CN109358087B - Material high-temperature directional solidification experimental device and experimental method in hypergravity environment - Google Patents
Material high-temperature directional solidification experimental device and experimental method in hypergravity environment Download PDFInfo
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- CN109358087B CN109358087B CN201811417528.3A CN201811417528A CN109358087B CN 109358087 B CN109358087 B CN 109358087B CN 201811417528 A CN201811417528 A CN 201811417528A CN 109358087 B CN109358087 B CN 109358087B
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- 239000000463 material Substances 0.000 title claims abstract description 59
- 238000007711 solidification Methods 0.000 title claims abstract description 35
- 230000008023 solidification Effects 0.000 title claims abstract description 35
- 238000002474 experimental method Methods 0.000 title claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 119
- 239000003708 ampul Substances 0.000 claims abstract description 53
- 239000000758 substrate Substances 0.000 claims abstract description 53
- 230000008018 melting Effects 0.000 claims abstract description 5
- 238000002844 melting Methods 0.000 claims abstract description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 15
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 230000005484 gravity Effects 0.000 claims description 7
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 claims description 7
- DECCZIUVGMLHKQ-UHFFFAOYSA-N rhenium tungsten Chemical compound [W].[Re] DECCZIUVGMLHKQ-UHFFFAOYSA-N 0.000 claims description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- 229910000629 Rh alloy Inorganic materials 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 14
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- 229910010293 ceramic material Inorganic materials 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
Abstract
The invention provides a high-temperature directional solidification experimental device and method for materials in a hypergravity environment, comprising the following steps: a centrifuge unit having a first experimental unit and a second experimental unit; an ampoule unit mounted to the first experiment unit; a temperature control unit; and a control unit; the ampoule unit is provided with: the ampoule comprises an ampoule sleeve with a hollow inner cavity, a secondary heating component which is nested and installed at the bottom of the inner side of the ampoule sleeve, a meltable substrate bin which is installed at an opening at the upper part of the secondary heating component, a meltable substrate which is placed in the hollow inner cavity of the meltable substrate bin, a crucible pipe which is nested into the ampoule sleeve and the meltable substrate bin, and a main heating component which is arranged between the ampoule sleeve and the crucible pipe; the meltable substrate flows into the hollow cavity of the sub-heating assembly below after melting. According to the invention, the directional solidification of the sample material under the condition of supergravity can be simply and conveniently realized without using a mechanical transmission mechanism such as a gear screw rod and the like and a motor and the like.
Description
Technical Field
The invention relates to the technical field of high-temperature directional solidification research of materials in a hypergravity environment, in particular to a high-temperature directional solidification experimental device and method of materials in a hypergravity environment.
Background
Directional solidification is a technique in which a forced means is used in the solidification process to establish a temperature gradient in a specific direction in an uncured melt of a solidified metal sample, so that the melt is solidified in a desired crystal orientation in a direction opposite to a heat flow after nucleation on a gas wall. The directional solidification technology has the greatest advantages that the prepared alloy material eliminates the influence between the interface of the matrix phase and the reinforcing phase, and effectively improves the comprehensive performance of the alloy. Meanwhile, the technology is also an important means for studying the solidification theory and the metal solidification rule by the scholars. The technology was originally established and perfected in the development of superalloys. The technology is adopted and developed to eliminate the transverse grain boundary generated in the crystallization process, so as to improve the unidirectional mechanical property of the material. The directional solidification technology provides an extremely effective means for the research of solidification theory of metals and the development of novel high-temperature alloys and the like.
Unlike the simple solidification and casting of common materials, the realization of directional solidification experiments needs to realize the descending or the movement of a temperature field through the external arrangement of a motor, a mechanism and the like to achieve the experimental purpose of directional solidification, and the engineering difficulty of using the motor and the mechanism under the hypergravity environment is extremely large, and the space in a centrifuge assembly is limited. At present, simple solidification of materials is realized in a supergravity environment generated by a centrifugal machine, but a scientific experiment for directional solidification of controllable materials is difficult to realize, and as mentioned above, the directional solidification experiment has great significance to the study of materialics.
