CN114808107A - 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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- CN114808107A CN114808107A CN202210355085.XA CN202210355085A CN114808107A CN 114808107 A CN114808107 A CN 114808107A CN 202210355085 A CN202210355085 A CN 202210355085A CN 114808107 A CN114808107 A CN 114808107A
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- 239000013078 crystal Substances 0.000 title claims abstract description 118
- 238000002109 crystal growth method Methods 0.000 title claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 35
- 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
- 238000000034 method Methods 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 8
- 239000004568 cement Substances 0.000 claims description 7
- 229910052810 boron oxide Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- 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
- 238000007493 shaping process Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000004065 semiconductor Substances 0.000 abstract description 7
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 12
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- 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
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 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
- 238000005520 cutting process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 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
- 238000007789 sealing Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
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, wherein the crystal growth single crystal furnace comprises a pressure container, a heater is arranged in the pressure container, the heater comprises a heater shell, and a furnace core group is arranged in the center of the interior of the heater shell; a heating wire is sleeved outside the furnace core group, a first temperature control group and a second temperature control group are arranged between the heating wire 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 located on the outer wall of the furnace core group, the middle part of the furnace core group is provided with an accommodating cavity, and the end part of the furnace core group is provided with a ceramic fiber blanket. The invention can reduce the generation of polycrystal during the crystal growth and improve the crystal forming rate of the 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 crystallization rate of the existing indium phosphide single crystal growth is generally about 30 percent, which is an important factor for restricting the rapid development of the indium phosphide material. The 5G-generation technological innovation has brought about a 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 velocity, 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 ultimate 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, heat conductivity and electron average velocity. In addition, at present, the optical communication device mainly adopts indium phosphide-based materials, and indium phosphide-based lasers, modulators, detectors and modules thereof with high digital code rate and good wavelength monochromaticity are widely applied to optical networks, so that the rapid development of the transmission quantity of internet data information is promoted, and the requirements of people on the development of networks in the directions of higher speed and wider bandwidth are continuously met.
At present, indium phosphide single crystal growth is mainly carried out by putting seed crystal into a boron nitride crucible seed crystal cavity, putting polycrystal material, boron nitride, red phosphorus and the like into the crucible body, vacuumizing the crucible body by using a quartz tube, welding and sealing, putting the crucible body into a single crystal furnace, heating, melting all polycrystal material and the upper part of the seed crystal, cooling to enable the polycrystal material and the upper part of the seed crystal to grow upwards along the seed crystal, starting shouldering and growing beyond the seed crystal cavity in the upwards process, and gradually expanding the diameter of a grown 4-inch indium phosphide single crystal from about 10mm to about 100 mm; the diameter is enlarged in the shouldering process, the solid-liquid interface is gradually enlarged from a small value in the enlarging process, the shape control of the solid-liquid interface is very difficult, when the crystal begins to nucleate at the contact position of the interface edge and the boron nitride crucible, twin crystal lines growing inwards are very easily generated, when two twin crystal lines extend and meet towards the interior of the crystal, polycrystal is directly generated at the meeting position, and the whole crystal becomes polycrystal. According to the actual production statistics, 80% of all the ingots which are not grown into single crystals are caused by the above situation, and the solution of the problem has a great effect on the improvement of 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 growth is finished, boron oxide between a crystal bar and a boron nitride crucible is difficult to dissolve in the demolding process, and the demolding time is prolonged; in addition, the damage amount to the seed crystal cavity is large in the demolding process, a slender quartz rod is required to be wrapped in the center of a wet felt in the manufacturing process of the furnace core group in the original process, two temperature measuring thermocouples are manufactured around the quartz rod, a plurality of layers of wet felts and quartz sleeves are wrapped outside the quartz rod, and the quartz rod is manufactured into a shape matched with the quartz tube.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a crystal growth single crystal furnace, a crucible and a crystal growth method, which can reduce the generation of polycrystals during crystal growth and increase the crystal yield of single crystal growth.
