WO2020118998A1 - 一种制备高成品率晶体的生长方法及装置 - Google Patents

一种制备高成品率晶体的生长方法及装置 Download PDF

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Publication number
WO2020118998A1
WO2020118998A1 PCT/CN2019/083280 CN2019083280W WO2020118998A1 WO 2020118998 A1 WO2020118998 A1 WO 2020118998A1 CN 2019083280 W CN2019083280 W CN 2019083280W WO 2020118998 A1 WO2020118998 A1 WO 2020118998A1
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Prior art keywords
crucible
crystal
auxiliary
main
growth
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PCT/CN2019/083280
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English (en)
French (fr)
Inventor
孙聂枫
王书杰
孙同年
刘惠生
邵会民
史艳磊
Original Assignee
中国电子科技集团公司第十三研究所
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Priority claimed from CN201822103824.8U external-priority patent/CN209508451U/zh
Priority claimed from CN201811532438.9A external-priority patent/CN109487329B/zh
Application filed by 中国电子科技集团公司第十三研究所 filed Critical 中国电子科技集团公司第十三研究所
Priority to US16/627,934 priority Critical patent/US11242615B2/en
Publication of WO2020118998A1 publication Critical patent/WO2020118998A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/002—Crucibles or containers for supporting the melt
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/003—Heating or cooling of the melt or the crystallised material
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/006—Controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/14—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method characterised by the seed, e.g. its crystallographic orientation
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/002—Continuous growth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10—Crucibles or containers for supporting the melt
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
    • C30B35/002—Crucibles or containers

Definitions

  • the invention relates to the technical field of compound semiconductor single crystal growth, in particular to a growth method and device for preparing high-yield crystals.
  • VFG Vertical Gradient Freeze
  • the growth process is roughly as follows: the synthesized compound semiconductor polycrystalline material, seed crystal, sealant, etc. are put into the crucible and Sealed in the vacuum furnace body, through temperature gradient control, the polycrystal is melted and welded with the seed crystal, and the single crystal grows slowly from the seed crystal end.
  • the invention patent of 201410293610.5 discloses a R-VGF method for growing high-quality compound semiconductor single crystals. Based on the VGF method for single crystal growth, The rotation process is added to obtain a uniformly distributed radial temperature field, which is conducive to effective heat dissipation in the axial temperature field. The process method is mainly to obtain a temperature field environment suitable for the growth of high-quality single crystals.
  • the monitoring of multiple thermocouples on the right side of the hot zone is complicated.
  • the present invention provides a growth method and device for preparing high yield crystals, which uses an auxiliary crucible added to the main crucible to correct the crystals caused by twinning
  • the change of the technical scheme has achieved an increase in the overall crystal growth yield, and the processing difficulty is low and the stability is good.
  • the technical scheme adopted by the present invention is: a growth method for preparing high-yield crystals, which is prepared by using a crystal growth crucible and a matching heating furnace.
  • the crystal growth crucible structure includes a seed crystal portion and growth in sequence from bottom to top
  • the main crucible of the main part, the constricted neck and the feeding growth part and the auxiliary crucible dispersedly arranged on the constricted neck of the main crucible, the method includes feeding, evacuation, main crucible material, auxiliary crucible material, main crucible cooling 1.
  • the auxiliary crucible is cooled down and dismantled in order to remove the crystal ingot.
  • the feeding step is to put the seed crystal into the seed crystal part according to the crystal plane index (h 1 k 1 l 1 ) perpendicular to the crystal growth direction, and crush the polycrystal
  • the materials are put into the main crucible growth part, the feeding growth part and the auxiliary crucible, and then the sealant is added to control the angle between the auxiliary crucible and the center line of the main crucible is ⁇ , and the angle between the center line of the auxiliary crucible is ⁇ or ⁇ Multiple, ⁇ and ⁇ satisfy
  • (h 1 k 1 l 1 ) is the crystal plane index perpendicular to the crystal growth direction; after twinning occurs, the crystal plane perpendicular to the crystal ingot along the crystal growth direction changes to (h 2 k 2 l 2 ); (h 3 k 3 l 3 ) and (h 4 k 4 l 4 ) are the crystal plane indexes perpendicular to the crystal growth crystal plane and passing through the twinning lines on the adjacent crystal growth crystal plane.
  • the auxiliary crucible structure includes a connection portion connected to the neck of the main crucible, a branch growth portion, and a balance tube in order from the bottom to the top.
  • the top of the balance tube is higher than the neck of the crystal growth crucible.
  • 1Feeding Put the seed crystal into the seed crystal part according to the crystal plane index perpendicular to the crystal growth direction, put the polycrystalline scrap into the main crucible growth part, the feed growth part and the auxiliary crucible, and then put the sealant;
  • 3Chemical material of main crucible With the heating component of the main crucible and temperature measuring thermocouple, the main crucible forms a temperature gradient with the temperature rising from bottom to top, and the temperature at the seed crystal part is controlled to be lower than the melting point of the crystal, so that the temperature in the main crucible Polycrystalline material melting;
  • each auxiliary crucible With the help of the heating components and temperature measuring thermocouples supporting each auxiliary crucible, the temperature of each auxiliary crucible is controlled from bottom to top, so that each auxiliary crucible forms a temperature gradient from bottom to top, and the polycrystalline material in the auxiliary crucible melt;
  • the main crucible is controlled to form a temperature gradient with the temperature decreasing from bottom to top with the heating assembly of the main crucible and temperature measuring thermocouple, and the temperature at the seed crystal part is controlled to be lower than the crystal melting point;
  • Auxiliary crucibles are cooled in sequence: from bottom to top, the temperature of each auxiliary crucible is controlled in turn.
  • the auxiliary crucible is controlled to form a temperature gradient that sequentially decreases from bottom to top. Make the crystal melting point isotherms of the auxiliary crucible and the main crucible the same;
  • the invention also provides a high-yield crystal growth crucible, including a main crucible.
  • the main crucible structure includes a seed crystal part and a growth part in sequence from bottom to top.
  • the main crucible is provided with an auxiliary crucible along the circumferential direction.
  • the main crucible includes a seed crystal portion, a growth portion, a constricted neck portion, and a feed growth portion in sequence from bottom to top.
  • the auxiliary crucible is provided in the constricted neck portion of the main crucible; in the auxiliary crucible structure, from bottom to top In turn, it includes a connecting portion connected to the neck of the main crucible, a branch growth portion, and a balance tube, and the top of the balance tube is higher than the neck of the main crucible.
  • a growth method for preparing a high-yield InP crystal the method includes the following steps:
  • 1Feeding Put the seed crystal into the seed crystal part according to the crystal plane index (h 1 k 1 l 1 ) perpendicular to the crystal growth direction, and put the polycrystalline scrap into the main crucible growth part, feeding growth part and auxiliary Put the sealant into the crucible;
  • 3Chemical material of main crucible With the heating component of the main crucible and temperature measuring thermocouple, the main crucible forms a temperature gradient with the temperature rising from bottom to top, and the temperature at the seed crystal part is controlled to be lower than 1060-1065°C, so that the main crucible The polycrystalline material inside melts;
  • each auxiliary crucible With the help of the heating components and temperature measuring thermocouples supporting each auxiliary crucible, the temperature of each auxiliary crucible is controlled from bottom to top, so that each auxiliary crucible forms a temperature gradient from bottom to top, and the polycrystalline material in the auxiliary crucible melt;
  • Cooling of the main crucible control the main crucible to form a temperature gradient that sequentially decreases from bottom to top with the help of the heating component of the main crucible and temperature measuring thermocouple, and control the temperature at the seed crystal part to be lower than 1060-1065°C;
  • Auxiliary crucibles are cooled in sequence: from bottom to top, the temperature of each auxiliary crucible is controlled in turn.
  • the auxiliary crucible is controlled to form a temperature gradient that sequentially decreases from bottom to top.
  • the auxiliary crucible is the same as the 1062°C isotherm in the main crucible;
  • the crystal direction is ⁇ 100>
  • the axial direction of the auxiliary crucible is parallel to the ⁇ 011> crystal direction of the seed crystal.
  • the included angle between the center lines of the auxiliary crucibles is 90°, 180° or 360°.
  • the crystal direction is ⁇ 111>, and the angle between the center lines of the auxiliary crucibles is 60° or 120°.
  • a growth method for preparing high-yield crystals is provided, which is manufactured by a heating furnace, a crystal growth crucible and a matching control system.
  • the structure of the crystal growth crucible includes a main crucible and an auxiliary crucible, and the main crucible is from bottom to top The seed crystal part, the growth part, the constricted neck and the feeding growth part in sequence.
  • the auxiliary crucible is dispersed and arranged on the constricted neck of the main crucible.
  • the method steps are as follows: feeding, vacuuming, main crucible material, auxiliary crucible material Material, cooling of the main crucible, cooling of the auxiliary crucible and dismantling of the ingot in order.