Disclosure of Invention
Problems to be solved by the invention:
in view of the above problems, an object of the present invention is to provide an apparatus and an experimental method capable of controllably performing a directional solidification experiment of a material at a high temperature in a hypergravity environment without using an external device.
Technical means for solving the problems:
the invention provides a high-temperature directional solidification experimental device for materials in a hypergravity environment, which comprises the following components:
a centrifuge unit having a first experimental unit and a second experimental unit mirrored in the first experimental unit;
an ampoule unit mounted to the first experiment unit;
a temperature control unit for controlling the temperature of the device; and
a control unit that controls the temperature control unit and the centrifuge unit;
the ampoule unit is provided with: the ampoule comprises an ampoule sleeve with a hollow inner cavity, a secondary heating component which is nested and installed at the bottom of the inner side of the ampoule sleeve and provided with the hollow inner cavity, a meltable substrate bin which is installed at an opening at the upper part of the secondary heating component and provided with the hollow inner cavity, a meltable substrate which is placed in the hollow inner cavity of the meltable substrate bin, a crucible pipe which is nested into the ampoule sleeve and the meltable substrate bin and is abutted with the upper end face of the meltable substrate, and a main heating component which is arranged between the ampoule sleeve and the crucible pipe;
the meltable substrate flows into the hollow cavity of the sub-heating assembly below after melting.
According to the experimental device for directionally solidifying the material at high temperature in the hypergravity environment, provided by the invention, ampoule units used for experimental samples of the material are systematically improved, ampoule sleeves are used as external supporting members, and the main heating assembly, the auxiliary heating assembly, the crucible tube, the meltable substrate bin and other assemblies are integrated into a whole to form the main body part of the experimental device, so that the directional solidification of the sample material under the hypergravity condition can be simply and conveniently realized without using mechanical transmission mechanisms such as a gear screw and the like and peripheral equipment such as a motor and the like. Therefore, the method solves the problem that the directional solidification of the material cannot be carried out by the conventional means under the condition of supergravity, and has very important scientific significance.
In the present invention, the main heating unit may include: the main heating element, a main heating resistance wire wound on the main heating element and a main heating control thermocouple; the sub-heating assembly includes: the auxiliary heating element, the auxiliary heating resistance wire wound on the auxiliary heating element and the auxiliary heating temperature control thermocouple. Therefore, two sets of independently controlled heating systems can be formed, and key system support is provided for realizing directional solidification experiments in a hypergravity environment.
In the present invention, the ampoule sleeve may be provided with a hole for drawing out a heating resistance wire electrode and a hole for mounting a thermocouple at positions corresponding to the main heating unit and the sub heating unit, respectively.
In the present invention, the ampoule sleeve may be formed of a high purity alumina or toughened zirconia material. Therefore, the ampoule sleeve manufactured by the materials can still provide effective protection for a heating system and an experimental sample under the severe experimental environment of the simultaneous actions of supergravity and high temperature.
In the invention, the bottom of the meltable substrate bin is provided with a drain hole communicated with the hollow inner cavity of the auxiliary heating assembly, and the meltable substrate bin is of a double-fillet bottom sealing structure. Therefore, the double-fillet back cover structure can form self pressure which is generated by dispersing a structure similar to a vault in a hypergravity environment, and the bottom drain hole can be provided with different apertures from 0.1mm to 5mm according to simulation calculation, so that the speed of removing a high-temperature area by a sample can be regulated according to the requirement of a material science experiment through the aperture.
In the present invention, the meltable substrate may be high-strength pressure-resistant glass, and the pressure-resistant strength is 650 to 1900mpa. Therefore, the device not only meets the mechanical requirement under the hypergravity, but also has the characteristic of easy softening or melting from the bottom after heating, and can be remelted for reuse after experiments, and the repeated utilization rate is high.
