Patent Grant
9371574
The present invention relates to an Ni3(Si, Ti)-based intermetallic compound to which W is added and to a method for producing the same.
Ni3Si intermetallic compounds, which are nickel intermetallic compounds, have excellent characteristics such as high-temperature strength, corrosion resistance and oxidation resistance. However, polycrystalline Ni3Si intermetallic compounds are brittle as being prone to intergranular fracture, and therefore an intermetallic compound having enhanced ductility and enabled for plastic working at room temperature has been desired. To this end, research and development for improving the Ni3Si intermetallic compounds has been promoted.
For example, an Ni3(Si, Ti)-based intermetallic compound, which is a nickel intermetallic compound, is known as a workable (ductile) intermetallic compound (see Non-Patent Document 1, for example).
In regard to such an Ni3(Si, Ti)-based intermetallic compound, for example, a method for producing a foil of an Ni3(Si, Ti)-based intermetallic compound composed of Ni, Si, Ti and B is known, and it is known that the foil of the Ni3(Si, Ti)-based intermetallic compound produced according to this method has enhanced strength characteristics in a range of temperature from room temperature to 600° C. (see Patent Document 1, for example). The Ni3(Si, Ti)-based intermetallic compound is expected to be applied to catalyst carriers for automobile exhaust control systems and aircraft structural materials, for example.
In addition, an Ni3(Si, Ti)-based intermetallic compound containing specified amounts of Nb and Cr is known as an Ni3(Si, Ti)-based intermetallic compound enabled for plastic working, and it is known that the Ni3(Si, Ti)-based intermetallic compound can be easily worked into a foil (see Patent Document 2, for example).
Furthermore, Ni3(Si, Ti)-based intermetallic compounds containing Ni, Si, Ti and Cu are known as Ni3(Si, Ti)-based intermetallic compounds having ductility, though their workability into a foil is not known (see Patent Documents 3 and 4, for example). Besides, an Ni-based superalloy to which high-concentration Co and Ti are added is known, though it is not an Ni3(Si, Ti)-based intermetallic compound (see Patent Document 5, for example). This alloy has a gamma prime phase including (Ni/Co)3(Al/Ti/Ta).
However, conventional Ni3(Si, Ti)-based intermetallic compounds have not been sufficiently considered for mechanical characteristics, for example, mechanical characteristics after plastic working (such as strength and ductility of a foil produced by rolling). Even in the case of Ni3(Si, Ti)-based intermetallic compounds that have been sufficiently considered for mechanical characteristics, the ductility is gradually reduced when a foil produced by rolling is subjected to a high temperature, for example, and an expensive metal (for example, Nb) is added in order to enhance the ductility at high temperatures and the oxidation resistance. It is therefore desired to sufficiently consider an Ni3(Si, Ti)-based intermetallic compound for mechanical characteristics and enhance the Ni3(Si, Ti)-based intermetallic compound in ductility at high temperatures. Furthermore, an Ni3(Si, Ti)-based intermetallic compound that can be formed with relatively inexpensive metals is desired.
The present invention provides an Ni3(Si, Ti)-based intermetallic compound having enhanced ductility at high temperatures and more enhanced strength characteristics.
The present invention provides an Ni3(Si, Ti)-based intermetallic compound characterized by containing from 25 to 500 ppm by weight of B with respect to a weight of an intermetallic compound having a composition of 100% by atom in total consisting of Ni as a main component, from 7.5 to 12.5% by atom of Si, from 4.5 to 11.5% by atom of Ti and from 0.5 to 5.0% by atom of W.
The inventors of the present invention have originated addition of a high melting point metal element in place of Ti in Ni3(Si, Ti) and made intensive studies. As a result, the inventors of the present invention have found that an Ni3(Si, Ti)-based intermetallic compound containing W in addition to Ni, Si, Ti and B has excellent ductility characteristics in a range of temperature from room temperature to high temperatures to reach completion of the present invention. Having excellent ductility characteristics at high temperatures in particular, the intermetallic compound of the present invention can be plastically worked at high temperatures. Accordingly, the intermetallic compound of the present invention can be worked into a desired shape in fewer steps. In addition, the intermetallic compound of the present invention has ductility at high temperatures to prevent rapid progress of metal fracture at high temperatures.
