CN115029783B - Indium arsenide monocrystal growth method based on VB method and VGF method - Google Patents
Indium arsenide monocrystal growth method based on VB method and VGF method Download PDFInfo
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- CN115029783B CN115029783B CN202210496774.2A CN202210496774A CN115029783B CN 115029783 B CN115029783 B CN 115029783B CN 202210496774 A CN202210496774 A CN 202210496774A CN 115029783 B CN115029783 B CN 115029783B
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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
- 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
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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
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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
- C30B11/003—Heating or cooling of the melt or the crystallised material
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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
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Abstract
An indium arsenide single crystal growth method based on VB method and VGF method, relates to an indium arsenide single crystal growth device, a charging method and a crystal growth process based on VB method and VGF method. The growth device consists of a heating furnace body, a thermal field system, a supporting system, a container system and a crucible descending device, and the growth method comprises the steps of charging, material melting, seed crystal receiving, shouldering, constant diameter growth and cooling annealing. The charging container is divided into an upper crucible, a lower crucible and a quartz ampoule bottle, and by utilizing reasonable collocation design of conical materials, round cake materials and ladder-shaped materials, the charging structure is stable, good material melting at high temperature is facilitated, the crystallization rate can be effectively improved by 31%, seed crystal embryo is obtained through synthesis of indium arsenide polycrystal, charging and single crystal growth, seed crystal is obtained through seed crystal embryo processing, single crystal growth is carried out, and finally low dislocation indium arsenide single crystal which is far lower than LEC growth is grown.
Description
Technical Field
The invention belongs to the field of compound semiconductor crystal growth, and in particular relates to a growing device, a charging process and a crystal growth method for growing indium arsenide monocrystal by combining a VB method and a VGF method.
Background
Indium arsenide (InAs) has a relatively high electron mobility and mobility ratio (μe/μh=70), and is an ideal substrate material for ultra-long wavelength lasers and detectors.
Indium arsenide has a melting point of 942 ℃ and a dissociation pressure of 0.33atm, and due to the low melting point and dissociation pressure, currently, the growth method mainly adopted for indium arsenide single crystals is the LEC method, namely the liquid-sealed Czochralski method. The main disadvantages of this method are high equipment cost, large crystal stress, high dislocation density, easy generation of twinning caused by dross on the surface of the melt, and the rate of crystallization is only about 33%, so that it is unfavorable for growing large-size low dislocation crystals.
Disclosure of Invention
The invention aims to provide an indium arsenide growth device combining a VB method and a VGF method, a charging process, a seed crystal acquisition method and a single crystal growth process.
The method for growing the indium arsenide monocrystal based on the combination of the VB method and the VGF method comprises the steps of charging, melting, inoculating seed crystal, shouldering, constant diameter growth, cooling and annealing, and is characterized in that:
the charging is specifically as follows:
the method comprises the steps of firstly, placing a first conical material into the bottom of a PBN lower crucible, then, placing 2 bridging trapezoidal materials to form a cylindrical bridging structure, then, respectively placing arsenic particles and diboron trioxide on two sides of the bridging structure, then, placing round cake materials on the bridging structure, and finally, placing a standard trapezoidal material on the round cake materials;
firstly, placing a second conical material into the bottom of the PBN upper crucible, then placing round cakes upwards, then oppositely stacking the large surface of a standard trapezoid material on the round cakes downwards, oppositely stacking 2 standard trapezoid materials on the standard trapezoid material according to the shape of a cylinder, and placing 2 standard trapezoid materials beside the standard trapezoid material;
in the equal-diameter growth process, the crucible descending speed is 1.2mm/h, and equal-diameter growth ending is performed.
Further, the material melting is divided into two stages, specifically:
the first stage is to raise the temperature to preliminary feed the crucible: setting heating temperatures of all temperature zones, wherein the first heating zone is 860 ℃, the second heating zone is 940 ℃, the third heating zone is 1029 ℃, the fourth heating zone is 1029 ℃, the fifth heating zone is 1019 ℃, and the sixth heating zone is 1019 ℃;
the second stage is to integrate the materials, and the heating temperature is raised to 860 ℃ for the first heating zone, 988 ℃ for the second heating zone, 1000 ℃ for the third heating zone, 1000 ℃ for the fourth heating zone, 1006 ℃ for the fifth zone and 1006 ℃ for the sixth zone.
