0330
1.756
1.784
1.882
1.985
2.005
2.096
0.362
10568
1.438
0.2927
0.048


0334
1.683
1.719
1.84
1.967
1.992
2.113
0.856
3306
0.874
0.3474
0.083


0335
1.748
1.780
1.893
2.008
2.031
2.137
0.486
5009
1.119
0.2891
0.067


0339
1.599
1.641
1.776
1.910
1.938
2.062
0.489
4985
0.770

0.066


0442
1.612
1.654
1.780
1.897
1.919
2.022
0.412
5510
0.606

0.057


























TABLE 24





Batch






Hc


PHys 1.5 T


93/
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
Br T
Ws/kg

























0323
1.672
1.701
1.811
1.937
1.964
2.089
0.348
8185
1.297
0.064


0328
1.693
1.721
1.823
1.934
1.957
2.063
0.511
8157
1.37
0.057


0329
1.778
1.804
1.9
1.998
2.017
2.105
0.383
11748
1.475
0.048


0330
1.759
1.786
1.883
1.983
2.004
2.093
0.344
14191
1.46
0.049


0334
1.684
1.717
1.837
1.966
1.992
2.113
0.753
4701
1.202
0.076


0335
1.749
1.781
1.892
2.008
2.031
2.136
0.457
5275
1.174
0.070





















TABLE 25








Av. atomic
Density



Batch

Density
weight of main
using the



93/
μmax
(g/cm3)
elements
rule of three
Δρ (%)







323
 9.047
7.942
56.371
7.942
  0.00%


325
 4.722
7.923
56.296
7.931
−0.11%


327
 4.605
7.918
56.292
7.931
−0.17%


328
13.859
7.917
56.286
7.930
−0.16%


329
15.658
7.912
56.283
7.930
−0.22%


330
22.271
7.909
56.281
7.929
−0.26%


420
20.281
7.905
56.262
7.927
−0.27%


422
11.411
7.894
56.224
7.921
−0.34%


423
 7.626
7.882
56.202
7.918
−0.46%


428
 8.640
7.911
56.279
7.929
−0.23%


429
10.832
7.911
56.279
7.929
−0.23%


430
 9.229
7.914
56.280
7.929
−0.19%


431
 9.119
7.910
56.278
7.929
−0.24%


432
11.109
7.910
56.277
7.929
−0.24%


433
12.767
7.911
56.284
7.930
−0.23%


434
11.386
7.913
56.290
7.931
−0.22%


435
15.751
7.912
56.304
7.933
−0.26%


436
13.814
7.921
56.403
7.947
−0.32%


437
13.273
7.908
56.266
7.927
−0.24%


438
15.090
7.917
56.380
7.943
−0.32%


440
15.730
7.910
56.274
7.928
−0.24%


441
16.232
7.913
56.283
7.930
−0.21%


76/4988
12.150
7.899
56.249
7.925
−0.33%


0502
11.770
7.909
56.277
7.929
−0.25%


0503
11.708
7.910
56.276
7.929
−0.24%


0504
21.461
7.898
56.232
7.922
−0.31%


0505
25.320
7.894
56.192
7.917
−0.29%



























TABLE 26





Batch







Hc

Br
PHys 1.5 T


93/
Annealing
B20 T
B25 T
B50 T
B90 T
B100 T
B160 T
A/cm
μmax
in T
Ws/kg


























0329
4 h 1050° C. +
1.808
1.833
1.925
2.018
2.035
2.115
0.369
17227
1.528
0.046



10 h 910° C.


0330
4 h 1050° C. +
1.813
1.839
1.930
2.021
2.039
2.118
0.354
19591
1.514
0.046



10 h 910° C.


0330
4 h 1050° C.
1.815
1.840
1.934
2.027
2.045
2.122
0.305
22271
1.514
0.045



Cooling



50° C./h +



10 h, 910° C.


0420
4 h 1000° C. +
1.798
1.824
1.914
2.006
2.024
2.104
0.347
20281
1.548
0.042



60 h 950° C.


