Quartz crucible assembly and growth furnace for indium antimonide crystal growth

CN224633600UActive Publication Date: 2026-08-14GUANGDONG JINGZHI OPTOELECTRONICS TECH CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-06-13
Publication Date
2026-08-14

AI Technical Summary

Technical Problem

[0004]但是,第二石英坩埚置于第一石英坩埚内时在底部周缘接触第一石英坩埚的内周壁,在直拉法生长晶体过程中第一石英坩埚旋转时,第二石英坩埚会相对第一石英坩埚位移,从而造成晶体生长液面波动,从而影响晶体质量

Benefits of technology

[0012]在根据本公开的用于锑化铟晶体生长的石英坩埚组件以及生长炉中,通过第一石英坩埚的周壁和第二石英坩埚的周部之间形成有沿上下方向相对彼此滑动而沿周向和径向限制的滑动副,在直拉法生长晶体过程中第一石英坩埚旋转时,第二石英坩埚受到滑动副的限制而与第一石英坩埚在周向上卡在一起旋转,第二石英坩埚不会相对第一石英坩埚位移,从而避免第二石英坩埚的移动造成晶体生长液面(即锑化铟料形成的熔体的液面)波动,从而避免影响晶体质量。

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Abstract

A quartz crucible assembly and a growth furnace for growing indium antimonide crystals are provided. The quartz crucible assembly includes a first quartz crucible and a second quartz crucible; the first quartz crucible has a bottom wall and a peripheral wall, which form an upwardly open and bottom- and peripherally closed inner cavity; the second quartz crucible has a peripheral portion and a hollow frustum-shaped portion, the peripheral portion being cylindrical, the hollow frustum-shaped portion being located inside the peripheral portion and lower than the peripheral portion, the hollow frustum-shaped portion and the peripheral portion forming a bottom surface, and the hollow frustum-shaped portion forming a trumpet-shaped cavity communicating with the inner cavity of the first quartz crucible; a sliding pair is formed between the peripheral wall of the first quartz crucible and the peripheral portion of the second quartz crucible, which slides relative to each other in the vertical direction and is restricted in the circumferential and radial directions; the first quartz crucible is configured to hold indium antimonide material at the bottom of the inner cavity; the second quartz crucible is configured to be placed inside the first quartz crucible, on the indium antimonide material in the first quartz crucible, and engages with the peripheral wall of the first quartz crucible through the sliding pair.
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Description

Technical Field

[0001] This disclosure relates to the field of crystal growth, and more specifically to a quartz crucible assembly and growth furnace for the growth of indium antimonide crystals. Background Technology

[0002] InSb, a group III-V semiconductor crystal material, possesses an extremely narrow bandgap, very low effective electron mass, and extremely high electron mobility, along with stable physicochemical properties. Based on these superior properties, it has found significant applications in industrial technologies such as magnetoresistive devices and Hall effect devices. Of particular note is that, due to InSb's intrinsic absorption in the 3-5 μm wavelength range, InSb-based infrared detectors exhibit extremely high quantum efficiency and responsivity, making InSb the preferred material for mid-wave infrared detectors. With the development of next-generation ultra-large-scale infrared focal plane array devices such as megapixel sensors, the demand for large-size, high-quality InSb crystals is increasing to reduce detector manufacturing costs and improve production efficiency. Large-size InSb crystal growth technology has become a primary key issue to be addressed. Diameter control, dislocation density control, and electrical parameter control technologies all need to be solved during the crystal growth stage, while the temperature gradient is a crucial factor determining the success of crystal growth.

[0003] Chinese patent document CN222411985U discloses a quartz crucible assembly and a growth furnace for growing indium antimonide crystals. The quartz crucible assembly includes a first quartz crucible and a second quartz crucible. The first quartz crucible has an inner cavity that is open upwards and closed at the bottom and periphery. The second quartz crucible is funnel-shaped, wider at the bottom and narrower at the top, hollow inside, and open upwards and downwards. The first quartz crucible is configured to hold indium antimonide material to be grown using the Czochralski method at the bottom of the inner cavity. The second quartz crucible is configured to be placed inside the first quartz crucible, on top of the indium antimonide material, and to contact the inner peripheral wall of the first quartz crucible at its bottom periphery. The growth furnace for growing indium antimonide crystals utilizes the quartz crucible assembly to grow crystals using the Czochralski method, thereby reducing dislocations in the obtained indium antimonide crystal and improving its quality.

