CN117702275A - Indium phosphide single crystal growth method based on double-layer crucible - Google Patents
Indium phosphide single crystal growth method based on double-layer crucible Download PDFInfo
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- CN117702275A CN117702275A CN202410164286.0A CN202410164286A CN117702275A CN 117702275 A CN117702275 A CN 117702275A CN 202410164286 A CN202410164286 A CN 202410164286A CN 117702275 A CN117702275 A CN 117702275A
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- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000002109 crystal growth method Methods 0.000 title description 2
- 239000013078 crystal Substances 0.000 claims abstract description 120
- 238000000034 method Methods 0.000 claims abstract description 46
- 229910052810 boron oxide Inorganic materials 0.000 claims abstract description 42
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000000463 material Substances 0.000 claims abstract description 39
- 239000010453 quartz Substances 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000001816 cooling Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000155 melt Substances 0.000 claims abstract description 15
- 238000007789 sealing Methods 0.000 claims abstract description 7
- 238000005520 cutting process Methods 0.000 claims abstract description 5
- 238000010899 nucleation Methods 0.000 claims description 31
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000002019 doping agent Substances 0.000 claims description 4
- 238000010583 slow cooling Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 description 6
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The scheme provides a growth method of indium phosphide monocrystal based on a double-layer crucible, which comprises the following steps: 1) Placing the single crystal growth material into a double-layer crucible, then placing the double-layer crucible into a quartz tube, and sealing the quartz tube; 2) Filling a quartz tube filled with materials into a single crystal furnace to be heated according to a set program until indium phosphide polycrystal materials are completely melted to obtain a melt, and enabling melted boron oxide to flow into the bottom of an inner crucible and overflow into a gap between the inner crucible and an outer crucible; 3) Adjusting the temperature of the single crystal furnace to enable the upper part of the seed crystal to be melted, and cooling according to a set degree after the temperature field of the single crystal furnace is stable until the whole melt is solidified into crystals; 4) Cutting a quartz tube, taking out a double-layer crucible, placing the double-layer crucible in hot water to separate an inner crucible from an outer crucible and separate crystals and boron oxide in the inner crucible, improving the demolding efficiency and the crucible utilization rate through the design of the double-layer crucible, avoiding the leakage risk, and changing the heat transfer in the growth process of the indium phosphide single crystal so as to improve the growth yield of the single crystal.
Description
Technical Field
The application relates to the field of indium phosphide crystals, in particular to a method for growing an indium phosphide single crystal based on a double-layer crucible.
Background
At present, the growth of indium phosphide monocrystal is mainly characterized by that the seed crystal is placed into the seed crystal cavity of boron nitride crucible, and the polycrystal material, boron nitride and red phosphorus are placed into the crucible body, then the crucible body is vacuum-pumped by means of quartz tube, welded and sealed, and placed into the monocrystal furnace, and heated. In order to prevent boron oxide and molten polycrystal materials from leaking out of the crucible in the growth process of indium phosphide monocrystal, a method is to cut and polish the crucible by using a high-purity BN rod: cutting a BN rod to be about 1-2 cm in length, polishing the BN rod into a round table shape with one end slightly smaller than a crucible seed crystal cavity and the other end larger than the crucible seed crystal cavity by using fine sand paper, then plugging the boron oxide crucible seed crystal cavity with the smaller end, and gradually twisting the BN rod inwards until the BN rod can be well fixed, thereby ensuring that seed crystals and materials in the crucible cannot leak out in the growth process after the seed crystals are mounted, and ensuring the tightness of the lower part of the crucible. The BN rod plugged in the production process has the risk of falling, the small mouth of the crucible is broken in the thermal expansion and cold contraction process due to the stress of the BN rod in the demolding process, and the small mouth of the boron oxide crucible is scrapped after being used once, so that the production cost of the indium phosphide monocrystal is greatly increased; another method is to design a crucible cap, the inner diameter of the crucible cap is about the outer diameter of a seed crystal cavity, the crucible cap is worn at the top end of a small mouth of a boron oxide crucible in the using process, seed crystals and materials are filled in the crucible cap, and the lower part of the crucible is sealed. It should be noted that, in the prior art, one side of the seed crystal cavity is closed, hot water cannot enter from one side of the seed crystal to dissolve boron oxide in the demolding process, so that the seed crystal is clung to the crucible, the crucible seed crystal cavity is pulled in the demolding process to cause damage, and meanwhile, the demolding efficiency is greatly reduced.
