This application claims priority to Swedish Patent Application No. 1451548-0, filed on Dec. 16, 2014, the entire contents of which are incorporated herein by reference.
The present invention relates to a sampling device for thermal analysis of solidifying metal, especially for thermal analysis in the production of castings.
Thermal analysis is a technique monitoring variations in temperature change of certain molten substances during solidification and subsequent solid state transformations to be able to determine the microstructure and hence properties of the substances in solid form. This is accomplished by obtaining a representative sample from the melt, transferring it into a sample vessel and recording and evaluating a time-dependent temperature change in the sample during solidification, by means of temperature responsive means, such as thermocouples or other devices known in the art.
When using thermal analysis for controlling solidification processes in molten materials, such as cast-iron or aluminium alloys, a most critical issue is to provide for a controlled, even and reproducible rate of heat removal from the sample. The reason for this is to make it possible to measure temperature changes during phase transformations, the knowledge of which is essential in order to predict microstructures and control certain solidification processes.
Thermal analysis is a heat balance. The ultimate shape, and thus the resolution, of the cooling curve is determined by the balance between the latent heat liberated during solidification and the heat transferred from the metal to the sampling device and from the sampling device to the atmosphere. It is evident that the amount of heat liberated by the solidification of a 200 gram sample of, for example cast iron, is fixed. If the 200 gram sample is contained in a vessel that has a high heat capacity, the heat liberated by the solidification will be less able to prevail over the heat transferred to and from the vessel. The result is that a sampling vessel with high thermal mass and/or a high cooling rate will provide less resolution in the cooling curves. High heat transfer from the vessel to the atmosphere will also result in fast cooling of the sample, which influences the development of the microstructure. For instance, fast cooling caused by the vessel will alter the solidification behaviour of the iron by inducing chill by increasing the undercooling. In order to extract as much information as possible from the heat liberated by the solidification, it is necessary to design a thermal analysis sampling device such that it neither masks nor dilutes the information provided by the solidification. The other major requirement of a thermal analysis sampling device is that it must ensure consistent sampling conditions. Because the differences in the liberated heat between a good microstructure and an out-of-spec microstructure can be very small, it is critical that all variations measured are due to differences in the material to be analysed and not due to differences in the sampling technique.
Sampling devices for thermal analysis may be constructed of a variety of materials as long as the material is able to withstand the temperature of the melt to be analysed at least in the sense of being dimensionally stable at the high temperature and not causing any undesired reaction with the molten sample. For example, it is previously known to construct the sampling devices from graphite, ceramic materials, steel, or a combination thereof.
Thermal analysis sampling devices commonly used in the evaluation of cast iron microstructures are typically constructed of chemically bonded sand, also known as “sand cups” within the technical field. These types of sampling devices do however have certain shortcomings which affect the accuracy of microstructure prediction during thermal analysis. Sand cups typically have thick sand walls to ensure safe containment of the molten iron, which results in high heat capacity causing the vessel to serve as a heat sink that extracts heat from the sampled iron, and thereby influencing the solidification behaviour. Sand cups typically have open surfaces resulting in large radiation heat losses and thus imbalanced heat losses from the top, sides and bottom of the sample volume. In addition, the change in radiated heat transfer on solidification causes the thermal hot spot to move during the solidification process. Furthermore, sand cups, especially those filled from the open surface of the cup, are liable to variation in both the sample volume (operator consistency) and entrainment of oxygen during filling. Moreover, thermocouples found in conventional sand cups are rigidly mounted and consumed with each analysis. Therefore, variations in the thermocouple calibration and the location of the measurement junction directly influence the accuracy of the thermal analysis. The location of the simplified connection of these thermocouples lead to biases due to the uneven heat transfer conditions of the 2 wires as they pass separately from the sample to the rudimentary connector.
EP 1 925 936 discloses a sampling device for thermal analysis of molten metal which solves the drawbacks of conventional sampling devices constructed of chemically bonded sand. The sampling device is a container comprising one common filling inlet on the upper side of said container and at least two cavities, each cavity having a protective tube adapted for enclosing a temperature responsive member. The common filling inlet is branched into at least two filling channels ending in said cavities. The sampling device is manufactured of steel or a moulded fibrous refractory cloth material.