  • the feeding step When the feeding step is carried out, put the seed crystal into the seed crystal part of the main crucible according to the crystal growth direction ⁇ h 1 k 1 l 1 >, and then In the main crucible growth part, the feeding growth part and the auxiliary crucible, polycrystalline scrap is put, and then the sealing agent is used to seal the polycrystalline material during the heating process.
  • the main concept of the invention to improve the crystal growth rate is to use the auxiliary crucible to correct the main crucible crystal
  • the twin crystal orientation generated during the growth process is based on the crystal orientation of the crystal growth in the main crucible according to different crystal types (or the crystal orientation along the crystal growth method when the seed crystal is placed), the crystal growth direction and the twin crystal orientation The relationship is achieved by controlling the angle between the auxiliary crucible and the main crucible and the relative position between the auxiliary crucible and the auxiliary crucible.
  • the seed crystal in the main crucible has a crystal plane index (h 1 k 1 l 1 ) perpendicular to the crystal growth direction Put it into the seed crystal part, put the polycrystalline scrap into the main crucible growth part, feed growth part and auxiliary crucible, and then put the sealant.
  • the angle between the auxiliary crucible and the center line of the main crucible needs to be controlled as ⁇
  • the angle between the center lines of the auxiliary crucible is ⁇ or a multiple of ⁇
  • ⁇ and ⁇ satisfy the following formula
  • (h 1 k 1 l 1 ) is the crystal plane index perpendicular to the crystal growth direction; after twinning occurs, the crystal plane perpendicular to the crystal ingot along the crystal growth direction changes to (h 2 k 2 l 2 ); (h 3 k 3 l 3 ) and (h 4 k 4 l 4 ) are the crystal plane indexes perpendicular to the crystal growth crystal plane and passing through the twinning lines on the adjacent crystal growth crystal plane.
  • the beneficial effects of the present invention are: (1) The growth method for preparing high-yield crystals provided by the present invention changes the crystal orientation change brought by twins by adding an auxiliary crucible on the main crucible, thereby realizing an increase in the finished product in the auxiliary crucible For the growth process of crystals with large probability of dislocations, this method achieves an increase in overall yield; (2) The crucible position can be customized according to the influence of twins on the crystal growth direction. It is suitable for a variety of crystal preparation processes and significantly improves the finished product. Rate, which reduces the difficulty of crystal processing and improves the utilization rate of materials.
  • FIG. 1 is a schematic structural diagram of a main crucible and an auxiliary crucible a, an auxiliary crucible b, and a supporting thermocouple in Embodiment 1 of the present invention
  • FIG. 2 is a schematic diagram of the structure of the main crucible and auxiliary crucible c, auxiliary crucible d and supporting thermocouple in Embodiment 1 of the present invention
  • FIG. 3 is a schematic diagram of the hot zone distribution of the heater supporting the main crucible in Embodiment 1 of the present invention.
  • FIG. 4 is a schematic diagram of the hot zone distribution of the auxiliary crucible a supporting heater in Embodiment 1 of the present invention
  • FIG. 5 is a schematic diagram of the hot zone distribution of the auxiliary crucible b supporting heater in Embodiment 1 of the present invention.
  • FIG. 6 is a schematic diagram of the distribution of the hot zone of the auxiliary crucible heater in Embodiment 1 of the present invention.
  • FIG. 7 is a schematic diagram of the hot zone distribution of the auxiliary crucible d supporting heater in Embodiment 1 of the present invention.
  • Example 8 is a schematic diagram of the structure of the main crucible in Example 1 of the present invention.
  • FIG. 9 is a schematic diagram of the position of the main crucible and the auxiliary crucible when the crystal growth crucible in Embodiment 1 of the present invention is viewed from above;
  • thermocouple a in the figure, 6: main crucible; 6-1: seed crystal part; 6-2: growth part; 6-3: necking down; 6-4: feeding growth part; 7: heating wire bearing layer; 8: insulation layer ; 9: heating wire; 10: seed crystal; 11: thermocouple a; 12: thermocouple b;
  • 13-1 ⁇ 14 main crucible thermocouple a ⁇ n, namely 13-1: main crucible thermocouple a; 13-2: main crucible thermocouple b; 13-3: main crucible thermocouple Couple c; 13-4: Main crucible thermocouple d; 13-5: Main crucible thermocouple e; 13-6: Main crucible thermocouple f; 13-7: Main crucible thermocouple g ; 13-8: main crucible thermocouple h; 13-9: main crucible thermocouple i; 13-10: main crucible thermocouple j; 13-11: main crucible thermocouple k; 13 -12: main crucible temperature measurement thermocouple l; 13-13: main crucible temperature measurement thermocouple m; 13-14: main crucible temperature measurement thermocouple n;
  • 15 auxiliary crucible a
  • 15-1 auxiliary crucible a growth part
  • 15-2 auxiliary crucible a balance tube
  • 14-1 ⁇ 7 auxiliary crucible a thermocouple a ⁇ g, namely 14-1: auxiliary crucible a thermocouple a; 14-2: auxiliary crucible a thermocouple b; 14-3: auxiliary crucible a temperature measuring thermocouple c; 14-4: auxiliary crucible a temperature measuring thermocouple d; 14-5: auxiliary crucible a temperature measuring thermocouple e; 14-6: auxiliary crucible a temperature measuring thermocouple f; 14-7: Auxiliary crucible a temperature measuring thermocouple g;
  • 16 auxiliary crucible b
  • 16-1 auxiliary crucible b growth part
  • 16-2 auxiliary crucible b balance tube
  • auxiliary crucible b temperature measurement thermocouple a ⁇ g namely 17-1: auxiliary crucible b temperature measurement thermocouple a; 17-2: auxiliary crucible b temperature measurement thermocouple b; 17-3: auxiliary crucible b thermocouple c; 17-4: auxiliary crucible b thermocouple d; 17-5: auxiliary crucible b thermocouple e; 17-6: auxiliary crucible b thermocouple f; 17-7: Auxiliary crucible b temperature measurement thermocouple g;
  • auxiliary crucible d temperature measurement thermocouple a ⁇ g namely 19-1: auxiliary crucible d temperature measurement thermocouple a; 19-2: auxiliary crucible d temperature measurement thermocouple b; 19-3: auxiliary crucible d temperature measuring thermocouple c; 19-4: auxiliary crucible d temperature measuring thermocouple d; 19-5: auxiliary crucible d temperature measuring thermocouple e; 19-6: auxiliary crucible d temperature measuring thermocouple f; 19-7: Auxiliary crucible d temperature measuring thermocouple g;
  • 20-1 ⁇ 6 auxiliary crucible c temperature measuring thermocouple a ⁇ f, namely 20-1: auxiliary crucible c temperature measuring thermocouple a; 20-2: auxiliary crucible c temperature measuring thermocouple b; 20-3: auxiliary crucible c temperature measuring thermocouple c; 20-4: auxiliary crucible c temperature measuring thermocouple d; 20-5: auxiliary crucible c temperature measuring thermocouple e; 20-6: auxiliary crucible c temperature measuring thermocouple f;
  • 21 auxiliary crucible c
  • 21-1 auxiliary crucible c growth part
  • 21-2 auxiliary crucible c balance tube
  • auxiliary crucible d 22: auxiliary crucible d; 22-1: auxiliary crucible d growth part; 22-2: auxiliary crucible d balance tube.
  • a crystal growth furnace, crucible and supporting heating components, control system, etc. are used.
  • the core of this method is to increase the auxiliary crucible on the main crucible to correct the crystal orientation change caused by twinning, so as to achieve the overall crystal growth finished product The rate of increase. That is, an auxiliary crucible is added to the main crucible, and a heating component, a temperature measuring thermocouple and other structures are provided.
  • the specific structure of the device is as follows:
  • the crystal growth crucible includes a main crucible 6 and an auxiliary crucible, which are respectively equipped with heating components and temperature measuring thermocouples.
  • the structure of the main crucible 6 is shown in FIG. 8, and the seed crystal part 6 is arranged from bottom to top -1, the growth part 6-2, the constricted neck 6-3 and the feeding growth part 6-4, the arrangement of the constricted neck 6-3 is conducive to improving the utilization rate of crystal materials and improving the growth stability of crystals.
  • the auxiliary crucible is distributed on the constricted neck 6-3 of the main crucible 6 in a dendritic shape.
  • the crystal plane index of the seed crystal 10 perpendicular to the crystal growth direction in the main crucible 6 is (h 1 k 1 l 1 ).
  • the angle between is ⁇
  • the angle between the center lines of the auxiliary crucible is ⁇ or a multiple of ⁇
  • ⁇ and ⁇ satisfy the following formula
  • the crystal plane perpendicular to the ingot along the crystal growth direction is transformed into (h 2 k 2 l 2 ); (h 3 k 3 l 3 ) and (h 4 k 4 l 4 ) are perpendicular to the crystal The crystal plane index of the growing crystal plane passing through the twins on the adjacent crystal growth crystal plane.
  • the twin crystals can be grown in the auxiliary crucible according to the design crystal direction.
