CN107829134A - A kind of aluminum-nitride single crystal grower and method without seed crystal adhesive technology - Google Patents
A kind of aluminum-nitride single crystal grower and method without seed crystal adhesive technology Download PDFInfo
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- CN107829134A CN107829134A CN201711171129.9A CN201711171129A CN107829134A CN 107829134 A CN107829134 A CN 107829134A CN 201711171129 A CN201711171129 A CN 201711171129A CN 107829134 A CN107829134 A CN 107829134A
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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
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Abstract
The invention discloses a kind of aluminum-nitride single crystal grower and technique without seed crystal adhesive technology, it is related to semiconductor fabrication.Grower includes：Heating system, infrared temperature measurement system, seed crystal, growth crucible, crucible dividing plate and double-layer nested formula crucible；Heating system is placed in outermost；Crucible bottom has temperature difference with top；Crucible is placed in insulation material；Seed crystal is placed in the bottom of crucible；Double-layer nested formula crucible is placed on the upside of crucible dividing plate, including inner crucible and outer crucible vertically；The height of the wall of inside and outside crucible keeps identical；High purity silicon nitride aluminium powder is filled between the side wall of inside and outside crucible.The present invention can reduce the incorporation of aluminum-nitride single crystal impurity element, its crystal mass is improved, increases monocrystalline usable area, at the same it is easy to use, the preparation of the aluminum-nitride single crystal of low cost is advantageously implemented, can avoid growing so as to influence aluminum-nitride single crystal using bonding seed crystal technology.
Description
Technical field
The present invention relates to semiconductor- fabricating device and technique, more particularly to a kind of aluminium nitride without seed crystal adhesive technology
(AlN) single-crystal growing apparatus and process.
Background technology
The energy gap of third generation semi-conducting material is generally higher than 3.0 electron volts, therefore the wide bandgap semiconductor that is otherwise known as,
Aluminium nitride material just belongs to wherein, and it has high heat conductance, high breakdown field strength, high saturated electrons drift speed and high bonding energy etc.
Excellent properties, possess huge application prospect in terms of high temperature, high frequency, high power and radioresistance device, for aluminum-nitride single crystal
The research and development of material has become a focus of semiconductor applications.At present, mainly using physical vapor transport (PVT)
Method prepare aluminum-nitride single crystal, physical vapor transport method refers to artificial using the difference of heat-insulation system throughout thickness
High-temperature region and low-temperature space are set, and solid feed is evaporated in high-temperature region, and the diffusion of steam and transporting for gas phase are utilized along thermograde
Crystal is grown in low-temperature space, monocrystalline can be gone out using crystal raw material spontaneous nucleation growth using this method, but spontaneous nucleation is only
Grade little crystal grain can be obtained.More than 1 inch monocrystal must then utilize seed deposition and obtain.Physical carbon burdening has
The features such as growth rate is fast, crystalline perfection is good, substantial amounts of research show that physical carbon burdening is to prepare large scale aluminium nitride
One of most effective approach of monocrystalline.
Among the process using physical vapor transport method, existing traditional device and technique typically set crucible top
Low-temperature space is set to, bottom is arranged to high-temperature region, and seed crystal is bonded on crucible top cover.But compared with silicon carbide monocrystal growth,
Using seed crystal adhesive technology, then there is great difficulty in aluminum-nitride single crystal growth course:
(1) seed crystal adhesive technology need to use high temperature adhesive (heatproof is up to more than 2300 DEG C), can reach such high temperature
The main carbonaceous component of bonding agent, carbon (C) are the main impurity sources of AlN monocrystalline, have serious harm to its crystal mass, also simultaneously
There are corrosion and brittle conduct to tungsten crucible tungsten heater assembly.But non-carbon-containing high temperature adhesive species is seldom, it is expensive and
Adhesive effect is substantially not so good as carbon containing bonding agent；
(2) seed crystal adhesive technology is strict to technical process requirement, and coating uneven curing process easily forms micro- stomata, its
The difference of thermal conductivity will cause seed crystal face thermal field skewness, influence the usable area of monocrystalline；
(3) once bonding is insecure, easily cause seed crystal in growth course and come off and cause whole the failure of an experiment etc. to be permitted
More problems.
