CN108085745A - A kind of aluminum nitride crystal growth is prepared with homo-substrate and expanding growing method - Google Patents
A kind of aluminum nitride crystal growth is prepared with homo-substrate and expanding growing method Download PDFInfo
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- CN108085745A CN108085745A CN201711454088.4A CN201711454088A CN108085745A CN 108085745 A CN108085745 A CN 108085745A CN 201711454088 A CN201711454088 A CN 201711454088A CN 108085745 A CN108085745 A CN 108085745A
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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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- 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
- C30B23/025—Epitaxial-layer growth characterised by the substrate
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Abstract
It is prepared the invention discloses a kind of aluminum nitride crystal growth with homo-substrate and expanding growing method, this method method mainly includes：It is first brilliant prepare, prepared by substrate, crystal growth.The present processes do not overcome key issue of the aluminum nitride crystal growth in the process without homo-substrate singly, can also use metal heater insulation construction and carry out preparing high quality aluminum-nitride single crystal material；Likewise, using the scheme of the invention, aluminum-nitride single crystal size can also effectively be expanded, therefore this method is also an important technology method of expanding growth in aluminum nitride crystal growth.
Description
Technical field
The expanding field of manufacture, aluminum nitride crystal growth the present invention relates to aluminum nitride crystal growth substrate, specifically relates to
And a kind of aluminum nitride crystal growth is prepared with homo-substrate and expanding growing method.
Background technology
Aluminum nitride crystal material is one of important photoelectric semiconductor material, be prepare deep ultraviolet high performance device can not or
Scarce crystalline material；With the urgency of rapid development and the application of semi-conducting material, aluminum nitride crystal material grinds in country
Hair is also stepped up its investment, and is also in increasing trend with the relevant R＆D institution of aluminum nitride crystal material.
Aluminum nitride crystal material is no in former nature, it is entirely a kind of artificial synthesized crystalline material.To the greatest extent
Pipe belongs to close-packed hexagonal wurtzite structure crystalline material together with carborundum, and the growing method of mainstream is also all physical vapour deposition (PVD)
Method, but the growth difficulty of aluminum nitride crystal is significantly larger than carborundum crystals material；Its manufacturing cost is also than carborundum crystals material
Cost will costliness.This is also in the market without a major reason of large scale aluminum nitride crystal material sale existing.
Although there is small size aluminum nitride crystal material supply in the market, size about 5*5mm is limited to its growth technique
And the intrinsic property that such crystalline material is exclusive, so far, do not learn still on the aluminium nitride list for breaking through 10*10mm
The message that brilliant material is sold on the market.So large scale aluminum nitride single-crystal substrate is that there is an urgent need for solutions for current aluminum nitride crystal growth
Key issue certainly.It, can be fast by preparing aluminium nitride homogenous growth substrate in order to meet aluminium nitride from growth demand is multiplied
Fast-growing aluminum nitride crystal in large size.
The content of the invention
Using crystal controlling is not easy in no substrate spontaneous nucleation growth course during based on aluminum nitride crystal growth, in crystal growth
What is obtained to terminal stage is a polycrystalline ingot；And use foreign template growth not only easily in growth course because of substrate crystal
Die plate failure caused by temperature, pressure gap with aluminum nitride crystal, it is easier to introduce foreign atom impurity so as to cause life
Grow up to cocrystalization compound, reduce crystal quality；When foreign substrate is silicon carbide seed, metal heater-insulation construction is used
It is also easy to stove is caused seriously to pollute even to fail.It is always aluminium nitride development based on growing large-size aluminum nitride crystal material
Bottleneck factor, the current country, which there is no to possess, can grow the technical solution with large scale aluminium nitride homo-substrate, stop always
It is stagnant in small crystalline size research of technique level.
For the series of problems of above-mentioned growing aluminum nitride crystal material, the present invention provides a kind of aluminum nitride crystal growth use
Homo-substrate prepares and expanding growing method, does not thus overcome key of the aluminum nitride crystal growth in the process without homo-substrate singly
Problem can also use metal heater-insulation construction and carry out preparing high quality aluminum-nitride single crystal material；It should likewise, using
Scheme of the invention can also effectively expand aluminum-nitride single crystal size, therefore this method is also expanding growth in aluminum nitride crystal growth
An important technology method.
