CN114808107B - Crystal growth single crystal furnace, crucible and crystal growth method - Google Patents
Crystal growth single crystal furnace, crucible and crystal growth method Download PDFInfo
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- CN114808107B CN114808107B CN202210355085.XA CN202210355085A CN114808107B CN 114808107 B CN114808107 B CN 114808107B CN 202210355085 A CN202210355085 A CN 202210355085A CN 114808107 B CN114808107 B CN 114808107B
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- 239000013078 crystal Substances 0.000 title claims abstract description 101
- 238000002109 crystal growth method Methods 0.000 title claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 239000000919 ceramic Substances 0.000 claims abstract description 8
- 239000000835 fiber Substances 0.000 claims abstract description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims abstract description 5
- 239000010453 quartz Substances 0.000 claims description 46
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 46
- 229910052582 BN Inorganic materials 0.000 claims description 24
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 8
- 229910052810 boron oxide Inorganic materials 0.000 claims description 7
- 239000004568 cement Substances 0.000 claims description 7
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000007493 shaping process Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 238000002425 crystallisation Methods 0.000 abstract description 8
- 230000008025 crystallization Effects 0.000 abstract description 8
- 239000004065 semiconductor Substances 0.000 abstract description 7
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 13
- 238000011161 development Methods 0.000 description 4
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
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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
-
- 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
- C30B11/006—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
- 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
Abstract
The invention relates to the field of semiconductor production, and discloses a crystal growth single crystal furnace, a crucible and a crystal growth method, which comprise a pressure container, wherein a heater is arranged in the pressure container, the heater comprises a heater shell, and a furnace core group is arranged at the central position inside the heater shell; the furnace core group is sleeved with heating wires, a first temperature control group and a second temperature control group are arranged between the heating wires and the heater shell, and the first temperature control group and the second temperature control group are symmetrically arranged along the central line of the furnace core group; the first temperature control group comprises a plurality of first thermocouple groups, and the second temperature control group comprises a plurality of second thermocouple groups; alumina powder is arranged between the heater shell and the furnace core group, the first thermocouple group and the second thermocouple group are both positioned on the outer wall of the furnace core group, the middle part of the furnace core group is provided with a containing cavity, and the end part of the furnace core group is provided with a Du Re ceramic fiber blanket. The invention can reduce the generation of polycrystal during the growth of crystal and improve the crystallization rate of single crystal growth.
Description
Technical Field
The invention relates to the technical field of semiconductor production, in particular to a crystal growth single crystal furnace, a crucible and a crystal growth method.
Background
Indium phosphide is an important compound semiconductor material, and the current crystallization rate of growing single crystals of indium phosphide is generally about 30%, so that the indium phosphide is an important factor for restricting the rapid development of the indium phosphide material. The technological innovation in the 5G era has brought about the vigorous development of second-generation semiconductor materials represented by indium phosphide (InP) and gallium arsenide (GaAs). The InP crystal has the advantages of high saturated electron drift speed, strong radiation resistance, good thermal conductivity, high photoelectric conversion efficiency and the like, and is widely applied to the fields of optical communication, high-frequency millimeter wave devices, photoelectric integrated circuits, solar cells for outer space and the like. The indium phosphide semiconductor material has the advantages of high electron limiting drift velocity, good radiation resistance and good heat conduction, and compared with gallium arsenide semiconductor material, the indium phosphide semiconductor material has the characteristics of high breakdown electric field, high heat conductivity and high electron average velocity. In addition, at present, an indium phosphide-based material is mainly adopted in an optical communication device, an indium phosphide-based laser, a modulator, a detector and a module thereof, which have high digital rate and good wavelength monochromaticity, are widely applied to an optical network, so that the rapid development of the data information transmission quantity of the Internet is promoted, and the requirements of people on the development of the network to a higher speed and wider bandwidth direction are continuously met.