As can be seen here, the method for bonding seed crystal traditional in physical vapor transport method easily influences the aluminium nitride list of generation
Brilliant quality, so there is an urgent need to a kind of the aluminum-nitride single crystal grower and technique of no seed crystal adhesive technology.
The content of the invention
For overcome the deficiencies in the prior art, the present invention proposes a kind of aluminum-nitride single crystal without seed crystal adhesive technology and given birth to
Growth device and technique, the present invention can reduce the incorporation of aluminum-nitride single crystal impurity element, improve its crystal mass, increase monocrystalline can
With area, while this device and comparison of processes are simple, are advantageously implemented the preparation of the aluminum-nitride single crystal of low cost, are one
Kind can be avoided using bonding seed crystal technology so as to influence the device and technique that aluminum-nitride single crystal grows.
Technical scheme provided by the invention is：
A kind of aluminum-nitride single crystal grower without seed crystal adhesive technology, including：Heating system, infrared temperature measurement system,
Seed crystal, growth crucible, crucible dividing plate and double-layer nested formula crucible；Heating system is in outermost；Heating system by induction coil and
Graphite is formed, and crucible is placed in insulation material, and crucible bottom center is provided with shed, and infrared temperature measurement system is carried out by under shed
Infrared measurement of temperature；Seed crystal is placed in the bottom of crucible；A big hole is left in the centre of crucible dividing plate, is uniformly distributed on dividing plate
Multiple small sircle holes；Place double-layer nested formula crucible vertically on the upside of dividing plate, inner crucible only has side wall, hollow bottomless；Outer layer earthenware
Crucible includes side wall and bottom；Inner crucible wall is identical with the height holding of outer layer sidewall of crucible；The side wall of inner crucible and outer crucible
Side wall between fill high purity silicon nitride aluminium powder.
In above-mentioned aluminum-nitride single crystal grower, further：
Heating system is improved to existing heat-insulation system so that top insulation material thickness is more than bottom, makes bottom
Heat-insulating property is weaker than top, is inverted its thermograde, and the temperature difference at guarantee crucible bottom and top is at 50-500 DEG C or so；
Heating system can use the various ways such as sensing heating, resistance heating；The present invention is when it is implemented, induction coil leads to
Enter electric current to heat the mode of graphite heating；
Crucible can choose the tantalum crucible or tungsten earthenware of the tantalum carbide ceramics crucible of ramet powder sintering, metal tantalum surface carbonation
Crucible；Crucible bottom center leaves the diameter of opening between 5mm-10mm；The material of crucible can be ramet (TaC), tantalum
(Ta), boron nitride (BN), tungsten (W) etc., the diameter of crucible can be in the range of 50mm-150mm, highly can be in 70mm-300mm
In the range of；
The diameter of the inner crucible of double-layer nested formula crucible can be between 20mm-75mm, inner crucible wall and outer crucible
The height of wall keeps identical, and highly between 35mm-195mm, and the distance between inside and outside sidewall of crucible is in 20mm-60mm scopes
It is interior.
The present invention also provides a kind of aluminum-nitride single crystal grower using above-mentioned no seed crystal adhesive technology and prepares aluminium nitride
The method of monocrystalline, comprises the following steps：
1) carry out being heated to high temperature using heating system；
2) high temperature makes the high purity silicon nitride aluminium powder distillation vapour China in double-layer nested formula crucible, forms aluminium nitride gas；Nitridation
Sidewall of crucible of the aluminium gas along double-layer nested formula crucible moves upward to the top up to double-layer nested formula crucible；
3) crucible top is different with the heat-insulation system thickness of bottom, and there is 50-500 DEG C or so of temperature therebetween
Difference, there is 40-200 DEG C or so of temperature difference between crucible dividing plate and crucible bottom, there is thermograde (thermal field) in crucible,
Part is low-temperature space where seed crystal, and crucible top is high-temperature region；
4) in the presence of thermal field, source gas is from crucible top along thermograde direction while interior from double-layer nested crucible
The inwall of the outer wall of crucible and outer crucible moves downward；
5) when source gas reaches the bottom seed crystal face of crucible, source gas is sublimated as aluminum-nitride single crystal solid；
Thus aluminum-nitride single crystal is prepared.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention proposes a kind of the aluminum-nitride single crystal grower and technique of no seed crystal adhesive technology, can avoid using
Bonding seed crystal technology grows so as to influence aluminum-nitride single crystal.The area and thickness of the AlN monocrystalline of present invention increase growth, are improved single
Brilliant rate, reduce the dislocation density on its surface and eliminate crackle；The incorporation of aluminum-nitride single crystal impurity element can be reduced, it is brilliant to improve it
Weight, increase monocrystalline usable area, while this device and comparison of processes are simple, are advantageously implemented the nitridation of low cost
The preparation of aluminium monocrystalline.