  • Auxiliary crucibles can be provided with multiple or multiple layers, such as 2, 4, 8 etc., in the height direction of the constriction of the main crucible 6.
  • the structure of the auxiliary crucible includes, from bottom to top, a connection part connected to the neck 6-3 of the main crucible 6, a branch growth part, and a balance tube, and the top of the balance tube is higher than the neck of the crystal growth crucible 6
  • the connection section and the branch growth section are used to grow crystals
  • the balance tube prevents the formation of pores or voids that cannot be eliminated by the gas in the branch growth section, thereby growing continuous crystals.
  • the preparation of InP crystals is taken as an example.
  • the crystal orientation is ⁇ 100> when the seed crystal is placed, the growth direction of the InP crystal is ⁇ 100>, the twin crystals appear in the ⁇ 110> crystal direction, and the center line of the auxiliary crucible ⁇ 011> crystal direction parallel to the seed crystal, ⁇ 100> and ⁇ 110> are 90°, the angle between the center lines of the auxiliary crucibles is 90° or 180° or 360°, this embodiment is provided with an auxiliary crucible a15, auxiliary crucible b16, auxiliary crucible c21 and auxiliary crucible d22, a total of 90° between the center lines of auxiliary crucibles, see Figure 9 for the top view;
  • the auxiliary crucible structure includes the main Crucible 6 shrink neck 6-3 connection part, branch growth part and balance tube, the growth part is used to grow crystals, and the branch growth part is also used to grow crystals, but it can grow in accordance with the crystal direction after twins appear
  • the balance tube is mainly to prevent
  • Auxiliary crucible a15 is provided with auxiliary crucible a growth part 15-1 and auxiliary crucible a balance tube 15-2; auxiliary crucible b is provided with auxiliary crucible b growth part 16-1 and auxiliary crucible b balance tube 16-2; auxiliary crucible c 21 Auxiliary crucible c growth part 21-1 and auxiliary crucible c balance tube 21-2 are provided; auxiliary crucible d is provided with auxiliary crucible d growth part 22-1 and auxiliary crucible d balance tube 22-2; the top of the balance tube is higher than The crystal growth crucible 6 shrinks the neck 6-3, as shown in Figure 4-7.
  • the main crucible 6 and the auxiliary crucible are provided with heating components and temperature measuring thermocouples on the periphery of the crucible respectively. See Figure 1-7.
  • the main crucible 6 is provided with a heating wire around the periphery and is divided into 13 main shown in Figure 3 according to the heating area.
  • the heating wires arranged around the auxiliary crucible a 15 are divided into 5 heating zones according to the area, and the heating zones a to e of the auxiliary crucible a are represented by 3-1 to 5, respectively; there are temperature measuring thermocouples in each heating zone, respectively 14 -1 ⁇ 7 indicate the auxiliary crucible a temperature measurement thermocouple a ⁇ g.
  • the heating wires arranged around the auxiliary crucible d22 are divided into 5 heating zones according to the area, and the heating zones a to e of the auxiliary crucible d are represented by 5-1 to 5, respectively; there are temperature measuring thermocouples in each heating zone, respectively 19 -1 to 7 indicate the auxiliary crucible d temperature measurement thermocouple a to f.
  • the heating wires arranged around the auxiliary crucible b16 are divided into 5 heating zones according to the area, and the heating zones a to e of the auxiliary crucible b are represented by 2-1 to 5 respectively; there are temperature measuring thermocouples in each heating zone, respectively 17 -1 ⁇ 7 indicate auxiliary crucible b temperature measurement thermocouple a ⁇ g.
  • the heating wires arranged around the auxiliary crucible 21 are divided into 5 heating zones according to the area, and the heating zones a to e of the auxiliary crucible c are represented by 4-1 to 5, respectively; there are temperature measuring thermocouples in each heating zone, respectively 20 -1 ⁇ 6 indicate the auxiliary crucible c temperature measuring thermocouple a ⁇ g.
  • the method for preparing high-yield InP crystals includes the following steps:
  • Feeding Put the seed crystal 10 into the seed crystal section 6-1 of the main crucible 6 according to the crystal growth direction ⁇ 100>, and put the polycrystalline scrap into the growth section 6 of the main crucible 6 through the feed growth section 6-4 -2. Feeding growth section 6-4 and auxiliary crucible a15, auxiliary crucible b16, auxiliary crucible c21 and auxiliary crucible d22, respectively, then add sealant separately.
  • the total sealant uses boron oxide 18, and put boron oxide 18 separately Enter the main crucible 6, auxiliary crucible a balance tube 15-2, auxiliary crucible b balance tube 16-2, auxiliary crucible c balance tube 21-2 and auxiliary crucible d balance tube 22-2, and ensure that boron oxide 18 melts in each The thickness in the crucible is approximately equal;
  • each auxiliary crucible With the help of the heating components and temperature measuring thermocouples supporting each auxiliary crucible, the temperature of each auxiliary crucible is controlled from bottom to top, so that each auxiliary crucible forms a temperature gradient from bottom to top, and the polycrystalline material in the auxiliary crucible Melting; specifically, the heating control process of the four auxiliary crucibles is as follows:
  • thermocouple g14-7 By controlling heating zone a3-1 of auxiliary crucible a15, heating zone b3-2 of auxiliary crucible a, heating zone c3-3 of auxiliary crucible a, heating zone d3-4 of auxiliary crucible a, heating of auxiliary crucible a Zone e3-5 corresponds to the power of the heating wire and controls the melting of the polycrystalline material in the auxiliary crucible a15, so that the main crucible thermocouple e13-5, the auxiliary crucible a thermocouple a14-1, and the thermocouple b14-2 , Auxiliary crucible a thermocouple c14-3, auxiliary crucible a thermocouple d14-4, auxiliary crucible a thermocouple e14-5, auxiliary crucible a thermocouple f14-6, auxiliary crucible a thermocouple The temperature of thermocouple g14-7 rises in turn;
  • the heating zone e5-5 corresponds to the power of the heating wire, and controls the melting of the polycrystalline material in the auxiliary crucible d22, so that the main crucible thermocouple g13-7, the auxiliary crucible thermocouple a19-1, and the auxiliary crucible d thermocouple Couple b19-2, auxiliary crucible d thermocouple c19-3, auxiliary crucible d thermocouple d19-4, auxiliary crucible d thermocouple e19-5, auxiliary crucible d thermocouple f19-6, auxiliary The temperature of crucible d thermocouple g19-7 rises in turn;
  • the heating zone e2-5 corresponds to the power of the heating wire and controls the melting of the polycrystalline material in the auxiliary crucible b16, so that the main crucible temperature measuring thermocouple i13-9, the auxiliary crucible b temperature measuring thermocouple a17-1, the auxiliary crucible b temperature measuring heat Couple b17-2, auxiliary crucible b thermocouple c17-3, auxiliary crucible b thermocouple d17-4, auxiliary crucible b thermocouple e17-5, auxiliary crucible b thermocouple f17-6, auxiliary The temperature of the crucible b thermocouple g17-7 rises in turn;
  • the heating zone e4-5 corresponds to the power of the heating wire and controls the melting of the polycrystalline material in the auxiliary crucible c21, so that the main crucible thermocouple j13-10, the auxiliary crucible c thermocouple a20-1, and the auxiliary crucible c thermostat Couple b20-2, auxiliary crucible c thermocouple c20-3, auxiliary crucible c thermocouple d20-4, auxiliary crucible c thermocouple e20-5, auxiliary crucible c thermocouple f20-6 temperature Increase in turn.
  • Cooling of the main crucible 6 The main crucible 6 is controlled to form a temperature gradient with the temperature decreasing from the bottom to the top by means of the heating component of the main crucible 6 and the thermocouple, and the temperature at the seed crystal section 6-1 is controlled to be lower than the melting point of InP; , Control the main heating zone a1-1, main heating zone b1-2, main heating zone c1-3, main heating zone d1-4, main heating zone e1-5, main heating zone f1-6, main heating zone g1- 7.
  • Auxiliary crucibles are cooled in sequence: from bottom to top, the temperature of each auxiliary crucible is controlled in turn.
  • the auxiliary crucible is controlled to form a temperature gradient that sequentially decreases from the bottom to the top, so that the auxiliary
  • the 1062°C isotherm in the crucible is the same as the 1062°C isotherm in the main crucible 6; specifically,
  • the heating zone d3-4 of the auxiliary crucible a and the heating zone e3-5 of the auxiliary crucible a correspond to the power of the heating wire, so that the temperature measurement thermocouple a14-1 of the auxiliary crucible a, the temperature couple b14-2, and the auxiliary crucible a Thermocouple c14-3, auxiliary crucible a thermocouple d14-4, auxiliary crucible a thermocouple e14-5, auxiliary crucible a thermocouple f14-6, auxiliary crucible a thermocouple g14-7 The temperature decreases in turn.