In addition, the Ni3(Si, Ti)-based intermetallic compound of the present invention can be easily worked into a foil or a sheet (hereinafter, also referred to as foil), and the foil has excellent ductility and strength. The Ni3(Si, Ti)-based intermetallic compound of the present invention is therefore suitable for materials of foils.
In addition, since W, which is less expensive than Nb, is used in the Ni3(Si, Ti)-based intermetallic compound of the present invention, the material cost is relatively low.
Further, the inventors of the present invention have found that the intermetallic compound of the present invention has superior strength characteristics to the Ni3(Si, Ti)-based intermetallic compound disclosed in Patent Document 1, which is composed of Ni, Si, Ti and B.
According to an aspect, an Ni3(Si, Ti)-based intermetallic compound of the present invention is characterized by containing an intermetallic compound having a composition of 100% by atom in total consisting of Ni as a main component, from 7.5 to 12.5% by atom of Si, from 4.5 to 11.5% by atom of Ti and from 0.5 to 5.0% by atom of W, and from 25 to 500 ppm by weight of B with respect to the weight of the intermetallic compound.
First, various embodiments of the present invention will be exemplified. In this specification, “from A to B” means that numerical values A and B are included in the range. In this specification, in addition, an intermetallic compound based on a composition of Ni3(Si, Ti) is referred to as “Ni3(Si, Ti)-based intermetallic compound”.
According to an embodiment of the present invention, in addition to the above-described configuration of the invention, the intermetallic compound may comprise an L12 phase and an Ni solid solution phase.
According to an embodiment of the present invention, the intermetallic compound preferably contains an intermetallic compound having a composition of 100% by atom in total consisting of Ni as a main component, from 7.5 to 12.5% by atom of Si, from 5.5 to 11.5% by atom of Ti and from 0.5 to 4.0% by atom of W, and from 25 to 500 ppm by weight of B with respect to the weight of the intermetallic compound. More preferably, the intermetallic compound contains an intermetallic compound having a composition of 100% by atom in total consisting of Ni as a main component, from 10.0 to 12.0% by atom of Si, from 6.5 to 10.5% by atom of Ti and from 1.0 to 3.0% by atom of W, and from 25 to 100 ppm by weight of B with respect to the weight of the intermetallic compound. Furthermore, the intermetallic compound according to the embodiments may comprise an L12 phase and an Ni solid solution phase.
Alternatively, according to an embodiment of the present invention, the intermetallic compound may contain an intermetallic compound having a composition of 100% by atom in total consisting of Ni as a main component, from 10.0 to 12.0% by atom of Si, from 9.5 to 12.0% by atom of Ti and from 9.5 to 12.0% by atom of W, and from 25 to 100 ppm by weight of B with respect to the weight of the intermetallic compound. In this embodiment, the intermetallic compound preferably contains from 5.5 to 11.5% by atom of Ti and from 0.5 to 4.0% by atom of W, and more preferably contains from 6.5 to 10.5% by atom of Ti and from 1.0 to 3.0% by atom of W.
According to an embodiment of the present invention, the intermetallic compound may be obtained through cold rolling at a rolling reduction of 85-99%. Such cold rolling allows production of an intermetallic compound having excellent strength (for example, tensile strength).
According to an embodiment of the present invention, the intermetallic compound may be obtained through annealing at 300-1050° C. performed after the cold rolling. The annealing may be performed at from 650 to 1050° C.; the annealing performed at a temperature of 650° C. or more allows production of an intermetallic compound having excellent ductility.
The present invention also provides a rolled foil of the Ni3(Si, Ti)-based intermetallic compound according to the invention, the foil having a thickness of 20-300 μm. According to the present invention, the rolled foil of the Ni3(Si, Ti)-based intermetallic compound having excellent ductility characteristics can be produced. Here, the rolled foil includes a rolled sheet, and the rolled foil obtained by the cold rolling or the rolled foil obtained by the cold rolling and the annealing has excellent ductility and strength.
