CN107829134B - Aluminum nitride single crystal growth device and method without seed crystal bonding technology - Google Patents
Aluminum nitride single crystal growth device and method without seed crystal bonding technology Download PDFInfo
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- CN107829134B CN107829134B CN201711171129.9A CN201711171129A CN107829134B CN 107829134 B CN107829134 B CN 107829134B CN 201711171129 A CN201711171129 A CN 201711171129A CN 107829134 B CN107829134 B CN 107829134B
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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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
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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
- C30B29/403—AIII-nitrides
Abstract
The invention discloses an aluminum nitride single crystal growth device and process without a seed crystal bonding technology, and relates to a semiconductor manufacturing technology. The growing device comprises: the device comprises a heating system, an infrared temperature measuring system, seed crystals, a growth crucible, a crucible partition plate and a double-layer nested crucible; the heating system is arranged at the outermost side; the bottom and the top of the crucible have temperature difference; the crucible is arranged in the heat insulation material; placing seed crystals at the bottom of the crucible; the double-layer nested crucible is vertically arranged on the upper side of the crucible partition plate and comprises an inner-layer crucible and an outer-layer crucible; the height of the walls of the inner and outer layer crucibles remains the same; high-purity aluminum nitride powder is filled between the side walls of the inner and outer layer crucibles. The method can reduce the doping of impurity elements of the aluminum nitride single crystal, improve the crystal quality of the aluminum nitride single crystal, increase the usable area of the single crystal, is simple and easy to use, is beneficial to realizing the preparation of the aluminum nitride single crystal with low cost, and can avoid the influence on the growth of the aluminum nitride single crystal due to the use of a seed crystal bonding technology.
Description
Technical Field
The invention relates to a semiconductor manufacturing device and a semiconductor manufacturing process, in particular to an aluminum nitride (AlN) single crystal growing device and a process method which do not need a seed crystal bonding technology.
Background
The third generation semiconductor material has a forbidden band width generally greater than 3.0 ev, so it is also called as wide band gap semiconductor, and the aluminum nitride material belongs to it, and it has excellent performances such as high thermal conductivity, high breakdown field strength, high saturated electron drift rate and high bonding energy, and has a huge application prospect in high temperature, high frequency, high power and anti-radiation devices, and research and development of aluminum nitride single crystal material has become a hot spot in the semiconductor field. At present, the method of Physical Vapor Transport (PVT) is mainly adopted to prepare the aluminum nitride single crystal, the method of physical vapor transport refers to that a high-temperature area and a low-temperature area are artificially arranged at different thicknesses of each part by using a heat preservation system, solid raw materials are evaporated in the high-temperature area, and crystals grow in the low-temperature area by using the diffusion of steam and the transport of vapor along a temperature gradient. More than 1 inch of single crystals must be obtained using seed deposition. The physical vapor transport method has the characteristics of high growth rate, good crystal integrity and the like, and a large number of researches show that the physical vapor transport method is one of the most effective ways for preparing the large-size aluminum nitride single crystal.
In the process of using the physical vapor transport method, the top of the crucible is generally set to be a low-temperature region and the bottom is set to be a high-temperature region by the conventional device and process, and the seed crystal is bonded on the crucible top cover. However, compared with the growth of silicon carbide single crystal, the seed crystal bonding technology is used in the growth process of aluminum nitride single crystal, which has great difficulty:
the seed crystal bonding technology needs a high-temperature adhesive (with the temperature resistance of more than 2300 ℃), the adhesive capable of reaching the high temperature mainly contains carbon, carbon (C) is a main impurity source of AlN single crystals and has serious harm to the crystal quality of the AlN single crystals, and meanwhile, the adhesive can corrode and embrittle tungsten heater components of a tungsten crucible. But the non-carbon-containing high-temperature adhesive has few types, high price and obviously inferior bonding effect to the carbon-containing adhesive;
secondly, the seed crystal bonding technology has strict requirements on the technological process, micro pores are easily formed in the uneven coating and curing process, and the difference of the thermal conductivity of the micro pores causes uneven distribution of the temperature field on the surface of the seed crystal, thereby influencing the usable area of the single crystal;
and (III) once the bonding is not firm, the seed crystal is easy to fall off in the growth process, so that the whole experiment fails and other problems are easily caused.
Therefore, the quality of the generated aluminum nitride single crystal is easily influenced by the traditional method for adhering the seed crystal in the physical vapor transport method, so that the aluminum nitride single crystal growth device and the aluminum nitride single crystal growth process adopting the seed crystal-free adhering technology are urgently needed.
