CN220999935U - Cooling device for halide crystal growth - Google Patents
Cooling device for halide crystal growth Download PDFInfo
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- CN220999935U CN220999935U CN202322787521.3U CN202322787521U CN220999935U CN 220999935 U CN220999935 U CN 220999935U CN 202322787521 U CN202322787521 U CN 202322787521U CN 220999935 U CN220999935 U CN 220999935U
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- frame
- cooling
- heat conducting
- resistant container
- temperature resistant
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- 238000001816 cooling Methods 0.000 title claims abstract description 92
- 239000013078 crystal Substances 0.000 title claims abstract description 54
- 150000004820 halides Chemical class 0.000 title claims abstract description 37
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 11
- 229910052802 copper Inorganic materials 0.000 claims description 11
- 239000010949 copper Substances 0.000 claims description 11
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 5
- 239000010931 gold Substances 0.000 claims description 5
- 238000009529 body temperature measurement Methods 0.000 claims description 4
- 239000000155 melt Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 6
- XQPRBTXUXXVTKB-UHFFFAOYSA-M caesium iodide Chemical compound [I-].[Cs+] XQPRBTXUXXVTKB-UHFFFAOYSA-M 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 239000000498 cooling water Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 2
- 229910000431 copper oxide Inorganic materials 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229910000619 316 stainless steel Inorganic materials 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- CMJCEVKJYRZMIA-UHFFFAOYSA-M thallium(i) iodide Chemical compound [Tl]I CMJCEVKJYRZMIA-UHFFFAOYSA-M 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The utility model belongs to the technical field of cooling devices, and particularly relates to a cooling device for halide crystal growth. The cooling device comprises a growth furnace, a heating piece, a heat conducting frame, a high-temperature resistant container, a cooling frame and a lifting platform; one end of the heat conducting frame is provided with a high-temperature resistant container, one end of the heat conducting frame, which is far away from the high-temperature resistant container, is clamped on the cooling frame, and one end of the cooling frame, which is far away from the heat conducting frame, is connected with a lifting platform; the heat conducting frame, the high temperature resistant container and the cooling frame are positioned in the growth furnace, and a heating element is arranged on the furnace wall of the growth furnace, which is close to one side surface of the high temperature resistant container. The device slowly descends through the heat conducting frame for supporting the high-temperature resistant container, directionally solidifies the melt to obtain single crystals, and accurately controls the temperature gradient to improve the quality of the crystals.
Description
Technical Field
The utility model belongs to the technical field of cooling devices, and particularly provides a cooling device for halide crystal growth.
Background
In growing halide crystals, a drop-down crystal growth technique is currently commonly used, but in the drop-down crystal growth technique, in order to produce a large-size halide single crystal, a growth gradient of more than 20 ℃/cm is generally required, a lower cooling stage is required to have a good heat conduction capability, and pure copper is generally used as a heat conduction member in order to ensure a good heat conduction capability.
However, the following problems exist in selecting copper as the heat conducting member: the growth temperature of part of halide is 621 ℃, copper can be rapidly oxidized at the temperature to generate a copper oxide interlayer with poor heat conduction capability, the heat conduction capability and the heat conduction non-uniformity are greatly influenced, the actual crystal growth interface temperature is unstable, and the crystal quality is reduced; meanwhile, the process of removing the oxide layer on the copper surface is additionally added after the growth link, so that the production cost is increased.
In addition, the crystal is continuously lowered in the crystal growth process, the distance between the growth interface and the heat conduction frame is increased, and the actual growth gradient is reduced due to the reduction of the heat transfer rate in unit time. Therefore, the growth environment temperature needs to be monitored and controlled in real time, and the growth interface gradient is kept stable.
Therefore, the above-described problems are to be solved.
Disclosure of utility model
The utility model aims to: in order to overcome the defects, the utility model aims to provide a cooling device for the growth of halide crystals, which can accurately control the growth temperature of the halide crystals, avoid the oxidation of a heat conduction device by the surrounding environment, and prevent the unstable crystallization temperature caused by the reduction of the heat transfer effect of the oxidized heat conduction device.