In the present invention, the main heating element and the sub heating element may be made of high purity alumina, and the main heating resistance wire and the sub heating resistance wire may be made of tungsten-rhenium, tungsten, molybdenum, or platinum-rhodium alloy. Therefore, the high-temperature refractory metal can show excellent mechanical properties in a supergravity environment, and the service life of the high-temperature refractory metal serving as a heating element can reach thousands of hours, so that the high-temperature refractory metal heating element has high reliability.
In the invention, the main heating temperature control thermocouple and the auxiliary heating temperature control thermocouple are platinum rhodium 40 or tungsten rhenium thermocouples.
In the present invention, the crucible tube may be made of high-purity alumina, and the lower end may be thickened. Therefore, the thickened bottom has a heat insulation function, so that the influence on the high-temperature heating of the meltable base material in the experimental process can be eliminated, and the hydraulic pressure generated by the liquefied material in the experimental process plays a certain supporting role.
The invention provides a high-temperature directional solidification experiment method for materials in a hypergravity environment, which comprises the steps of heating the materials in a crucible tube through a main heating assembly under a preset hypergravity field, heating the meltable base materials in a meltable base material bin through a secondary heating assembly after the set temperature is reached, so that the meltable base materials are controllably melted, the melted meltable base materials flow into a cavity at the lower side under the influence of gravity, and the crucible tube gradually moves downwards, so that the materials which are locally separated from a high-temperature area are directionally solidified.
According to the invention, after the centrifugal machine is in a working state and reaches a preset gravity value, the main heating component is controlled by the temperature control unit to heat the test sample material, after the material reaches a set temperature, the auxiliary heating component is started by the temperature control unit, the meltable substrate in the meltable substrate bin is gradually melted from the bottom, the melted meltable substrate flows out under the influence of gravity, and the material moves downwards along with the meltable substrate to partially leave a high-temperature area of the main heating component, so that the controllable directional solidification of the material under the hypergravity is realized.
The invention has the following effects:
the invention can provide the experimental device and the experimental method for controllably performing the high-temperature directional solidification of the material under the hypergravity environment without using external equipment.
Drawings
FIG. 1 is a schematic view of the structure of an experimental device according to the present invention in an experimental state;
fig. 2 is a structural cross-sectional view of an ampoule unit of the experimental apparatus according to the present invention;
symbol description:
1. an ampoule sleeve;
2. a main heating member;
3. a main heating resistance wire;
4. a main heating temperature control thermocouple;
5. a crucible tube;
6. experimental object materials;
7. a meltable substrate cartridge;
8. a meltable substrate;
9. a sub-heating member;
10. a secondary heating resistance wire;
11. an auxiliary heating temperature control thermocouple;
12. a thermal insulation assembly;
13. a hanging basket;
14. an I-shaped arm;
15. a basket shaft;
16. a heating wire electrode bus;
17. a conductive slip ring;
18. a second experimental unit;
19. thermocouple electrode buses;
20. a temperature control unit;
21. an electrically conductive slip ring output bus;
22. a control unit;
23. a first experimental unit.
Detailed Description
The invention will be further described in connection with the following embodiments, it being understood that the following embodiments are only illustrative of the invention and not limiting thereof. The same or corresponding reference numerals in the drawings denote the same parts, and a repetitive description thereof will be omitted. Meanwhile, the following embodiments are only for further illustrating the present invention, and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adaptations of the present invention by those skilled in the art should and are within the scope of the present invention. The specific process parameters and the like described below are also merely examples of suitable ranges, i.e., one skilled in the art can make a suitable selection from the description herein and are not intended to be limited to the specific values described below.
Disclosed herein is a directional solidification experimental device, fig. 1 is a schematic structural view of the experimental device according to the present invention in an experimental state, and fig. 2 is a structural cross-sectional view of an ampoule unit of the experimental device according to the present invention. As shown in fig. 1, the experimental apparatus includes a centrifuge unit a, an ampoule unit B, a temperature control unit 20, and a control unit 22. The centrifuge unit a includes a first experimental unit 23 to which the ampoule unit B is attached, and a second experimental unit 18 that is mirror-weighted with the first experimental unit 23.