Disclosure of Invention
The embodiment of the application provides a growth method of indium phosphide single crystal based on a double-layer crucible, which improves the demolding efficiency and the crucible utilization rate, avoids the leakage risk, and can change the heat transfer in the growth process of the indium phosphide single crystal so as to improve the growth yield of the single crystal.
In a first aspect, embodiments of the present application provide a method for growing an indium phosphide crystal based on a double-layer crucible, including:
1) Placing a single crystal growth material into a double-layer crucible, then placing the double-layer crucible into a quartz tube, and sealing the quartz tube to obtain the quartz tube filled with the material, wherein the double-layer crucible consists of an inner crucible and an outer crucible with gaps, the inner crucible is arranged on the inner side of the outer crucible, the top of the inner crucible is lower than the top of the outer crucible, and the single crystal growth material comprises seed crystals, indium phosphide polycrystal material, red phosphorus, boron oxide and doping agents;
2) Filling a quartz tube filled with materials into a single crystal furnace to carry out temperature rise by a set program until indium phosphide polycrystal materials are completely melted to obtain a melt, wherein in the temperature rise process, melted boron oxide flows into the bottom of an inner crucible and overflows into a gap between the inner crucible and an outer crucible;
3) Adjusting the temperature of the single crystal furnace to enable the upper part of the seed crystal to be melted, and cooling according to a set degree after the temperature field of the single crystal furnace is stable until the whole melt is solidified into crystals;
4) Cutting a quartz tube, taking out the double-layer crucible, placing the double-layer crucible in hot water at 65-80 ℃ to separate the inner crucible from the outer crucible and the crystal and boron oxide in the inner crucible, and taking out the crystal.
The main contributions and innovation points of the invention are as follows:
the demolding efficiency and the crucible utilization rate are improved. The double-layer crucible consisting of the inner crucible and the outer crucible is designed, boron oxide between the gaps of the inner crucible and the outer crucible is easier to dissolve into water to separate the inner crucible from the outer crucible in the growth process and the demolding process of indium phosphide single crystals, after the inner crucible and the outer crucible are separated, hot water enters from the upper end and the lower end of the inner crucible to dissolve the boron oxide between the crystal and the inner crucible, the stress born by a seed crystal cavity corresponding to the seeding stage is reduced, compared with the original mode of sealing the seed crystal cavity, the boron oxide at the seed crystal part of the scheme cannot be basically dissolved, so that the crystal is separated from the crystal after the crystal is disconnected in the demolding process, the problem of difficult demolding is solved by the double-layer crucible, the damage probability of the seed crystal cavity of the crucible in the demolding process is reduced, and the demolding efficiency and the crucible use rate are improved. Avoiding the risk of material leakage. The double-layer crucible completely avoids the risk that seed crystals slide out due to the fact that a small mouth of the crucible is not plugged or a crucible cap is not fixed in the single crystal growth process of the original process, and then polycrystalline materials or liquid sealing agents leak out, so that loss caused by crucible breakage due to material leakage is reduced. The heat transfer in the growth process of the indium phosphide single crystal is changed to improve the yield of single crystal growth. The liquid boron oxide between the double-layer crucible also serves as a buffer layer, when the power of the external heating wire of the double-layer crucible is unstable, the actual temperature is fluctuated, the temperature fluctuation is reduced due to the arrangement of the buffer layer, meanwhile, a heat shield is also provided, rapid heat exchange between the melt and the hearth of the single crystal furnace is blocked, and the influence of the abnormality of the external heating wire on the growth of crystals inside the double-layer crucible is reduced. The details of one or more embodiments of the application are set forth in the accompanying drawings and the description below to provide a more thorough understanding of the other features, objects, and advantages of the application.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute an undue limitation to the application. In the drawings:
fig. 1 is a schematic view of the overall structure of a double-layered crucible provided according to an embodiment of the present application;
fig. 2 is a schematic view of a specific structure of a double-layered crucible provided according to an embodiment of the present application;
in the figure: the inner crucible comprises an inner crucible body 11, an inner crucible constant diameter part 111, an inner crucible shoulder-placing part 112, an inner crucible seeding part 113, an outer crucible body 12, an outer crucible constant diameter part 121, an outer crucible shoulder-placing part 122 and an outer crucible seeding part 123.