At present, growing indium phosphide single crystal mainly comprises the steps of putting seed crystal into a seed crystal cavity of a boron nitride crucible, putting polycrystal material, boron nitride, red phosphorus and the like into the crucible, vacuumizing by using a quartz tube, welding and sealing, putting the crucible into a single crystal furnace, heating, melting all polycrystal material and the upper part of the seed crystal, cooling to enable the polycrystal material to grow upwards along the seed crystal, starting shoulder-placing growth beyond the seed crystal cavity in the upward process, and gradually expanding the diameter of the grown 4-inch indium phosphide single crystal from about 10mm to about 100 mm; during shouldering, the diameter is enlarged, the solid-liquid interface is gradually enlarged from small, the shape of the solid-liquid interface is difficult to control, when the crystal starts to nucleate at the contact position of the interface edge and the boron nitride crucible, an inward-growing twin line is easy to generate, when the two twin lines extend to the inner part of the crystal to meet, polycrystal is directly generated at the intersection position, and the whole crystal becomes polycrystal. According to practical production statistics, 80% of all crystal rods which are not grown into single crystals are caused by the conditions, and the problem is solved, so that the problem has a great effect on improving the crystallization rate.
In the original growth process, the quartz tube and the crucible used for charging are required to be made into specific shapes, so that the manufacturing cost of the crucible is increased, the original small seed crystal is not beneficial to demolding after the growth is finished, boron oxide between the crystal bar and the boron nitride crucible is difficult to dissolve in the demolding process, and the demolding time is prolonged; in addition, the damage quantity to the seed crystal cavity is larger in the demolding process, the slender quartz rod needs to be wrapped in the center of the wet felt in the original process furnace core group manufacturing process, two temperature thermocouples are manufactured around the quartz rod, the multilayer wet felt and the quartz sleeve are wrapped outside, the quartz rod and the quartz sleeve are manufactured into a shape matched with the quartz tube, the manufacturing process is extremely complex, the period about ten days is needed for manufacturing, the furnace core group manufactured by the process is complex, the furnace core group is extremely easy to damage in the production process, and the furnace core group basically needs to be manufactured again after being damaged and cannot be maintained.
Disclosure of Invention
Accordingly, the present invention is directed to a crystal growth single crystal furnace, a crucible, and a crystal growth method, which can reduce the generation of polycrystal during crystal growth and increase the crystallization rate of single crystal growth.
The invention solves the technical problems by the following technical means:
the crystal growth single crystal furnace comprises a pressure container, wherein a heater is arranged in the pressure container, the heater comprises a heater shell, and a furnace core group is arranged at the central position inside the heater shell; the furnace core group is sleeved with heating wires, a first temperature control group and a second temperature control group are arranged between the heating wires and the heater shell, and the first temperature control group and the second temperature control group are symmetrically arranged along the central line of the furnace core group; the first temperature control group comprises a plurality of first thermocouple groups, and the second temperature control group comprises a plurality of second thermocouple groups; alumina powder is arranged between the heater shell and the furnace core group, the first thermocouple group and the second thermocouple group are both positioned on the outer wall of the furnace core group, the middle part of the furnace core group is provided with a containing cavity, and the end part of the furnace core group is provided with a Du Re ceramic fiber blanket.
Further, the furnace core group comprises a quartz rod, a wet felt is arranged outside the quartz rod, a hearth pipe is sleeved outside the wet felt, and the diameter of the quartz rod is 50% -80% of the inner diameter of the hearth pipe. Therefore, when the furnace core group is prepared, the preparation process is simple, the diameter of the quartz rod is greatly increased compared with that of the quartz rod in the prior art, so that the heat conduction of the center of the furnace body is more sufficient, the center temperature of crystals on the same horizontal line is lower in the growth cooling process, crystal nuclei are preferentially formed, a slightly convex solid-liquid interface is formed, part of twin crystals or polycrystal which begin to nucleate at the crucible wall and begin to grow inwards are avoided, and the crystallization rate of crystal growth is further improved.
Further, the first temperature control group comprises a first temperature control area, a second temperature control area, a third temperature control area and a fourth temperature control area, a first temperature control thermocouple is arranged in the center of the first temperature control area, a second temperature control thermocouple is arranged in the center of the second temperature control area, a third temperature control thermocouple is arranged in the center of the third temperature control area, a fourth temperature control thermocouple is arranged in the center of the fourth temperature control area, and the first temperature control thermocouple, the second temperature control thermocouple, the third temperature control thermocouple and the fourth temperature control thermocouple are all arranged on the outer wall of the hearth pipe. According to the invention, four temperature control areas are arranged on one side of the outer wall of the hearth pipe, so that the hearth pipe can be precisely controlled in temperature, and the crystallization rate and quality of single crystal growth are improved.