The technical scheme is as follows: in order to achieve the above object, the present utility model provides a cooling device for halide crystal growth, comprising: the device comprises a growth furnace, a heating piece, a heat conduction frame, a high-temperature resistant container, a cooling frame and a lifting platform; one end of the heat conducting frame is provided with a high-temperature resistant container, one end of the heat conducting frame, which is far away from the high-temperature resistant container, is clamped on the cooling frame, a lifting device for lifting the heat conducting frame is also arranged on the heat conducting frame, and one end of the cooling frame, which is far away from the heat conducting frame, is connected with a lifting platform; the heat conducting frame, the high temperature resistant container and the cooling frame are positioned in the growth furnace, and a heating element is arranged on the furnace wall of the growth furnace, which is close to one side surface of the high temperature resistant container. In the cooling device for the growth of the halide crystal, when the halide crystal is grown, raw materials are firstly placed into a high-temperature-resistant container, then are put into a crystal growth furnace to be melted, and a heat conduction frame for supporting the high-temperature-resistant container slowly descends to directionally solidify a melt to obtain a single crystal.
Further, in the cooling device for halide crystal growth, the heat conducting frame comprises a base, a supporting block and a carrying block; one end of the base is clamped in the cooling frame, the other end of the base is connected with a carrying block, a first groove is formed in the surface of one side of the carrying block, which is close to the high-temperature resistant container, the high-temperature resistant container is embedded in the first groove of the carrying block, and a supporting block surrounding the base is arranged on the base. According to the cooling device for the growth of the halide crystal, the high-temperature resistant container is clamped by the grooves formed in the carrying blocks, so that the high-temperature resistant container can be fixed, and the high-temperature resistant container can be taken down at any time.
Further, in the cooling device for halide crystal growth, the heat conducting frame is made of pure copper, and a layer of gold film is plated on the base of the heat conducting frame. According to the cooling device for the halide crystal growth, pure copper is selected as a material of the heat conducting frame, so that the heat transfer capacity of the heat conducting frame is improved, meanwhile, a gold film is plated on a base contacted with the cooling frame, copper oxide with poor heat conductivity is prevented from being generated on the surface of copper, the growth gradient is reduced, and the service life and the recycling rate are improved.
Further, in the above-mentioned cooling device for growth of halide crystal, the pulling device includes layer board, connecting sleeve and pull ring, and the supporting shoe is close to cooling frame one side surface and is connected with the layer board, and the one end that the layer board is close to the growth furnace is connected with the connecting sleeve, and the connecting sleeve arranges along the growth furnace direction of height, and the one end that the cooling frame was kept away from to the connecting sleeve is provided with the pull ring. According to the cooling device for the growth of the halide crystal, the lifting device is arranged on the heat conduction frame, so that the heat conduction frame and the high-temperature-resistant container can be conveniently taken out at any time, and fragments generated when the high-temperature-resistant container bursts can be prevented from flying into the growth furnace by the lifting device.
Furthermore, in the cooling device for halide crystal growth, a temperature measuring device is also arranged in the heat conducting frame, the temperature measuring device is a thermocouple, and the thermocouple is arranged in the base. According to the cooling device for the growth of the halide crystal, the thermocouple is arranged in the heat conduction frame, so that the temperature condition of the heat conduction frame can be conveniently observed at any time, the temperature gradient is ensured to be unchanged, and the quality degradation of the crystal in the middle and later stages of the growth caused by the gradient change is prevented.
Further, in the cooling device for halide crystal growth, the cooling frame is a water cooling frame, a water flow channel is arranged in the cooling frame, the water flow channel is arranged around the heat conducting frame, and a water inlet pipe and a water outlet pipe are respectively arranged at two ends of the water flow channel. In the cooling device for the growth of the halide crystal, the water cooling frame is used for cooling the crystal, and the temperature difference of the crystal are flexibly adjusted by adjusting the temperature of cooling water and the flow of cooling water so as to change the heat transfer rate of the crystal.