  • the 1062°C isotherm in the auxiliary crucible a15 is approximately the same as the 1062°C isotherm in the main crucible 6;
  • thermocouple g13-7 By analogy, after the main crucible temperature measuring thermocouple g13-7 is lower than 1062°C, by adjusting the heating zone a5-1 of auxiliary crucible d22, heating zone b5-2 of auxiliary crucible d, heating zone of auxiliary crucible d c5-3, auxiliary crucible d heating zone d5-4, auxiliary crucible d heating zone e5-5 corresponds to the heating wire power, so that auxiliary crucible d temperature measuring thermocouple a19-1, auxiliary crucible d temperature measuring thermocouple b19- 2.
  • thermocouple g19-7 Auxiliary crucible d thermocouple c19-3, auxiliary crucible d thermocouple d19-4, auxiliary crucible d thermocouple e19-5, auxiliary crucible d thermocouple f19-6, auxiliary crucible d
  • the temperature of the thermocouple g19-7 decreases sequentially.
  • thermocouple e13-9 is lower than 1062°C
  • the heating zone a2-1 of auxiliary crucible b16, heating zone b2-2 of auxiliary crucible b, heating zone of auxiliary crucible b c2-3, the heating zone d2-4 of the auxiliary crucible b, the heating zone e2-5 of the auxiliary crucible b correspond to the power of the heating wire, so that the main crucible temperature measuring thermocouple i13-9, the auxiliary crucible b temperature measuring thermocouple a17-1 , Auxiliary crucible b thermocouple b17-2, auxiliary crucible b thermocouple c17-3, auxiliary crucible b thermocouple d17-4, auxiliary crucible b thermocouple e17-5, auxiliary crucible b thermocouple The temperature of the thermocouple f17-6 and the auxiliary crucible b temperature measurement thermocouple g17-7 decrease
  • thermocouple j13-10 is lower than 1062°C
  • heating zone a4-1 of auxiliary crucible c21, heating zone b4-2 of auxiliary crucible c, heating zone of auxiliary crucible c c4-3, auxiliary crucible c heating zone d4-4, auxiliary crucible c heating zone e4-5 corresponds to the heating wire power, so that auxiliary crucible c temperature measuring thermocouple a20-1, auxiliary crucible c temperature measuring thermocouple b20- 2.
  • auxiliary crucible c thermocouple c20-3, auxiliary crucible c thermocouple d20-4, auxiliary crucible c thermocouple e20-5, auxiliary crucible c thermocouple f20-6 decrease in turn.
  • thermocouple n13-14 Auxiliary crucible a thermocouple g14-7, auxiliary crucible b thermocouple g17-7, auxiliary crucible d thermocouple f20-6, auxiliary crucible c thermocouple g19-7 are all lower than 1062°C. Slowly lower the temperature to room temperature, dismantle the furnace and take out the crystal ingot.
  • Example 1 differs from Example 1 in that no auxiliary crucible is provided.
  • Example 1 Comparing the products of Example 1 and the comparative example, it was found that the InP crystal prepared in Example 1 had a yield of 32%, and the comparative example had a yield of about 11.4%. It has been found through multiple experiments that the crystal yield prepared by the method of the present invention Increased to more than 30%, compared with the current common crucible, single crucible crystal growth yield of about 10%, increased by more than 3 times, economic efficiency is very high, and the equipment is simple, easy to control, suitable for industrial production.

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Abstract

本发明提供一种制备高成品率晶体的生长方法，属于单晶生长技术领域，通过根据不同晶体类型、依据主坩埚中晶体生长的晶向、晶体生长方向与孪晶晶向的关系，在坩埚上设置辅助坩埚，控制辅助坩埚与主坩埚之间的角度、辅助坩埚与辅助坩埚之间的相对位置来实现以辅助坩埚矫正主坩埚晶体生长过程中产生的孪晶晶向。有益效果是本发明提供的制备高成品率晶体的生长方法，通过主坩埚上增加的辅助坩埚来改变孪晶带来的晶向改变，对于大概率位错晶体生长过程，该方法实现了总体成品率的提高；可以依据孪晶对晶体生长方向的影响定制设计坩埚位置，适用于多种晶体制备工艺，显著提高成品率，减少了晶体加工难度，提高了材料的利用率。