The invention solves the technical problems by the following technical means:
a 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 in the center of the inside of the heater shell; a heating wire is sleeved outside the furnace core group, a first temperature control group and a second temperature control group are arranged between the heating wire 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 located on the outer wall of the furnace core group, the middle part of the furnace core group is provided with an accommodating cavity, and the end part of the furnace core group is provided with a 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. So, when preparing the core group, preparation simple process, and with the quartz rod diameter greatly increased of the diameter ratio prior art of quartz rod, make furnace body center heat-conduction more abundant, the crystal central temperature on same water flat line is on the low side at growth cooling in-process, preferentially forms the crystal nucleus, forms the solid-liquid interface of little protruding, has avoided the part to begin the nucleation at the crucible wall and begins twin crystal or the polycrystal of ingrowth, further improves the crystallization rate of crystal growth.
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, the four temperature control areas are arranged on one side of the outer wall of the hearth pipe, so that the temperature of the hearth pipe can be accurately controlled, 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, the fifth temperature control thermocouple is arranged on the outer side of the hearth pipe at the end part of the quartz rod positioned in the hearth pipe, and the distance between every two adjacent temperature control 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 30 mm. The 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 measured accurately, and the crystallization rate and the quality of single crystal growth are improved through accurate temperature control.
Further, the interval of heating wires in the first temperature control area is 150mm, the interval of heating wires in the second temperature control area is 250mm, the interval of heating wires in the third temperature control area is 150mm, and the interval of heating wires in the fourth temperature control area is 150 mm. Therefore, 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 wires are arranged in the high-temperature-resistant cement layer. The high-temperature-resistant cement layer can fix the heating wire, so that the heating wire is prevented from moving in the process.
Further, a heater bracket is arranged between the heater shell and the pressure container. The heater support 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 the polycrystalline material, the seed crystal, the boron oxide and the red phosphorus raw material and then putting the processed raw material into a boron nitride flat-bottom crucible;
s2, placing the boron nitride flat-bottom crucible into a quartz crucible, and sintering by using oxyhydrogen flame to seal the boron nitride flat-bottom crucible into the quartz crucible in vacuum;
s3, preparing a quartz rod, wrapping the quartz rod with a wet aluminum silicate felt, 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 gap at the end part with a Dethermic ceramic fiber blanket;
and S4, heating the heater, controlling the temperature of the four temperature zones through the first temperature control thermocouple, the second temperature control thermocouple, the third temperature control thermocouple and the fourth temperature control thermocouple, and after the seed crystals are molten, 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, and then cooling to enable crystals to grow from bottom to top, wherein a solid-liquid interface gradually moves upwards, and the growth of the crystals is completed.
Further, the baking temperature of the furnace core group is 1000-. During heating, the crystal is encapsulated by the molten boron nitride when the temperature is about 450 ℃, and the polycrystalline material is completely molten when the temperature is about 1070 ℃, so that the upper part of the seed crystal is molten.
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 the quartz crucible and the boron nitride crucible are easy to manufacture, the manufacturing process is simplified, the manufacturing cost is reduced compared with a special-shaped crucible, and the parts which are easy to damage do not exist in the transportation and use processes, thereby reducing the probability of damage and further reducing the cost.
2. The seed crystals used for producing the indium phosphide single crystal and the gallium arsenide single crystal are all very fine, the seed crystals with the diameter of about 8mm are placed into a small mouth of a special-shaped crucible, the temperature is reduced after the melting part is melted, the growth is carried out upwards, the diameter is gradually enlarged, twin crystals and polycrystal are very easy to appear in the enlarging process.
3. According to the single crystal growth method, as the size of the grown seed crystal is the same as that of the grown target, after the growth is finished, the whole crystal bar is a perfect crystal, only the part with higher impurity enrichment at the tail part of the crystal needs to be cut, and the head part of the crystal can be cut and then continuously used as the seed crystal for the next single crystal growth, so that the effect of recycling is achieved; compared with the prior art, the invention only occupies a larger amount of finished products at the early stage, but the seed crystals are hardly consumed in the process after the mass production, thereby reducing the production cost.