Detailed Description
Reference will now be made in detail to exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, the same numbers in different drawings refer to the same or similar elements, unless otherwise indicated. The implementations described in the following exemplary embodiments do not represent all implementations consistent with one or more embodiments of the present specification. Rather, they are merely examples of apparatus and methods consistent with aspects of one or more embodiments of the present description as detailed in the accompanying claims.
It should be noted that: in other embodiments, the steps of the corresponding method are not necessarily performed in the order shown and described in this specification. In some other embodiments, the method may include more or fewer steps than described in this specification. Furthermore, individual steps described in this specification, in other embodiments, may be described as being split into multiple steps; while various steps described in this specification may be combined into a single step in other embodiments.
Example 1
The utility model provides a growing method of indium phosphide crystal based on double-deck crucible, the problem that the drawing of patterns inefficiency and material leakage etc. brought by the growth of indium phosphide crystal in traditional technology has been improved through the double-deck crucible of original design, and specifically, the growing method of indium phosphide crystal based on double-deck crucible that this scheme provided includes following steps:
1) Placing a single crystal growth material into a double-layer crucible, then placing the double-layer crucible into a quartz tube, and sealing the quartz tube to obtain the quartz tube filled with the material, wherein the double-layer crucible consists of an inner crucible 11 and an outer crucible 12 with gaps, the inner crucible 11 is arranged on the inner side of the outer crucible 12, and the top of the inner crucible 11 is lower than the top of the outer crucible 12, wherein the single crystal growth material comprises seed crystal, indium phosphide polycrystal material, red phosphorus, boron oxide and doping agent;
2) Loading a quartz tube filled with materials into a single crystal furnace to carry out temperature rise by a set program until indium phosphide polycrystal materials are completely melted to obtain a melt, wherein in the temperature rise process, melted boron oxide flows into the bottom of an inner crucible 11 and overflows into a gap between the inner crucible 11 and an outer crucible 12;
3) Adjusting the temperature of the single crystal furnace to enable the upper part of the seed crystal to be melted, and cooling according to a set degree after the temperature field of the single crystal furnace is stable until the whole melt is solidified into crystals;
4) Cutting a quartz tube, taking out the double-layer crucible, placing the double-layer crucible in 65-80 ℃ hot water to separate the inner crucible 11 and the outer crucible 12 and separate the crystal and boron oxide in the inner crucible 11, and taking out the crystal.
The structure of the double-layer crucible provided in this embodiment is shown in fig. 1, the inner crucible 11 and the outer crucible 12 have the same shape, the outer crucible 12 has a structure with one side being conducted and one side being closed, and the inner crucible 11 has a structure with two sides being conducted.
Specifically, the inner crucible 11 is integrally formed by an inner crucible constant diameter portion 111, an inner crucible shoulder 112 and an inner crucible seeding portion 113 which are sequentially connected, wherein the inner crucible constant diameter portion 111 and the inner crucible seeding portion 113 are in a cylindrical structure with two ends being conducted, and the inner crucible shoulder 112 is in a conical structure with two ends being conducted. In some embodiments, inner crucible constant diameter portion 111 and inner crucible seeding portion 113 are cylinders that remain the same in diameter, and the diameter of inner crucible shoulder 112 tapers from inner crucible constant diameter portion 111 toward inner crucible seeding portion 113.
The outer crucible 12 is composed of an outer crucible constant diameter part 121, an outer crucible placing shoulder part 122 and an outer crucible seeding part 123 which are connected in sequence, wherein the outer crucible constant diameter part 121 is of a cylindrical structure with two ends being conducted, the outer crucible placing shoulder part 122 is of a conical cylinder structure with two ends being conducted, the outer crucible seeding part 123 is of a cylindrical structure with one side being conducted, and one end of the outer crucible seeding part 123 close to the outer crucible placing shoulder part 122 is conducted. In some embodiments, outer crucible constant diameter portion 121 and outer crucible seeding portion 123 are cylinders that remain the same in diameter, and outer crucible shoulder 122 tapers in diameter from outer crucible constant diameter portion 121 toward outer crucible seeding portion 123.