[0004] However, when the second quartz crucible is placed inside the first quartz crucible, its bottom periphery contacts the inner wall of the first quartz crucible. During the Czochralski crystal growth process, when the first quartz crucible rotates, the second quartz crucible will shift relative to the first quartz crucible, causing fluctuations in the crystal growth liquid surface and thus affecting the crystal quality.

[0005] Furthermore, the quartz crucible assembly needs further improvement to further enhance the crystal growth temperature field, further reduce the dislocations in the obtained indium antimonide crystal, and thus further improve the quality of the indium antimonide crystal. Utility Model Content

[0006] In view of the problems existing in the background art, one object of this disclosure is to provide a quartz crucible assembly and growth furnace for indium antimonide crystal growth, which can avoid the crystal growth liquid surface fluctuation caused by the movement of the second quartz crucible.

[0007] Another object of this disclosure is to provide a quartz crucible assembly and growth furnace for the growth of indium antimonide crystals, which can change the temperature distribution within a first quartz crucible.

[0008] Another object of this disclosure is to provide a quartz crucible assembly and growth furnace for growing indium antimonide crystals, which can reduce the dislocations in the obtained indium antimonide crystals.

[0009] Therefore, a quartz crucible assembly for indium antimonide crystal growth is provided. The quartz crucible assembly includes a first quartz crucible and a second quartz crucible. The first quartz crucible has a bottom wall and a peripheral wall, which form an upwardly open, bottom-side and peripheral-side-closed cylindrical cavity. The second quartz crucible has a peripheral portion and a hollow frustum-shaped portion. The peripheral portion is cylindrical, and the hollow frustum-shaped portion is located inside the peripheral portion and lower than the peripheral portion. The hollow frustum-shaped portion and the peripheral portion are integrally connected at the bottom to form an annular bottom surface. The hollow frustum-shaped portion is smaller at the top and larger at the bottom, with a central... The cavity is hollow, open to the top and open to the bottom, and communicates with the inner cavity of the first quartz crucible; a sliding pair is formed between the peripheral wall of the first quartz crucible and the peripheral portion of the second quartz crucible, which slides relative to each other in the vertical direction and is restricted in the circumferential and radial directions; the first quartz crucible is configured to hold indium antimonide material for growing indium antimonide crystals by Czochralski method at the bottom of the inner cavity; the second quartz crucible is configured to be placed inside the first quartz crucible, on the indium antimonide material of the first quartz crucible, and cooperate with the peripheral wall of the first quartz crucible through the sliding pair.

[0010] A growth furnace for growing indium antimonide crystals is provided. The growth furnace includes a furnace body, a heater, a quartz crucible assembly, a seed crystal, and a crystal pulling rod. The quartz crucible assembly is supported and fixed inside the furnace body. The heater is located inside the furnace body and is used to heat the indium antimonide material inside the first quartz crucible of the quartz crucible assembly from the outside to form an indium antimonide melt. The seed crystal is fixed to the end of the crystal pulling rod. The crystal pulling rod is disposed in the furnace body, located above the quartz crucible assembly, and is capable of reciprocating in the vertical direction. The crystal pulling rod is configured to drive the seed crystal downward into the second quartz crucible of the quartz crucible assembly, immersing it from the surface of the indium antimonide melt, and then the crystal pulling rod is pulled upward to grow indium antimonide crystals to form indium antimonide ingots.

[0011] The beneficial effects of this disclosure are as follows.

[0012] In the quartz crucible assembly and growth furnace for indium antimonide crystal growth according to this disclosure, a sliding pair is formed between the peripheral wall of the first quartz crucible and the periphery of the second quartz crucible. This sliding pair slides relative to each other in the vertical direction and is restricted in the circumferential and radial directions. During the Czochralski crystal growth process, when the first quartz crucible rotates, the second quartz crucible is restricted by the sliding pair and rotates together with the first quartz crucible in the circumferential direction. The second quartz crucible will not be displaced relative to the first quartz crucible, thereby avoiding fluctuations in the crystal growth liquid surface (i.e., the liquid surface of the melt formed by the indium antimonide material) caused by the movement of the second quartz crucible, thus avoiding affecting the crystal quality.