Description

一种制备高成品率晶体的生长方法及装置 技术领域
本发明涉及化合物半导体单晶生长技术领域，具体涉及一种制备高成品率晶体的生长方法及装置。
背景技术
垂直温度梯度凝固法(Vertical Gradient Freeze,简称VGF)是制备高品质磷化铟晶体的优选方法，其生长过程大致如下：将合成好的化合物半导体多晶料及籽晶、密封剂等装入坩埚并密封在抽真空的炉体中，通过温度梯度控制，使多晶熔化后与籽晶进行熔接，单晶从籽晶端向上缓慢生长，在实际晶体生产中，需有序、精确控制升温化料、温度保持、缓慢降温等过程，由于装置、控制及传到、对流、辐射等，热场极其复杂，控制难度大，尤其是对于磷化铟等的单晶生长过程，由于其离解压高，需高温高压生长环境，而其层错能低，非常容易出现孪晶缺陷，同时，其临界剪切应力小，使得制备高质量磷化铟晶体非常困难，由于孪晶出现几率高，造成成品率低，成本居高不下，对其在光纤通讯、微电子、太阳能领域的广泛应用带来了限制。
提高晶体生长成品率是单晶生长领域一直致力研究的热点和难点，201410293610.5的发明专利公开了一种R-VGF法生长高质量化合物半导体单晶工艺，在VGF法单晶生长工艺的基础上，加入旋转工艺，从而获得均匀分布的径向温场，有利于轴向温场进行有效散热，其工艺方法主要在于获得适宜高质量单晶生长的温场环境，但在实际应用中，由于每个热区右多个热偶监控，线路较复杂，另一方面，由于旋转，造成坩埚、炉体等位置对中性出现偏差的几率增大，反而降低了成品率，还造成产品一致性较差。因此，研究开发稳定性好、成品率高的单晶生长方法及配套装置是本领域急需解决的技术问题。
发明内容
为解决现有VGF法单晶生长成品率低、成本高的技术问题，本发明提供一种制备高成品率晶体的生长方法及装置，采用在主坩埚上增加辅助坩埚从而矫正孪晶引起的晶向改变的技术方案，实现了总体晶体生长成品率的提高，且加工难度低、稳定性好。
本发明采用的技术方案是：一种制备高成品率晶体的生长方法，采用晶体生长坩埚及配套的加热炉制备，所述晶体生长坩埚结构中包括由下往上依次设有籽晶部、生长部、缩颈部及投料生长部的主坩埚和分散设置在主坩埚的缩颈部上的辅助坩埚，所述方法依次包括投料、抽真空、主坩埚化料、辅助坩埚化料、主坩埚降温、辅助坩埚依次降温和拆炉去除晶 锭，所述投料步骤为将籽晶按与晶体生长方向垂直的晶面指数为(h 1 k 1 l 1)放入至籽晶部，将多晶碎料分别投入至主坩埚生长部、投料生长部及辅助坩埚中，再投入密封剂，控制辅助坩埚与主坩埚中心线的夹角为θ，辅助坩埚中心线之间的夹角为φ或φ的倍数，θ、φ满足
cos θ＝∣(h 1h 2+k 1k 2+l 1l 2)∣/[(h 1 2+l 1 2+k 1 2)(h 2 2+l 2 2+k 2 2)] 0.5，
cos φ＝∣(h 3h 4+k 3k 4+l 3l 4)∣/[(h 3 2+l 3 2+k 3 2)(h 4 2+l 4 2+k 4 2)] 0.5
其中，(h 1 k 1 l 1)为与晶体生长方向垂直的晶面指数；出现孪晶后，与晶锭沿晶体生长方向垂直的晶面转变为(h 2 k 2 l 2)；(h 3 k 3 l 3)和(h 4 k 4 l 4)为垂直于晶体生长晶面、且经过相邻晶体生长晶面上的孪晶线的晶面指数。
进一步的，所述辅助坩埚结构中由下至上依次包括与主坩埚缩颈部连接的连接部、分支生长部和平衡管，所述平衡管顶端高于晶体生长坩埚缩颈部。
进一步的，所述方法步骤具体如下：
①投料：将籽晶按与晶体生长方向垂直的晶面指数为放入至籽晶部，将多晶碎料分别投入至主坩埚生长部、投料生长部及辅助坩埚中，再投入密封剂；
②抽真空：对炉体抽真空，冲入惰性气体至1.8-2.5MPa；
③主坩埚化料：借助主坩埚的加热组件及测温热偶使主坩埚形成由下至上温度依次升高的温度梯度，且控制籽晶部处的温度低于晶体熔点，使主坩埚内的多晶料熔化；
④辅助坩埚化料：借助各辅助坩埚配套的加热组件及测温热偶由下至上依次控制各辅助坩埚升温，使各辅助坩埚形成由下至上升温的温度梯度，使辅助坩埚内的多晶料熔化；
⑤主坩埚降温：借助主坩埚的加热组件及测温热偶控制主坩埚形成由下至上温度依次降低的温度梯度，且控制籽晶部处的温度低于晶体熔点；
⑥辅助坩埚依次降温：由下至上，依次控制使各辅助坩埚降温，在辅助坩埚与主坩埚(6)连接处温度低于晶体熔点时，控制辅助坩埚形成由下至上温度依次降低的温度梯度，使辅助坩埚与主坩埚内晶体熔点等温线相同；
⑦当各辅助坩埚平衡管处温度均低于晶体熔点时，控制加热组件使主坩埚、辅助坩埚缓慢降温至室温，拆炉去除晶锭。
本发明还提供一种高成品率晶体生长坩埚，包括主坩埚，所述主坩埚结构由下往上依次包括籽晶部、生长部，主坩埚上沿周向呈设置有辅助坩埚。
进一步的，所述辅助坩埚与主坩埚中心线的夹角为θ，cosθ＝∣(h 1h 2+k 1k 2+l 1l 2)∣/[(h 1 2+l 1 2+k 1 2)(h 2 2+l 2 2+k 2 2)] 0.5，其中，h 1 k 1 l 1 h 2 k 2 l 2为晶面指数，与晶体生长方向垂直的晶面为(h 1 k 1 l 1)；出现孪晶后，与晶锭沿晶体生长方向垂直的晶面转变为(h 2 k 2 l 2)。
进一步的，所述主坩埚由下往上依次包括籽晶部、生长部、缩颈部及投料生长部，所述辅助坩埚设置在主坩埚的缩颈部；所述辅助坩埚结构中由下至上依次包括与主坩埚缩颈部连接的连接部、分支生长部和平衡管，所述平衡管顶端高于主坩埚的缩颈部。
进一步的，所述辅助坩埚中心线之间的夹角为φ或φ的倍数，cos φ＝∣(h 3h 4+k 3k 4+l 3l 4)∣/[(h 3 2+l 3 2+k 3 2)(h 4 2+l 4 2+k 4 2)] 0.5，其中，(h 3 k 3 l 3)和(h 4 k 4 l 4)为垂直于晶体生长晶面、且经过相邻晶体生长晶面上的孪晶线的晶面指数。一种制备高成品率InP晶体的生长方法，所述方法包括以下步骤：
①投料：将籽晶按与晶体生长方向垂直的晶面指数为(h 1 k 1 l 1)放入至籽晶部，将多晶碎料分别投入至主坩埚生长部、投料生长部及辅助坩埚中，再投入密封剂；
②抽真空：对炉体抽真空，冲入惰性气体至1.8-2.5MPa；
③主坩埚化料：借助主坩埚的加热组件及测温热偶使主坩埚形成由下至上温度依次升高的温度梯度，且控制籽晶部处的温度低于1060-1065℃，使主坩埚内的多晶料熔化；
④辅助坩埚化料：借助各辅助坩埚配套的加热组件及测温热偶由下至上依次控制各辅助坩埚升温，使各辅助坩埚形成由下至上升温的温度梯度，使辅助坩埚内的多晶料熔化；
⑤主坩埚降温：借助主坩埚的加热组件及测温热偶控制主坩埚形成由下至上温度依次降低的温度梯度，且控制籽晶部处的温度低于1060-1065℃；
⑥辅助坩埚依次降温：由下至上，依次控制使各辅助坩埚降温，在辅助坩埚与主坩埚连接处温度低于1060-1065℃时，控制辅助坩埚形成由下至上温度依次降低的温度梯度，使辅助坩埚与主坩埚内1062℃等温线相同；
⑦当各辅助坩埚平衡管处温度均低于晶体熔点时，控制加热组件使主坩埚、辅助坩埚缓慢降温至室温，拆炉去除晶锭。
进一步的，所述投料步骤中籽晶放入时晶向为<100>，所述辅助坩埚轴向平行于籽晶的<011>晶向。
进一步的，所述辅助坩埚中心线之间的夹角为90°或180°或360°。
进一步的，所述投料步骤中籽晶放入时晶向为<111>，所述辅助坩埚中心线之间的夹角为60°或120°。
上述技术方案中，提供一种制备高成品率晶体的生长方法，通过加热炉、晶体生长坩埚及配套的控制系统制作，晶体生长坩埚的结构中包括主坩埚和辅助坩埚，主坩埚由下往上依次是籽晶部、生长部、缩颈部及投料生长部，辅助坩埚分散设置在主坩埚的缩颈部上，所述方法步骤依次如下：投料、抽真空、主坩埚化料、辅助坩埚化料、主坩埚降温、辅助坩 埚依次降温和拆炉去除晶锭，投料步骤进行时，将籽晶按晶体生长晶向<h 1 k 1 l 1>放入至主坩埚的籽晶部，再向主坩埚生长部、投料生长部及辅助坩埚中投入多晶碎料，然后再投入密封剂用于加热过程中密封多晶料，本发明提高晶体生长率的主要构思在于采用辅助坩埚矫正主坩埚晶体生长过程中产生的孪晶晶向，通过根据不同晶体类型、依据主坩埚中晶体生长的晶向(或籽晶放入时沿晶体生长方法的晶向)、晶体生长方向与孪晶晶向的关系，控制辅助坩埚与主坩埚之间的角度、辅助坩埚与辅助坩埚之间的相对位置来实现，主坩埚中籽晶按与晶体生长方向垂直的晶面指数为(h 1 k 1 l 1)放入至籽晶部，将多晶碎料分别投入至主坩埚生长部、投料生长部及辅助坩埚中，再投入密封剂，该情况下，需控制辅助坩埚与主坩埚中心线的夹角为θ，辅助坩埚中心线之间的夹角为φ或φ的倍数，θ、φ满足下述公式