Furthermore, the temperature thermocouple adopts an R-type thermocouple.
According to the invention, the VB method and VGF method are combined to grow the indium arsenide crystal, so that the crystal with ultralow dislocation can be grown, the single crystal rate is high, the uniformity of electrical parameters such as carrier concentration and mobility is far better than that of the LEC method, the growth equipment is simple, and the growth benefit is greatly improved.
Drawings
FIG. 1 is a schematic diagram showing the structure of a growing apparatus for rapidly growing indium arsenide single crystals by combining the VB method and the VGF method according to the present invention.
FIG. 2 is a schematic diagram of the PBN lower crucible loading of the present invention.
FIG. 3 is a schematic diagram of the loading of a PBN upper crucible of the present invention.
1. A furnace core; 2. an inner support tube; 3. an inner insulation sleeve; 4. an outer support tube; 5. an outer insulation sleeve; 6. a furnace; 7. applying heat preservation cotton; 8. a first heater; 9. a second heater; 10. a third heater; 11. a fourth heater; 12. a fifth heater; 13. a sixth heater; 14. a first temperature thermocouple; 15. a second temperature thermocouple; 16. a third temperature thermocouple; 17. a fourth temperature thermocouple; 18. a fifth temperature thermocouple; 19. a sixth temperature thermocouple; 20. an indium arsenide seed crystal; 21. a first cone material; 22. bridging trapezoid materials; 23. round cake materials; 24. standard trapezoid materials; 25. a second taper; 26. quartz ampoule bottle; a pbn lower crucible; a pbn upper crucible; 29. diboron trioxide; 30. arsenic particles.
Detailed Description
The objects, technical solutions and advantages of the present invention will become more apparent by the following detailed description of the present invention with reference to the accompanying drawings.
Example 1: the device adopted by the method for growing the indium arsenide monocrystal based on the VB method and the VGF method is shown in figure 1. Consists of a heating furnace body, a thermal field system, a supporting system, a container system and a crucible descending device. The heating furnace body comprises 6 heating areas and 6 temperature control devices for controlling the temperature of the heating areas, wherein the first heating area 8, the second heating area 9, the third heating area 10, the fourth heating area 11, the fifth heating area 12 and the sixth heating area 13 are arranged in sequence from bottom to top. The thermal field system comprises a bottom heat preservation and radiation system, a middle heat preservation system and a top heat preservation system; the bottom heat preservation and heat dissipation system consists of a furnace core 1, an inner support tube 2, an inner heat preservation sleeve 3, an outer support tube 4 and an outer heat preservation sleeve 5; the middle heat preservation system consists of a hearth 6 and heat preservation cotton; the top heat preservation system consists of upper heat preservation cotton 7. The support system consists of an inner support tube 2, an outer support tube 4 and a bottom aluminum alloy structural platform. The container system includes a quartz ampoule 26, a PBN lower crucible 27, and a PBN upper crucible 28.
The first heating zone 8, the second heating zone 9, the third heating zone 10, the fourth heating zone 11, the fifth heating zone 12 and the sixth heating zone 13 are respectively and correspondingly provided with a first temperature thermocouple 14, a second temperature thermocouple 15, a third temperature thermocouple 16, a fourth temperature thermocouple 17, a fifth temperature thermocouple 18 and a sixth temperature thermocouple 19. The first temperature thermocouple 14 is positioned at the bottom of the seed crystal, the second temperature thermocouple 15 is positioned at the middle of the seed crystal, the third temperature thermocouple 16 is positioned at the middle of the shoulder, the fourth temperature thermocouple 17 is positioned at the intersection of the end of the shoulder and the equal diameter, the fifth temperature thermocouple 18 is positioned at the end of the equal diameter, and the sixth temperature thermocouple 19 is positioned at the middle of the upper crucible
Preferably, the temperature thermocouple is an R-type thermocouple.