[0013] In the quartz crucible assembly and growth furnace for indium antimonide crystal growth according to this disclosure, the overlapping portion of the hollow frustum and the periphery reduces the temperature gradient at the solid-liquid interface, decreasing the thermal stress during crystal growth and thus reducing dislocation generation. The portion of the periphery extending beyond the hollow frustum increases the temperature gradient away from the solid-liquid interface, allowing the latent heat of crystallization generated at the solid-liquid interface to be released from the crystal, thereby improving the crystal growth interface and preventing concave interfaces and dislocation generation. In other words, the cylindrical periphery and hollow frustum design of the second quartz crucible can alter the temperature distribution within the first quartz crucible. As verified, the quartz crucible assembly of this disclosure, when used for indium antimonide crystal growth, can reduce the dislocations in the obtained indium antimonide crystal. Attached Figure Description

[0014] Figure 1 This is a schematic cross-sectional view of a growth furnace for growing indium antimonide crystals according to this disclosure.

[0015] Figure 2 This is a perspective view of the first quartz crucible of the quartz crucible assembly for indium antimonide crystal growth according to the present disclosure.

[0016] Figure 3 yes Figure 2 A half-section 3D view.

[0017] Figure 4 This is a three-dimensional view of the second quartz crucible in the quartz crucible assembly.

[0018] Figure 5 yes Figure 4 A half-section 3D view.

[0019] Figure 6 This is a cross-sectional view of the first quartz crucible, with example dimensions indicated.

[0020] Figure 7 This is a cross-sectional view of the second quartz crucible, with example dimensions indicated.

[0021] Figure 8 This is an EPD distribution diagram of the indium antimonide crystal slice from Example 1.

[0022] Figure 9 This is the dislocation EPD distribution diagram of the indium antimonide crystal slice of Comparative Example 1.

[0023] The reference numerals in the attached figures are explained as follows:

[0024] 100 growth furnace 32 second quartz crucible

[0025] 1 Furnace body 321 perimeter

[0026] 11. Top cover 322. Hollow truncated circular section

[0027] 12-inch middle cylinder 322a cavity

[0028] 13 base 323 bottom surface

[0029] 2 heater G groove

[0030] 21 Graphite heater B convex strip

[0031] 22 Graphite Double-Layer Insulation Cover P Sliding Pair

[0032] 221 inner layer 4 seed crystals

[0033] 222 outer layer 5 crystal pull rods

[0034] 23 carbon felt 6 vacuum interface

[0035] 3 Quartz Crucible Assembly 7 Gas Inlet

[0036] 31 First Quartz Crucible 8 Supports

[0037] 311 bottom wall S screw

[0038] 312 peripheral wall 200 indium antimonide material

[0039] 313 inner cavity Detailed Implementation

[0040] The accompanying drawings illustrate embodiments of this disclosure, and it will be understood that the disclosed embodiments are merely examples of this disclosure, which can be implemented in various forms. Therefore, the specific details disclosed herein should not be construed as limiting, but are intended only as the basis for the claims and as an illustrative basis to teach those skilled in the art how to implement this disclosure in various ways.

[0041] [Quartz crucible assembly for indium antimonide crystal growth]

[0042] Reference Figures 1 to 7 The quartz crucible assembly 3 for indium antimonide crystal growth according to this disclosure includes a first quartz crucible 31 and a second quartz crucible 32.