Specifically, in the present embodiment, the centrifuge unit a is an i-shaped centrifuge, i-shaped arms 14 are formed at both ends, a basket shaft 15 and a basket 13 supported by the basket shaft 15 are respectively provided on the two i-shaped arms 14, and a heat insulation assembly 12 is further provided in the basket 13, thereby forming a first experimental unit 23 and a second experimental unit 18. The second experimental unit 18 is a necessary configuration of the i-centrifuge for balancing the arms, i.e. the two baskets 13 are required to have a mass substantially equal to the centre of mass so that the experimentally set gravitational field can be generated efficiently. The related technologies and indexes are based on the existing centrifuge production requirements, and all the centrifuges on the market can be used as long as the required gravitational field can be met.
As shown in fig. 1, the ampoule unit B is vertically installed in the heat insulation assembly 12 in the basket 13 of the first experiment unit 23. Specifically, as shown in fig. 2, ampoule unit B includes: the ampoule sleeve 1 as an external supporting member, a crucible tube 5 which is nested in the ampoule sleeve 1 and leaves a certain space with the bottom thereof, a main heating assembly arranged between the ampoule sleeve 1 and the crucible tube 5, a secondary heating assembly arranged at the bottom of the inner side of the ampoule sleeve 1, and a meltable substrate bin 7 arranged between the secondary heating assembly and the bottom of the outer side of the crucible tube 5. The meltable substrate 8 is stored in the meltable substrate bin 7, and the experimental object material 6 is placed in the crucible tube 5.
Wherein the main heating assembly further comprises: a main heating element 2, a main heating resistance wire 3 and a main heating temperature control thermocouple 4. Accordingly, the sub-heating assembly further comprises: a secondary heating element 9, a secondary heating resistance wire 10 and a secondary heating temperature control thermocouple 11. In the present embodiment, the ampoule jacket 1 has a hollow cylindrical structure with rounded bottom, and two holes (left side in the drawing) for drawing out the heater wire electrode are formed on one side of the ampoule jacket 1 at positions corresponding to the main heater unit and the sub heater unit, for example, the size may be 1mm to 5mm, and two holes (right side in the drawing) for mounting the thermocouple are formed on the other side, for example, the size may be 2mm to 6mm, and the ampoule jacket 1 is preferably made of high-purity alumina, and the wall thickness is preferably 2mm to 5 mm.
In the present embodiment, the high purity alumina as the material of the ampoule sleeve 1 is produced by sintering, with a purity of 99% to 99.9%. The high-purity aluminum oxide ceramic part can still keep good mechanical properties at high temperature, can still keep tensile strength at about 170Mpa at 1000 ℃ and can still keep elastic modulus at 275Gpa. In addition, the toughened zirconia material can be selected, and the compressive strength of the toughened zirconia material can reach 800Mpa at 1200 ℃, and the density is higher than that of high-purity alumina, so that the weight of the finished product is heavier than that of the high-purity alumina.
As shown in fig. 2, the auxiliary heating assembly is embedded and mounted at the bottom of the inner side of the ampoule sleeve 1, the auxiliary heating member 9 is formed into a hollow cylindrical structure with rounded dome structure back cover, the outer side is formed with a thread groove for uniformly winding the auxiliary heating resistance wire 10, and the end opening is provided with a step portion 9a for mounting the meltable substrate chamber 7. The auxiliary heating member 9 should be a high temperature resistant ceramic material, and the present invention is preferably high purity alumina having a purity of 99% -99.9% in consideration of mechanical properties under a supergravity environment, and the width of the thread groove may be adaptively increased by 0.2mm according to the wire diameter of the auxiliary heating resistance wire 10, but is not limited thereto. The secondary heating resistance wire 10 is made of refractory metals with high strength and high temperature resistance, such as tungsten-rhenium, tungsten, molybdenum, platinum-rhodium alloy, etc., and the wire diameter can be 0.5mm-1.2mm according to the resistance design, but is not limited to the specification. In this embodiment, the surface of the thread groove may be uniformly coated with high-strength alumina ceramic glue after the auxiliary heating resistance wire 10 is mounted, so as to reinforce the whole structure, the auxiliary heating element 9 is solidified and then placed at the bottom of the ampoule sleeve 1, and then the electrode of the auxiliary heating element 9 is led out through the hole at the lower side of the ampoule sleeve 1.