The method for growing the indium arsenide monocrystal based on the combination of the VB method and the VGF method comprises the following steps:
s1, charging:
6N arsenic and 6N indium are mixed according to the mass ratio of 0.652:1, synthesizing indium arsenide polycrystal, cutting and polishing the polycrystal material to obtain a bridging trapezoid material 22 and a standard trapezoid material 24;
as shown in FIG. 2, the PBN lower crucible charging method comprises the steps of placing a first conical material 21 at the bottom of the PBN lower crucible, then placing 2 pieces of bridging trapezoidal materials 22 to form a cylindrical bridging structure for stable supporting, then respectively placing arsenic particles 30 and diboron trioxide 29 at two sides of the bridging structure, then placing round cake materials 23 on the bridging structure, and finally placing a standard trapezoidal material 24 on the round cake materials 23;
as shown in FIG. 3, the loading method of the PBN upper crucible is that a second conical material 25 is put at the bottom of the PBN upper crucible, a round cake material 23 is put upwards, the large surface of a standard trapezoid material 24 is oppositely stacked on the round cake material 23 downwards, 2 standard trapezoid materials 24 are oppositely stacked on the standard trapezoid material 24 according to the shape of a cylinder, and 2 standard trapezoid materials 24 are put beside the standard trapezoid materials;
the charging mode mainly ensures that the whole structure is stable after charging and is designed according to the principle of pre-feeding upper materials in the heating and material-melting process, wherein the total weight of the indium arsenide polycrystal material is 4kg, the diboron trioxide is 32g, the arsenic is 2g, and the material is baked after charging, and then a oxyhydrogen flame tube is used for sealing.
S2, charging:
installing a bottom temperature thermocouple, wherein the first temperature thermocouple 14 is positioned at the bottom of the seed crystal, the second temperature thermocouple 15 is positioned at the middle of the seed crystal, and the third temperature thermocouple 16 is positioned at the middle of the shoulder; the charging container system is arranged in the single crystal furnace, a temperature thermocouple is arranged, a fourth temperature thermocouple 17 is positioned at the intersection of the shoulder placing end and the equal diameter, a fifth temperature thermocouple 18 is positioned at the equal diameter end, and a sixth temperature thermocouple 19 is positioned at the middle part of the upper crucible.
S3, heating for 20 hours to preliminarily feed materials to the crucible:
setting heating temperatures of all temperature zones, wherein the first heating zone is 860 ℃, the second heating zone is 940 ℃, the third heating zone is 1029 ℃, the fourth heating zone is 1029 ℃, the fifth heating zone is 1019 ℃, and the sixth heating zone is 1019 ℃;
the actual measurement temperature of the temperature thermocouple is as follows: TC (TC) 1 ＝898.8℃，TC 2 ＝909.1℃，TC 3 ＝924.5℃，TC 4 ＝939.9℃，TC 5 ＝951.7℃，TC 6 If the actual measurement does not reach the preset temperature, = 917.6 ℃, the set temperature needs to be correspondingly adjusted, so that the actual temperature meets the set requirement temperature.
S4, preparing the integrated material for 28 hours before inoculation:
heating to a temperature such that the first heating zone is 860 ℃, the second heating zone is 988 ℃, the third heating zone is 1000 ℃, the fourth heating zone is 1000 ℃, the fifth zone is 1006 ℃, and the sixth zone is 1006 ℃;
the actual measurement temperature of the temperature thermocouple is as follows: TC (TC) 1 ＝925.15℃，TC 2 ＝934.3℃，TC 3 ＝942.6℃，TC 4 ＝951.0℃，TC 5 ＝954.2℃，TC 6 = 953.8 ℃, incubated for 2 hours.
S5, inoculating seed crystals:
over 8 hours, TC is first added 1 -TC 6 The temperature is reduced by 0.1 to 5.5 ℃ and the recrystallization after seed crystal remelting is carried out.
S6, shouldering:
cooling for 20 hours to obtain a first region 826.8 ℃, a second region 954.8 ℃, a third region 1008.7 ℃, a fourth region 1011.9 ℃, a fifth region 1005.9 and a sixth region 1005.9 ℃;
the actual measurement temperature of the temperature thermocouple is as follows: TC (TC) 1 ＝908.3℃，TC 2 ＝921.7℃，TC 3 ＝930.6℃，TC 4 ＝943.5℃，TC 5 ＝950.4℃，TC 6 If the actual measurement does not reach the preset temperature, = 952.7 ℃, the set temperature needs to be correspondingly adjusted, so that the actual temperature meets the set requirement temperature.
S7, equal-diameter growth:
the constant diameter growth of the crucible descending speed is 1.2mm/h and ends.