[0043] The first quartz crucible 31 has a bottom wall 311 and a peripheral wall 312, which form a cylindrical inner cavity 313 that is open upwards and closed at the bottom and peripheral sides. The second quartz crucible 32 has a peripheral portion 321 and a hollow frustum 322. The peripheral portion 321 is cylindrical, and the hollow frustum 322 is located inside the peripheral portion 321 and is lower than the peripheral portion 321. The hollow frustum 322 and the peripheral portion 321 are integrally connected at the bottom to form an annular bottom surface 323. The hollow frustum 322 forms a trumpet-shaped cavity 322a that is smaller at the top and larger at the bottom, hollow inside, and open upwards and downwards, communicating with the inner cavity 313 of the first quartz crucible 31. A sliding pair P is formed between the peripheral wall 312 of the first quartz crucible 31 and the peripheral portion 321 of the second quartz crucible 32, which slides relative to each other in the vertical direction and is restricted in the circumferential and radial directions. The first quartz crucible 31 is configured to hold indium antimonide material 200, on which indium antimonide crystals will be grown by the Czochralski method, at the bottom of the inner cavity 313. The second quartz crucible 32 is configured to be placed inside the first quartz crucible 31, on the indium antimonide material 200 in the first quartz crucible 31, and to engage with the peripheral wall 312 of the first quartz crucible 31 via a sliding pair P.

[0044] In the quartz crucible assembly 3 for indium antimonide crystal growth according to this disclosure, a sliding pair P is formed between the peripheral wall 312 of the first quartz crucible 31 and the peripheral portion 321 of the second quartz crucible 32, which slides relative to each other in the vertical direction and is restricted in the circumferential and radial directions. During the Czochralski crystal growth process, when the first quartz crucible 31 rotates, the second quartz crucible 32 is restricted by the sliding pair P and rotates together with the first quartz crucible 31 in the circumferential direction. The second quartz crucible 32 will not be displaced relative to the first quartz crucible 31, thereby avoiding fluctuations in the crystal growth liquid surface (i.e., the liquid surface of the melt formed by the indium antimonide material 200) caused by the movement of the second quartz crucible 32, thus avoiding affecting the crystal quality.

[0045] In the quartz crucible assembly 3 for indium antimonide crystal growth according to this disclosure, the overlapping portion of the hollow frustum portion 322 and the periphery 321 reduces the temperature gradient at the solid-liquid interface, thereby reducing the thermal stress during crystal growth and thus reducing dislocation generation. The portion of the periphery 321 extending beyond the hollow frustum portion 322 increases the temperature gradient away from the solid-liquid interface, allowing the latent heat of crystallization generated at the solid-liquid interface to be released from the crystal, thereby improving the crystal growth interface and avoiding concave interfaces and dislocation generation. That is, the design of the cylindrical periphery 321 and the hollow frustum portion 322 of the second quartz crucible 32 can change the temperature distribution within the first quartz crucible 31. As will be verified later, the quartz crucible assembly 3 of this disclosure can reduce the dislocations in the obtained indium antimonide crystal when used for indium antimonide crystal growth.

[0046] Specifically, such as Figures 1 to 7As shown, one of the peripheral wall 312 of the first quartz crucible 31 and the peripheral portion 321 of the second quartz crucible 32 is provided with a protrusion B extending in the vertical direction, and the other of the peripheral wall 312 of the first quartz crucible 31 and the peripheral portion 321 of the second quartz crucible 32 is provided with a groove G extending in the vertical direction. The groove G and the groove G form a sliding pair P.

[0047] Furthermore, the peripheral wall 312 of the first quartz crucible 31 is provided with a groove G; the peripheral portion 321 of the second quartz crucible 32 is provided with a protrusion B, which is located at the lower part of the peripheral portion 321 of the second quartz crucible 32.

[0048] In one example, the groove G is provided along the entire height of the peripheral wall 312; the bottom surface of the protrusion B is flush with the bottom surface 323 of the second quartz crucible 32, and the height of the protrusion B exceeds half the height of the periphery 321 of the second quartz crucible 32; the height of the hollow frustum portion 322 is half the height of the periphery 321 of the second quartz crucible 32.

[0049] In the example shown in the figure, the number of grooves G and ridges B are both eight, and they are evenly distributed along the circumference. Of course, this is not the only possibility; the number of grooves G and ridges B can be set to more or less than eight depending on the actual situation.