Disclosure of Invention
The invention provides a device and a process for growing aluminum nitride single crystals without seed crystal bonding technology in order to overcome the defects of the prior art, the device and the process can reduce the doping of impurity elements of the aluminum nitride single crystals, improve the crystal quality of the aluminum nitride single crystals and increase the usable area of the single crystals, meanwhile, the device and the process are simpler, are beneficial to realizing the preparation of the aluminum nitride single crystals with low cost, and are a device and a process which can avoid the influence on the growth of the aluminum nitride single crystals caused by the use of the seed crystal bonding technology.
The technical scheme provided by the invention is as follows:
an aluminum nitride single crystal growth apparatus without a seed crystal bonding technique, comprising: the device comprises a heating system, an infrared temperature measuring system, seed crystals, a growth crucible, a crucible partition plate and a double-layer nested crucible; the heating system is arranged at the outermost side; the heating system consists of an induction coil and graphite, the crucible is arranged in a heat insulation material, a lower opening is arranged in the center of the bottom of the crucible, and the infrared temperature measurement system carries out infrared temperature measurement through the lower opening; placing seed crystals at the bottom of the crucible; a large round hole is reserved in the middle of the crucible partition plate, and a plurality of small round holes are uniformly distributed on the partition plate; a double-layer nested crucible is vertically arranged on the upper side of the partition plate, the inner layer crucible only has a side wall, and is hollow and bottomless; the outer crucible comprises a side wall and a bottom; the heights of the inner crucible wall and the outer crucible wall are kept the same; high-purity aluminum nitride powder is filled between the side wall of the inner crucible and the side wall of the outer crucible.
In the above aluminum nitride single crystal growth apparatus, further:
the heating system improves the existing heat preservation system, so that the thickness of the heat preservation material at the top is larger than that at the bottom, the heat preservation performance at the bottom is weaker than that at the top, the temperature gradient is inverted, and the temperature difference between the bottom and the top of the crucible is ensured to be about 50-500 ℃;
the heating system can adopt various modes such as induction heating, resistance heating and the like; when the graphite heating device is specifically implemented, the induction coil is electrified to heat the graphite in a heating mode;
the crucible can be a tantalum carbide ceramic crucible sintered by tantalum carbide powder, a tantalum crucible carbonized on the surface of metal tantalum or a tungsten crucible; the diameter of an opening left in the middle of the bottom of the crucible is between 5mm and 10 mm; the material of the crucible can be tantalum carbide (TaC), tantalum (Ta), Boron Nitride (BN), tungsten (W) and the like, the diameter of the crucible can be in the range of 50mm-150mm, and the height of the crucible can be in the range of 70mm-300 mm;
the diameter of the inner crucible of the double-layer nested crucible can be 20mm-75mm, the height of the inner crucible wall and the outer crucible wall is kept the same, the height is 35mm-195mm, and the distance between the inner crucible wall and the outer crucible wall is 20mm-60 mm.
The invention also provides a method for preparing the aluminum nitride single crystal by using the aluminum nitride single crystal growth device of the seedless crystal bonding technology, which comprises the following steps:
1) heating to high temperature by using a heating system;
2) sublimating the high-purity aluminum nitride powder in the double-layer nested crucible at high temperature to form aluminum nitride gas; the aluminum nitride gas moves upwards along the crucible wall of the double-layer nested crucible to reach the top of the double-layer nested crucible;
3) the thicknesses of the heat preservation systems at the top and the bottom of the crucible are different, a temperature difference of about 50-500 ℃ exists between the heat preservation systems, a temperature difference of about 40-200 ℃ exists between the partition plate of the crucible and the bottom of the crucible, a temperature gradient (temperature field) appears in the crucible, the part of the seed crystal is a low-temperature area, and the top of the crucible is a high-temperature area;
4) under the action of a temperature field, source gas simultaneously moves downwards from the top of the crucible along the direction of temperature gradient from the outer wall of the inner crucible and the inner wall of the outer crucible in the double-layer nested crucible;
5) when the source gas reaches the surface of the seed crystal at the bottom of the crucible, the source gas is desublimated into aluminum nitride single crystal solid;
thereby preparing an aluminum nitride single crystal.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides an aluminum nitride single crystal growth device and process based on a seedless bonding technology, which can avoid the influence on the growth of the aluminum nitride single crystal due to the use of the seed bonding technology. The invention increases the area and thickness of the AlN single crystal, improves the single crystal rate, reduces the dislocation density of the surface and eliminates cracks; the doping of impurity elements of the aluminum nitride single crystal can be reduced, the crystal quality of the aluminum nitride single crystal is improved, the usable area of the single crystal is increased, and meanwhile, the device and the process method are simpler, and the preparation of the aluminum nitride single crystal with low cost is facilitated.