0420
4 h 1050° C.
1.767
1.793
1.889
1.988
2.007
2.094
0.378
14388
1.456
0.049



Cooling



150° C./h


0505
4 h 1050° C.
1.809
1.837
1.935
2.031
2.049
2.129
0.279
13981
1.290
0.046



Cooling



150° C./h


0505
4 h 1050° C. +
1.787
1.813
1.912
2.011
2.031
2.118
0.297
15480
1.362
0.047



10 h 910° C.


0505
4 h 1050° C. +
1.790
1.817
1.914
2.012
2.032
2.117
0.244
25320
1.524
0.043



10 h 910° C. +



10 h 930° C. +



10 h 940° C.


504
4 h 1050° C.
1.772
1.801
1.899
1.998
2.018
2.109
0.394
10716
1.303
0.055



Cooling



150° C./h


504
4 h 1050° C. +
1.776
1.803
1.900
1.999
2.019
2.109
0.351
14009
1.396
0.051



10 h 910° C.


504
4 h 1050° C. +
1.774
1.800
1.894
1.993
2.011
2.098
0.294
21461
1.52
0.046



10 h 910° C. +



10 h 930° C. +



10 h 940° C.





















TABLE 27









C in
S in



Batch
Annealing
ppmw
ppmw





















93/0435
Unannealed
32
36




4 h 1050° C., H2 + 10 h 910° C., H2
15
12




(two annealing processes)





93/0440
Unannealed
30
13




4 h 1050° C., 10 h 910° C., H2
14
6




(one annealing process)





93/0505
unannealed
30
8




4 h 1050° C., H2
12
4




(one annealing process)






4 h 1050° C., H2 + 10 h 910° C., H2
16
4




(two annealing processes)





76/4998
Unannealed
20
48




4 h 1050° C., H2, 10 h 910° C., H2
21
23




(one annealing process)





76/5180
unannealed
26
60




4 h 1050° C., H2
17
40




(one annealing process)






4 h 1050° C., H2 + 10 h 930° C., H2
15
36




(two annealing processes)





76/5180
Unannealed
26
60




6 h 1050° C., H2
17
31




(one annealing process)






6 h 1050° C., H2 + 10 h 930° C., H2
17
28




(two annealing processes)





























TABLE 28







Dims.

B20
B25
B50
B90
B100
B160
Hc Rings

PHyst. at 1.5 T


batch
sample
(mm)
final annealing
in T
in T
in T
in T
in T
in T
in A/cm
μmax
in Ws/kg















from hot rolling thickness of 1.9 mm



















7604988A
without int. anneal
0.35
4 h, 1050° C.
1.704
1.734
1.836
1.946
1.968
2.069
0.428
10836
0.054


7604988A
without int. anneal
0.35
4 h, 1050° C. +
1.702
1.732
1.834
1.944
1.965
2.068
0.429
11635
0.053





10 h, 910° C.


7604988A
without int. anneal
0.20
4 h, 1050° C.
1.723
1.753
1.857
1.964
1.985
2.080
0.423
10555
0.054


7604988A
without int. anneal
0.20
4 h, 1050° C. +
1.724
1.753
1.860
1.969
1.989
2.086
0.458
10478
0.054





10 h, 910° C.


7604988A
with int. anneal 1 h
0.20
4 h, 1050° C.
1.736
1.764
1.868
1.972
1.993
2.086
0.417
11196
0.053



750° C.


7604988A
with int. anneal 1 h
0.20
4 h, 1050° C. +
1.738
1.766
1.868
1.973
1.994
2.088
0.421
12467
0.052



750° C.

10 h, 910° C.


7604988A
with int. anneal 1 h
0.20
4 h, 1050° C.
1.740
1.769
1.872
1.976
1.996
2.088
0.437
10452
0.054



1050° C.


7604988A
with int. anneal 1 h
0.20
4 h, 1050° C. +
1.740
1.769
1.872
1.977
1.998
2.092
0.458
10668
0.054



1050° C.

10 h, 910° C.







from hot rolling thickness of 2.6 mm



















7604988B
without int. anneal
0.35
4 h, 1050° C.
1.707
1.735
1.838
1.945
1.968
2.067
0.394
11778
0.052


7604988B
without int. anneal
0.35
4 h, 1050° C. +
1.709
1.737
1.839
1.948
1.970
2.072
0.406
12741
0.052





10 h, 910° C.