According to another aspect, the present invention provides a method for producing a rolled sheet or foil of an Ni3(Si, Ti)-based intermetallic compound, the method comprising: an ingot preparation step of preparing an ingot containing an intermetallic compound having a composition of 100% by atom in total consisting of Ni as a main component, from 7.5 to 12.5% by atom of Si, from 4.5 to 11.5% by atom of Ti and from 0.5 to 5.0% by atom of W, and from 25 to 500 ppm by weight of B with respect to the weight of the intermetallic compound; a homogenization heat treatment step of performing homogenization heat treatment on the ingot; a thermomechanical heat treatment step of repeating rolling at a rolling reduction of 10% or more and annealing at 900-1100° C. on the ingot after the homogenization heat treatment step three times or more to prepare a sheet material; and a cold rolling step of performing cold rolling on the sheet material at a rolling reduction of 85-99%.
In the method for producing a rolled sheet or foil of an intermetallic compound of the present invention, the rolling in the thermomechanical heat treatment step may be cold rolling or warm rolling at 350° C. or lower. Furthermore, the rolling in the thermomechanical heat treatment step may be warm rolling at 250-350° C.
The various embodiments shown herein may be combined with one another.
[Content of Each Element]
Next, the content of each element will be described.
The content of Ni is, for example, from 78.5 to 81.0% by atom, and preferably from 78.5 to 80.5% by atom. Specific examples of the content of Ni include 78.5, 79.0, 79.5, 80.0, 80.5 and 81.0% by atom. The content of Ni may be between any two of the numeral values exemplified here.
The content of Si is from 7.5 to 12.5% by atom, and preferably from 10.0 to 12.0% by atom. Specific examples of the content of Si include 7.5, 8.0, 8.5, 9.0, 9.5, 10.0, 10.5, 11.0, 11.5, 12.0 and 12.5% by atom. The content of Si may be between any two of the numeral values exemplified here.
The content of Ti is from 4.5 to 11.5% by atom, preferably from 5.5 to 11.5% by atom, and more preferably from 6.5 to 10.5% by atom. Specific examples of the content of Ti include 4.5, 5.0, 5.5, 6.0, 6.5, 7.0, 7.5, 8.0, 8.5, 9.0, 9.5, 10.0, 10.5, 11.0 and 11.5% by atom. The content of Ti may be between any two of the numeral values exemplified here.
The content of W is from 0.5 to 5.0% by atom, preferably from 0.5 to 4.0% by atom, and more preferably from 1.0 to 3.0% by atom. Specific examples of the content of W include 0.5, 1.0, 1.5, 2.0, 2.5, 3.0, 3.5, 4.0, 4.5 and 5.0% by atom. The content of W may be between any two of the numeral values exemplified here.
The content of each element is adjusted appropriately so that the total content of Ni, Si, Ti and W is 100% by atom.
The content of B is from 25 to 500 ppm by weight and preferably from 25 to 100 ppm by weight. Specific examples of the content of B include 25, 40, 50, 60, 75, 100, 150, 200, 300, 400 and 500 ppm by weight. The content of B may be between any two of the numeral values exemplified here.
According to an embodiment of the present invention, specific compositions of the intermetallic compound are obtained by adding the above-mentioned content of B to the compositions shown in Tables 1-3, for example.
[Rolled Sheet or Foil and Method for Producing the Same]
Next, a rolled sheet or foil of an Ni3(Si, Ti)-based intermetallic compound will be described.
The rolled sheet or foil of an Ni3(Si, Ti)-based intermetallic compound is obtained by forming an Ni3(Si, Ti)-based intermetallic compound having a composition of the embodiment into a sheet or a foil. Though not particularly limited, the thickness of the rolled sheet or foil of an Ni3(Si, Ti)-based intermetallic compound is, for example, 10 μm-10 mm, preferably 10-1000 μm, and more preferably 20-300 μm. Hereinafter, production steps of the rolled sheet or foil will be described.
(1) Ingot Preparation Step
First, an ingot having a composition mentioned in the embodiment is prepared. For example, the ingot can be obtained by weighing appropriate amounts of Ni, Si, Ti, W and B to compose an Ni3(Si, Ti)-based intermetallic compound having a composition of the embodiment, heating and melting the components in a melting furnace, and pouring the resulting molten metal into a mold for casting. The melting furnace is not particularly limited as long as it can melt such metals, and usable examples thereof include a vacuum induction melting furnace and an arc melting furnace.