Further, the second temperature control group comprises a fifth temperature control thermocouple, a sixth temperature control thermocouple, a seventh temperature control thermocouple, an eighth temperature control thermocouple and a ninth temperature control thermocouple which are all positioned on the outer wall of the hearth pipe, wherein the fifth temperature control thermocouple is arranged on the outer side of the hearth pipe, which is positioned at the end part of the quartz rod in the hearth pipe, and the distance between two adjacent temperature thermocouples of the fifth temperature control thermocouple, the sixth temperature control thermocouple, the seventh temperature control thermocouple, the eighth temperature control thermocouple and the ninth temperature control thermocouple is 30mm. According to the invention, five temperature measuring points are arranged on the other side of the outer wall of the hearth pipe, the temperature of the accommodating cavity in the hearth pipe is precisely measured, and the crystallization rate and quality of single crystal growth are improved through precise temperature control.
Further, the distance between the heating wires in the first temperature control area is 150mm, the distance between the heating wires in the second temperature control area is 250mm, the distance between the heating wires in the third temperature control area is 150mm, and the distance between the heating wires in the fourth temperature control area is 150mm. Thus, the temperature of each temperature control area can be accurately controlled.
Further, a high-temperature-resistant cement layer is arranged outside the hearth pipe, and the heating wire is arranged in the high-temperature-resistant cement layer. The high-temperature-resistant cement layer can fix the heating wire, and the heating wire is prevented from moving in the process.
Further, a heater bracket is arranged between the heater shell and the pressure vessel. The heater bracket stably supports the whole heater.
The invention also discloses a crystal growth crucible which is applied to the crystal growth single crystal furnace and is a cylindrical flat bottom crucible made of boron nitride material.
The invention also discloses a crystal growth method using the crystal growth single crystal furnace and the crucible, which comprises the following steps:
s1, processing polycrystalline materials, seed crystals, boron oxide and red phosphorus raw materials, and then loading the processed polycrystalline materials, seed crystals, boron oxide and red phosphorus raw materials into a boron nitride flat-bottom crucible;
s2, placing the boron nitride flat-bottom crucible into a quartz crucible, and vacuum sealing the boron nitride flat-bottom crucible into the quartz crucible by using oxyhydrogen flame sintering;
s3, preparing a quartz rod, wrapping the quartz rod by using a wet felt of aluminum silicate, then placing the quartz rod into a hearth pipe, and baking and shaping the quartz rod into a furnace core group; assembling the furnace core into the heater, and filling the gaps of the end parts by using Du Re ceramic fiber blankets;
and S4, heating the heater, controlling the temperature of the four temperature areas through the first temperature control thermocouple, the second temperature control thermocouple, the third temperature control thermocouple and the fourth temperature control thermocouple, and after seed crystals are melted, sequentially heating the fifth temperature control thermocouple, the sixth temperature control thermocouple, the seventh temperature control thermocouple, the eighth temperature control thermocouple and the ninth temperature control thermocouple, then cooling to enable crystals to grow from bottom to top, gradually moving up a solid-liquid interface, and completing crystal growth.
Further, the baking temperature of the furnace core group is 1000-1200 ℃, and the setting temperature of the first, second, third and fourth temperature control thermocouples is 1000-1090 ℃. When heating, the boron nitride is heated to about 450 ℃ to melt the crystal, the crystal is wrapped and sealed, and the polycrystalline material is completely melted at about 1070 ℃ to melt the upper part of the seed crystal.
The invention has the beneficial effects that:
1. the quartz crucible and the boron nitride crucible used in the invention have simple shapes, and particularly, the boron nitride crucible can be directly a cylindrical flat bottom crucible, so that the manufacturing process is easy to manufacture, the manufacturing cost is reduced relative to a special-shaped crucible, and the easy-to-damage parts are not existed in the transportation and use processes, so that the damage probability is reduced, and the cost can be reduced.
2. The seed crystal used for producing the indium phosphide monocrystal and the gallium arsenide monocrystal at present is very fine, the seed crystal with the diameter of about 8mm is filled into a small mouth of a special-shaped crucible, the molten part is cooled and grown upwards, and the diameter is gradually enlarged, but twin crystals and polycrystal are very easy to appear in the enlarging process.