Brief description of the drawings
Fig. 1 is the structure chart of the provided by the invention aluminum-nitride single crystal that need not be bonded seed crystal technology grower；
Wherein, 1- heating systems, 2- crucibles, the double-layer nested formula crucibles of 3-, 4- aluminum nitride source powder, 5- dividing plates, 6- seed crystals.
Fig. 2 is the temperature profile in crucible in aluminum-nitride single crystal growth course of the embodiment of the present invention.Ordinate is growth
Temperature (unit：Degree Celsius), abscissa is the position (unit in crucible：Millimeter).
Embodiment
Below in conjunction with the accompanying drawings, the present invention, the model of but do not limit the invention in any way are further described by embodiment
Enclose.
The invention provides a kind of aluminum-nitride single crystal grower and process without seed crystal adhesive technology.
Fig. 1 is the structure chart of the provided by the invention aluminum-nitride single crystal that need not be bonded seed crystal technology grower；Wherein,
1 is heating system, and 2 be crucible, and 3 be double-layer nested formula crucible, and 4 be aluminum nitride source powder, and 5 be dividing plate, and 6 be seed crystal.Wherein：
(1) grower outermost is heating system.Heating system can use a variety of sides such as sensing heating, resistance heating
Formula, better than top to manufacture thermograde, this patent will pass the heat-insulating property of the general heat-insulation system bottom of traditional grower
Bulk cargo is put heat-insulation system and adjusted, and top insulation material thickness is more than bottom, it is therefore an objective to and make bottom heat-insulating property be weaker than top,
It is inverted its thermograde, the temperature difference at guarantee crucible bottom and top is at 50-500 DEG C or so, specific Temperature Distribution example
As shown in figure (2), while crucible bottom center leaves opening, and the diameter of opening ensures infrared measurement of temperature system between 5mm-10mm
System can be by carrying out infrared measurement of temperature here.
(2) crucible is placed in insulation material, and the material of crucible can be ramet (TaC), tantalum (Ta), boron nitride (BN),
Tungsten (W) etc., the diameter of crucible can be in the range of 50mm-150mm, highly can be in the range of 70mm-300mm.
(3) seed crystal is placed in the bottom of crucible, the material of seed crystal can select 6H-SiC chips, 4H-SiC chips, hot pressing
AlN ceramic piece etc., seed crystal diameter can be in the range of 40mm-140mm.
(4) dividing plate is placed in crucible medium position, the size of dividing plate is in the range of 55mm-140mm, dividing plate and crucible bottom
Distance is between 20mm-50mm, and for the temperature difference of guarantee dividing plate and crucible bottom at 40-200 DEG C or so, the centre of dividing plate leaves one
Individual big hole, the diameter of circular hole are also uniformly dispersed with some small circular holes between 20mm-75mm on dividing plate, and diameter exists
7mm or so.
(5) a double-layer nested formula crucible is placed vertically on the upside of dividing plate, inner crucible only has side wall, hollow bottomless.It is interior
The diameter of crucible can be between 20mm-75mm, and inner crucible wall is identical with the height holding of outer layer sidewall of crucible, highly exists
Between 35mm-195mm, and the distance between inside and outside sidewall of crucible is in the range of 20mm-60mm, between crucible inside and outside wall
Fill high purity silicon nitride aluminium powder.
When it is implemented, comprised the following steps using above-mentioned grower growing aluminum nitride monocrystalline：
(1) growth crucible is heated using heating system.