The meltable base material chamber 7 is formed into a hollow cylindrical structure with a double rounded dome structure as a back cover, a boss portion 7a fitted with a stepped portion 9a of the sub heater 9 is formed at the lower portion, and a drain hole 7b of 0.2mm to 5mm is formed in the middle of the bottom portion for guiding out the melted meltable base material 8 into the hollow cavity of the sub heater 9.
The meltable substrate 8 stored in the hollow cavity of the meltable substrate bin 7 is a cylinder with a solid round bottom structure in normal state, and in the embodiment, high-strength pressure-resistant glass is selected, so that the high-strength pressure-resistant glass not only meets the mechanical requirement under the hypergravity, but also has the characteristic of easily softening or melting from the bottom after heating, but the material selection is not limited to the above, and can be selected according to the actual design requirement. The height of the meltable substrate 8 is reduced by 2mm to 5mm from the inner height of the hollow cavity of the meltable substrate holder 7, so that a certain space is reserved for installing the crucible tube 5 described later.
The crucible tube 5 is formed in a hollow cylindrical structure with a rounded bottom structure, is inserted vertically into the meltable substrate chamber 7, has an outer diameter that is in contact with the inner diameter of the hollow cavity of the meltable substrate chamber 7, and has a bottom that is in contact with the end surface of the meltable substrate 8. In the present embodiment, the crucible tube 5 is made of a high-purity alumina material, and the bottom sealing of the lower end is thickened to provide a heat insulating function, whereby the influence of high-temperature heating on the meltable base material 8 can be eliminated during the experiment. In the present embodiment, the high purity alumina as the material of the crucible tube 5 has a purity of 99% to 99.9%, and the crucible tube 5 may have a bottom (i.e., lower end) thickness of 5mm to 100mm according to actual use.
The crucible tube 5 contains a subject material 6, which may be, for example, a non-cermet or a metal, but is not limited thereto. The subject material 6 should have a structure corresponding to the hollow cavity inside the crucible tube 5, i.e., a solid cylinder which should be prefabricated into a rounded bottom structure, and an outer diameter consistent with the inner diameter of the crucible tube 5.
In the present embodiment, the main heating resistance wire 3 is a high-strength high-temperature refractory metal, for example, tungsten rhenium, tungsten, molybdenum, platinum rhodium alloy, etc., and the wire diameter may be 0.5mm to 1.2mm according to the resistance design, but the present invention is not limited thereto, and the main heating resistance wire 3 can heat the crucible tube 5 and the experimental object material 6 therein after being energized. The main heating member 2 is formed in a hollow cylindrical structure, and a screw groove for winding the main heating resistance wire 3 is formed at the outer side thereof, and the width of the screw groove is increased by 0.2mm compared with the wire diameter adaptability of the main heating resistance wire 3, and the material is high-purity alumina, but is not limited thereto. Specifically, the main heating resistance wire 3 is uniformly wound in the thread groove of the main heating element 2, high-strength alumina ceramic glue is uniformly smeared on the surface of the thread groove after winding is completed, so that the whole structure is reinforced, the main heating element is tightly nested between the experimental crucible tube 5 and the ampoule sleeve 1 after being integrally solidified, and then the electrode of the main heating element is led out through the hole on the upper side of the ampoule sleeve 1.
The main structure of ampoule unit B is basically complete, the auxiliary heating element is installed in ampoule sleeve 1 bottom, the auxiliary heating element top is meltable substrate storehouse 7, meltable substrate 8 is in meltable substrate storehouse 7 inside, meltable substrate 8 is supported under crucible tube 5, the main heating element parcel is outside crucible tube 5. Then, the main heating and temperature controlling thermocouple 4 and the sub heating and temperature controlling thermocouple 11 are inserted from the holes on the other side of the ampoule sleeve 1, respectively. In the present embodiment, the two thermocouples 4 and 11 are made of a material resistant to high temperature and high strength, for example, platinum rhodium 40, tungsten rhenium thermocouples, or the like, and the wire diameter is preferably 0.3mm to 1mm, but the present invention is not limited thereto.