Other examples of previously known sampling devices are disclosed in WO 96/23206 and EP 1 034 419. Said sampling devices comprise a container intended to contain a sample quantity of liquid metal during analysis, and a sensor for thermal analysis. The container of such sampling devices is intended to be immersed in a molten bath of the material to be analysed in order to fill the container with a consistent sample quantity. The container is thereafter removed from the molten bath and the sample quantity is allowed to solidify while recording the time-dependent temperature change during said solidification.
While the sampling devices described above solve at least some of the problems associated with conventional sampling devices constructed of chemically bonded sand, they may be less preferred in certain circumstances. For example, they often tend to have higher production cost than sand cups. They are also not designed to fill multiple vessels simultaneously.
The object of the invention is a sampling device for thermal analysis which may be easily manufactured in a cost-effective manner and which ensures that reliable results during thermal analysis are consistently achieved irrespective of the skill and discipline of the operator.
The object is achieved by a sampling device in accordance with independent claim 1. Embodiments are defined by the dependent claims.
The sampling device for thermal analysis of solidifying metal according to the present invention comprises an upper side and a lower side. The uppermost portion of the upper side defines a horizontal first plane. The sampling device comprises at least two cavities adapted to be filled with a molten metal to be analysed. The cavities are each intended to substantially enclose the molten metal during thermal analysis and are as such only provided with openings necessary for their function, such as the filling opening and a possible ventilation hole or channel for venting out gaseous substances from the cavity during filling. For the purpose of thermal analysis, a respective temperature responsive means is provided at least partly inside each of the cavities, and the cavities are thus adapted for containing such a temperature responsive means. The sampling device further comprises one common filling inlet having an inlet opening on the upper side of the sampling device. It is preferred that the common filling inlet is the single filling inlet of the sampling device. The common filling inlet is at a distance from the upper side of the sampling device branched into a plurality of filling channels, such as two filling channels. Each filling channel opens up into a respective cavity. The inlet opening of the common filling inlet is arranged in a second plane essentially parallel to the first plane below said first plane. Thus, the inlet opening of the common filling inlet is arranged vertically below the uppermost portion of the upper side of the sampling device.
Suitably the inlet opening of the common filling inlet may be arranged in a horizontal plane which is arranged at a distance from the first plane which is at least 20%, preferably at least 25%, of the distance between the first plane and a horizontal plane tangent to an uppermost internal surface of at least one of the first cavity and the second cavity. In case of cavities having different distances between the first plane and their respective uppermost internal surface, the horizontal plane tangent to an uppermost internal surface of a cavity is preferably the horizontal plane tangent to an uppermost internal surface of the cavity having the smallest distance to the first plane.
The inlet opening of the common filling inlet may be arranged essentially in a horizontal plane tangent to an uppermost internal surface of at least one of the first cavity and the second cavity.
The sampling device may furthermore comprise open ventilation channels or holes connecting a cavity through the upper surface to the open atmosphere. The purpose of such a ventilation hole or channel is to enable gaseous substances from the cavity to be vented out from the cavity during for example filling. Each cavity is suitably substantially enclosed except for the respective filling channel and the respective ventilation channel/hole.
The sampling device may further comprise a ring shaped recess arranged in the upper side of the sampling device radially outside of and concentric with the opening of the common filling inlet. The purpose of such a recess is to (at least temporarily) accommodate any excess molten metal after filling of the sampling device. Alternatively, the sampling device may comprise a run-off channel on the upper side of the device connected to the filling inlet. The purpose of such a channel is to drain away any excess molten metal from the filling inlet so that the total volume of the filling inlet is consistent from one sample to the next. The run-off channel is adapted to remove the excess molten in a safe direction, i.e. away from operators or other sensitive apparatus.
The cavities may or may not have the same internal volume, have the same geometrical shape, and/or be arranged with their respective centres in the same horizontal plane (i.e. with their centres arranged at the same vertical distance from the first plane). It is also plausible to arrange the cavities of the sampling device such that each of the cavities has its uppermost internal surface arranged in the same horizontal plane, irrespective of whether or not the cavities have the same internal volume and/or geometrical shape.