[0050] Reference Figure 4 , Figure 6 and Figure 7 In one example, the bottom wall 311 of the first quartz crucible 31 has a wall thickness of 10 mm, the height of the peripheral wall 312 of the first quartz crucible 31 is 200 mm, the wall thickness of the peripheral wall 312 of the first quartz crucible 31 is 10 mm, and the inner diameter of the peripheral wall 312 of the first quartz crucible 31 is 216 mm; the height of the periphery 321 of the second quartz crucible 32 is 150 mm, the wall thickness of the periphery 321 of the second quartz crucible 32 is 5 mm, and the height of the periphery 321 of the second quartz crucible 32 is 150 mm, the wall thickness of the periphery 321 of the second quartz crucible 32 is 5 mm, and the inner diameter of the periphery 321 of the second quartz crucible 32 is 216 mm. The outer diameter of part 321 is 214 mm; the height of the hollow frustum 322 of the second quartz crucible 32 is 75 mm, the outer diameter of the top surface of the hollow frustum 322 is 150 mm, the wall thickness of the hollow frustum 322 is 10 mm, and the cone angle of the cavity 322a of the hollow frustum 322 is 54°; the circumferential length of the convex rib B is 5 mm, the radial dimension of the convex rib B is 5 mm, the height of the convex rib B is 90 mm, and the convex rib B and the groove G are fitted with a 1 mm gap.

[0051] [Growth furnace for indium antimonide crystal growth]

[0052] Reference Figure 1 and combined Figure 2 and Figure 3 The growth furnace 100 for growing indium antimonide crystals according to this disclosure includes a furnace body 1, a heater 2, the aforementioned quartz crucible assembly 3, a seed crystal 4, and a crystal pulling rod 5.

[0053] The quartz crucible assembly 3 is supported and fixed inside the furnace body 1. The heater 2 is located inside the furnace body 1 and is configured to heat the first quartz crucible 31 of the quartz crucible assembly 3 from the outside to form indium antimonide melt from the indium antimonide material 200 inside the first quartz crucible 31. The seed crystal 4 is fixed to the end of the crystal pulling rod 5. The crystal pulling rod 5 is located above the quartz crucible assembly 3 in the furnace body 1 and can reciprocate in the vertical direction. The crystal pulling rod 5 is configured to drive the seed crystal 4 downwards into the second quartz crucible 32 of the quartz crucible assembly 3, immersing it from the surface of the indium antimonide melt. Then, the crystal pulling rod 5 pulls the crystal upwards to grow indium antimonide crystals to form indium antimonide ingots.

[0054] like Figure 1 As shown, the furnace body 1 includes a top cover 11, a middle cylinder 12 and a base 13 arranged sequentially from top to bottom. The top cover 11 and the middle cylinder 12 are detachably assembled by screws S, and the middle cylinder 12 and the base 13 are detachably assembled by screws S.

[0055] like Figure 1 As shown, in one example, the heater 2 includes a graphite heater 21, a graphite double-layer insulation cover 22, and a carbon felt 23; the graphite heater 21 is disposed around the first quartz crucible 31, and the graphite double-layer insulation cover 22 is disposed around the graphite heater 21. Further, the graphite double-layer insulation cover 22 includes an inner layer 221 and an outer layer 222; the carbon felt 23 is filled between the inner layer 221 and the outer layer 222 of the graphite double-layer insulation cover 22.

[0056] The composition and effects of the quartz crucible assembly 3 are explained above and will not be repeated here.

[0057] In addition, the first quartz crucible 31 is fixed on the bracket 8 during operation. The bracket 8 is connected to an external rotating mechanism (not shown) and an external lifting mechanism (not shown) so that it can rotate and rise simultaneously during crystal growth, so that the liquid surface in the first quartz crucible 31 is within the range heated by the heater 2. The rotation of the first quartz crucible 31 is opposite to the rotation of the crystal pulling rod 5.

[0058] Seed crystal 4 can be an indium antimonide single crystal with a purity of 7N or higher.

[0059] The crystal pulling rod 5 is connected to the corresponding rotating mechanism (not shown) and the corresponding lifting mechanism (not shown), and can move upward linearly while rotating.

[0060] like Figure 1 As shown, the growth furnace 100 also includes a vacuum port 6, which is located on the base 13.