S8, entering cooling annealing:
the cooling process is divided into four stages, specifically as follows:
the first stage of the cooling process: TC (TC) 1 -TC 6 The cooling speed is 2.1-2.6 ℃/h;
the second stage of the cooling process: TC (TC) 1 -TC 6 The cooling speed is 16.9-36.8 ℃/h;
third stage of cooling process: TC (TC) 1 -TC 6 The cooling speed is 27-32 ℃/h;
the fourth stage of the cooling process: TC (TC) 1 -TC 6 The cooling speed is 10.7-11.3 ℃/h.
When the temperature is lower than 80 ℃, the furnace is opened, the crystal is taken out, and is put into hot methanol for soaking, so that the indium arsenide crystal is separated from the PBN crucible, after the crystal is demoulded, the crystal bar is cut into sections according to the length of 40mm, and the part with larger crystal grains is selected from the sections and is drilled by an electric drill; and (3) utilizing an X-ray orientation instrument to orient the crystal orientation, selecting a proper embryo, and orienting, processing and obtaining the indium arsenide seed crystal 20 with the (111) crystal orientation without clamp crystal, notch and cavity.
The crystal growth is again the same as before except that the indium arsenide seed 22 is first charged into the bottom of the PBN lower crucible 27.
From the obtained crystal head-to-tail cutting test piece of the indium arsenide seed crystal 20, the carrier concentration, mobility and dislocation density of indium arsenide were tested. As shown in Table 1, the average dislocation of the head and tail of the indium arsenide crystal grown by the VGF and VB combined growth method is 1423cm, respectively, compared with the conventional LEC method -1 And 1612cm -1 16000-20000cm far below LEC method -1 . The head and tail carrier concentrations were 2.2E+16 (cm) -3 ) And 2.8E+16 (cm) -3 ) The carrier concentration uniformity is superior to LEC. Head-to-tail mobility of 3.4E+4 (v. S), respectively -1 And 4.1E+4 (v. S) -1 Mobility uniformity is superior to LEC.
TABLE 1
Example 2: and respectively growing 1 furnace 4 inch indium phosphide single crystals by adopting crucible descending speeds of 0.4mm/h, 0.8mm/h, 1.2mm/h, 1.6mm/h and 1.8mm/h, wherein the dosage of the indium phosphide single crystals is 4 Kg+/-50 g, and testing dislocation, carrier concentration, electron mobility and crystal yield of the grown crystals.
The method is characterized in that a testing method under the condition of 100 times of a metallographic microscope (137 lattice) is adopted for crystal dislocation, and single-point calculation is carried out; for the carrier concentration of the crystal, adopting a Hall 4 probe test method for electron mobility; the crystal to crystal ratio was calculated using conventional measurements.
Cutting the grown crystal with the crucible pulling speed of 0.4mm/h head and tail to obtain wafers with the thickness of 1mm, corroding and grinding by a chemical method, and observing dislocation by a wafer dislocation recognition counter to obtain the crystal: head average dislocation 5005, tail average dislocation 5513, crystallization rate 33%.
The qualified length of the grown crystal with the pulling speed of 0.8mm/h is 4 inches and 15mm, the crystal is cut from the head to the tail to obtain wafers with the thickness of 1mm, and the wafer dislocation recognition counter is adopted to observe dislocation after the crystal is corroded and ground by a chemical method to obtain the crystal: head average dislocation 2210, tail average dislocation 2612, and crystallization rate 51%.
Cutting the grown crystal from the head to the tail at the pull speed of 1.2mm/h to obtain wafers with the thickness of 1mm, corroding and grinding by a chemical method, and observing dislocation by a wafer dislocation recognition counter to obtain the crystal: the average dislocation of the head piece is 1423, the average dislocation of the tail piece is 1612, and the crystallization rate is 61%.
Cutting the grown crystal from the head to the tail at the pull speed of 1.6mm/h to obtain wafers with the thickness of 1mm, corroding and grinding by a chemical method, and observing dislocation by a wafer dislocation recognition counter to obtain the crystal: the average dislocation of the head piece is 3305, the average dislocation of the tail piece is 4100, and the crystallization rate is 39%.
Cutting the grown crystal from the head to the tail at the pull speed of 1.8mm/h to obtain wafers with the thickness of 1mm, corroding and grinding by a chemical method, and observing dislocation by a wafer dislocation recognition counter to obtain the crystal: the average dislocation of the head piece is 5210, the average dislocation of the tail piece is 6011, and the crystallization rate is 45%.