When the inner crucible 11 is placed on the outer crucible 12, the position where the inner crucible constant diameter portion 111 meets the inner crucible shoulder portion 112 is on the same level as the position where the outer crucible constant diameter portion 121 meets the outer crucible shoulder portion 122, and the position where the inner crucible shoulder portion 112 meets the inner crucible seeding portion 113 is on the same level as the position where the outer crucible shoulder portion 122 meets the outer crucible seeding portion 123.
As shown in fig. 2, the shoulder angle of the outer crucible shoulder 122 is larger than the shoulder angle of the inner crucible shoulder 112, so that the gap between the outer crucible shoulder 122 and the inner crucible shoulder 112 gradually increases toward the direction in which the outer crucible seeding portion 123 is located, the gap between the inner crucible constant diameter portion 111 and the outer crucible constant diameter portion 121 is uniform, the gap between the inner crucible seeding portion 113 and the outer crucible seeding portion 123 is uniform, and the gap between the inner crucible seeding portion 113 and the outer crucible seeding portion 123 is smaller than the gap between the inner crucible constant diameter portion 111 and the outer crucible constant diameter portion 121. The design of the scheme has the advantages that: the thickness of the filling layer formed between the inner crucible and the outer crucible can be gradually thickened towards the crystal guiding part 123 of the outer crucible, and as the boron oxide is a poor heat conductor, the crystallization latent heat generated by the solid-liquid interface is prevented from being transmitted from the radial direction, the heat conducted out from the crucible wall in the shouldering process is reduced, the axial heat dissipation is increased, the driving force of the axial crystal growth is improved, and the smoothness or the slight convexity of the crystal growth interface is ensured.
In some embodiments, the top height of the inner crucible 11 is greater than 4cm below the top height of the outer crucible 12.
In some embodiments, the shoulder angle of the inner crucible shoulder 112 is 90 °.
In some specific embodiments, the gap between inner crucible constant diameter portion 111 and outer crucible constant diameter portion 121 is between 1-1.5mm, and the gap between inner crucible seeding portion 113 and outer crucible seeding portion 123 is between 0.5-1.2 mm.
After seed crystal, indium phosphide polycrystal material, red phosphorus, boron oxide and doping agent are sequentially placed in an inner crucible 11, a double-layer crucible filled with the materials is placed in a quartz tube, and a quartz cap is placed in an opening of the quartz tube and then sealed by oxyhydrogen flame vacuum welding. It should be noted that, because the double-layer crucible structure is adopted in the scheme, the risk that seed crystals slide out and polycrystalline materials or liquid sealing agents leak out due to the fact that small mouths of the crucible are not plugged or a crucible cap is not fixed in the traditional process can be completely avoided, and further loss caused by crucible breakage due to material leakage is reduced.
In the scheme, in the step of loading a quartz tube filled with materials into a single crystal furnace to carry out temperature rise by a set program until indium phosphide polycrystal materials are completely melted to obtain a melt, red phosphorus in an inner crucible 11 is vaporized in a first temperature rise stage, boron oxide begins to melt in a second temperature rise stage, part of the melted boron oxide flows into the bottom of the inner crucible 11, part of the melted boron oxide overflows from the top of the inner crucible 11 and enters a gap between the inner crucible 11 and an outer crucible 22, and in a third temperature rise stage, the indium phosphide polycrystal materials are completely melted to obtain the melt, and the melt is wrapped by the boron oxide.
Specifically, the temperature rise setting program is set as follows: vacuumizing the single crystal furnace in the first temperature rising stage, and uniformly rising the temperature from room temperature to 350 ℃ in 1 h; the second temperature rising stage is performed with air intake: keeping the temperature at 350 ℃ for 1h, and in the third heating stage: the temperature is raised for 5 hours at a constant speed to be between 1065 ℃ and 1085 ℃.
Since the top of the inner crucible 11 of the double-layered crucible of the present embodiment is lower than the top of the outer crucible 12, liquid boron oxide after melting the boron oxide in the inner crucible 11 can overflow from the inner crucible 11 to the gap between the inner crucible 11 and the outer crucible 12. The liquid boron oxide which overflows the gap between the inner crucible 11 and the outer crucible 12 can play a role of a buffer layer to slow down the influence caused by the temperature fluctuation outside the quartz tube, and also play a role of a heat shield to block the rapid heat exchange between the melt and the single crystal furnace, so that the influence of the heating element of the single crystal furnace on the growth of the internal crystal is reduced.