Further, in the above-mentioned cooling device for halide crystal growth, the cooling frame includes first standpipe, second standpipe and connecting pipe, first standpipe and second standpipe interval arrangement, and first standpipe is close to lift platform one end and is connected with the inlet tube, and second standpipe is close to lift platform one end and is connected with the outlet pipe, and first standpipe and second standpipe are connected respectively at the connecting pipe both ends, and the cooling frame is "H" shape, and connecting pipe, first standpipe and second standpipe are being close to heat conduction frame one side and form the second recess, and the heat conduction frame card is established in the second recess. According to the cooling device for the growth of the halide crystals, the heat conducting frame is clamped on the cooling frame, so that the cooling frame can sufficiently cool the heat conducting frame and can play a supporting role, and the heat conducting frame can be conveniently removed from the cooling frame at any time.
Further, in the cooling device for halide crystal growth, a temperature control device and a temperature measuring device are provided in the furnace wall of the growth furnace. The temperature control device is a temperature control thermocouple, and the temperature measurement device is a temperature measurement thermocouple.
The technical scheme can be seen that the utility model has the following beneficial effects: in the cooling device for the growth of the halide crystal, the high-temperature resistant container, the heat conducting frame and the cooling frame are clamped, so that the whole device has strong flexibility and is convenient to take down at any time; the heat conducting frame is made of pure copper, so that the heat conducting capacity is high, meanwhile, the surface is plated with gold, and the influence of an oxide film on the surface of copper on the heat conducting capacity is prevented; the cooling rack adopts water cooling, and the temperature is flexibly adjusted by setting the temperature and the flow of cooling water; the device is provided with a thermocouple, and the temperature of the device is measured and regulated in real time, so that the cooling temperature is ensured to be stable.
Drawings
FIG. 1 is a schematic structural view of a cooling device for halide crystal growth;
FIG. 2 is a schematic structural view of a heat conducting frame;
Fig. 3 is a side view of a thermally conductive frame.
In the figure: 1. a growth furnace; 2. a heating member; 3. a heat conduction frame; 31. a base; 32. a support block; 33. a carrying block; 4. a high temperature resistant container; 5. a cooling rack; 51. a first standpipe; 52. a second standpipe; 53. a connecting pipe; 54. a water inlet pipe; 55. a water outlet pipe; 6. a lifting platform; 71. a supporting plate; 72. a connecting sleeve; 73. and (5) a pull ring.
Detailed Description
The cooling device for the growth of the halide crystal shown in fig. 1 comprises a growth furnace 1, a heating element 2, a heat conduction frame 3, a high-temperature resistant container 4, a cooling frame 5 and a lifting platform 6; one end of the heat conducting frame 3 is provided with a high-temperature resistant container 4, one end of the heat conducting frame 3 far away from the high-temperature resistant container 4 is clamped on the cooling frame 5, the heat conducting frame 3 is also provided with a lifting device for lifting the heat conducting frame 3, and one end of the cooling frame 5 far away from the heat conducting frame 3 is connected with a lifting platform 6; the heat conduction frame 3, the high temperature resistant container 4 and the cooling frame 5 are positioned in the growth furnace 1, and the furnace wall of the growth furnace 1, which is close to one side surface of the high temperature resistant container 4, is provided with a heating element 2. Wherein, heating element 2 is heating resistance wire, and high temperature resistant container 4 is the crucible.
The heat conduction frame 3 as shown in fig. 2 and 3 includes a base 31, a support block 32, and a carrier block 33; one end of the base 31 is clamped in the cooling frame 5, the other end of the base 31 is connected with a carrying block 33, a first groove is formed in the surface, close to one side of the high-temperature resistant container 4, of the carrying block 33, the high-temperature resistant container 4 is embedded in the first groove of the carrying block 33, the first groove is V-shaped, and a supporting block 32 surrounding the base 31 is arranged on the base 31. The heat conducting frame 3 is made of T1 pure copper, and is wholly subjected to electroless gold plating, and the plating thickness is 50um.