Drawings
FIG. 1 is a structural diagram of an apparatus for growing a single crystal of aluminum nitride according to the present invention without the need for bonding a seed crystal;
the method comprises the following steps of 1-heating system, 2-crucible, 3-double-layer nested crucible, 4-aluminum nitride source powder, 5-partition plate and 6-seed crystal.
FIG. 2 is a graph showing the temperature distribution in the crucible during the growth of an aluminum nitride single crystal according to the embodiment of the present invention. The ordinate is the temperature of growth (unit: degrees centigrade) and the abscissa is the position in the crucible (unit: mm).
Detailed Description
The invention will be further described by way of examples, without in any way limiting the scope of the invention, with reference to the accompanying drawings.
The invention provides an aluminum nitride single crystal growth device and a process method without a seed crystal bonding technology.
FIG. 1 is a structural diagram of an aluminum nitride single crystal growth apparatus of the present invention without bonding a seed crystal; wherein, 1 is a heating system, 2 is a crucible, 3 is a double-layer nested crucible, 4 is aluminum nitride source powder, 5 is a partition plate, and 6 is seed crystal. Wherein:
(1) the outermost side of the growing device is a heating system. The heating system can adopt multiple modes such as induction heating, resistance heating and the like, the heat preservation performance of the bottom of a common heat preservation system of a traditional growing device is superior to that of the top to manufacture a temperature gradient, the heat preservation system of the traditional growing device is adjusted, the thickness of a heat preservation material of the top is more than that of the bottom, the heat preservation performance of the bottom is weaker than that of the top, the temperature gradient is inverted, the temperature difference between the bottom and the top of the crucible is ensured to be about 50-500 ℃, the specific temperature distribution is shown in a graph (2), an opening is left in the center of the bottom of the crucible, the diameter of the opening is between 5mm and 10mm, and the infrared temperature measurement system can carry out infrared temperature measurement.
(2) The crucible is placed in a heat-insulating material, the material of the crucible can be tantalum carbide (TaC), tantalum (Ta), Boron Nitride (BN), tungsten (W) and the like, the diameter of the crucible can be within the range of 50mm-150mm, and the height of the crucible can be within the range of 70mm-300 mm.
(3) And a seed crystal is placed at the bottom of the crucible, the material of the seed crystal can be selected from a 6H-SiC wafer, a 4H-SiC wafer, a hot-pressed AlN ceramic wafer and the like, and the diameter of the seed crystal can be in the range of 40mm-140 mm.
(4) A partition plate is placed in the middle of a crucible, the size of the partition plate is within the range of 55mm-140mm, the distance between the partition plate and the bottom of the crucible is 20mm-50mm, the temperature difference between the partition plate and the bottom of the crucible is guaranteed to be about 40-200 ℃, a large round hole is reserved in the middle of the partition plate, the diameter of the round hole is 20mm-75mm, a plurality of small round holes are uniformly distributed on the partition plate, and the diameter of the round holes is about 7 mm.
(5) A double-layer nested crucible is vertically arranged on the upper side of the partition plate, the inner layer crucible only has a side wall, and the crucible is hollow and has no bottom. The diameter of the inner crucible can be 20mm-75mm, the height of the inner crucible wall and the outer crucible wall is kept the same, and the height is between
35mm-195mm, the distance between the inner and outer crucible walls is 20mm-60mm, and high-purity aluminum nitride powder is filled between the inner and outer crucible walls.
In specific implementation, the growth of the aluminum nitride single crystal by using the growth device comprises the following steps:
(1) and heating the growth crucible by using a heating system.
(2) The high-purity aluminum nitride powder in the double-layer nested crucible is sublimated and vaporized at the high temperature of about 2000 ℃. The vaporized aluminum nitride moves up the crucible wall of the double nested crucible to the top of the crucible.
(3) Because the thicknesses of the heat insulating materials at the top and the bottom of the crucible are different, the temperature difference between the heat insulating materials at the top and the bottom of the crucible is about 50-500 ℃, the temperature difference between the partition board and the bottom of the crucible is about 40-200 ℃, the temperature gradient occurs in the crucible, and the part where the seed crystal is located is a low-temperature region. The top of the crucible is a high temperature zone.