As shown in fig. 1, two sets of heater wire electrodes and thermocouple electrodes respectively led out from four holes of ampoule sleeve 1 form two sets of heater wire electrode buses 16 and two sets of thermocouple electrode buses 19 respectively by a zigzag path method, and the specific path method is not limited thereto. The central part of the centrifuge unit a is also provided with a conductive slip ring 17 for controlling the two heating components in the ampoule unit B, and two groups of buses 16 and 19 are connected with the conductive slip ring 17 through two sides of the i-shaped arm 14 and are respectively connected with the temperature control unit 20 and the control unit 22 through a conductive slip ring output bus 21, and at the same time, the temperature control unit 20 and the control unit 22 are connected, for example, through an RS485 bus which is not shown.
In this embodiment, the temperature control method is specifically as follows: the main heating control thermocouple 4 and the auxiliary heating control thermocouple 11 are connected to the conductive slip ring 17 through wires, then the conductive slip ring 17 is connected to the temperature control unit 20 through wires to acquire real-time millivolt voltage signals of the thermocouples and convert the millivolt voltage signals into corresponding temperature values, output voltage is adjusted through a fuzzy mathematical algorithm, and the adjusted voltage acts on the main heating resistance wire 3 and the auxiliary heating resistance wire 10 through the conductive slip ring 17 system again, so that real-time temperature control is realized. And the temperature value in the experimental process is acquired in real time through an RS485 bus which is not shown and connected with a computer and a temperature control system and is stored in a hard disk of the computer system so as to be convenient for data analysis and data mining after the experiment is finished.
In a specific operation, after the control unit 22 receives the instruction, the centrifuge unit a is set and started, the i-arm 14 of the centrifuge starts to rotate at a high speed to generate a gravity field, after reaching the set gravity value, the control unit 22 sends the instruction to the temperature control unit 20, after receiving the instruction, the temperature control unit 20 starts to heat the experimental object material 6 in the crucible tube 5 until reaching the set experimental temperature, at this time, the control unit 22 sends the instruction to the temperature control unit 20, after receiving the instruction, the temperature control unit 20 starts to controllably heat the bottom end surface of the meltable substrate 8 in the meltable substrate bin 7, so that the bottom of the meltable substrate 8 starts to be gradually melted, and the melted meltable substrate 8 flows into the hollow cavity of the auxiliary heating member 9 through the drain hole 7b of the meltable substrate bin 7 under the influence of gravity. Therefore, the meltable base material 8 slowly moves downwards to drive the whole crucible tube 5 to move downwards, and finally, part of the experimental object material 6 in the crucible tube 5 moves out of a high temperature area generated by the original main heating piece 2, so that the aim of directional solidification of the material under the hypergravity environment is fulfilled.
In summary, compared with the prior art of simple solidification and casting of materials under a hypergravity field, the invention can realize directional solidification of the materials under the hypergravity environment, and compared with the prior art of controllable directional solidification of the materials by means of external devices such as a motor, a mechanism and the like, the invention does not depend on any external equipment, can realize controllable directional solidification of the materials under the hypergravity field, greatly reduces experimental difficulty, greatly improves operability, and is very significant in the research field.