cos θ＝∣(h 1h 2+k 1k 2+l 1l 2)∣/[(h 1 2+l 1 2+k 1 2)(h 2 2+l 2 2+k 2 2)] 0.5，
cos φ＝∣(h 3h 4+k 3k 4+l 3l 4)∣/[(h 3 2+l 3 2+k 3 2)(h 4 2+l 4 2+k 4 2)] 0.5
来实现矫正。
其中，(h 1 k 1 l 1)为与晶体生长方向垂直的晶面指数；出现孪晶后，与晶锭沿晶体生长方向垂直的晶面转变为(h 2 k 2 l 2)；(h 3 k 3 l 3)和(h 4 k 4 l 4)为垂直于晶体生长晶面、且经过相邻晶体生长晶面上的孪晶线的晶面指数。
本发明的有益效果是：(1)本发明提供的制备高成品率晶体的生长方法，通过主坩埚上增加的辅助坩埚来改变孪晶带来的晶向改变，实现了在辅助坩埚中增加成品晶体，对于大概率位错晶体生长过程，该方法实现了总体成品率的提高；(2)可以依据孪晶对晶体生长方向的影响定制设计坩埚位置，适用于多种晶体制备工艺，显著提高成品率，减少了晶体加工难度，提高了材料的利用率。
附图说明
图1为本发明实施例1中主坩埚与辅助坩埚a、辅助坩埚b及配套热偶的结构示意图；
图2为本发明实施例1中主坩埚与辅助坩埚c、辅助坩埚d及配套热偶的结构示意图；
图3为本发明实施例1中主坩埚配套加热器的热区分布示意图；
图4为本发明实施例1中辅助坩埚a配套加热器的热区分布示意图；
图5为本发明实施例1中辅助坩埚b配套加热器的热区分布示意图；
图6为本发明实施例1中辅助坩埚c配套加热器的热区分布示意图；
图7为本发明实施例1中辅助坩埚d配套加热器的热区分布示意图；
图8为本发明实施例1中主坩埚结构示意图；
图9为本发明实施例1中晶体生长坩埚俯视时主坩埚与辅助坩埚位置示意图；
图中，6：主坩埚；6-1：籽晶部；6-2：生长部；6-3：缩颈部；6-4：投料生长部；7：加热丝承载层；8：保温层；9：加热丝；10：籽晶；11：热偶a；12：热偶b；
13-1～14：主坩埚测温热偶a～n，即13-1：主坩埚测温热偶a；13-2：主坩埚测温热偶b；13-3：主坩埚测温热偶c；13-4：主坩埚测温热偶d；13-5：主坩埚测温热偶e；13-6：主坩埚测温热偶f；13-7：主坩埚测温热偶g；13-8：主坩埚测温热偶h；13-9：主坩埚测温热偶i；13-10：主坩埚测温热偶j；13-11：主坩埚测温热偶k；13-12：主坩埚测温热偶l；13-13：主坩埚测温热偶m；13-14：主坩埚测温热偶n；
15：辅助坩埚a；15-1：辅助坩埚a生长部；15-2：辅助坩埚a平衡管；
14-1～7：辅助坩埚a测温热偶a～g，即14-1：辅助坩埚a测温热偶a；14-2：辅助坩埚a测温热偶b；14-3：辅助坩埚a测温热偶c；14-4：辅助坩埚a测温热偶d；14-5：辅助坩埚a测温热偶e；14-6：辅助坩埚a测温热偶f；14-7：辅助坩埚a测温热偶g；
16：辅助坩埚b；16-1：辅助坩埚b生长部；16-2：辅助坩埚b平衡管；
17-1～7：辅助坩埚b测温热偶a～g，即17-1：辅助坩埚b测温热偶a；17-2：辅助坩埚b测温热偶b；17-3：辅助坩埚b测温热偶c；17-4：辅助坩埚b测温热偶d；17-5：辅助坩埚b测温热偶e；17-6：辅助坩埚b测温热偶f；17-7：辅助坩埚b测温热偶g；
18：氧化硼；
19-1～7：辅助坩埚d测温热偶a～g，即19-1：辅助坩埚d测温热偶a；19-2：辅助坩埚d测温热偶b；19-3：辅助坩埚d测温热偶c；19-4：辅助坩埚d测温热偶d；19-5：辅助坩埚d测温热偶e；19-6：辅助坩埚d测温热偶f；19-7：辅助坩埚d测温热偶g；
20-1～6：辅助坩埚c测温热偶a～f，即20-1：辅助坩埚c测温热偶a；20-2：辅助坩埚c测温热偶b；20-3：辅助坩埚c测温热偶c；20-4：辅助坩埚c测温热偶d；20-5：辅助坩埚c测温热偶e；20-6：辅助坩埚c测温热偶f；
21：辅助坩埚c；21-1：辅助坩埚c生长部；21-2：辅助坩埚c平衡管；
22：辅助坩埚d；22-1：辅助坩埚d生长部；22-2：辅助坩埚d平衡管。
各坩埚热区标号：1-1：主加热区a；1-2：主加热区b；1-3：主加热区c；1-4：主加热区d；1-5：主加热区e；1-6：主加热区f；1-7：主加热区g；1-8：主加热区h；1-9：主加热区i；1-10：主加热区j；1-11：主加热区k；1-12：主加热区l；1-13：主加热区m；3-1：辅助坩埚a的加热区a；3-2：辅助坩埚a的加热区b；3-3：辅助坩埚a的加热区c；3-4：辅助坩埚a的加热区d；3-5：辅助坩埚a的加热区e；
2-1：辅助坩埚b的加热区a；2-2：辅助坩埚b的加热区b；2-3：辅助坩埚b的加热区c；2-4：辅助坩埚b的加热区d；2-5：辅助坩埚b的加热区e；
4-1：辅助坩埚c的加热区a；4-2：辅助坩埚c的加热区b；4-3：辅助坩埚c的加热区c；4-4：辅助坩埚c的加热区d；4-5：辅助坩埚c的加热区e；
5-1：辅助坩埚d的加热区a；5-2：辅助坩埚d的加热区b；5-3：辅助坩埚d的加热区c；5-4：辅助坩埚d的加热区d；5-5：辅助坩埚d的加热区e。
具体实施方式
以下以具体实施例详细说明本发明所提供的一种制备高成品率晶体的生长方法及装置，但不以任何形式限制本发明的保护范围，所属领域技术人员根据技术方案所进行的改善修改或者类似替换，均应包含在本发明的保护范围之内。
实施例1
制备高成品率晶体，采用晶体生长炉、坩埚及配套的加热组件、控制系统等，本方法核心在于利用在主坩埚上增加辅助坩埚从而矫正孪晶引起的晶向改变，从而实现总体晶体生长成品率的提高。即在主坩埚上增加辅助坩埚，配套设置加热组件、测温热偶等结构，装置结构具体如下：
参见图1-8所示，晶体生长坩埚包括主坩埚6和辅助坩埚，分别配套有加热组件、测温热偶，主坩埚6结构参见图8所示，由下往上依次为籽晶部6-1、生长部6-2、缩颈部6-3和投料生长部6-4，缩颈部6-3的设置有利于提高晶体材料利用率及提高晶体的生长稳定性。辅助坩埚呈树枝状分散设置在主坩埚6的缩颈部6-3上，辅助坩埚与主坩埚6的相对位置及辅助坩埚的位置，主要取决于晶体类型、主坩埚6中晶体生长的晶向(籽晶方向)与孪晶晶向的关系，主坩埚6中籽晶10与晶体生长方向垂直的晶面指数为(h 1 k 1 l 1)放置，则需控制辅助坩埚与主坩埚中心线的夹角为θ，辅助坩埚中心线之间的夹角为φ或φ的倍数，θ、φ满足下述公式
cos θ＝∣(h 1h 2+k 1k 2+l 1l 2)∣/[(h 1 2+l 1 2+k 1 2)(h 2 2+l 2 2+k 2 2)] 0.5，
cos φ＝∣(h 3h 4+k 3k 4+l 3l 4)∣/[(h 3 2+l 3 2+k 3 2)(h 4 2+l 4 2+k 4 2)] 0.5
其中，出现孪晶后，与晶锭沿晶体生长方向垂直的晶面转变为(h 2 k 2 l 2)；(h 3 k 3 l 3)和(h 4 k 4 l 4)为垂直于晶体生长晶面、且经过相邻晶体生长晶面上的孪晶线的晶面指数。
辅助坩埚按照角度θ和φ布置后，可以实现孪晶晶体在辅助坩埚中按着设计晶向进行生长。辅助坩埚可在主坩埚6的缩颈部沿高度方向设置多个、多层，如2个、4个、8个等。
所述辅助坩埚的结构优选的是，由下至上依次包括与主坩埚6缩颈部6-3连接的连接部、分支生长部和平衡管，所述平衡管顶端高于晶体生长坩埚6缩颈部6-3，连接部、分支生长部均用于生长晶体，平衡管可防止在分支生长部气体无法排除所形成气孔或者空洞，从而生长连续晶体。本实施例以制备InP晶体为例，投料步骤中籽晶放入时晶向为<100>，InP晶体生长方向为<100>，孪晶出现在<110>晶向上，所述辅助坩埚中心线平行于籽晶的<011>晶向，<100>与<110>成90°，所述辅助坩埚中心线之间的夹角为90°或180°或360°，本实施例设置有辅助坩埚a15、辅助坩埚b16、辅助坩埚c21和辅助坩埚d22共4个，辅助坩埚中心线之间互成90°设置，俯视图参见附图9所示；所述辅助坩埚结构中由下至上依次包括与主坩埚6缩颈部6-3连接的连接部、分支生长部和平衡管，生长部用于生长晶体，分支生长部也用于生长晶体，但是其可以在出现孪晶后在生长出符合晶向要求的晶体，平衡管主要是防止在分支生长部气体无法排出，形成气孔或者孔洞。辅助坩埚a15设有辅助坩埚a生长部15-1和辅助坩埚a平衡管15-2；辅助坩埚b设有辅助坩埚b生长部16-1和辅助坩埚b平衡管16-2；辅助坩埚c 21设有辅助坩埚c生长部21-1和辅助坩埚c平衡管21-2；辅助坩埚d设有辅助坩埚d生长部22-1和辅助坩埚d平衡管22-2；所述平衡管顶端高于晶体生长坩埚6缩颈部6-3，如图4-7所示。