The lifting device comprises a supporting plate 71, a connecting sleeve 72 and a pull ring 73, wherein the supporting plate 71 is connected to the surface of one side of the supporting block 32, which is close to the cooling frame 5, one end of the supporting plate 71, which is close to the growth furnace 1, is connected with the connecting sleeve 72, the connecting sleeve 72 is arranged along the height direction of the growth furnace 1, and the pull ring 73 is arranged at one end of the connecting sleeve 72, which is far away from the cooling frame 5. The material of the lifting device is 45# carbon steel, and the inner diameter of the connecting sleeve 72 is 2mm larger than the outer diameter of the heat conducting frame 3.
The cooling frame 5 is the water-cooling frame, be provided with the rivers passageway in the cooling frame 5, the cooling frame 5 includes first standpipe 51, second standpipe 52 and connecting pipe 53, first standpipe 51 and second standpipe 52 interval arrangement, first standpipe 51 is close to lift platform 6 one end and is connected with inlet tube 54, second standpipe 52 is close to lift platform 6 one end and is connected with outlet pipe 55, first standpipe 51 and second standpipe 52 are connected respectively at connecting pipe 53 both ends, the cooling frame 5 is "H" shape, connecting pipe 53, first standpipe 51 and second standpipe 52 form the second recess in being close to heat conduction frame 3 one side, heat conduction frame 3 card is established in the second recess. The whole wall thickness of the cooling frame 5 is 3mm, the material is 316 stainless steel, and the outer diameter is 120mm.
A thermocouple is installed in the heat conducting frame 3 for detecting the temperature at the crystallization position, and a through hole is provided in the cooling frame 5 for installing the thermocouple. A furnace wall of the growth furnace 1 is provided with a temperature control thermocouple and a temperature thermocouple.
The growth process is operated as follows: 10000g of cesium iodide raw material and 20g of thallium iodide raw material are mixed in a glove box to form cesium iodide crystals, the cesium iodide crystals are placed in a crucible, and the crucible is sealed by oxyhydrogen flame after being vacuumized to 1 x 10 -4 Pa. Before the crystal grows, the heat conduction frame 3 is fixedly connected with the lifting device and is arranged on the cooling frame 5, and the sealed quartz crucible is arranged on the heat conduction frame 3; the cooling water temperature is set to 20 ℃, and the flow is set to 50L/h; heating the growth furnace at a speed of 100 ℃/h, enabling the temperature-controlled thermocouple to reach 750 ℃, enabling the temperature-measuring thermocouple of the furnace body to be higher than the melting point of cesium iodide by about 50 ℃ at the moment, enabling the cesium iodide crystal raw material in the quartz crucible to be completely melted, and preserving heat for 12h; after the end of the incubation, the growth started and was decreased at a constant rate of 1mm/h by 400mm. After the lowering is finished, the temperature of the furnace body is reduced at a speed of 30 ℃/h, water cooling is closed after the temperature reaches the room temperature, a special hook is used for inserting a pull ring 73, and the lifting device is lifted. At this time, the quartz crucible and the heat conduction frame 3 are simultaneously lifted, and the whole growth process is finished.
The above embodiments are illustrative for the purpose of illustrating the technical concept and features of the present utility model so that those skilled in the art can understand the content of the present utility model and implement it accordingly, and thus do not limit the scope of the present utility model. All equivalent changes or modifications made in accordance with the spirit of the present utility model should be construed to be included in the scope of the present utility model.