To achieve the above object, the present invention uses following technical scheme：
A kind of aluminum nitride crystal growth is prepared with homo-substrate and expanding growing method, and described method includes following steps：
1) member is brilliant prepares：It is processed using physical vapour deposition (PVD) growing aluminum nitride crystal, and to it, is prepared into isometric circle
Column construction member is brilliant, and the wherein brilliant end face of aluminium nitride member is { 0001 } family of crystal planes；
2) prepared by substrate：Bond member crystalline substance in order with aluminium nitride adhesive special on clean seed crystal support, it is brilliant viscous according to member
The different member crystalline substance of diameter is equably bonded on seed crystal support by knot planning by order, forms blank substrate；Again by blank substrate into
Row sintering curing；Then crystal orientation deviation measuring and calculating is carried out, determines that crystal is carried out epi- again after the brilliant crystal orientation deviation of each member is reasonable
Ready is processed；
3) crystal growth：Aluminium nitride substrate template and aluminium nitride growth material source are placed in same crucible, first make aluminium nitride
Substrate template is in high-temperature position, and high temperature pretreatment is carried out to aluminium nitride substrate；Substrate and material are adjusted by the stretching structure of stove
The position relationship in source realizes that material source is in high-temperature position, and substrate is located at deposition growing position and carries out aluminum nitride crystal growth.
Further, the method for the brilliant preparation of member is specially in step 1)：Using physical vapour deposition (PVD) growing aluminum nitride monocrystal,
Aluminium nitride column crystal is pressed and is equidistantly cut perpendicular to (0001) crystal orientation direction, prepares the circle that end face is { 0001 } sets of crystal planes
Column rotation volume elements is brilliant, and to each end face mark (0001) and (000-1) face；And it is divided into different brackets by the difference of first brilliant diameter.
Further, the brilliant process of member is bonded in step 2) is specially：One layer of aluminium nitride is uniformly applied on the seed crystal support of crystallization
The brilliant demand according to technique of member of different-diameter is successively bonded on seed crystal support, forms blank lining by adhesive special in order
Bottom；During the bonding process, first Jingjing face in same substrate face must be consistent, while first whisker in substrate surface is in same level
On face, 0~1 ° of crystal orientation deviation；More than whole operation process operates under constant temperature, and temperature is 25~85 DEG C.
Further, it is firm to first brilliant group using dead ring in step 2) substrate preparation process, while ensure that each first intergranular is brilliant
Zone of reasonableness to deviation at 0~1 °；The blank substrate consolidated is placed in seed crystal again to fire in frock, places it in high temperature furnace
In, the regular weight that 2~200kg is suppressed in frock, furnace chamber pressure 10 are fired in seed crystal-1~106Pa, using nitrogen or argon gas as
Protective gas, 200~1500 DEG C of temperature, 0.5~50h of constant temperature time；The dead ring on blank material source is removed afterwards, and at cleaning
Reason, orients again, determines member Jingjing to deviation in 0~1 ゜ zone of reasonableness；If crystal orientation deviation is excessive, crystal orientation is carried out by force and is rectified
Just, if crystal orientation deviation is excessive, quantity is excessive, failed sample must be bonded and cured again；To blank substrate epi-ready
Rank is processed, and obtains aluminium nitride substrate template.
Further, the process of step 3) crystal growth is specially：Substrate template is placed in growth material source in same growth room,
Substrate template is first made to be in high-temperature position to be pre-processed, treatment temperature be 2000~2600 DEG C, the time be 5~300min, furnace pressure
For 10~120KPa, 10~500sccm of nitrogen or argon stream rate；It is real again by adjusting crucible and the position relationship of coil
Existing material source is in high-temperature position, and substrate is located at deposition growing position, and the wherein brilliant group template growth condition of aluminium nitride member is 1800~2260
DEG C, 20~120KPa of furnace pressure, 10~1000sccm of nitrogen.
The present invention has following advantageous effects：
The present processes are not overcome singly during aluminum nitride crystal growth without the key issue of homo-substrate, can be with
It carries out preparing high quality aluminum-nitride single crystal material using metal heater-insulation construction；Likewise, using the scheme of the invention, go back
Aluminum-nitride single crystal size can effectively be expanded, therefore this method is also an important skill of expanding growth in aluminum nitride crystal growth
Art method.
Description of the drawings
Fig. 1 is that the first crystalline substance of plurality of specifications (diameter) of the embodiment of the present invention 1 prepares aluminium nitride substrate；
Fig. 2 is that the first crystalline substance of plurality of specifications (diameter) of the embodiment of the present invention 2 prepares aluminium nitride substrate；
Wherein：11st, 21- seed crystal supports, 12,22- dead rings, 13,14,15,16,23,24,25 be respectively that diameter specifications differ
Equidistant member it is brilliant.