主坩埚6、辅助坩埚分别在坩埚外围设置加热组件、测温热偶，参见图1-7所示，主坩埚6外围设置加热丝，并根据加热区域不同分为图3所示的13个主加热区，分别以1-1～13表示主加热区a～m；在各加热区设有测温热偶，参见图1所示，分别以13-1～14表示主坩埚测温热偶a～n。
辅助坩埚a 15外围设置的加热丝根据区域分为5个加热区，分别以3-1～5表示辅助坩埚a的加热区a～e；在各加热区设有测温热偶，分别以14-1～7表示辅助坩埚a测温热偶a～g。
辅助坩埚d 22外围设置的加热丝根据区域分为5个加热区，分别以5-1～5表示辅助坩埚d的加热区a～e；在各加热区设有测温热偶，分别以19-1～7表示辅助坩埚d测温热偶a～f。
辅助坩埚b 16外围设置的加热丝根据区域分为5个加热区，分别以2-1～5表示辅助坩埚b的加热区a～e；在各加热区设有测温热偶，分别以17-1～7表示辅助坩埚b测温热偶a～g。
辅助坩埚c 21外围设置的加热丝根据区域分为5个加热区，分别以4-1～5表示辅助坩埚c的加热区a～e；在各加热区设有测温热偶，分别以20-1～6表示辅助坩埚c测温热偶 a～g。
以合成InP晶体为例，说明本制备高成品率InP晶体的方法，包括以下步骤：
①投料：将籽晶10按照晶体生长晶向<100>放入至主坩埚6的籽晶部6-1，将多晶碎料通过投料生长部6-4别投入至主坩埚6生长部6-2、投料生长部6-4及辅助坩埚a15、辅助坩埚b16、辅助坩埚c21和辅助坩埚d22中，再分别加入密封剂，本实施例总密封剂采用氧化硼18，将氧化硼18分别放入主坩埚6、辅助坩埚a平衡管15-2、辅助坩埚b平衡管16-2、辅助坩埚c平衡管21-2和辅助坩埚d平衡管22-2，且保证氧化硼18熔化后在各坩埚中的厚度大致相等；
②抽真空：对炉体抽真空至10 -5Pa，冲入惰性气体至2MPa；
③主坩埚6化料：借助主坩埚6的加热组件及测温热偶使主坩埚6形成由下至上温度依次升高的温度梯度，且控制籽晶部6-1处的温度低于InP熔点(1062℃)，使主坩埚6内的多晶料熔化；具体的，控制主加热区a1-1、主加热区b1-2、主加热区c1-3、主加热区d1-4、主加热区e1-5、主加热区f1-6、主加热区g1-7、主加热区h1-8、主加热区i1-9、主加热区j1-10、主加热区k1-11、主加热区l1-12、主加热区m1-13对应加热丝的加热功率，使得热偶a11、热偶b12、主坩埚测温热偶a13-1、主坩埚测温热偶b13-2、主坩埚测温热偶c13-3、主坩埚测温热偶d13-4、主坩埚测温热偶e13-5、主坩埚测温热偶f13-6、主坩埚测温热偶g13-7、主坩埚测温热偶h13-8；主坩埚测温热偶i13-9；主坩埚测温热偶j13-10；主坩埚测温热偶k13-11、主坩埚测温热偶l13-12、主坩埚测温热偶m13-13、主坩埚测温热偶n13-14的温度依次升高，同时使得热偶a11处的温度低于1062℃。
④辅助坩埚化料：借助各辅助坩埚配套的加热组件及测温热偶由下至上依次控制各辅助坩埚升温，使各辅助坩埚形成由下至上升温的温度梯度，使辅助坩埚内的多晶料熔化；具体的，4个辅助坩埚的升温控制过程如下：
④-1通过控制辅助坩埚a15的加热区a3-1、辅助坩埚a的加热区b3-2、辅助坩埚a的加热区c3-3、辅助坩埚a的加热区d3-4、辅助坩埚a的加热区e3-5对应加热丝的功率，控制辅助坩埚a15内多晶料的熔化，使得主坩埚测温热偶e13-5、辅助坩埚a测温热偶a14-1、测温热偶b14-2、辅助坩埚a测温热偶c14-3、辅助坩埚a测温热偶d14-4、辅助坩埚a测温热偶e14-5、辅助坩埚a测温热偶f14-6、辅助坩埚a测温热偶g14-7的温度依次升高；
④-2然后通过控制辅助坩埚d22的加热区a5-1、辅助坩埚d的加热区b5-2、辅助坩埚d的加热区c5-3、辅助坩埚d的加热区d5-4、辅助坩埚d的加热区e5-5对应加热丝的功率，控制辅助坩埚d22内的多晶料熔化，使得主坩埚测温热偶g13-7、辅助坩埚d测温热偶a19-1、 辅助坩埚d测温热偶b19-2、辅助坩埚d测温热偶c19-3、辅助坩埚d测温热偶d19-4、辅助坩埚d测温热偶e19-5、辅助坩埚d测温热偶f19-6、辅助坩埚d测温热偶g19-7的温度依次升高；
④-3然后通过控制辅助坩埚b16的加热区a2-1、辅助坩埚b的加热区b2-2、辅助坩埚b的加热区c2-3、辅助坩埚b的加热区d2-4、辅助坩埚b的加热区e2-5对应加热丝的功率，控制辅助坩埚b16内的多晶料熔化，使得主坩埚测温热偶i13-9、辅助坩埚b测温热偶a17-1、辅助坩埚b测温热偶b17-2、辅助坩埚b测温热偶c17-3、辅助坩埚b测温热偶d17-4、辅助坩埚b测温热偶e17-5、辅助坩埚b测温热偶f17-6、辅助坩埚b测温热偶g17-7的温度依次升高；
④-4然后通过控制辅助坩埚c的加热区a4-1、辅助坩埚c的加热区b4-2、辅助坩埚c的加热区c4-3、辅助坩埚c的加热区d4-4、辅助坩埚c的加热区e4-5对应加热丝的功率，控制辅助坩埚c21内多晶料的熔化，使得主坩埚测温热偶j13-10、辅助坩埚c测温热偶a20-1、辅助坩埚c测温热偶b20-2、辅助坩埚c测温热偶c20-3、辅助坩埚c测温热偶d20-4、辅助坩埚c测温热偶e20-5、辅助坩埚c测温热偶f20-6的温度依次升高。
⑤主坩埚6降温：借助主坩埚6的加热组件及测温热偶控制主坩埚6形成由下至上温度依次降低的温度梯度，且控制籽晶部6-1处的温度低于InP熔点；具体的，控制主加热区a1-1、主加热区b1-2、主加热区c1-3、主加热区d1-4、主加热区e1-5、主加热区f1-6、主加热区g1-7、主加热区h1-8、主加热区i1-9、主加热区j1-10、主加热区k1-11、主加热区l1-12、主加热区m1-13对应加热丝的加热功率，使得热偶a11、热偶b12、主坩埚测温热偶a13-1、主坩埚测温热偶b13-2、主坩埚测温热偶c13-3、主坩埚测温热偶d13-4、主坩埚测温热偶e13-5，主坩埚测温热偶f13-6、主坩埚测温热偶g13-7、主坩埚测温热偶h13-8、主坩埚测温热偶i13-9、主坩埚测温热偶j13-10、主坩埚测温热偶k13-11、主坩埚测温热偶l13-12、主坩埚测温热偶m13-13、主坩埚测温热偶n13-14温度依次降低到1062℃以下。
⑥辅助坩埚依次降温：由下至上，依次控制使各辅助坩埚降温，在辅助坩埚与主坩埚6连接处温度低于InP熔点时，控制辅助坩埚形成由下至上温度依次降低的温度梯度，使辅助坩埚内的1062℃等温线与主坩埚6内1062℃等温线相同；具体的，
⑥-1在主坩埚测温热偶e13-5低于1062℃以后，通过调控辅助坩埚a的加热区a3-1、辅助坩埚a的加热区b3-2、辅助坩埚a的加热区c3-3、辅助坩埚a的加热区d3-4、辅助坩埚a的加热区e3-5对应加热丝的功率，使得辅助坩埚a测温热偶a14-1、测温热偶b14-2、辅助坩埚a测温热偶c14-3、辅助坩埚a测温热偶d14-4、辅助坩埚a测温热偶e14-5、辅助坩埚a 测温热偶f14-6、辅助坩埚a测温热偶g14-7的温度依次降低。通过监控上述热偶控制辅助坩埚a15内的1062℃等温线与主坩埚6内1062℃等温线大致相同；
⑥-2依次类推，在主坩埚测温热偶g13-7低于1062℃以后，通过调控辅助坩埚d22的加热区a5-1、辅助坩埚d的加热区b5-2、辅助坩埚d的加热区c5-3、辅助坩埚d的加热区d5-4、辅助坩埚d的加热区e5-5对应加热丝的功率，使得辅助坩埚d测温热偶a19-1、辅助坩埚d测温热偶b19-2、辅助坩埚d测温热偶c19-3、辅助坩埚d测温热偶d19-4、辅助坩埚d测温热偶e19-5、辅助坩埚d测温热偶f19-6、辅助坩埚d测温热偶g19-7的温度依次降低。通过监控上述热偶保证辅助坩埚d22内的1062℃等温线与主坩埚6内1062℃等温线大致相同。
⑥-3依次类推，在主坩埚测温热偶e13-9低于1062℃以后，通过调控辅助坩埚b16的加热区a2-1、辅助坩埚b的加热区b2-2、辅助坩埚b的加热区c2-3、辅助坩埚b的加热区d2-4、辅助坩埚b的加热区e2-5对应加热丝的功率，使得主坩埚测温热偶i13-9、辅助坩埚b测温热偶a17-1、辅助坩埚b测温热偶b17-2、辅助坩埚b测温热偶c17-3、辅助坩埚b测温热偶d17-4、辅助坩埚b测温热偶e17-5、辅助坩埚b测温热偶f17-6、辅助坩埚b测温热偶g17-7的温度依次降低。通过监控上述热偶保证辅助坩埚b16内的1062℃等温线与主坩埚6内1062℃等温线大致相同。