[0061] In addition, refer to Figure 1 The growth furnace 100 also includes a gas inlet 7, which is located on the top cover 11.

[0062] [test]

[0063] Example 1

[0064] Example 1 uses the following steps:

[0065] S1, Indium antimonide material 200 is loaded into the first quartz crucible 31 of the growth furnace 100. The bottom wall 311 of the first quartz crucible 31 has a wall thickness of 10mm, the height of the peripheral wall 312 of the first quartz crucible 31 is 200mm, the wall thickness of the peripheral wall 312 of the first quartz crucible 31 is 10mm, the inner diameter of the peripheral wall 312 of the first quartz crucible 31 is 216mm, and the groove G is set along the entire height of the peripheral wall 312. The number of grooves G is eight.

[0066] S2, the second quartz crucible 32 is placed inside the first quartz crucible 31. The second quartz crucible 32 is positioned on the indium antimonide material 200 of the first quartz crucible 31 and engages with the peripheral wall 312 of the first quartz crucible 31 via a sliding pair P. The height of the peripheral portion 321 of the second quartz crucible 32 is 150 mm, the wall thickness of the peripheral portion 321 of the second quartz crucible 32 is 5 mm, and the outer diameter of the peripheral portion 321 of the second quartz crucible 32 is 214 mm. The hollow frustum 322 of crucible 32 has a height of 75 mm, an outer diameter of the top surface of the hollow frustum 322 has a diameter of 150 mm, a wall thickness of 10 mm, and a cone angle of 54° for the cavity 322a of the hollow frustum 322. There are eight protrusions B, with a circumferential length of 5 mm, a radial dimension of 5 mm, a height of 90 mm, and the protrusions B are fitted with the groove G with a 1 mm gap.

[0067] S3, Evacuate, remove gas, and check for leaks in the growth furnace 100 to achieve a vacuum inside the growth furnace 100. The vacuum pressure is below 10 Pa (monitored by a pressure gauge (not shown). Evacuation and gas removal are performed alternately 2-3 times by a vacuum pump to evacuate the growth furnace 100 and to fill the growth furnace 100 with nitrogen. The vacuum port 6 for evacuation is located at the bottom of the growth furnace 100. Nitrogen is used for gas removal through the gas inlet 7 located at the top of the growth furnace 100.

[0068] S4. After step S3 is completed, the top cover 11 and the middle cylinder 12 are locked with the corresponding screws S, and the middle cylinder 12 and the base 13 are locked with the corresponding screws S. Then, the vacuum port 6 and the gas inlet 8 are closed.

[0069] S5, reopen the gas inlet 7 and fill the growth furnace 100 with a nitrogen-hydrogen mixture to bring the pressure inside the growth furnace 100 to 0.1 MPa (monitored by a pressure gauge), then close the gas inlet 7.

[0070] S6, heating of the first quartz crucible 31 is started, and the indium antimonide material 200 inside the first quartz crucible 31 is heated to melt. The heater 2 includes a graphite heater 21, a graphite double-layer heat insulation cover 22, and a carbon felt 23. The graphite heater 21 is arranged around the first quartz crucible 31, the graphite double-layer heat insulation cover 22 is arranged around the graphite heater 21, and the carbon felt 33 is filled between the inner layer 221 and the outer layer 222 of the graphite double-layer heat insulation cover 22. The heater 2 that heats the first quartz crucible 31 is the only heating device in the growth furnace 100.

[0071] S7, when the pressure inside the melt growth furnace 100, where the indium antimonide material 200 has completely melted to form a melt, rises to 0.15 MPa (monitored by a pressure gauge), the temperature of the first quartz crucible 31 is kept constant, wherein the formation of the melt is observed and confirmed through an observation window (not shown) provided in the growth furnace 100;

[0072] S8. After step S7, the crystal pulling rod 5 drives the seed crystal 4 downward to enter the hollow frustum 322 of the second quartz crucible 32 of the quartz crucible assembly 3, immersing it from the surface of the indium antimonide melt. Then, the crystal pulling rod 5 pulls upward to grow the indium antimonide crystal to form an indium antimonide crystal rod. During the indium crystal growth process, the first quartz crucible 31 and the crystal pulling rod 5 maintain opposite rotation speeds. The rotation speed of the first quartz crucible 31 is 1 rpm, and the rotation speed of the crystal pulling rod 5 is 3 rpm. The seed crystal 4 is an indium antimonide single crystal with a purity of 7N.