(2) 2000 DEG C or so of high temperature makes the high purity silicon nitride aluminium powder distillation vaporization in double-layer nested formula crucible.Vaporization
Sidewall of crucible of the aluminium nitride along double-layer nested formula crucible is moved upward to up to crucible top.
(3) because crucible top is different with the insulation material thickness of bottom, there is 50-500 DEG C or so therebetween
Temperature difference, there is 40-200 DEG C or so of temperature difference between dividing plate and crucible bottom, there is thermograde, seed crystal institute in crucible
It is low-temperature space in part.Crucible top is high-temperature region.
(4) in the presence of thermal field, source gas is from crucible top along thermograde direction while out of double-layer nested crucible
Wall and outer wall move downward.
(5) when source gas reaches the bottom seed crystal face of crucible, source gas is sublimated as aluminum-nitride single crystal solid.
Following several schemes are without the aluminum-nitride single crystal grower of seed crystal adhesive technology and the implementation of method using this
Example, Fig. 2 is the temperature profile in crucible in aluminum-nitride single crystal growth course of the embodiment of the present invention；Its specific similarities and differences is as following
Shown in form.
It is specific as follows：
Embodiment one：The aluminium nitride without seed crystal adhesive technology is utilized in the carbonization tantalum crucible of powder metallurgy pressing sintering
Single-crystal growing apparatus completes the growth of high-purity single-crystal aluminum nitride.
Specific growth course is as follows：
(1) induction coil is passed through electric current to graphite heating.
(2) heat insulation layer structure is adjusted, top insulation material thickness is more than bottom, crucible top temperature is higher than bottom temperature
About 400 DEG C of degree.Diameter 9mm openings are left immediately below simultaneously, ensure that infrared temperature measurement system can enter to crucible bottom thermal field condition
Row non-contact infrared measures.
(3) crucible chooses the tantalum carbide ceramics crucible of ramet powder sintering, and tantalum carbide ceramics crucible size is diameter 70mm,
High 100mm.
(4) seed crystal is placed in the bottom of tantalum carbide ceramics crucible, selection seed crystal is (0001) direction 6H- ready in advance
SiC seed crystals, a diameter of 50mm of seed crystal.
(5) dividing plate is placed in tantalum carbide ceramics crucible middle and lower part position, dividing plate is apart from the bottom of tantalum carbide ceramics crucible
Distance is 20mm.A big hole is left in a diameter of 70mm of dividing plate, the centre of dividing plate, a diameter of 30mm of circular hole, on dividing plate
Circular hole, Circularhole diameter 7mm are dispersed with evenly.
(6) double-layer nested formula crucible, a diameter of 25mm of inner crucible are placed vertically on the upside of dividing plate, inner crucible only has
Side wall, it is hollow bottomless.Inner crucible wall is identical with the height holding of outer layer sidewall of crucible, is highly 50mm, and inside and outside sidewall of crucible it
Between distance be 10mm, high purity silicon nitride aluminium powder is placed in crucible inside and outside wall junction, places 35g every time.
(7) equipment is heated to 2000 DEG C of high temperature above using heating system, crucible top temperature is 2500 DEG C, bottom temperature
Spend for 2100 DEG C.
(8) high temperature makes aluminum nitride powder distil, and is moved in tantalum carbide ceramics crucible along thermograde direction to low-temperature space,
Low temperature seed crystal face is sublimated as aluminium nitride solid, the growth of completion high-purity single-crystal aluminum nitride.
Embodiment two：The aluminum-nitride single crystal grower without seed crystal adhesive technology is utilized in the metal tantalum crucible of carbonization
Complete the growth of high-purity single-crystal aluminum nitride.
Specific growth course is as follows：
(1) induction coil is passed through electric current to graphite heating.
(2) heat insulation layer structure is adjusted, top insulation material thickness is more than bottom, crucible top temperature is higher than bottom temperature
About 400 DEG C of degree.Diameter 9mm openings are left immediately below simultaneously, ensure that infrared temperature measurement system can enter to crucible bottom thermal field condition
Row non-contact infrared measures.
(3) crucible chooses the tantalum crucible of metal tantalum surface carbonation, and the metal tantalum crucible size of carbonization is diameter 80mm, high
100mm。
(4) seed crystal is placed in the bottom of the metal tantalum crucible of carbonization, selection seed crystal is (0001) direction ready in advance
6H-SiC seed crystals, a diameter of 50mm of seed crystal.