7604988B
without int. anneal
0.20
4 h, 1050° C.
1.736
1.766
1.869
1.974
1.994
2.087
0.416
10529
0.053


7604988B
without int. anneal
0.20
4 h, 1050° C. +
1.734
1.763
1.867
1.974
1.994
2.089
0.441
11174
0.052





10 h, 910° C.


7604988B
with int. anneal 1 h
0.20
4 h, 1050° C.
1.762
1.790
1.888
1.989
2.009
2.096
0.383
12943
0.050



750° C.


7604988B
with int. anneal 1 h
0.20
4 h, 1050° C. +
1.762
1.790
1.890
1.991
2.011
2.100
0.390
14125
0.049



750° C.

10 h, 910° C.


7604988B
with int. anneal 1 h
0.20
4 h, 1050° C.
1.753
1.783
1.883
1.985
2.005
2.094
0.395
12036
0.052



1050° C.


7604988B
with int. anneal 1 h
0.20
4 h, 1050° C. +
1.758
1.786
1.886
1.989
2.009
2.098
0.399
13094
0.049



1050° C.

10 h, 910° C.







from slab section hot and cold rolled in the pilot plant



















7604988A
without int. anneal
0.35
10 h 1050° C.
1.728
1.757
1.858
1.963
1.984
2.078
0.299
18717
0.043





Abk. 50° C./h;





10 h 930° C. OK


7604988A
without int. Anneal
0.35
4 h, 1050° C.
1.732
1.761
1.860
1.965
1.985
2.077
0.485
8633
0.050





Abk. 10° C./h


7604988A
without int. anneal
0.35
100 h, 910° C.
1.584
1.612
1.711
1.824
1.849
1.972
0.578
5190
0.068


7604988A
without int. anneal
0.35
4 h, 1050° C.
1.734
1.763
1.861
1.965
1.985
2.079
0.410
9315
0.050


7604988A
without int. anneal
0.35
10 h 1050° C.
1.725
1.754
1.855
1.961
1.982
2.077
0.311
12150
0.043





Abk. 50° C./h;





10 h 930° C. OK


7604988A
without int. anneal
0.35
2 h 1050° C.;
1.735
1.765
1.867
1.972
1.993
2.090
0.422
9001
0.050





4 h 910° C.


7605180A
head
0.35
4 h 1050° C.
1.760
1.787
1.888
1.990
2.010
2.101
0.388
9138
0.053


7605180A
head
0.35
4 h 1050° C. +
1.759
1.786
1.886
1.986
2.006
2.097
0.368
14130
0.050





10 h 930° C.


7605180B
head
0.35
6 h 1050° C.
1.782
1.810
1.908
2.008
2.028
2.114
0.334
10925
0.051


7605180B
head
0.35
6 h 1050° C. +
1.782
1.809
1.907
2.005
2.025
2.111
0.254
22632
0.039





10 h 930° C.


7605180A
foot
0.35
6 h 1050° C.
1.784
1.811
1.907
2.004
2.023
2.109
0.370
9222
0.052


7605180A
foot
0.35
6 h 1050° C. +
1.791
1.817
1.912
2.010
2.030
2.115
0.287
18397
0.041





10 h 930° C.




















TABLE 29






1st onset
1st onset





heating
cooling
Best Hc in



Batch 93/
(T custom-character2)
(T custom-character1)
A/cm
Annealing







323
940
932
0.348
4 h 1150° C. +






10 h 910° C.


328
934
914
0.369
4 h 1050° C.






Cooling at






50° C./h + 10 h,






910° C.


329
952
933
0.367
4 h 1050° C. +






10 h 910° C.


330
980
958
0.282
10 h 1050° C.






Cooling at






50° C./h to






930° C.






10 h OK


420
988
964
0.347
4 h 1000° C. +






60 h 950° C.


422
1017 
979
0.382
4 h 1100° C. +






10 h 960° C.


423
1037 
994
0.593
4 h 950° C.


428
951
934
0.540
4 h 1050° C. +






10 h 910° C.


429
947
934
0.465
4 h 1050° C. +






10 h 910° C.


430
944
932
0.520
4 h 1050° C. +






10 h 910° C.


431
950
931
0.572
4 h 1050° C. +






10 h 910° C.