[0073] S9. After the crystal growth is completed, stop heating, cool down, and replace the gas in the furnace with nitrogen again through the vacuum pump via the vacuum port 6 and the gas inlet 7. Then open the growth furnace 100 and cut the crystal rod off the crystal pulling rod 5.

[0074] S10, perform EPD (Etch pits Density) detection on the crystal rod slices.

[0075] Comparative Example 1

[0076] Except for step S1, which does not use the second quartz crucible 32, step S2, which does not involve it, and step S8, which involves "the crystal pulling rod 5 driving the seed crystal 4 downward to enter the first quartz crucible 31 of the quartz crucible assembly 3", the rest is the same as in embodiment 1.

[0077] Figure 8 This is an EPD distribution diagram of dislocations on an indium antimonide crystal slice from Example 1. Based on Figure 5 The dislocation EPD distribution diagram shows that the average number of dislocations in indium antimonide crystal is 13 / cm. 2 .

[0078] Figure 9 This is the dislocation EPD distribution diagram of the indium antimonide crystal slice of Comparative Example 1. Comparative Example 1 only uses the first quartz crucible 31 (i.e., without the second quartz crucible 32), based on... Figure 9 The dislocation EPD distribution diagram shows that the average number of dislocations in indium antimonide crystal is 94 / cm. 2 .

[0079] Several exemplary embodiments have been described in detail above, but this document is not intended to limit itself to the explicitly disclosed combinations. Therefore, unless otherwise stated, the various features disclosed herein can be combined to form several other combinations, which are not shown for simplicity.

Claims

1. A quartz crucible assembly for indium antimonide crystal growth, characterized in that, The quartz crucible assembly (3) includes a first quartz crucible (31) and a second quartz crucible (32); The first quartz crucible (31) has a bottom wall (311) and a peripheral wall (312), which together form a cylindrical inner cavity (313) that is open to the top and closed on the bottom and periphery. The second quartz crucible (32) has a periphery (321) and a hollow frustum (322). The periphery (321) is cylindrical. The hollow frustum (322) is located inside the periphery (321) and is lower than the periphery (321). The hollow frustum (322) and the periphery (321) are integrally connected at the bottom to form an annular bottom surface (323). The hollow frustum (322) forms a trumpet-shaped cavity (322a) that is smaller at the top and larger at the bottom, hollow inside, and open upwards and downwards, communicating with the inner cavity (313) of the first quartz crucible (31). A sliding pair (P) is formed between the peripheral wall (312) of the first quartz crucible (31) and the peripheral portion (321) of the second quartz crucible (32), which slides relative to each other in the vertical direction and is restricted in the circumferential and radial directions. The first quartz crucible (31) is configured to hold indium antimonide material (200) for growing indium antimonide crystals by Czochralski method at the bottom of the inner cavity (313); The second quartz crucible (32) is configured to be placed inside the first quartz crucible (31), on the indium antimonide material (200) of the first quartz crucible (31), and to engage with the peripheral wall (312) of the first quartz crucible (31) via a sliding pair (P).

2. The quartz crucible assembly for indium antimonide crystal growth according to claim 1, characterized in that, One of the peripheral wall (312) of the first quartz crucible (31) and the peripheral portion (321) of the second quartz crucible (32) is provided with a protrusion (B) extending in the vertical direction. The peripheral wall (312) of the first quartz crucible (31) and the peripheral portion (321) of the second quartz crucible (32) are provided with a groove (G) extending in the vertical direction, and the groove (G) forms a sliding pair (P) with the groove (G).

3. The quartz crucible assembly for indium antimonide crystal growth according to claim 2, characterized in that, The peripheral wall (312) of the first quartz crucible (31) is provided with a groove (G); The second quartz crucible (32) has a raised strip (B) on its periphery (321), and the raised strip (B) is located at the lower part of the periphery (321) of the second quartz crucible (32).