4. The boron nitride crucible used in the invention has simple appearance, and can better promote water molecules to enter a gap between the crucible and a crystal bar in the demolding process after growth is finished, promote sufficient dissolution of boron nitride, make demolding easier, and simultaneously reduce the loss of the boron nitride crucible in the demolding process.
5. The invention belongs to equal-diameter growth in the growth process of single crystals, and because the diameter is not expanded, the effective length of the crystal bar grown by the invention is longer due to the same weight of the fed materials.
6. According to the invention, the diameter of the quartz rod is increased, so that the heat conduction at the center of the furnace body is more sufficient, the temperature of the center of the crystal on the same horizontal line is lower in the growth and cooling processes, a crystal nucleus is preferentially formed, a slightly convex solid-liquid interface is formed, twin crystals or polycrystal which are partially nucleated on the crucible wall and grow inwards are avoided, and the crystal forming rate of the 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 polycrystalline material is easier to fill, and the requirement on the cutting shape of the polycrystalline material is not high, so that the time for selecting and filling the polycrystalline material is shortened, and the working efficiency is improved.
Drawings
FIG. 1 is a schematic view showing the structure of a single crystal growing furnace and a crucible according to the present invention.
The device comprises a pressure container 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 Dethermite ceramic fiber blanket 10, a boron nitride flat-bottom crucible 11, a quartz crucible 12, seed crystals 13 and boron oxide 14, wherein the heating wire is arranged in the furnace;
a first temperature-controlled thermocouple T1, a second temperature-controlled thermocouple T2, a third temperature-controlled thermocouple T3, a fourth temperature-controlled thermocouple T4, a fifth temperature-controlled thermocouple T5, a sixth temperature-controlled thermocouple T6, a seventh temperature-controlled thermocouple T7, an eighth temperature-controlled thermocouple T8, and a ninth temperature-controlled thermocouple T9.
Detailed Description
The invention will be described in detail below with reference to the following drawings:
as shown in fig. 1: the crystal growth single crystal furnace comprises a pressure container 1, a heater is arranged in the pressure container 1 and comprises a heater shell 2, a heater support 3 is arranged between the heater shell 2 and the pressure container 1, a furnace core group is arranged at the center inside the heater shell 2 and comprises a quartz rod 4, an aluminum silicate wet felt 5 is arranged outside the quartz rod 4, a hearth pipe 6 is arranged outside the wet felt 5, the diameter of the quartz rod 4 is 50% -80% of the inner diameter of the hearth pipe 6, and the preferred embodiment is 65%; a heating wire 7 is sleeved outside the hearth group, a high-temperature-resistant cement layer is arranged outside the hearth 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 center line of the hearth 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; alumina powder 8 is arranged between the heater shell 2 and the hearth group, the first thermocouple group and the second thermocouple group are both positioned on the outer wall of the hearth tube 6, the middle part of the hearth tube 6 is provided with an accommodating cavity 9, and the upper end part of the hearth tube 6 is provided with a Detherm 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, a first temperature control thermocouple T1 is arranged in the center of the first temperature control area, a second temperature control thermocouple T2 is arranged in the center of the second temperature control area, a third temperature control thermocouple T3 is arranged in the center of the third temperature control area, a fourth temperature control thermocouple T4 is arranged in 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 located on the outer wall of the hearth pipe 6, the fifth temperature control thermocouple T5 is arranged on the outer side of the hearth pipe 6 at the end part of the quartz rod 4 located in the hearth pipe 6, and the distance between two adjacent temperature measurement 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 30 mm.
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 150 mm.
The crystal growth crucible of the present embodiment is a cylindrical boron nitride flat-bottomed crucible 11.