In the step of adjusting the temperature of the single crystal furnace to promote the upper part of the seed crystal to melt, the temperature of the single crystal furnace is controlled to 1045-1055 ℃, and when the upper part of the seed crystal is melted, the temperature of the seed crystal of the whole melt is gradually increased to form a gradient zone, wherein the temperature of the gradient zone is 1000-1080 ℃. The temperature of the single crystal furnace is regulated to be approximately that the upper temperature of the seed crystal is smaller than 1060 ℃ and the lower temperature of the seed crystal is larger than 1030 ℃.
And cooling according to a set degree after the temperature field of the single crystal furnace is stable until the whole melt is solidified into crystals, cooling according to the single crystal growth rate to know that the whole melt is solidified into crystals, and taking the quartz tube out of the single crystal furnace after cooling.
The setting procedure of the temperature reduction is as follows: the first cooling stage is a slow cooling stage: the low temperature area is cooled at the average speed of 3-5 ℃ per hour, the high temperature area is cooled at the average speed of 0.2-0.3 ℃ per hour for about 80 hours, the second cooling stage and the third cooling stage are rapid cooling, the second stage is 9 hours and uniformly cooling to 300 ℃, and the third stage is 6 hours and uniformly cooling to 600 ℃.
In some embodiments, the low temperature zone is cooled at an average rate of about 4 ℃ per hour and the high temperature zone is cooled at about 0.25 ℃ per hour.
In the step of separating the inner crucible 11 and the outer crucible 12 and separating the crystal and the boron oxide in the inner crucible 11 by placing the double-layered crucible in hot water of 65 to 80 c, the hot water first enters the gap between the inner crucible 11 and the outer crucible 11 to melt the boron oxide in the gap to separate the inner crucible 11 and the outer crucible 12, and then the hot water enters the gap between the melt and the inner crucible 11 from the inner crucible 11 to dissolve the boron oxide to separate the crystal and the boron oxide, so that simple demoulding of the crystal is achieved.
In some embodiments, hot water enters the gap between the melt and the inner crucible 11 from the bottom of the inner crucible 11. In addition, in some embodiments, the temperature of the hot water of the present protocol is 70 ℃.
According to the scheme, the double-layer crucible structure is adopted, the boron oxide between gaps is easy to dissolve into water in the demolding process, so that the inner crucible 11 and the outer crucible 12 are separated, hot water enters from the upper end and the lower end of the inner crucible 11, the boron oxide between the crystal and the inner crucible 11 is dissolved, the problem of difficult demolding is solved by the double-layer crucible, the probability of damage to a seed crystal cavity of the crucible in the demolding process is reduced, and the demolding efficiency and the crucible use rate are improved.
The present invention is not limited to the above-described preferred embodiments, and any person who can obtain other various products under the teaching of the present invention, however, any change in shape or structure of the product is within the scope of the present invention, and all the products having the same or similar technical solutions as the present application are included.
Claims (10)
1. A method for growing an indium phosphide crystal on the basis of a double-layer crucible, comprising: 1) Placing a single crystal growth material into a double-layer crucible, then placing the double-layer crucible into a quartz tube, and sealing the quartz tube to obtain the quartz tube filled with the material, wherein the double-layer crucible consists of an inner crucible and an outer crucible with gaps, the inner crucible is arranged on the inner side of the outer crucible, the top of the inner crucible is lower than the top of the outer crucible, and the single crystal growth material comprises seed crystals, indium phosphide polycrystal material, red phosphorus, boron oxide and doping agents;
2) Filling a quartz tube filled with materials into a single crystal furnace to carry out temperature rise by a set program until indium phosphide polycrystal materials are completely melted to obtain a melt, wherein in the temperature rise process, melted boron oxide flows into the bottom of an inner crucible and overflows into a gap between the inner crucible and an outer crucible;
3) Adjusting the temperature of the single crystal furnace to enable the upper part of the seed crystal to be melted, and cooling according to a set degree after the temperature field of the single crystal furnace is stable until the whole melt is solidified into crystals;
4) Cutting a quartz tube, taking out the double-layer crucible, placing the double-layer crucible in hot water at 65-80 ℃ to separate the inner crucible from the outer crucible and the crystal and boron oxide in the inner crucible, and taking out the crystal.
2. The method for growing an indium phosphide crystal on the basis of a double-layer crucible as set forth in claim 1, wherein the inner crucible and the outer crucible are identical in shape, the outer crucible has a structure of single-side conduction and single-side closure, and the inner crucible has a structure of double-side conduction.