The carrier concentration and electron mobility of the sample wafer after dislocation detection, which is obtained by taking 1cm x 1cm small pieces, are tested by using a Hall 4 probe and are shown in Table 2:
TABLE 2
It can be seen from Table 2 that at a pull rate of the crucible of 1.2mm/h, the crystal dislocation, carrier concentration, electron mobility, and crystal yield were superior to the other pull rates.
The conventional charging method does not use the conical materials 21 and 25 and the round cake material 23, and has no requirement on the size and the bridging combination of the bridging trapezoidal material 22 and the round cake material 23. The improvement of the method of the invention uses the conical materials 21 and 25 and the round cake material 23, the size of the conical materials is regulated, and meanwhile, the bridging trapezoid material 22 and the round cake material 23 are combined in a bridging way, so that the crystallization rate can be effectively improved by 31%, as shown in table 3.
TABLE 3 Table 3
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explanation of the principles of the present invention and are in no way limiting of the invention. Accordingly, any modification, equivalent replacement, improvement, etc. made without departing from the spirit and scope of the present invention should be included in the scope of the present invention. Furthermore, the appended claims are intended to cover all such changes and modifications that fall within the scope and boundary of the appended claims, or equivalents of such scope and boundary.
Claims (5)
1. The method for growing the indium arsenide monocrystal based on the combination of the VB method and the VGF method comprises the steps of charging, melting, inoculating seed crystal, shouldering, constant diameter growth, cooling and annealing, and is characterized in that:
the charging is specifically as follows:
the method comprises the steps of firstly, placing a first conical material into the bottom of a PBN lower crucible, then, placing 2 bridging trapezoidal materials to form a cylindrical bridging structure, then, respectively placing arsenic particles and diboron trioxide on two sides of the bridging structure, then, placing round cake materials on the bridging structure, and finally, placing a standard trapezoidal material on the round cake materials;
firstly, placing a second conical material into the bottom of the PBN upper crucible, then placing round cake materials upwards, then oppositely stacking the large surface of the standard trapezoid materials downwards on the round cake materials, oppositely stacking 2 standard trapezoid materials on the standard trapezoid materials according to the shape of a cylinder, and placing 2 standard trapezoid materials beside the standard trapezoid materials;
in the equal-diameter growth process, the crucible descending speed is 1.2mm/h, and equal-diameter growth ending is performed.
2. The method for growing indium arsenide single crystal based on the combination of VB method and VGF method as set forth in claim 1, wherein the melting is divided into two stages, specifically:
the first stage is to raise the temperature to preliminary feed the crucible: setting heating temperatures of all temperature zones, wherein the first heating zone is 860 ℃, the second heating zone is 940 ℃, the third heating zone is 1029 ℃, the fourth heating zone is 1029 ℃, the fifth heating zone is 1019 ℃, and the sixth heating zone is 1019 ℃;
the second stage of integration material is heated to a temperature that makes the first heating area 860 ℃, the second heating area 988 ℃, the third heating area 1000 ℃, the fourth heating area 1000 ℃, the fifth area 1006 ℃ and the sixth area 1006 ℃;
furthermore, the temperature thermocouple adopts an R-type thermocouple.
3. The method for growing indium arsenide single crystal based on the combination of VB method and VGF method according to claim 1, wherein said seed grafting process is performed for 8 hours by first applying TC 1 - TC 6 The temperature is reduced by 0.1 to 5.5 ℃ and the recrystallization after seed crystal remelting is carried out.
4. The method for growing indium arsenide single crystal based on the combination of VB method and VGF method according to claim 1, wherein the shouldering process is carried out for 20 hours to lower the temperature of the first region 826.8 ℃, the second region 954.8 ℃, the third region 1008.7 ℃, the fourth region 1011.9 ℃, the fifth region 1005.9 ℃ and the sixth region 1005.9 ℃.
5. The method for growing indium arsenide single crystal based on the combination of VB method and VGF method according to claim 1, wherein the cooling annealing process is divided into four stages, specifically:
the first stage of the cooling process: TC (TC) 1 -TC 6 The cooling speed is 2.1-2.6 ℃/h;
the second stage of the cooling process: TC (TC) 1 -TC 6 The cooling speed is 16.9-36.8 ℃/h;
third stage of cooling process: TC (TC) 1 -TC 6 The cooling speed is 27-32 ℃/h;
the fourth stage of the cooling process: TC (TC) 1 -TC 6 The cooling speed is 10.7-11.3 ℃/h.
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