3. According to the single crystal growth method, as the grown seed crystal is the same as the grown target size, after the growth is completed, the whole crystal bar is a perfect crystal, only the part with higher impurity enrichment at the tail part of the crystal is needed to be cut, and the head part can be used as the seed crystal for the next single crystal growth after being cut, so that the effect of recycling is achieved; therefore, compared with the existing process, the invention only occupies larger finished product amount of the prior seed crystal, but the seed crystal of the process is hardly consumed after mass production, thereby reducing the production cost.
4. The boron nitride crucible used in the invention has simple appearance, can better promote water molecules to enter the gap between the crucible and the crystal bar in the demolding process after the growth is finished, promote the full dissolution of boron nitride, make the demolding easier, and simultaneously reduce the loss of the boron nitride crucible in the demolding process.
5. In the growth process of single crystals, the invention belongs to equal diameter growth, and the invention has no stage of shoulder diameter expansion, so the crystal rods grown by the invention have longer effective length with the same weight of feeding.
6. According to the invention, by increasing the diameter of the quartz rod, the heat conduction of the center of the furnace body is more sufficient, the center temperature of the crystal on the same horizontal line is lower in the growth cooling process, crystal nuclei are preferentially formed, a slightly convex solid-liquid interface is formed, part of twin crystals or polycrystal which begin to nucleate and grow inwards on the crucible wall is avoided, and the crystallization rate of crystal growth is improved.
7. Because the crucible is in the shape of a flat bottom of a cylinder, compared with a special-shaped crucible, the filling of the polycrystalline material is easier, the cutting shape of the polycrystalline material is not too high, the time for selecting and filling the material is shortened, and the working efficiency is improved.
Drawings
FIG. 1 is a schematic diagram of a crystal growth furnace and a crucible according to the present invention.
The furnace comprises a pressure vessel 1, a heater shell 2, a heater bracket 3, a quartz rod 4, a wet felt 5, a hearth pipe 6, a heating wire 7, alumina powder 8, a containing cavity 9, a Du Re ceramic fiber blanket 10, a boron nitride flat bottom crucible 11, a quartz crucible 12, a seed crystal 13 and boron oxide 14;
the first temperature-control thermocouple T1, the second temperature-control thermocouple T2, the third temperature-control thermocouple T3 and the fourth temperature-control thermocouple T4, the fifth temperature-control thermocouple T5, the sixth temperature-control thermocouple T6, the seventh temperature-control thermocouple T7, the eighth temperature-control thermocouple T8 and the ninth temperature-control thermocouple T9.
Detailed Description
The invention will be described in detail below with reference to the attached drawings:
as shown in fig. 1: the crystal growth single crystal furnace comprises a pressure vessel 1, wherein a heater is arranged in the pressure vessel 1, the heater comprises a heater shell 2, a heater bracket 3 is arranged between the heater shell 2 and the pressure vessel 1, a furnace core group is arranged in the central position inside the heater shell 2, the furnace core group comprises a quartz rod 4, a wet felt 5 of aluminum silicate is arranged outside the quartz rod 4, a hearth tube 6 is sleeved outside the wet felt 5, the diameter of the quartz rod 4 is 50-80% of the inner diameter of the hearth tube 6, and the preferred embodiment is 65%; the furnace core group is sleeved with a heating wire 7, a high-temperature-resistant cement layer is arranged outside the furnace pipe 6, the heating wire 7 is arranged in the high-temperature-resistant cement layer, a first temperature control group and a second temperature control group are arranged between the heating wire 7 and the heater shell 2, and the first temperature control group and the second temperature control group are symmetrically arranged along the central line of the furnace pipe 6; the first temperature control group comprises a plurality of first thermocouple groups, and the second temperature control group comprises a plurality of second thermocouple groups; an alumina powder 8 is arranged between the heater shell 2 and the furnace core group, the first thermocouple group and the second thermocouple group are both positioned on the outer wall of the furnace pipe 6, the middle part of the furnace pipe 6 is provided with a containing cavity 9, and the upper end part of the furnace pipe 6 is provided with a Du Re ceramic fiber blanket 10.