(2) Homogenization Heat Treatment Step
Homogenization heat treatment is performed on the ingot obtained in the ingot preparation step. The homogenization heat treatment renders the elements in the ingot free from segregation, so that the composition of the whole ingot can be homogeneous and uniform. In the homogenization heat treatment, the ingot was put in a vacuum and heat-treated at 950-1100° C. for 24-48 hours, for example.
(3) Thermomechanical Heat Treatment Step
Next, rolling and annealing is repeatedly performed on the ingot after the homogenization heat treatment to form the ingot into a sheet to obtain a sheet material. First, the ingot given the homogenization heat treatment is rolled into a sheet material. After the rolling, annealing is performed to eliminate work-hardening, and then rolling is further performed. The rolling and the annealing are performed repeatedly to form the ingot into a sheet material having a desired thickness.
The rolling process is not particularly limited; for example, a sample can be caused to pass through a rolling machine to be rolled. For example, when the material is rolled with a rolling machine, it is preferable that the rolling is performed at a rolling reduction of 0.5-1.5% per pass and 10-20 passes of rolling is performed. Such rolling with a rolling machine is repeated so that the rolling reduction of the entire rolling process is 10% or more, preferably 10-50%, and more preferably 15-30%. In this specification, the “rolling reduction” means a total thickness reduction by a plurality of passes of rolling, unless stated clearly with “per pass”.
The rolling temperature is not particularly limited; the rolling may be cold rolling or warm rolling. While cold rolling is acceptable, warm rolling at a temperature of 350° C. or less (preferably, 250-350° C.) is desirable in this embodiment. It is thereby possible to reduce the number of times of annealing, if any, to be performed after the rolling. Ordinary metals are more workable at a higher rolling temperature, whereas the Ni3(Si, Ti)-based intermetallic compound prefers warm rolling at a temperature of 350° C. or less (more preferably, 250-350° C.), because it has yield strength showing inverse temperature dependency and therefore becomes less deformable when the temperature is raised.
The annealing can be performed under any condition as long as it can eliminate work-hardening of the sample. In the annealing, the material is retained in a vacuum at 900-1100° C. for 1-5 hours, for example.
The rolling and the annealing are repeated until a sheet material having a desired thickness is obtained. Specifically, the rolling and the annealing are repeated three times or more, and preferably four times or more.
(4) Full Annealing Step
Full annealing may be performed on the sheet material given the thermomechanical heat treatment. The full annealing can eliminate the internal stress of the sheet material given the thermomechanical heat treatment. The full annealing is therefore preferable as a treatment prior to the cold rolling to be described next. In the full annealing, the sheet material is put in a vacuum and heat-treated at 900-1050° C. for 0.5-5 hours, for example.
(5) Cold Rolling Step
Next, cold rolling is performed on the sheet material at a rolling reduction of 85-99%. As a result of the cold rolling, a desired rolled sheet or foil of an Ni3(Si, Ti)-based intermetallic compound is obtained. The cold rolling process is not particularly limited; for example, the sheet material can be caused to pass through a rolling machine to be cold-rolled.
When one-time cold rolling is insufficient for obtaining a foil having a desired thickness, annealing may be performed after the cold rolling, and then cold rolling may be performed again to further reduce the thickness. In the annealing, the material is retained in a vacuum at 800-1000° C. for 0.5-2 hours, for example.
In addition, the strength characteristics of the sample can be enhanced by work-hardening due to the cold rolling. The rolled sheet or foil of an Ni3(Si, Ti)-based intermetallic compound after the cold rolling therefore has very high strength characteristics and can be used as a structural material.
(6) Annealing Step
Annealing can be performed on the rolled sheet or foil of an Ni3(Si, Ti)-based intermetallic compound obtained in the cold rolling step. The annealing is performed in a vacuum at 100-1050° C. The annealing time is 0.5-2 hours, for example. The annealing step enhances the ductility characteristics of the sheet or the foil. In addition, when the sheet or the foil is used at a temperature of 100-700° C., the annealing at a temperature equal to or higher than the use temperature can stabilize the characteristics of the sheet or the foil.
[Demonstration Experiment 1]
Next, an effect demonstration experiment for verifying the effect of the present invention will be described. In the effect demonstration experiment, Demonstration Experiment 1 for studying the characteristics of the target intermetallic compound was performed. Hereinafter, Demonstration Experiment 1 will be described.