Specific embodiment
In the following, refer to the attached drawing, more fully illustrates the present invention, shown in the drawings of the exemplary implementation of the present invention
Example.However, the present invention can be presented as a variety of various forms, it is not construed as being confined to the exemplary implementation described here
Example.And these embodiments are to provide, so that the present invention is fully and completely, and it will fully convey the scope of the invention to this
The those of ordinary skill in field.
It is prepared the present invention provides a kind of aluminum nitride crystal growth with homo-substrate and expanding growing method, thus not Dan Ke
Take during aluminum nitride crystal growth without the key issue of homo-substrate, can also use metal heater-insulation construction into
Row prepares high quality aluminum-nitride single crystal material；Likewise, using the scheme of the invention, aluminum-nitride single crystal size can also effectively be expanded
Greatly, thus this method be also expanding growth in aluminum nitride crystal growth an important technology method.This method mainly includes：Member
Prepared by crystalline substance, prepared by substrate, crystal growth.First crystalline substance in the invention refers to the most basic unit of composition aluminium nitride substrate, definitely
It is aluminium nitride crystal column or chip that ground, which is said,.
First brilliant preparation：Using physical vapour deposition (PVD) growing aluminum nitride crystal, aluminum nitride powder is utilized in aluminium nitride growth room
Shape or bulk crystal growth go out aluminium nitride column crystal or lamella crystal, and aluminium nitride column crystal is pressed perpendicular to certain crystal orientation
Direction is equidistantly cut, final to obtain with identical crystal orientation, highly consistent aluminium nitride crystal column or chip namely aluminium nitride
It is first brilliant.It is according to the cutting carried out perpendicular to (0001) crystal orientation direction in the present invention, obtains the circle that end face is { 0001 } sets of crystal planes
Column rotary body, and to each end face mark (0001) and (000-1) face.In order to which seed crystal support bare area will be reduced most possibly,
Preferably first crystalline substance is fallen into three classes by diameter.First brilliant difference according to diameter is divided into the present invention different etc.
Grade；Be to take second place labeled as B wherein by the brilliant mark of the member being relatively large in diameter, then according to diameter by subtract principle and so on C,
D……
It is prepared by substrate：The dirt on seed crystal support surface is first subjected to clean processing；It is equably applied with aluminium nitride adhesive special
It is put on seed crystal support, gradually will equably be bonded on seed crystal support labeled as the member of A is brilliant, again have B constituent element crystalline substances after bonding
In the gap formed after being placed in sequence that A constituent elements are brilliant and bonding, small tangent of diameter time is inserted into A groups again successively or B constituent elements are brilliant is formed
Gap in ... formed substrate blank；During the bonding process, first Jingjing face in same substrate face must be consistent, while substrate
First whisker in face is in same level, 0~1 ° of crystal orientation deviation, 0 ° of optimum error value；During more than whole operation
It is operated under constant temperature, temperature is 25~85 DEG C.Blank substrate is further cured, consolidates the brilliant phase on seed crystal support surface of member
To the relative position of position and first intergranular, first confined with dead ring, ensure that crystal orientation deviation occurs in first intergranular in fastener cycle, one
There is crystal orientation deviation in denier, then stops fastening, and first brilliant crystal orientation is corrected in time, it is ensured that each first intergranular crystal orientation deviation 0~
After in 1 ° of zone of reasonableness, blank substrate is placed in frock and is sintered curing, shape is placed in frock during sintering curing
Shape rule 2~200kg of weight, furnace chamber pressure 10-1~106Pa, using nitrogen or argon gas as protective gas, temperature 200~1500
DEG C, 0.5~50h of constant temperature time.Blank substrate removes dead ring after curing, and handles its surface ease glue is clean, again
Orientation determines member Jingjing to deviation in zone of reasonableness.If crystal orientation deviation is excessive, crystal orientation correction is carried out by force, if first intergranular
Crystal orientation deviation is big, quantity is excessive, then is determined as defective work, must bond and cure again.Determine that the crystal orientation deviation of member intergranular exists
After in zone of reasonableness, then blank substrate is processed to epi-ready, it is final to obtain suitable for aluminum nitride crystal growth
Substrate template.