The first temperature control group comprises a first temperature control area, a second temperature control area, a third temperature control area and a fourth temperature control area, the first temperature control area is provided with a first temperature control thermocouple T1 at the center, a second temperature control thermocouple T2 at the center of the second temperature control area, a third temperature control thermocouple T3 at the center of the third temperature control area, a fourth temperature control thermocouple T4 at the center of the fourth temperature control area, and the first temperature control thermocouple T1, the second temperature control thermocouple T2, the third temperature control thermocouple T3 and the fourth temperature control thermocouple T4 are all arranged on the outer wall of the hearth pipe 6. The second temperature control group comprises a fifth temperature control thermocouple T5, a sixth temperature control thermocouple T6, a seventh temperature control thermocouple T7, an eighth temperature control thermocouple T8 and a ninth temperature control thermocouple T9 which are all positioned on the outer wall of the hearth pipe 6, the fifth temperature control thermocouple T5 is arranged outside the hearth pipe 6 at the end part of the quartz rod 4 positioned in the hearth pipe 6, and the distance between two adjacent temperature measuring thermocouples of the fifth temperature control thermocouple T5, the sixth temperature control thermocouple T6, the seventh temperature control thermocouple T7, the eighth temperature control thermocouple T8 and the ninth temperature control thermocouple T9 is 30mm.
The distance between the heating wires 7 in the first temperature control area is 150mm, the distance between the heating wires 7 in the second temperature control area is 250mm, the distance between the heating wires 7 in the third temperature control area is 150mm, and the distance between the heating wires 7 in the fourth temperature control area is 150mm.
The crystal growth crucible of this embodiment is a cylindrical boron nitride flat bottom crucible 11.
The invention discloses a crystal growth method utilizing the crystal growth single crystal furnace and a crucible, which comprises the following steps:
the polycrystalline material, seed crystal 13, boron oxide, red phosphorus and other raw materials are processed and then are filled into a boron nitride flat bottom crucible 11. Then placing the boron nitride flat bottom crucible 11 into the quartz crucible 12, and vacuum sealing the boron nitride flat bottom crucible 11 into the quartz crucible 12 by using oxyhydrogen flame sintering; preparing a quartz rod 4, wrapping the quartz rod 4 by using a wet felt 5 of aluminum silicate, then placing the quartz rod into a hearth pipe 6, and baking and shaping the quartz rod into a furnace core group by using the temperature of 1000-1200 ℃; the furnace core was assembled inside the heater and the end voids were filled with Du Re ceramic fiber blanket 10. Then the external circuit, the air circuit and the water circuit are connected, and the furnace body is installed.
The temperature of the heater is raised, the temperature of four temperature areas is controlled through a first temperature control thermocouple T1, a second temperature control thermocouple T2, a third temperature control thermocouple T3 and a fourth temperature control thermocouple T4, the set temperature of the first temperature control thermocouple T1, the set temperature of the second temperature control thermocouple T2, the set temperature of the third temperature control thermocouple T3 and the set temperature of the fourth temperature control thermocouple T4 are 1000-1090 ℃, when the heater is heated, boron nitride is heated to about 450 ℃ to melt the crystal to wrap the liquid seal, the polycrystalline material is melted at about 1070 ℃ to completely melt the upper part of the seed crystal 13, the upper part of the seed crystal 13 is melted until the upper part of the seed crystal is melted, the fifth temperature control thermocouple T5, the sixth temperature control thermocouple T6, the seventh temperature control thermocouple T7, the eighth temperature control thermocouple T8 and the ninth temperature control thermocouple T9 are sequentially raised, then the crystal grows from bottom to top, the solid-liquid interface is gradually moved upwards, and the crystal growth is completed.
After the growth is completed, the quartz crucible 12 is taken out after the temperature is reduced, the quartz crucible is put into an ultrasonic hot water tank after the tube is opened to be separated from the crystal rod, then a section of perfect crystal is cut to be used as a seed crystal 13, the rest part of the crystal is cut, the crystal flows into the next working procedure to be processed into a product after the detection data are qualified, and the crystal is basically free from loss in the whole process.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention. The technology, shape, and construction parts of the present invention, which are not described in detail, are known in the art.