(4) Under the action of the temperature field, the source gas moves downwards from the top of the crucible along the direction of temperature gradient from the inner wall and the outer wall of the double-layer nested crucible simultaneously.
(5) When the source gas reaches the bottom seed surface of the crucible, the source gas condenses into an aluminum nitride single crystal solid.
The following schemes are embodiments of the aluminum nitride single crystal growth device and the method adopting the seed crystal bonding-free technology, and FIG. 2 is a temperature distribution diagram in a crucible in the aluminum nitride single crystal growth process of the embodiment of the invention; the specific differences are shown in the following table.
The method comprises the following specific steps:
the first embodiment is as follows: the growth of high-purity single-crystal aluminum nitride is completed in a tantalum carbide crucible pressed and sintered by powder metallurgy by using an aluminum nitride single-crystal growth device without a seed crystal bonding technology.
The specific growth process is as follows:
(1) the induction coil is electrified to heat the graphite.
(2) Adjusting the structure of the heat-insulating layer to make the thickness of the heat-insulating material at the top be greater than that at the bottom and make the temperature at the top of the crucible be higher than that at the bottom by about 400 ℃. Meanwhile, an opening with the diameter of 9mm is reserved right below the crucible, so that the infrared temperature measurement system can perform non-contact infrared measurement on the thermal field condition at the bottom of the crucible.
(3) The crucible is a tantalum carbide ceramic crucible sintered by tantalum carbide powder, and the size of the tantalum carbide ceramic crucible is 70mm in diameter and 100mm in height.
(4) Seed crystals are placed at the bottom of the tantalum carbide ceramic crucible, the seed crystals are selected to be prepared in advance and 6H-SiC seed crystals in the (0001) direction, and the diameter of the seed crystals is 50 mm.
(5) And a partition plate is arranged at the middle lower part of the tantalum carbide ceramic crucible, and the distance between the partition plate and the bottom of the tantalum carbide ceramic crucible is 20 mm. The diameter of the partition board is 70mm, a large round hole is reserved in the middle of the partition board, the diameter of the round hole is 30mm, the round holes are uniformly distributed in the partition board, and the diameter of the round hole is 7 mm.
(6) The double-layer nested crucible is vertically placed on the upper side of the partition plate, the diameter of the inner crucible is 25mm, the inner crucible only has a side wall, and the inner crucible is hollow and has no bottom. The height of the inner crucible wall and the outer crucible wall is kept the same, the height is 50mm, the distance between the inner crucible wall and the outer crucible wall is 10mm, and the high-purity aluminum nitride powder is placed at the joint of the inner crucible wall and the outer crucible wall and is placed by 35g each time.
(7) The equipment is heated to a high temperature of more than 2000 ℃ by a heating system, the temperature of the top of the crucible is 2500 ℃, and the temperature of the bottom of the crucible is 2100 ℃.
(8) The aluminum nitride powder is sublimated at high temperature, moves to a low-temperature area in the tantalum carbide ceramic crucible along the temperature gradient direction, and is sublimated to aluminum nitride solid on the surface of the low-temperature seed crystal, so that the growth of high-purity single crystal aluminum nitride is completed.
Example two: the growth of high purity single crystal aluminum nitride is accomplished in a carbonized tantalum metal crucible using an aluminum nitride single crystal growth apparatus that does not require a seed bonding technique.
The specific growth process is as follows:
(1) the induction coil is electrified to heat the graphite.
(2) Adjusting the structure of the heat-insulating layer to make the thickness of the heat-insulating material at the top be greater than that at the bottom and make the temperature at the top of the crucible be higher than that at the bottom by about 400 ℃. Meanwhile, an opening with the diameter of 9mm is reserved right below the crucible, so that the infrared temperature measurement system can perform non-contact infrared measurement on the thermal field condition at the bottom of the crucible.
(3) The crucible is a tantalum crucible with the carbonized surface of tantalum metal, and the size of the carbonized tantalum metal crucible is 80mm in diameter and 100mm in height.
(4) And placing seed crystals at the bottom of the carbonized metal tantalum crucible, and selecting the seed crystals as the prepared (0001) direction 6H-SiC seed crystals with the diameter of 50 mm.