(5) dividing plate, the bottom of the metal tantalum crucible of dividing plate distance carbonization are placed in the metal tantalum crucible medium position of carbonization
Distance be 20mm, a diameter of 80mm of dividing plate, a big hole, a diameter of 30mm of circular hole, in dividing plate are left in the centre of dividing plate
On be also uniformly dispersed with some small circular holes, a diameter of 7mm.
(6) double-layer nested formula crucible, a diameter of 30mm of inner crucible are placed vertically on the upside of dividing plate, inner crucible only has
Side wall, it is hollow bottomless.Inner crucible wall is identical with the height holding of outer layer sidewall of crucible, is highly 50mm, and inside and outside sidewall of crucible it
Between distance be 15mm, high purity silicon nitride aluminium powder is placed in crucible inside and outside wall junction, places 40g every time.
(7) equipment is heated to 2000 DEG C of high temperature above using heating system, crucible top temperature is 2500 DEG C, bottom temperature
Spend for 2100 DEG C..
(8) high temperature makes aluminum nitride powder distil, and is moved in the metal tantalum crucible of carbonization along thermograde direction to low-temperature space,
Sublimated in low temperature seed crystal face as aluminium nitride solid, the growth of completion high-purity single-crystal aluminum nitride.
Embodiment three：Utilized in tungsten crucible and complete high-purity without the aluminum-nitride single crystal grower of seed crystal adhesive technology
The growth of single-crystal aluminum nitride.
Specific growth course is as follows：
(1) electric current is passed through in high purity tungsten net (resistance heating) to heat it.
(2) insulation effect in top adjustment heat insulation layer structure (shape and the number of plies), is made as heat-insulation layer using multistage high purity tungsten screen
Fruit is more than bottom, and crucible top temperature is higher than about 400 DEG C of bottom temp.Diameter 9mm openings are left immediately below simultaneously, are ensured infrared
Temp measuring system can carry out non-contact infrared measurement to crucible bottom thermal field condition.
(3) crucible chooses high-purity tungsten crucible, and tungsten crucible size is diameter 70mm, high 100mm.
(4) seed crystal is placed in the bottom of tungsten crucible, selection seed crystal is (0001) direction ready in advance 6H-SiC seed crystals,
The a diameter of 50mm of seed crystal.
(5) dividing plate is placed in tungsten crucible middle and lower part position, distance of the dividing plate apart from the bottom of tungsten crucible is 20mm.Dividing plate is straight
Footpath is 70mm, and a big hole is left in the centre of dividing plate, a diameter of 30mm of circular hole, is evenly distributed circular hole on dividing plate, circle
Bore dia is 7mm.
(6) double-layer nested formula crucible, a diameter of 25mm of inner crucible are placed vertically on the upside of dividing plate, inner crucible only has
Side wall, it is hollow bottomless.Inner crucible wall is identical with the height holding of outer layer sidewall of crucible, is highly 50mm, and inside and outside sidewall of crucible it
Between distance be 10mm, high purity silicon nitride aluminium powder is placed in crucible inside and outside wall junction, places 35g every time.
(7) equipment is heated to 2000 DEG C of high temperature above using heating system, crucible top temperature is 2200 DEG C, bottom temperature
Spend for 1800 DEG C.
(8) high temperature makes aluminum nitride powder distil, and is moved in tungsten crucible along thermograde direction to low-temperature space, in low temperature seed crystal
Sublimate as aluminium nitride solid, the growth of completion high-purity single-crystal aluminum nitride on surface.
It should be noted that the purpose for publicizing and implementing example is that help further understands the present invention, but the skill of this area
Art personnel are appreciated that：Do not departing from the present invention and spirit and scope of the appended claims, various substitutions and modifications are all
It is possible.Therefore, the present invention should not be limited to embodiment disclosure of that, and the scope of protection of present invention is with claim
The scope that book defines is defined.