In the sampling device, a substance adapted to intentionally alter the solidification behaviour of the molten metal contained thereof during thermal analysis may be provided in at least one cavity. For example, if desired, the inner walls of one or more of the cavities facing the sample quantity may be provided with a reactive coating adapted to alter the solidification behaviour of the molten metal. Such a coating may for example be provided by brushing a slurry or the like of a suitable coating composition onto the inner wall of a cavity and allowing the coating composition to dry such as to form the coating. It is also possible to provide a coating on the walls of one cavity whereas another cavity of the sampling device is either free from such a coating or contains a different coating intended to alter the solidification in a different manner. Thereby, it may be possible to determine the solidification behaviour of the same melt simultaneously for different conditions or different purposes. Instead of a reactive coating, a powdery or granular substance may be provided to one or more cavities and only contained in the cavity without being coated on a wall of the cavity. The substance may also be contained in a sacrificial envelope to prevent its escape from the cavity during transport and handling. Alternatively, a paste of a substance may be adhered to a part of the wall of a cavity, for example as a “blob”.
The sampling device may comprise additional cavities adapted to be filled with molten metal to be analysed if desired. For example, the sampling device may comprise three, four or five cavities. The cavities suitably share the same common filling inlet, and are suitably arranged at equal distances from the common filling inlet.
Moreover, the sampling device may suitably comprise a protective tube adapted to contain at least one temperature responsive means during thermal analysis. Such a protective tube may extend through at least one wall of the sampling device and be open in one end to enable inserting a temperature responsive means. The protective tube may for example extend radially through a cavity and comprise at least one end opening adapted for inserting a temperature responsive means into the protective tube. Alternatively, the protective tube may comprise a closed end and extend radially into a cavity such that the closed end is arranged essentially in the centre of said cavity. The protective tube may if desired comprise a plurality of temperature responsive means.
The present disclosure also relates to a kit for thermal analysis comprising at least two, preferably a plurality of, temperature responsive means, such as thermocouples, and a sampling device as disclosed above. The number of temperature responsive means generally correspond to the number of cavities in the sampling device, but could also be more than the number of cavities of the sampling device in order to obtain cooling curves from different locations within a cavity.
The invention will be described below with reference to the accompanying drawings. The invention is not limited to the embodiments shown but may be varied within the scope of the appended claims. Moreover, the drawings shall not be considered drawn to scale as some features may be exaggerated in order to more clearly illustrate the features of the sampling device or the details thereof.
In the figures representing the present invention, the cavities are illustrated as sphere shaped which is a preferred embodiment. However, the cavities may also have other shapes such as oblate spheroid, sphere with a flat top or bottom, elipsoid, cube, square prism, regular polygon prism, 3 or more sided prism, etc. if desired without departing from the scope of the invention. Furthermore, the cavities may have the same shape, such as shown in the figures, or may be of different geometrical shapes if desired. Moreover, the size of the cavities may be the same or may differ from each other in the same sampling device to provide different solidification rates. In case of the cavities having different geometrical shape, the internal volume of the cavities need not necessarily be substantially different. The size and shape of the cavities can be adapted to the intended purpose by a person skilled in the art in view of the present disclosure.
In contrast to the prior art shown with reference to
The common filling inlet 4 ensures that the molten metal is filled into the sampling device 1 through only one inlet opening 7, thereby ensuring that an operator need not ensure equal amounts to be filled into the cavities as would be the case if each cavity would be filled separately. Each filling channel 5, 6 opens into a respective cavity 2, 3 of the sampling device at an inlet opening of a cavity. As shown in
Each of the cavities 2, 3 is provided with at least one temperature responsive means (not shown in the figure), at least during thermal analysis. The temperature responsive means is adapted to measure the temperature during the solidification of the molten metal and the measurements are recorded over time in order to determine the changes during the solidification process of the molten metal. In
As shown in
It has previously been considered necessary to arrange filling inlets well above the level of the cavities in order to ensure consistent filling of the cavities. However, the inventors have found that consistent filling of the cavities is still achieved despite the location of the filling inlet according to the present invention.