(5) The baffle is placed in carbonized metal tantalum crucible middle part position, and the distance of baffle apart from carbonized metal tantalum crucible's bottom is 20mm, and the baffle diameter is 80mm, leaves a big round hole in the centre of baffle, and the diameter of round hole is 30mm, and also even distribution is some little round holes on the baffle, and the diameter is 7 mm.
(6) The double-layer nested crucible is vertically placed on the upper side of the partition board, the diameter of the inner-layer crucible is 30mm, the inner-layer crucible only has a side wall, and the crucible is hollow and has no bottom. The height of the inner crucible wall and the outer crucible wall is kept the same, the height is 50mm, the distance between the inner crucible wall and the outer crucible wall is 15mm, and the high-purity aluminum nitride powder is placed at the joint of the inner crucible wall and the outer crucible wall and is placed by 40g each time.
(7) The equipment is heated to a high temperature of more than 2000 ℃ by a heating system, the temperature of the top of the crucible is 2500 ℃, and the temperature of the bottom of the crucible is 2100 ℃. .
(8) The aluminum nitride powder is sublimated at high temperature, moves to a low-temperature area in the carbonized metal tantalum crucible along the temperature gradient direction, and is sublimated to aluminum nitride solid on the surface of the low-temperature seed crystal, so that the growth of high-purity single crystal aluminum nitride is completed.
Example three: the growth of high-purity single-crystal aluminum nitride is completed in a tungsten crucible by using an aluminum nitride single-crystal growth device without a seed crystal bonding technology.
The specific growth process is as follows:
(1) the high-purity tungsten net (resistance heating) is heated by passing current through the high-purity tungsten net.
(2) The multi-section high-purity tungsten screen is used as a heat insulation layer, the structure (shape and number of layers) of the heat insulation layer is adjusted, so that the heat insulation effect of the top is greater than that of the bottom, and the temperature of the top of the crucible is about 400 ℃ higher than that of the bottom. Meanwhile, an opening with the diameter of 9mm is reserved right below the crucible, so that the infrared temperature measurement system can perform non-contact infrared measurement on the thermal field condition at the bottom of the crucible.
(3) The crucible is a high-purity tungsten crucible, and the size of the tungsten crucible is 70mm in diameter and 100mm in height.
(4) And placing seed crystals at the bottom of the tungsten crucible, wherein the seed crystals are selected from (0001) direction 6H-SiC seed crystals prepared in advance, and the diameter of the seed crystals is 50 mm.
(5) A partition plate is arranged at the middle lower part of the tungsten crucible, and the distance between the partition plate and the bottom of the tungsten crucible is 20 mm. The diameter of the partition board is 70mm, a large round hole is reserved in the middle of the partition board, the diameter of the round hole is 30mm, the round holes are uniformly distributed in the partition board, and the diameter of the round hole is 7 mm.
(6) The double-layer nested crucible is vertically placed on the upper side of the partition plate, the diameter of the inner crucible is 25mm, the inner crucible only has a side wall, and the inner crucible is hollow and has no bottom. The height of the inner crucible wall and the outer crucible wall is kept the same, the height is 50mm, the distance between the inner crucible wall and the outer crucible wall is 10mm, and the high-purity aluminum nitride powder is placed at the joint of the inner crucible wall and the outer crucible wall and is placed by 35g each time.
(7) The equipment is heated to a high temperature of more than 2000 ℃ by a heating system, the temperature of the top of the crucible is 2200 ℃, and the temperature of the bottom of the crucible is 1800 ℃.
(8) The aluminum nitride powder is sublimated at high temperature, moves to a low-temperature area in the tungsten crucible along the temperature gradient direction, and is sublimated to aluminum nitride solid on the surface of the low-temperature seed crystal, so that the growth of the high-purity single crystal aluminum nitride is completed.
It is noted that the disclosed embodiments are intended to aid in further understanding of the invention, but those skilled in the art will appreciate that: various substitutions and modifications are possible without departing from the spirit and scope of the invention and appended claims. Therefore, the invention should not be limited to the embodiments disclosed, but the scope of the invention is defined by the appended claims.