4. The quartz crucible assembly for indium antimonide crystal growth according to claim 3, characterized in that, The groove (G) is provided along the entire height of the peripheral wall (312); The bottom surface of the ridge (B) is flush with the bottom surface (323) of the second quartz crucible (32), and the height of the ridge (B) exceeds half the height of the periphery (321) of the second quartz crucible (32). The height of the hollow frustum (322) is half the height of the periphery (321) of the second quartz crucible (32).

5. The quartz crucible assembly for indium antimonide crystal growth according to claim 4, characterized in that, The number of grooves (G) and the number of ridges (B) are both eight, and they are equally spaced along the circumference.

6. The quartz crucible assembly for indium antimonide crystal growth according to claim 5, characterized in that, The bottom wall (311) of the first quartz crucible (31) has a wall thickness of 10 mm, the height of the peripheral wall (312) of the first quartz crucible (31) is 200 mm, the wall thickness of the peripheral wall (312) of the first quartz crucible (31) is 10 mm, and the inner diameter of the peripheral wall (312) of the first quartz crucible (31) is 216 mm. The height of the periphery (321) of the second quartz crucible (32) is 150 mm, the wall thickness of the periphery (321) of the second quartz crucible (32) is 5 mm, and the outer diameter of the periphery (321) of the second quartz crucible (32) is 214 mm. The hollow frustum portion (322) of the second quartz crucible (32) has a height of 75 mm, an outer diameter of the top surface of the hollow frustum portion (322) of 150 mm, a wall thickness of 10 mm, and a cone angle of 54° for the cavity (322a) of the hollow frustum portion (322). The circumferential length of the convex rib (B) is 5mm, the radial dimension of the convex rib (B) is 5mm, the height of the convex rib (B) is 90mm, and the convex rib (B) and the groove (G) are fitted with a 1mm gap.

7. A growth furnace for growing indium antimonide crystals, characterized in that, The growth furnace (100) includes a furnace body (1), a heater (2), a quartz crucible assembly (3) according to any one of claims 1-6, a seed crystal (4), and a crystal pulling rod (5); The quartz crucible assembly (3) is supported and fixed inside the furnace body (1); The heater (2) is located inside the furnace body (1). The heater (2) is used to heat from the outside of the first quartz crucible (31) of the quartz crucible assembly (3) to form indium antimonide melt from the indium antimonide material (200) inside the first quartz crucible (31). The seed crystal (4) is fixed to the end of the crystal pulling rod (5); The crystal pulling rod (5) is set in the furnace body (1), located above the quartz crucible assembly (3) and can move back and forth in the vertical direction. The crystal pulling rod (5) is configured to drive the seed crystal (4) downward into the second quartz crucible (32) of the quartz crucible assembly (3), immerse it from the surface of the indium antimonide melt, and then the crystal pulling rod (5) is pulled upward to grow indium antimonide crystal to form an indium antimonide crystal rod.

8. The growth furnace for indium antimonide crystal growth according to claim 7, characterized in that, The furnace body (1) includes a top cover (11), a middle cylinder (12) and a base (13) arranged sequentially from top to bottom. The top cover (11) and the middle cylinder (12) are detachably assembled by screws (S), and the middle cylinder (12) and the base (13) are detachably assembled by screws (S). The growth furnace (100) also includes a vacuum port (6), which is located on the base (13); The growth furnace (100) also includes a gas inlet (7), which is located on the top cover (11); 9. The growth furnace for indium antimonide crystal growth according to claim 7, characterized in that, The heater (2) includes a graphite heater (21), a graphite double-layer insulation cover (22), and a carbon felt (23); A graphite heater (21) is arranged around the first quartz crucible (31), and a graphite double-layer heat insulation cover (22) is arranged around the graphite heater (21).

10. The growth furnace for indium antimonide crystal growth according to claim 9, characterized in that, The graphite double-layer insulation cover (22) includes an inner layer (221) and an outer layer (222); Carbon felt (23) is filled between the inner layer (221) and the outer layer (222) of the graphite double-layer insulation cover (22).

Citation Information

Patent Citations

  • Quartz crucible assembly for indium antimonide crystal growth and growth furnace

    CN222411985U