3. The method for growing indium phosphide crystals based on a double-layer crucible as set forth in claim 1, wherein the inner crucible is composed of an inner crucible constant diameter portion, an inner crucible shoulder portion and an inner crucible seeding portion which are connected in sequence, wherein the inner crucible constant diameter portion and the inner crucible seeding portion are of a cylindrical structure with two ends being conducted, and the inner crucible shoulder portion is of a conical structure with two ends being conducted; the outer crucible is composed of an outer crucible constant diameter part, an outer crucible placing shoulder part and an outer crucible seeding part which are connected in sequence, wherein the outer crucible constant diameter part is of a cylindrical structure with two ends being communicated, the outer crucible placing shoulder part is of a conical cylinder structure with two ends being communicated, the outer crucible seeding part is of a cylindrical structure with one side being communicated, and one end of the outer crucible seeding part, which is close to the outer crucible placing shoulder part, is communicated.
4. A method for growing an indium phosphide crystal on the basis of a double-layer crucible as set forth in claim 3, wherein the gap between the outer crucible shoulder portion and the inner crucible shoulder portion gradually increases toward the direction in which the outer crucible seeding portion is located, the gap between the inner crucible isodiametric portion and the outer crucible isodiametric portion is uniform, the gap between the inner crucible seeding portion and the outer crucible seeding portion is uniform, and the gap between the inner crucible seeding portion and the outer crucible seeding portion is smaller than the gap between the inner crucible isodiametric portion and the outer crucible isodiametric portion.
5. The method for growing an indium phosphide crystal on the basis of a double-layer crucible as set forth in claim 4, wherein the shoulder angle of the shoulder portion of the outer crucible is larger than the shoulder angle of the shoulder portion of the inner crucible.
6. The method for growing an indium phosphide crystal on the basis of a double-layer crucible as set forth in claim 1, wherein in the step of charging a quartz tube filled with a material into a single-crystal furnace to be programmed to rise temperature until indium phosphide polycrystal material is completely melted to obtain a melt, wherein in the first rise period, red phosphorus in the inner crucible is vaporized, in the second rise period, boron oxide starts to melt and a part of the melted boron oxide flows into the bottom of the inner crucible, a part overflows from the top of the inner crucible into a gap between the inner crucible and the outer crucible, and in the third rise period, indium phosphide polycrystal material is completely melted to obtain a melt, and the melt is surrounded by boron oxide.
7. The method for growing an indium phosphide crystal according to claim 6, wherein the temperature-raising setting program is set as follows: vacuumizing the single crystal furnace in the first temperature rising stage, and uniformly rising the temperature from room temperature to 350 ℃ in 1 h; the second temperature rising stage is performed with air intake: keeping the temperature at 350 ℃ for 1h, and in the third heating stage: the temperature is raised for 5 hours at a constant speed to be between 1065 ℃ and 1085 ℃.
8. The method for growing an indium phosphide crystal on the basis of a double-layer crucible as set forth in claim 1, wherein when the upper portion of the seed crystal is melted, the seed crystal of the entire melt is gradually raised upward in temperature to form a gradient zone, wherein the temperature of the gradient zone is 1000 ℃ to 1080 ℃.
9. The method for growing indium phosphide crystal on the basis of double-layer crucible according to claim 1, wherein the set procedure of temperature reduction is as follows: the first cooling stage is a slow cooling stage: the low temperature area is cooled at the average speed of 3-5 ℃ per hour, the high temperature area is cooled at the average speed of 0.2-0.3 ℃ per hour, the second cooling stage and the third cooling stage are rapid cooling, the second stage is uniform cooling at 300 ℃ for 9 hours, and the third stage is uniform cooling at 600 ℃ for 6 hours.
10. The method for growing an indium phosphide crystal based on a double-layer crucible as set forth in claim 1, wherein in the step of separating the inner crucible and the outer crucible and separating the crystal and boron oxide in the inner crucible by placing the double-layer crucible in hot water at 65 to 80 ℃, the hot water first enters the gap between the inner crucible and the outer crucible to melt the boron oxide in the gap to separate the inner crucible and the outer crucible, and then the hot water enters the gap between the melt and the inner crucible from the inner crucible to dissolve the boron oxide to separate the crystal and the boron oxide.
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Citations (18)
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