⑥-4依次类推，在主坩埚测温热偶j13-10低于1062℃以后，通过调控辅助坩埚c21的加热区a4-1、辅助坩埚c的加热区b4-2、辅助坩埚c的加热区c4-3、辅助坩埚c的加热区d4-4、辅助坩埚c的加热区e4-5对应加热丝的功率，使得辅助坩埚c测温热偶a20-1、辅助坩埚c测温热偶b20-2、辅助坩埚c测温热偶c20-3、辅助坩埚c测温热偶d20-4、辅助坩埚c测温热偶e20-5、辅助坩埚c测温热偶f20-6的温度依次降低。通过监控上述热偶保证辅助坩埚c21内的1062℃等温线与主坩埚6内1062℃等温线大致相同。
⑦当各辅助坩埚平衡管处温度均低于InP熔点时，控制加热组件使主坩埚6、辅助坩埚缓慢降温至室温，拆炉去除晶锭，即待主坩埚6测温热偶n13-14、辅助坩埚a测温热偶g14-7、辅助坩埚b测温热偶g17-7、辅助坩埚d测温热偶f20-6、辅助坩埚c测温热偶g19-7均低于1062℃以后，缓慢降温至室温，拆炉取出晶锭。
对比例：与上述实施例1中主坩埚6结构相同，对主坩埚6的加热、降温等过程同
实施例1，与实施例1不同的是，没有设置辅助坩埚。
对比实施例1与对比例的产品发现，实施例1中制备的InP晶体，成品率32％，对比实施例中成品率约11.4％，多次试验统计发现，采用本发明方法制备的晶体成品率提高至 30％以上，相对于目前普通坩埚、单坩埚晶体生长约10％的成品率，提高3倍以上，经济效益非常高，且设备简单，易于控制，适宜工业化生产。

Claims (11)

  1. 一种制备高成品率晶体的生长方法，采用晶体生长坩埚及配套的加热炉制备，其特征在于，所述晶体生长坩埚结构中包括由下往上依次设有籽晶部(6-1)、生长部(6-2)、缩颈部(6-3)及投料生长部(6-4)的主坩埚(6)和分散设置在主坩埚(6)的缩颈部(6-3)上的辅助坩埚，所述方法依次包括投料、抽真空、主坩埚(6)化料、辅助坩埚化料、主坩埚(6)降温、辅助坩埚依次降温和拆炉去除晶锭，所述投料步骤为将籽晶(10)按与晶体生长方向垂直的晶面指数为(h 1k 1l 1)放入至籽晶部(6-1)，将多晶碎料分别投入至主坩埚(6)生长部(6-2)、投料生长部(6-4)及辅助坩埚中，再投入密封剂，控制辅助坩埚与主坩埚(6)中心线的夹角为θ，辅助坩埚中心线之间的夹角为φ或φ的倍数，θ、φ满足
    cosθ＝∣(h 1h 2+k 1k 2+l 1l 2)∣/[(h 1 2+l 1 2+k 1 2)(h 2 2+l 2 2+k 2 2)] 0.5，
    cosφ＝∣(h 3h 4+k 3k 4+l 3l 4)∣/[(h 3 2+l 3 2+k 3 2)(h 4 2+l 4 2+k 4 2)] 0.5
    其中，(h 1k 1l 1)为与晶体生长方向垂直的晶面指数；出现孪晶后，与晶锭沿晶体生长方向垂直的晶面转变为(h 2k 2l 2)；(h 3k 3l 3)和(h 4k 4l 4)为垂直于晶体生长晶面、且经过相邻晶体生长晶面上的孪晶线的晶面指数。
  2. 根据权利要求1所述的方法，其特征在于，所述辅助坩埚结构中由下至上依次包括与主坩埚(6)缩颈部(6-3)连接的连接部、分支生长部和平衡管，所述平衡管顶端高于晶体生长坩埚(6)缩颈部(6-3)。
  3. 根据权利要求1所述的方法，其特征在于，所述方法步骤具体如下：
    ①投料：将籽晶(10)按与晶体生长方向垂直的晶面指数为(h 1k 1l 1)放入至籽晶部(6-1)，将多晶碎料分别投入至主坩埚(6)生长部(6-2)、投料生长部(6-4)及辅助坩埚中，再投入密封剂；
    ②抽真空：对炉体抽真空，冲入惰性气体至1.8-2.5MPa；
    ③主坩埚(6)化料：借助主坩埚(6)的加热组件及测温热偶使主坩埚(6)形成由下至上温度依次升高的温度梯度，且控制籽晶部(6-1)处的温度低于晶体熔点，使主坩埚(6)内的多晶料熔化；
    ④辅助坩埚化料：借助各辅助坩埚配套的加热组件及测温热偶由下至上依次控制各辅助坩埚升温，使各辅助坩埚形成由下至上升温的温度梯度，使辅助坩埚内的多晶料熔化；
    ⑤主坩埚(6)降温：借助主坩埚(6)的加热组件及测温热偶控制主坩埚(6)形成由下至上温度依次降低的温度梯度，且控制籽晶部(6-1)处的温度低于晶体熔点；
    ⑥辅助坩埚依次降温：由下至上，依次控制使各辅助坩埚降温，在辅助坩埚与主坩埚(6)连接处温度低于晶体熔点时，控制辅助坩埚形成由下至上温度依次降低的温度梯度，使辅助 坩埚与主坩埚(6)内晶体熔点等温线相同；
    ⑦当各辅助坩埚平衡管处温度均低于晶体熔点时，控制加热组件使主坩埚(6)、辅助坩埚缓慢降温至室温，拆炉去除晶锭。
  4. 一种高成品率晶体生长坩埚，包括主坩埚(6)，其特征在于，所述主坩埚(6)结构由下往上依次包括主坩埚籽晶部(6-1)、主坩埚生长部(6-2)，主坩埚(6)上沿周向呈设置有辅助坩埚。
  5. 根据权利要4所述的晶体生长坩埚，其特征在于，所述辅助坩埚与主坩埚(6)中心线的夹角为θ，cosθ＝∣(h 1h 2+k 1k 2+l 1l 2)∣/[(h 1 2+l 1 2+k 1 2)(h 2 2+l 2 2+k 2 2)] 0.5，其中，h 1k 1l 1h 2k 2l 2为晶面指数，与晶体生长方向垂直的晶面为(h 1k 1l 1)；出现孪晶后，与晶锭沿晶体生长方向垂直的晶面转变为(h 2k 2l 2)。
  6. 根据权利要求4或5所述的晶体生长坩埚，其特征在于，所述主坩埚(6)由下往上依次包括籽晶部(6-1)、生长部(6-2)、缩颈部(6-3)和投料生长部(6-4)，所述辅助坩埚设置在主坩埚(6)的缩颈部(6-3)；所述辅助坩埚结构中由下至上依次包括与主坩埚(6)缩颈部(6-3)连接的连接部、分支生长部和平衡管，所述平衡管顶端高于主坩埚(6)的缩颈部(6-3)。
  7. 根据权利要4所述的晶体生长坩埚，其特征在于，所述辅助坩埚中心线之间的夹角为φ或φ的倍数，cosφ＝∣(h 3h 4+k 3k 4+l 3l 4)∣/[(h 3 2+l 3 2+k 3 2)(h 4 2+l 4 2+k 4 2)] 0.5，其中，(h 3k 3l 3)和(h 4k 4l 4)为垂直于晶体生长晶面、且经过相邻晶体生长晶面上的孪晶线的晶面指数。
  8. 一种制备高成品率InP晶体的生长方法，其特征在于，所述方法包括以下步骤：
    ①投料：将籽晶(10)按与晶体生长方向垂直的晶面指数为(h 1k 1l 1)放入至籽晶部(6-1)，将多晶碎料分别投入至主坩埚(6)生长部(6-2)、投料生长部(6-4)及辅助坩埚中，再投入密封剂；
    ②抽真空：对炉体抽真空，冲入惰性气体至1.8-2.5MPa；
    ③主坩埚(6)化料：借助主坩埚(6)的加热组件及测温热偶使主坩埚(6)形成由下至上温度依次升高的温度梯度，且控制籽晶部(6-1)处的温度低于1060-1065℃，使主坩埚(6)内的多晶料熔化；
    ④辅助坩埚化料：借助各辅助坩埚配套的加热组件及测温热偶由下至上依次控制各辅助坩埚升温，使各辅助坩埚形成由下至上升温的温度梯度，使辅助坩埚内的多晶料熔化；
    ⑤主坩埚(6)降温：借助主坩埚(6)的加热组件及测温热偶控制主坩埚(6)形成由下至上温度依次降低的温度梯度，且控制籽晶部(6-1)处的温度低于1060-1065℃；
    ⑥辅助坩埚依次降温：由下至上，依次控制使各辅助坩埚降温，在辅助坩埚与主坩埚(6)连接处温度低于1060-1065℃时，控制辅助坩埚形成由下至上温度依次降低的温度梯度，使辅助坩埚与主坩埚(6)内1062℃等温线相同；
    ⑦当各辅助坩埚平衡管处温度均低于晶体熔点时，控制加热组件使主坩埚(6)、辅助坩埚缓慢降温至室温，拆炉去除晶锭。
  9. 根据权利要求8所述的生长方法，其特征在于，所述投料步骤中籽晶(10)放入时晶向为<100>，所述辅助坩埚轴向平行于籽晶的<011>晶向。
  10. 根据权利要求9所述的生长方法，其特征在于，所述辅助坩埚中心线之间的夹角为90°或180°或360°。
  11. 根据权利要求8所述的生长方法，其特征在于，所述投料步骤中籽晶(10)放入时晶向为<111>，所述辅助坩埚中心线之间的夹角为60°或120°。
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