The crystal growth method using the crystal growth single crystal furnace and the crucible comprises the following steps:
polycrystalline materials, seed crystals 13, boron oxide, red phosphorus and other raw materials are processed and then put into a boron nitride flat-bottom crucible 11. Then, the boron nitride flat-bottom crucible 11 is placed into a quartz crucible 12, and the boron nitride flat-bottom crucible 11 is sealed into the quartz crucible 12 in a vacuum manner by oxyhydrogen flame sintering; preparing a quartz rod 4, wrapping the quartz rod 4 with a wet aluminum silicate felt 5, then placing the quartz rod into a hearth pipe 6, and baking and shaping the quartz rod into a furnace core group at the temperature of 1000-; the core was assembled inside the heater with the end gap filled with a dumet ceramic fiber blanket 10. Then, an external circuit, an air passage and a water passage are connected, and the furnace body is installed.
And (3) heating the heater, controlling the temperature of the four temperature zones by 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, wherein the set temperature of 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 is 1000-1090 ℃, during heating, the temperature is increased to about 450 ℃ to melt the crystal wrapping liquid seal, the polycrystalline material is completely melted at about 1070 ℃, so that the upper part of the seed crystal 13 is melted, and the temperature 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 sequentially increased, then the temperature is reduced to enable the crystal to grow from bottom to top, and the solid-liquid interface gradually moves upwards, and the growth of the crystal is completed.
After the growth is finished, the quartz crucible 12 is cooled and taken out, the tube is opened and then placed into an ultrasonic hot water tank to be separated from a crystal bar, a section of intact crystal is cut to serve as a seed crystal 13, the rest part of the intact crystal is detected, the qualified detection data flows into the next procedure to be processed into a product, and the crystal is basically free of loss in the whole process.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims. The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.
Claims (10)
1. A 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 in the center of the inside of the heater shell; the method is characterized in that: a heating wire is sleeved outside the furnace core group, a first temperature control group and a second temperature control group are arranged between the heating wire 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 located on the outer wall of the furnace core group, a containing cavity is arranged in the middle of the furnace core group, and a Dethermit ceramic fiber blanket is arranged at the end of the furnace core group.
2. The crystal growth single crystal furnace of claim 1, wherein: 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.
3. The crystal growth single crystal furnace of claim 1, wherein: 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.
4. The crystal growing single crystal furnace of claim 1, wherein: 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 located on the outer wall of the hearth pipe, the fifth temperature control thermocouple is arranged on the outer side of the hearth pipe at the end part of the quartz rod located in the hearth pipe, and the distance between every two adjacent temperature control 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 30 mm.
5. The crystal growth single crystal furnace of claim 2, wherein: the interval of the heating wires in the first temperature control area is 150mm, the interval of the heating wires in the second temperature control area is 250mm, the interval of the heating wires in the third temperature control area is 150mm, and the interval of the heating wires in the fourth temperature control area is 150 mm.
6. A crystal growing single crystal growing furnace according to any one of claims 1 to 5, wherein: and 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.
7. The crystal growth single crystal furnace of claim 6, wherein: and a heater bracket is arranged between the heater shell and the pressure container.
8. A crystal growth crucible, characterized in that: the crucible is applied to a crystal growth single crystal furnace as claimed in any one of claims 1 to 7, and is a cylindrical flat-bottomed crucible made of a boron nitride material.
9. A crystal growth method using the single crystal furnace of claim 7 and the crystal growth crucible of claim 8, characterized in that: the method comprises the following steps:
s1, processing the polycrystalline material, the seed crystal, the boron oxide and the red phosphorus raw material and then putting the processed raw material into a boron nitride flat-bottom crucible;
s2, placing the boron nitride flat-bottom crucible into a quartz crucible, and sintering by using oxyhydrogen flame to seal the boron nitride flat-bottom crucible into the quartz crucible in vacuum;
s3, preparing a quartz rod, wrapping the quartz rod with a wet aluminum silicate felt, 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 gap at the end part with a ceramic fiber blanket;
and S4, heating the heater, controlling the temperature of the four temperature zones through the first temperature control thermocouple, the second temperature control thermocouple, the third temperature control thermocouple and the fourth temperature control thermocouple, and after the seed crystals are molten, 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, and then cooling to enable crystals to grow from bottom to top, wherein a solid-liquid interface gradually moves upwards, and the growth of the crystals is completed.
10. A crystal growth method according to claim 9, characterized in that: the baking temperature of the furnace core group is 1000-.
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