Claims (8)
1. a kind of aluminum-nitride single crystal grower without seed crystal adhesive technology, including：Heating system, infrared temperature measurement system, seed
Crystalline substance, growth crucible, crucible dividing plate and double-layer nested formula crucible；Heating system is placed in the outermost of the grower, heating system
System is made up of induction coil and graphite；The top insulation material thickness of heating system is more than bottom insulation material so that bottom is protected
Warm nature can be weaker than top, and thermograde is inverted, and crucible bottom has temperature difference with top；Crucible is placed in insulation material, crucible
Bottom center is provided with shed；Infrared temperature measurement system carries out infrared measurement of temperature by under shed；Seed crystal is placed in the bottom of crucible；Earthenware
The centre of crucible dividing plate is provided with a big hole, and multiple small sircle holes are uniformly distributed on crucible dividing plate；Double-layer nested formula crucible is vertical
It is placed on the upside of crucible dividing plate, including inner crucible and outer crucible；Inner crucible only has side wall, hollow bottomless；Internal layer earthenware
The side wall of crucible is identical with the height holding of the wall of outer crucible；Filled between the side wall of inner crucible and the side wall of outer crucible high
Pure aluminum nitride powder.
2. the aluminum-nitride single crystal grower without seed crystal adhesive technology as claimed in claim 1, it is characterized in that, heating system
Mode of heating includes sensing heating or resistance heating.
3. the aluminum-nitride single crystal grower without seed crystal adhesive technology as claimed in claim 1, it is characterized in that, heating system
In, induction coil is passed through electric current and the mode of graphite heating is heated.
4. the aluminum-nitride single crystal grower without seed crystal adhesive technology as claimed in claim 1, it is characterized in that, crucible chooses carbon
Change tantalum carbide ceramics crucible, the tantalum crucible or tungsten crucible of metal tantalum surface carbonation of tantalum powder sintering；The material of crucible be ramet,
Tantalum, boron nitride or tungsten.
5. the aluminum-nitride single crystal grower without seed crystal adhesive technology as claimed in claim 1, it is characterized in that, the bottom of crucible
Diameter of the center provided with opening is between 5mm-10mm；A diameter of 50mm-150mm of crucible；The height of crucible is 70mm-
300mm。
6. the aluminum-nitride single crystal grower without seed crystal adhesive technology as claimed in claim 1, it is characterized in that, double-layer nested formula
A diameter of 20mm-75mm of the inner crucible of crucible；The height of inner crucible wall and outer layer sidewall of crucible is 35mm-195mm；Internal layer
The distance between sidewall of crucible and outer layer sidewall of crucible are 20mm-60mm.
7. a kind of aluminum-nitride single crystal grower using claim 1~6 Suo Shu without seed crystal adhesive technology prepares aluminium nitride
The method of monocrystalline, comprises the following steps：
1) carry out being heated to high temperature using heating system；
2) high temperature makes the high purity silicon nitride aluminium powder distillation vapour China in double-layer nested formula crucible, forms aluminium nitride gas；Aluminium nitride gas
Sidewall of crucible of the body along double-layer nested formula crucible moves upward to the top up to double-layer nested formula crucible；
3) crucible top and the heat-insulation system of bottom have temperature difference, also there is temperature difference, earthenware between crucible dividing plate and crucible bottom
Occurs thermograde in crucible, part where seed crystal is low-temperature space, and crucible top is high-temperature region；
4) in the presence of thermograde, source gas is from crucible top along thermograde direction while interior from double-layer nested crucible
The inwall of the outer wall of crucible and outer crucible moves downward；
5) when source gas reaches the seed crystal face of crucible bottom, source gas is sublimated as aluminum-nitride single crystal solid；
Thus aluminum-nitride single crystal is prepared.
8. the method for preparing aluminum-nitride single crystal as claimed in claim 7, it is characterized in that, in step 3), crucible top and bottom
Heat-insulation system temperature difference is 50-500 DEG C or so, and the temperature difference between crucible dividing plate and crucible bottom is 40-200 DEG C or so.
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| 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 |
| 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 |
| 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 |
| CN111472045A (en) * | 2020-04-30 | 2020-07-31 | 北京大学 | Aluminum nitride single crystal preparation method based on large-size seed crystals |
| CN113337886A (en) * | 2021-06-04 | 2021-09-03 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Thermal field device and method for high-quality single crystal growth by PVT (physical vapor transport) method |
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