(Sample Preparation)
(1) Ingot Sample Preparation Step
Table 4 shows the composition of an intermetallic compound prepared in Demonstration Experiment 1 and the composition of an intermetallic compound prepared for comparison, which is disclosed in Patent Document 1.
First, the respective metals (purity of each metal: 99.9% by weight or more) and B were weighted so as to form the two kinds of compositions shown in Table 4. Subsequently, the weighted metals and B were melted in an arc melting furnace and casted to prepare ingots each having a thickness of 10 mm or more. A melting chamber of the arc melting furnace was evacuated, and the atmosphere in the arc melting furnace is replaced with an inert gas (argon gas). Non-consumable tungsten electrodes were employed as electrodes of the furnace, and a water-cooling copper hearth was employed as a mold.
A sample containing 2.0 atomic % of W is an example of the present invention, which hereinafter is referred to as “Example Sample 1”. On the other hand, a sample not containing W is referred to as “Comparative Example Sample”, which may be simply referred to as “Ni3(Si, Ti)” in the drawings, meaning that it consists only of the basic composition.
(2) Homogenization Heat Treatment Step
Subsequently, a homogenization heat treatment step was performed in which each ingot was retained in a vacuum at 1050° C. for 48 hours for homogenization. The ingot obtained through the homogenization heat treatment is referred to as “homogenization heat-treated ingot”.
(3) Warm Rolling Step
Subsequently, the homogenization heat-treated ingot was cut into a thickness of 10 mm, and warm rolling and annealing process was repeated on the cut ingot five times to prepare a sheet material having a thickness of 2 mm. In the warm rolling, the sample was heated up to 300° C. in the atmosphere and subjected to 10-20 passes of rolling by using a 2-high rolling machine, provided that the rolling reduction was approximately 0.1 mm per pass. In addition, the sample was heated for each pass.
In the annealing process, the sample was retained in a vacuum at 1000° C. for 5 hours.
(4) Full Annealing Step
Subsequently, full annealing was performed in which the sheet material was retained in a vacuum at 1050° C. for 1 hour.
(5) Cold Rolling Step
Subsequently, cold rolling was performed on the sheet material obtained in the preceding step at room temperature to prepare a foil. The cold rolling was performed at a rolling reduction of 90%, during which annealing was not performed. The cold rolling process was performed by using a dies steel roll until the thickness of the sheet material reached approximately 0.5 mm, and then performed by using a carbide roll. The same 2-high rolling machine was used for both the dies steel roll and the carbide roll. The thickness of the foil prepared was 0.2 mm. Hereinafter, such a foil obtained by cold rolling without annealing after the cold rolling is referred to as “cold-rolled foil”.
(6) Annealing Step
Subsequently, the cold-rolled foil obtained in the preceding step was retained in a vacuum at 500, 600, 700, 800, 900 or 1000° C. for 1 hour for annealing. Hereinafter, the term “annealing” means annealing after the cold rolling, unless otherwise stated.
As described above, the sample was prepared.
(Sample Evaluation)
(1) Microstructure Observation
Microstructure observation was performed on the sample obtained after the homogenization heat treatment step (Example Sample 1). Specifically, an SEM photograph of the microstructure of the homogenization heat-treated ingot (Example Sample 1) was taken.
Further, an X-ray diffraction measurement was performed on the homogenization heat-treated ingot (Example Sample 1) in order to identify the constituent phases in the microstructure.
Further, EPMA was performed on Example Sample 1 for microstructure analysis.
As shown in
(2) Vickers' Hardness Test
Next, a Vickers' hardness test was performed on (i) homogenization heat-treated ingot (Example Sample 1), (ii) cold-rolled foil (Example Sample 1) and (iii) cold-rolled foil subjected to annealing at each temperature (Example Sample 1). In the Vickers' hardness test, a square pyramid diamond indenter was pushed into each sample. The load was mainly 300 g, and the retention time was 20 seconds.
(3) Room-Temperature Tensile Test
Next, a room-temperature tensile test was performed on (i) cold-rolled foil and (ii) cold-rolled foil subjected to annealing at each temperature of Example Sample 1 and Comparative Example Sample. The size of the samples used in the room-temperature tensile test was 10 mm in length of a parallel part and 4 mm in width. The room-temperature tensile test was performed in the atmosphere at room temperature and at a straining rate of 8.4×10−5 s−1.