Claims (9)
1. A cooling device for halide crystal growth, characterized by: comprises a growth furnace (1), a heating piece (2), a heat conduction frame (3), a high-temperature resistant container (4), a cooling frame (5) and a lifting platform (6); one end of the heat conducting frame (3) is provided with a high-temperature resistant container (4), one end, far away from the high-temperature resistant container (4), of the heat conducting frame (3) is clamped on the cooling frame (5), a lifting device for lifting the heat conducting frame (3) is further arranged on the heat conducting frame (3), and one end, far away from the heat conducting frame (3), of the cooling frame (5) is connected with the lifting platform (6); the heat conduction frame (3), the high-temperature resistant container (4) and the cooling frame (5) are positioned in the growth furnace (1), and a heating element (2) is arranged on the furnace wall, which is close to one side surface of the high-temperature resistant container (4), of the growth furnace (1).
2. The cooling device for halide crystal growth according to claim 1, wherein: the heat conduction frame (3) comprises a base (31), a supporting block (32) and a carrying block (33); the cooling rack is characterized in that one end of the base (31) is clamped in the cooling rack (5), the other end of the base (31) is connected with the carrying block (33), a first groove is formed in the surface, close to one side of the high-temperature resistant container (4), of the carrying block (33), the high-temperature resistant container (4) is embedded in the first groove of the carrying block (33), and the base (31) is provided with a supporting block (32) surrounding the base (31).
3. The cooling device for halide crystal growth according to claim 2, wherein: the heat conducting frame (3) is made of pure copper, and a layer of gold film is plated on the base (31) of the heat conducting frame (3).
4. The cooling device for halide crystal growth according to claim 2, wherein: the lifting device comprises a supporting plate (71), a connecting sleeve (72) and a pull ring (73), wherein the supporting block (32) is connected with the supporting plate (71) close to one side surface of the cooling frame (5), one end, close to the growing furnace (1), of the supporting plate (71) is connected with the connecting sleeve (72), the connecting sleeve (72) is arranged along the height direction of the growing furnace (1), and one end, far away from the cooling frame (5), of the connecting sleeve (72) is provided with the pull ring (73).
5. The cooling device for halide crystal growth according to claim 2, wherein: the heat conduction frame (3) is internally provided with a temperature measuring device, the temperature measuring device is a thermocouple, and the thermocouple is arranged in the base (31).
6. The cooling device for halide crystal growth according to claim 1, wherein: the cooling rack (5) is a water cooling rack, a water flow channel is arranged in the cooling rack (5), the water flow channel is arranged around the heat conduction rack (3), and a water inlet pipe (54) and a water outlet pipe (55) are respectively arranged at two ends of the water flow channel.
7. The cooling device for halide crystal growth according to claim 6, wherein: the cooling rack (5) comprises a first vertical pipe (51), a second vertical pipe (52) and a connecting pipe (53), wherein the first vertical pipe (51) and the second vertical pipe (52) are arranged at intervals, the first vertical pipe (51) is connected with a water inlet pipe (54) close to one end of the lifting platform (6), the second vertical pipe (52) is connected with a water outlet pipe (55) close to one end of the lifting platform (6), two ends of the connecting pipe (53) are respectively connected with the first vertical pipe (51) and the second vertical pipe (52), the cooling rack (5) is in an H shape, the connecting pipe (53), the first vertical pipe (51) and the second vertical pipe (52) form a second groove on one side close to the heat conducting rack (3), and the heat conducting rack (3) is clamped in the second groove.
8. The cooling device for halide crystal growth according to claim 1, wherein: a temperature control device and a temperature measuring device are arranged in the furnace wall of the growth furnace (1).
9. The cooling device for halide crystal growth according to claim 8, wherein: the temperature control device is a temperature control thermocouple, and the temperature measurement device is a temperature measurement thermocouple.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322787521.3U CN220999935U (en) | 2023-10-18 | 2023-10-18 | Cooling device for halide crystal growth |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322787521.3U CN220999935U (en) | 2023-10-18 | 2023-10-18 | Cooling device for halide crystal growth |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN220999935U true CN220999935U (en) | 2024-05-24 |
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ID=91116160
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202322787521.3U Active CN220999935U (en) | 2023-10-18 | 2023-10-18 | Cooling device for halide crystal growth |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN220999935U (en) |
-
2023
- 2023-10-18 CN CN202322787521.3U patent/CN220999935U/en active Active
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