Claims (7)
1. An aluminum nitride single crystal growth apparatus without a seed crystal bonding technique, comprising: the device comprises a heating system, an infrared temperature measuring system, seed crystals, a growth crucible, a crucible partition plate and a double-layer nested crucible; the heating system is arranged at the outermost side of the growing device and consists of an induction coil and graphite; the thickness of the top heat-insulating material of the heating system is larger than that of the bottom heat-insulating material, so that the bottom heat-insulating property is weaker than that of the top, the temperature gradient is inverted, and the bottom and the top of the crucible have a temperature difference; the crucible is arranged in the heat insulation material, and the center of the bottom of the crucible is provided with a lower opening; the infrared temperature measurement system carries out infrared temperature measurement through the lower opening; placing seed crystals at the bottom of the crucible; a large round hole is arranged in the middle of the crucible partition plate, and a plurality of small round holes are uniformly distributed on the crucible partition plate; the double-layer nested crucible is vertically arranged on the upper side of the crucible partition plate and comprises an inner-layer crucible and an outer-layer crucible; the inner layer crucible only has a side wall, and is hollow without a bottom; the height of the side wall of the inner crucible and the height of the wall of the outer crucible are kept the same; high-purity aluminum nitride powder is filled between the side wall of the inner crucible and the side wall of the outer crucible; the diameter of the inner layer crucible is 20mm-75 mm; the height of the inner crucible wall and the outer crucible wall is 35mm-195 mm; the distance between the inner crucible wall and the outer crucible wall is 20mm-60 mm.
2. An apparatus for growing an aluminum nitride single crystal without seed crystal bonding technique according to claim 1, wherein the heating system is heated by induction heating or resistance heating.
3. An apparatus for growing an aluminum nitride single crystal without seed crystal bonding as defined in claim 1, wherein the heating system is a heating system in which the induction coil is heated by supplying an electric current to heat the graphite.
4. An aluminum nitride single crystal growth apparatus according to claim 1 which does not require a seed bonding technique, wherein the crucible is selected from a tantalum carbide ceramic crucible sintered with tantalum carbide powder, a tantalum crucible carbonized on the surface of metallic tantalum or a tungsten crucible; the crucible is made of tantalum carbide, tantalum, boron nitride or tungsten.
5. An aluminum nitride single crystal growth apparatus without seed crystal bonding technique as defined in claim 1, wherein the diameter of the opening provided in the center of the bottom of the crucible is between 5mm and 10 mm; the diameter of the crucible is 50mm-150 mm; the height of the crucible is 70mm-300 mm.
6. A method for preparing an aluminum nitride single crystal by using the aluminum nitride single crystal growth device without seed crystal bonding technology as claimed in any one of claims 1 to 5, comprising the following steps:
1) heating to high temperature by using a heating system;
2) sublimating the high-purity aluminum nitride powder in the double-layer nested crucible at high temperature to form aluminum nitride gas; the aluminum nitride gas moves upwards along the crucible wall of the double-layer nested crucible to reach the top of the double-layer nested crucible;
3) the temperature difference exists between the heat preservation systems at the top and the bottom of the crucible, the temperature difference also exists between the crucible partition plate and the bottom of the crucible, the temperature gradient appears in the crucible, the part where the seed crystal is located is a low-temperature region, and the top of the crucible is a high-temperature region;
4) under the action of the temperature gradient, the source gas simultaneously moves downwards from the top of the crucible along the direction of the temperature gradient from the outer wall of the inner crucible and the inner wall of the outer crucible in the double-layer nested crucible;
5) when the source gas reaches the surface of the seed crystal at the bottom of the crucible, the source gas is desublimated into aluminum nitride single crystal solid;
thereby preparing an aluminum nitride single crystal.
7. The method of producing an aluminum nitride single crystal as defined in claim 6, wherein in the step 3), the temperature difference between the holding system at the top and bottom of the crucible is about 50 to 500 ℃ and the temperature difference between the crucible partition plate and the bottom of the crucible is about 40 to 200 ℃.
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| CN108624954A (en) * | 2018-03-29 | 2018-10-09 | 苏州奥趋光电技术有限公司 | A kind of method of isoepitaxial growth aluminum-nitride single crystal |
| CN108396375A (en) * | 2018-03-29 | 2018-08-14 | 苏州奥趋光电技术有限公司 | A kind of crucible device of isoepitaxial growth aluminum-nitride single crystal |
| CN109129833A (en) * | 2018-09-18 | 2019-01-04 | 北京大学 | Device and preparation method of the preparation for the carbonization tantalum crucible of growing aluminum nitride monocrystalline |
| CN111121454A (en) * | 2019-12-23 | 2020-05-08 | 武汉科技大学 | High-temperature sintering structure with double-layer nested structure |
| CN111334862A (en) * | 2020-04-08 | 2020-06-26 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Non-bonded seed crystal type tantalum crucible and crystal growth method |
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