432
946
925
0.516
4 h 1050° C. +






10 h 910° C.


433
949
929
0.412
4 h 1050° C. +






10 h 910° C.


434
944
921
0.495
4 h 1050° C. +






10 h 910° C.


435
953
932
0.404
4 h 1050° C. +






10 h 910° C.


436
952
931
0.402
4 h 1050° C. +






10 h 910° C.


437
954
934
0.409
4 h 1050° C. +






10 h 910° C.


438
955
934
0.406
4 h 1050° C. +






10 h 910° C.


439
958
936
0.578
4 h 1050° C.


440
954
934
0.331
4 h 1050° C. +






10 h 910° C.


441
952
932
0.313
4 h 1050° C. +






10 h 910° C.


443
#NV
1012 
0.792
4 h 1050° C.





OK = Furnace cooling


Cooling from T1 at 150 K/h unless otherwise indicated


Cooling from T2 at 150 K/h unless otherwise indicated


“+” signifies 2 separate annealing processes





Claims
  • 1. A method for the production of a soft magnetic alloy comprising: providing a preliminary product with a composition consisting essentially of:
  • 2. A method according to claim 1, wherein for a sample mass of 50 mg and a DSC heating rate of 10 Kelvin per minute the transition temperature TÜ1 is above 900° C.
  • 3. A method according to claim 1, wherein 960° C.≤T1<Tm.
  • 4. (canceled)
  • 5. A method according to claim 1, wherein the preliminary product is heat treated for a period of over 30 minutes at above TÜ2, and then cooled to T2.
  • 6. (canceled)
  • 7. A method according to claim 1, wherein the preliminary product is cooled from T1 to T2, heat treated at T2 for a period t2, 30 minutes being ≤t2≤20 hours, and then cooled from T2 to room temperature.
  • 8. A method according to claim 1, wherein the preliminary product is cooled from T1 to room temperature and then heated from room temperature to T2.
  • 9. (canceled)
  • 10. (canceled)
  • 11. (canceled)
  • 12. A method according to claim 1, wherein after heat treatment the soft magnetic alloy has a maximum permeability μmax≥5,000, and/or an electrical resistance ρ≥0.25 μΩm, hysteresis losses PHys≤0.07 J/kg at an amplitude of 1.5 T, and/or a coercive field strength Hc of ≤0.7 A/cm and/or an induction B≥1.90 T at 100 A/cm.
  • 13. A method according to claim 12, wherein after heat treatment the soft magnetic alloy has a maximum permeability μmax≥10,000, and/or an electrical resistance ρ≥0.25 μΩm, and/or hysteresis losses PHys≤0.06 J/kg at an amplitude of 1.5 T, and/or a coercive field strength Hc of ≤0.6 A/cm and an induction B≥1.95 T at 100 A/cm.
  • 14. A method according to claim 13, wherein after heat treatment the soft magnetic alloy has a maximum permeability μmax≥12,000, and/or an electrical resistance ρ≥0.30 μΩm, and/or hysteresis losses PHys≤0.05 J/kg at an amplitude of 1.5 T, and/or a coercive field strength Hc of ≤0.5 A/cm, and/or an induction B≥2.00 T at 100 A/cm.
  • 15. A method according to claim 1, wherein a maximum difference in coercive field strength Hc measured parallel to the direction of rolling, measured diagonally (45°) to the direction of rolling or measured perpendicular to the direction of rolling between these two directions is at most 6%.
  • 16. A method according to claim 1, wherein the heat treatment is carried out in a hydrogen-containing atmosphere or in an inert gas.
  • 17. (canceled)
  • 18. (canceled)
  • 19. A method according to claim 1, wherein the preliminary product has the form of one or more sheets or one or more laminated cores.
  • 20. A method according to claim 1, wherein the preliminary product initially has the form of a strip from which at least one sheet is produced by stamping, laser cutting or water jet cutting, wherein the heat treatment is performed on one or more sheets.
  • 21. A method according to claim 20, wherein following heat treatment several sheets are: stuck together by an insulating adhesive to form a laminated core, or surface oxidised to form an insulating layer and then stuck or laser welded together to form a laminated core, orcoated with an inorganic-organic hybrid coating and then further processed to form a laminated core.
  • 22. A method according to claim 1, wherein the preliminary product initially has the form of a laminated core and the heat treatment is carried out on one or more laminated cores.