Claims (3)
1. The crystal growth single crystal furnace comprises a pressure container and a crucible, wherein a heater is arranged in the pressure container, the heater comprises a heater shell, and a furnace core group is arranged at the central position inside the heater shell; the method is characterized in that: the furnace core group is sleeved with heating wires, a first temperature control group and a second temperature control group are arranged between the heating wires and the heater shell, and the first temperature control group and the second temperature control group are symmetrically arranged along the central line of the furnace core group; the first temperature control group comprises a plurality of first thermocouple groups, and the second temperature control group comprises a plurality of second thermocouple groups; alumina powder is arranged between the heater shell and the furnace core group, the first thermocouple group and the second thermocouple group are both positioned on the outer wall of the furnace core group, the middle part of the furnace core group is provided with a containing cavity, and the end part of the furnace core group is provided with a Du Re ceramic fiber blanket; the furnace core group comprises a quartz rod, a wet felt is arranged outside the quartz rod, a hearth pipe is sleeved outside the wet felt, and the diameter of the quartz rod is 50% -80% of the inner diameter of the hearth pipe; the first temperature control group comprises a first temperature control area, a second temperature control area, a third temperature control area and a fourth temperature control area, wherein a first temperature control thermocouple is arranged in the center of the first temperature control area, a second temperature control thermocouple is arranged in the center of the second temperature control area, a third temperature control thermocouple is arranged in the center of the third temperature control area, a fourth temperature control thermocouple is arranged in the center of the fourth temperature control area, and the first temperature control thermocouple, the second temperature control thermocouple, the third temperature control thermocouple and the fourth temperature control thermocouple are all arranged on the outer wall of the hearth pipe; the second temperature control group comprises a fifth temperature control thermocouple, a sixth temperature control thermocouple, a seventh temperature control thermocouple, an eighth temperature control thermocouple and a ninth temperature control thermocouple which are all positioned on the outer wall of the hearth pipe, wherein the fifth temperature control thermocouple is arranged on the outer side of the hearth pipe, which is positioned at the end part of the quartz rod in the hearth pipe, and the distance between two adjacent temperature measuring thermocouples of the fifth temperature control thermocouple, the sixth temperature control thermocouple, the seventh temperature control thermocouple, the eighth temperature control thermocouple and the ninth temperature control thermocouple is 30mm; the interval between the heating wires in the first temperature control area is 150mm, the interval between the heating wires in the second temperature control area is 250mm, the interval between the heating wires in the third temperature control area is 150mm, and the interval between the heating wires in the fourth temperature control area is 150mm; the furnace pipe is externally provided with a high-temperature-resistant cement layer, and the heating wire is arranged in the high-temperature-resistant cement layer; the crucible is a cylindrical flat bottom crucible made of boron nitride material.
2. A crystal growth single crystal furnace according to claim 1, wherein: a heater bracket is arranged between the heater shell and the pressure vessel.
3. A crystal growth method using the single crystal furnace of claim 1, characterized in that: the method comprises the following steps:
s1, processing polycrystalline materials, seed crystals, boron oxide and red phosphorus raw materials, and then loading the processed polycrystalline materials, seed crystals, boron oxide and red phosphorus raw materials into a boron nitride flat-bottom crucible;
s2, placing the boron nitride flat-bottom crucible into a quartz crucible, and vacuum sealing the boron nitride flat-bottom crucible into the quartz crucible by using oxyhydrogen flame sintering;
s3, preparing a quartz rod, wrapping the quartz rod by using a wet felt of aluminum silicate, then placing the quartz rod into a hearth pipe, and baking and shaping the quartz rod into a furnace core group; assembling the furnace core into the heater, and filling the gaps of the end parts by using Du Re ceramic fiber blankets;
s4, heating the heater, controlling the temperature of the four temperature areas through a first temperature control thermocouple, a second temperature control thermocouple, a third temperature control thermocouple and a fourth temperature control thermocouple, enabling the fifth temperature control thermocouple, the sixth temperature control thermocouple, the seventh temperature control thermocouple, the eighth temperature control thermocouple and the ninth temperature control thermocouple to rise in sequence after seed crystals are melted, then cooling to enable crystals to grow from bottom to top, enabling a solid-liquid interface to gradually move upwards, and completing crystal growth;
the baking temperature of the furnace core group is 1000-1200 ℃, and the setting temperature of the first temperature control thermocouple, the second temperature control thermocouple, the third temperature control thermocouple and the fourth temperature control thermocouple is 1000-1090 ℃.
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