The above embodiments further describe the objects, technical solutions and advantageous effects of the present invention in detail, it should be understood that the above is only one embodiment of the present invention and is not limited to the scope of the present invention, and the present invention may be embodied in various forms without departing from the gist of the essential characteristics of the present invention, and thus the embodiments of the present invention are intended to be illustrative and not limiting, since the scope of the present invention is defined by the claims rather than the specification, and all changes falling within the scope defined by the claims or the equivalent scope of the scope defined by the claims should be construed to be included in the claims. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A high-temperature directional solidification experimental device for a material in a hypergravity environment is characterized by comprising:
a centrifuge unit having a first experimental unit and a second experimental unit mirrored in the first experimental unit;
an ampoule unit mounted to the first experiment unit;
a temperature control unit for controlling the temperature of the device; and
a control unit that controls the temperature control unit and the centrifuge unit;
the ampoule unit is provided with: the ampoule comprises an ampoule sleeve with a hollow inner cavity, a secondary heating component which is nested and installed at the bottom of the inner side of the ampoule sleeve and provided with the hollow inner cavity, a meltable substrate bin which is installed at an opening at the upper part of the secondary heating component and provided with the hollow inner cavity, a meltable substrate which is placed in the hollow inner cavity of the meltable substrate bin, a crucible pipe which is nested into the ampoule sleeve and the meltable substrate bin and is abutted with the upper end face of the meltable substrate, and a main heating component which is arranged between the ampoule sleeve and the crucible pipe;
the meltable substrate flows into the hollow cavity of the sub-heating assembly below after melting.
2. The experimental device of claim 1, wherein the device comprises a plurality of sensors,
the main heating assembly includes: the main heating element, a main heating resistance wire wound on the main heating element and a main heating control thermocouple;
the sub-heating assembly includes: the auxiliary heating element, the auxiliary heating resistance wire wound on the auxiliary heating element and the auxiliary heating temperature control thermocouple.
3. The experimental device of claim 1, wherein the device comprises a plurality of sensors,
and holes for leading out heating resistance wire electrodes and holes for installing thermocouples are respectively formed on the ampoule sleeve at positions corresponding to the main heating assembly and the auxiliary heating assembly.
4. The experimental device of claim 1, wherein the device comprises a plurality of sensors,
the ampoule sleeve is formed of a high purity alumina or toughened zirconia material.
5. The experimental device of claim 1, wherein the device comprises a plurality of sensors,
the bottom of the meltable substrate bin is provided with a drain hole communicated with the hollow inner cavity of the auxiliary heating assembly, and the meltable substrate bin is of a double-fillet bottom sealing structure.
6. The experimental device of claim 1, wherein the device comprises a plurality of sensors,
the meltable substrate is high-strength pressure-resistant glass, and the pressure-resistant strength is 650-1900 MPa.
7. The experimental device of claim 2, wherein the device comprises a plurality of sensors,
the main heating element and the auxiliary heating element are made of high-purity aluminum oxide, and the main heating resistance wire and the auxiliary heating resistance wire are made of tungsten-rhenium, tungsten, molybdenum or platinum-rhodium alloy.
8. The experimental device of claim 2, wherein the device comprises a plurality of sensors,
the main heating temperature control thermocouple and the auxiliary heating temperature control thermocouple are platinum rhodium 40 or tungsten rhenium thermocouples.
9. The experimental device of claim 1, wherein the device comprises a plurality of sensors,
the crucible tube is made of high-purity alumina, and the lower end of the crucible tube is thickened.
10. A high-temperature directional solidification experimental method for materials in a hypergravity environment is characterized in that,
the experimental device according to any one of claims 1 to 9, wherein the material in the crucible tube is heated by the main heating assembly under a preset hypergravity field, after the set temperature is reached, the meltable substrate in the meltable substrate bin is heated by the auxiliary heating assembly to be controllably melted, the melted meltable substrate flows into the cavity on the lower side under the influence of gravity, and the crucible tube gradually moves downwards, so that the material locally leaving the high temperature area is directionally solidified.
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| CN110842168B (en) * | 2019-09-10 | 2023-10-27 | 浙江大学 | Directional solidification casting system carried on supergravity centrifugal machine |
| CN110846712B (en) * | 2019-09-10 | 2023-11-10 | 浙江大学 | Supergravity directional solidification casting furnace device |
| CN110523958B (en) * | 2019-09-10 | 2024-02-27 | 浙江大学 | Crucible device suitable for supergravity directional solidification |
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