  • 23. A method according to claim 1, also comprising: providing by use of vacuum induction melting, electroslag remelting or vacuum arc remelting of a molten mass consisting essentially of:
  • 24. A method according to claim 23, wherein the ingot is mechanically formed by hot rolling at temperatures of between 900° C. and 1300° C. to form a slab and then to form a hot strip with a thickness D1, and is then mechanically formed by cold rolling to form a band with a thickness D2, 0.05 mm≤D2≤1.0 mm and D2<D1.
  • 25. A method according to claim 24, wherein a hot strip of thickness D1 is initially produced by continuous casting and then mechanically formed by cold rolling to form a strip of thickness D2, 0.05 mm≤D2≤1.0 mm and D2<D1.
  • 26. A method according to claim 24, wherein the degree of cold working by cold rolling is >40%.
  • 27. (canceled)
  • 28. (canceled)
  • 29. A method according to claim 29, further comprising intermediate annealing.
  • 30. A method according to claim 1, wherein TÜ1≥Tc, wherein Tc the Curie temperature and Tc is ≥900° C.
  • 31. A method according to claim 30, wherein TÜ1>T2>Tc is selected.
  • 32. A method according to claim 1, wherein after heat treatment the average grain size is at least 100 μm.
  • 33. A method according to claim 1, wherein after heat treatment the measured density of the annealed alloy is more than 0.10% lower than the density calculated using the rule of three from the average atomic weight of the metallic elements in the alloy, the average atomic weight of the metallic elements in the corresponding binary FeCo alloy and the measured density of this annealed binary FeCo alloy.
  • 34. A method according to claim 1, wherein after heat treatment the measured density of the annealed alloy is 0.20% to 0.35% lower than the density calculated using the rule of three from the average atomic weight of the metallic elements in the alloy, the average atomic weight of the metallic elements in the corresponding binary FeCo alloy and the measured density of this annealed binary FeCo alloy.
  • 35. A method according to claim 23, wherein during heat treatment the sulphur content is reduced in a H2-containing inert gas atmosphere.
  • 36. A method according to claim 1, further comprising coating the preliminary product with an oxide layer for electrical insulation.
  • 37. (canceled)
  • 38. A method according to claim 36, wherein the preliminary product is heat treated in an atmosphere containing oxygen or water vapor to form an electrically insulating layer.
  • 39. A soft magnetic alloy consisting essentially of:
  • 40. A soft magnetic alloy according to claim 39, having a maximum permeability μmax≥12.000.
  • 41. A soft magnetic alloy according to claim 39, wherein the soft magnetic alloy has hysteresis losses of PHys≤0.05 J/kg and/or a coercive field strength Hc of ≤0.4 A/cm, and/or an induction B≥1.90 T at 100 A/cm.
  • 42. A soft magnetic alloy according to claim 39, wherein 10 wt %≤Co≤20 wt %.
  • 43. A soft magnetic alloy according to claim 39, wherein 0.5 wt %≤V≤4.0 wt %.
  • 44. A soft magnetic alloy according to claim 39, wherein 0.1 wt %≤Cr≤2.0 wt %.
  • 45. A soft magnetic alloy according to claim 39, wherein 0.1 wt %≤Si≤2.0 wt %.
  • 46. A soft magnetic alloy according to claim 39, wherein 0.1 wt %≤Cr+Si+Al+Mn≤1.5 wt %.
  • 47. An electric machine including a soft magnetic alloy according to claim 39.
Priority Claims (2)
Number Date Country Kind
10 2017 009 999.5 Oct 2017 DE national
10 2018 112 493.7 May 2018 DE national
Parent Case Info

This U.S. national phase patent application claims the benefit of PCT/EP2018/079339, filed Oct. 25, 2018, which claims the benefit of DE application no. 10 2017 009 999.5, filed Oct. 27, 2017, and DE application no. 10 2018 112 493.7, filed May 24, 2018, the entire contents of which are incorporated herein by reference for all purposes.

PCT Information
Filing Document Filing Date Country Kind
PCT/EP2018/079339 10/25/2018 WO 00