The sampling device according to the present invention comprises at least two cavities, irrespective of the embodiment thereof. This has the benefit of providing two separate results for the same molten metal sample, thereby increasing the accuracy of the readings. It is however also possible to analyse different aspects of the same melt at the same time by means of the two cavities. For example, one of the cavities may be free from any additions and thereby analysing the actual molten metal whereas another cavity may be provided with a substance influencing the solidification behaviour of the molten metal, for example with the purpose of studying the nucleating potential by adding an inoculant or analysing the carbon equivalent by adding sulphur and/or tellurium or by adding sulphur and/or reducible oxides to intentionally alter the growth behaviour of the graphite, or by adding materials to enhance the analysis of the solid state transformation of austenite to ferrite and pearlite. Addition of one or more substances adapted to alter the solidification behaviour of the molten metal may be made in accordance with any previously known method. For example, such a substance may be added in the form of a functional or reactive coating which is applied to the internal walls of a cavity by means of for example dipping, rinsing, spraying or brushing a coating composition comprising the substance. The substance may also in some cases be added in the form of a powder, granulate or the like merely introduced into the cavity without attaching the powder to the internal walls of the cavity, the powder/granulate optionally contained in a sacrificial envelope, or by forming a paste containing the substance, forming it into a small ball, “blob” or the like and adhering the ball to a part of the internal wall of the cavity.
The filling channels 5, 6 are illustrated in both
While
It is preferred that the central axis B of the common filling inlet corresponds to the central axis of the sampling device for all of the embodiments disclosed herein.
The sampling device may suitably further comprise open ventilation holes or channels 15 in the walls of the cavities connecting each cavity 2, 3 with the open atmosphere above the sample, such as shown in the exemplifying embodiment shown in
In accordance with the present invention, the inlet opening of the common filling inlet is arranged in a second plane which is parallel to a first plane constituting a horizontal plane which is tangent to the uppermost part of the upper side of the sampling device. The second plane is arranged at lower height than the first plane and may be arranged at any height between the first plane and a plane tangent to an uppermost part of an internal surface of a cavity, excluding the first plane but including the plane tangent to an uppermost part of an internal surface of a cavity. In case the cavities have different size or are arranged at different vertical distances within the sampling device, the plane tangent to an uppermost part of an internal surface of a cavity corresponds to said plane of the cavity having such an uppermost part of an internal surface closest to the uppermost part of the sampling device (the first plane).
Arranging the ventilation hole or channel in a plane other than the vertical plane extending through the centre of a cavity, such as a plane parallel to said vertical plane, may also provide additional advantages. For example, it is then possible to allow a potential protective tube 12 to extend through the cavity and be supported in the wall on the opposite side of the cavity such as shown in
While not shown in
The sampling device may be constructed of sand or sand based materials, especially chemically bonded sand. If desired the sampling device may in such a case also comprise an outer housing of another material, such as steel, if desired without departing from the scope of the invention. However, such an outer housing is not necessary and the sand itself provides sufficient stability of the sampling device. The sampling device may also be constructed of other types of materials such as synthetic sand or insulating refractories, a castable refractory, fibre cloth or coated steel. Also in the case of such materials, the sampling device may optionally comprise a housing (of the same or of a different material) if desired.
The sampling device may also optionally comprise external support means if desired. Such support means may for example be a supporting device serving the purpose of properly aligning temperature responsive means within one or more of the possible protective tubes during insertion thereof as well as during operation of the sampling device, i.e. during thermal analysis.
Any type of temperature responsive means that is suitable for measuring temperatures in molten metals, such as molten cast iron, may be used in connection with the sampling device according to the present invention. One example of such a temperature responsive means is a thermocouple.
The temperature responsive means may during thermal analysis suitably be arranged in a protective tube in order to ensure that the temperature responsive means is neither damaged nor consumed during the thermal analysis. Thus, the temperature responsive means may be removed from the sampling device after termination of the thermal analysis and reused in another sampling device. Furthermore, it is possible to arrange a plurality of temperature responsive means in the same protective tube if desired, for example for the purpose of obtaining cooling curves from different locations within a cavity, to increase the output of the temperature responsive means, or to reduce the measurement error.
The sampling device is not limited to the embodiments disclosed above and shown in the figures. For example, the protective tube need not be arranged vertically in the sampling device, but could for example be arranged essentially horizontally or angled to a horizontal and a vertical plane.
The sampling device according to the present invention is mainly developed for thermal analysis of grey cast iron (also known as lamellar cast iron-GJL), compacted graphite iron CGI (also known as vermicular graphite iron-GJV) and ductile iron (also known as nodular graphite iron or spheroidal graphite iron-GJS). However, the sampling device may also be used for analysing other molten substances, in particular molten metals, by means of thermal analysis.
Number | Date | Country | Kind |
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1451548-0 | Dec 2014 | SE | national |