Furthermore,
Subsequently, fracture surface observation was performed on Example Sample 1 after the tensile test to study its fracture form in the room-temperature tensile test.
In
(4) High-Temperature Tensile Test
Next, a tensile test was performed on Example Sample 1 and Comparative Example Sample, both subjected to annealing at 900° C. for 1 hour, at room temperature and high temperatures. The size of the foils used in the high-temperature tensile test was 10 mm in length of a parallel part and 4 mm in width. The high-temperature tensile test was performed in a vacuum at a straining rate of 8.4×10−5 s−1 from room temperature to 700° C.
Next,
Subsequently, fracture surface observation was performed on Example Sample 1 after the high-temperature tensile test, too.
In
As revealed by the results of Demonstration Experiment 1, Example Sample 1 has superior tensile strength and ductility to Comparative Example Sample at room temperature. Even at high temperatures, Example Sample 1 has superior tensile strength and higher ductility, in particular. Accordingly, Example Sample 1 has characteristics preventing rapid progress of metal fracture at high temperatures.
[Demonstration Experiment 2]
Next, Demonstration Experiment 2 was performed to see if intermetallic compounds similar to Example Sample 1 in Demonstration Experiment 1 can be obtained when the W content is varied. Hereinafter, Demonstration Experiment 2 will be described.
(Sample Preparation)
In Demonstration Experiment 2, samples having the two kinds of compositions shown in Table 6 were prepared. Table 6 shows the compositions of intermetallic compounds prepared in Demonstration Experiment 2.
The samples in Demonstration Experiment 2 were prepared through (1) Ingot sample preparation step and (2) Homogenization heat treatment step described above in Demonstration Experiment 1. That is, in (1) Ingot sample preparation step, the samples were prepared under the same conditions as in Demonstration Experiment 1 except that the respective metals (purity of each metal: 99.9% by weight or more) and B were weighted so as to form the two kinds of compositions shown in Table 6.
Both the samples shown in Table 6 are examples of the present invention, of which, hereinafter, the sample containing 0.5 atomic % of W is referred to as “Example Sample 2”, and the sample containing 4.0 atomic % of W is referred to as “Example Sample 3”.
(Sample Evaluation)
(1) Microstructure Observation
First, microstructure observation (SEM observation) was performed on the samples prepared.
On the other hand,
Meanwhile,
(2) Vickers' Hardness Test
Next, a Vickers' hardness test was performed on Example Samples 2 and 3. In the Vickers' hardness test, a square pyramid diamond indenter was pushed into each sample as in the case of Demonstration Experiment 1. The load was 1 kg and the retention time was 20 seconds.
Table 7 reveals that the samples have almost the same hardness, though the samples have greatly different microstructures, having greatly different volume fractions of the parent phase (L12 phase) or volume fractions of the second phase (fcc-Ni solid solution phase). The results lead to the expectation that Example Samples 2 and 3 as well as Example Sample 1 can be subjected to the same cold rolling step as in Demonstration Experiment 1 and produce comparable effects even when subjected to annealing.
The present invention can be applied to chemical equipment materials (catalyst carriers, chemical container members, and the like), electric/electronic materials and structural materials as materials alternative to stainless steel foils and nickel foils, for example. When applied to these materials, the intermetallic compound of the present invention is workable at high temperatures and easily produced as having excellent ductility characteristics at high temperatures. In addition, the intermetallic compound of the present invention can be attached to another structural member to protect the structure or can be used as a base material for a laminate as being capable of preventing rapid progress.
| Number | Date | Country | Kind |
|---|---|---|---|
| 2009-212085 | Sep 2009 | JP | national |
| Filing Document | Filing Date | Country | Kind | 371c Date |
|---|---|---|---|---|
| PCT/JP2010/065835 | 9/14/2010 | WO | 00 | 3/26/2012 |
| Publishing Document | Publishing Date | Country | Kind |
|---|---|---|---|
| WO2011/030904 | 3/17/2011 | WO | A |
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| 3311470 | Evans et al. | Mar 1967 | A |
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| Number | Date | Country | |
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| 20120216922 A1 | Aug 2012 | US |