Crystal growth：Aluminium nitride substrate template is placed in aluminium nitride growth material source in same crucible, first makes aluminium nitride substrate
Template is in high-temperature position, and high temperature pretreatment is carried out to aluminium nitride substrate, and treatment temperature is 2000~2600 DEG C, the time for 5~
300min, furnace pressure are 10~120KPa, 10~500sccm of nitrogen or argon stream rate.It is adjusted by the stretching structure of stove
The position relationship of substrate and material source realizes that material source is in high-temperature position, and substrate is located at deposition growing position, the wherein brilliant group mould of aluminium nitride member
Plate growth conditions is 1800~2260 DEG C, 20~120KPa of furnace pressure, 10~1000sccm of nitrogen.
With reference to specific embodiment, the present invention is further illustrated：
Embodiment 1
It is prepared as shown in Figure 1, member is brilliant：Aluminium nitride material source is placed in carbonization tantalum crucible, growth temperature is 2220 DEG C, furnace pressure
Growth obtains aluminum-nitride single crystal under the conditions of 80KPa, stream of nitrogen gas rate 500sccm, monocrystalline is carried out preparatory processing, according to vertical
Equidistantly cut in (0001) crystal orientation direction, select suitable fixture by the crystal pro cessing after cutting into cylinder rotary body 13,
14、15、16；The end face of crystal is finally respectively labeled as (0001) and (000-1) face.
It is prepared by substrate：The dirt on 11 surface of seed crystal support is first subjected to clean processing；With aluminium nitride adhesive special equably
It is applied on seed crystal support 11, first 13 is gradually equably bonded in the member crystalline substance being relatively large in diameter on seed crystal support 11, then can be with by diameter
The member crystalline substance 15 of approximate tangent calking is equably bonded in the gap that first crystalline substance 13 is formed.It is opposite between brilliant for the ease of firm member
Position, then first crystalline substance 14 is bonded in first brilliant 13 peripheries in an orderly manner, it is similarly, the approximate tangent calking of diameter is brilliant in first crystalline substance 13 and member
Between 14；It is prepared into substrate blank；During the bonding process, first Jingjing face in same substrate face must be consistent, while substrate surface
Interior first whisker is in same level, 0~1 ° of crystal orientation deviation, 0 ° of optimum error value；During more than whole operation
It is operated under constant temperature, temperature is 65 DEG C.By blank substrate curing process；With the firm brilliant relative position on seed crystal support surface of member
And the relative position of first intergranular, first confined with dead ring 12, ensure that crystal orientation deviation occurs in first intergranular in fastener cycle, once go out
Existing crystal orientation deviation, then stop fastening, and first brilliant crystal orientation is corrected in time, it is ensured that each member intergranular crystal orientation deviation is at 0~1 °
After in zone of reasonableness, blank substrate is placed in frock and is sintered curing, place shape rule during sintering curing in frock
Then weight 15kg, furnace chamber pressure 1000Pa, using argon gas as protective gas, 950 DEG C of temperature, constant temperature time 8h.
Blank substrate removes dead ring 12 after curing, and to the clean processing of its surface ease glue, while orient again,
It is 0 ゜ to determine that member Jingjing finely controls first intergranular deviation to deviation in zone of reasonableness, present case.If crystal orientation deviation is more than 1 ゜,
Carry out crystal orientation correction by force, if the crystal orientation deviation of first intergranular is big, quantity is excessive, be determined as defective work, must bond again and
Cure.After determining the crystal orientation deviation of member intergranular in the reasonable scope, then blank substrate is processed to epi-ready, finally
Obtain the substrate template suitable for aluminum nitride crystal growth.
Crystal growth：It is placed in aluminium nitride substrate template and aluminium nitride growth material source in same crucible, first serves as a contrast aluminium nitride
End template is in high-temperature position, and high temperature pretreatment is carried out to aluminium nitride substrate, and treatment temperature is 2000~2600 DEG C, the time for 5~
300min, furnace pressure are 10~120KPa, 10~500sccm of nitrogen or argon stream rate.It is adjusted by the stretching structure of stove
The position relationship of substrate and material source realizes that material source is in high-temperature position, and substrate is located at deposition growing position, the wherein brilliant group mould of aluminium nitride member
Plate growth conditions is 2220 DEG C, furnace pressure 60KPa, nitrogen 500sccm.
Embodiment 2
It is prepared as shown in Fig. 2, member is brilliant：Aluminium nitride material source is placed in carbonization tantalum crucible, growth temperature is 2220 DEG C, furnace pressure
Growth obtains aluminum-nitride single crystal under the conditions of 80KPa, stream of nitrogen gas rate 500sccm, monocrystalline is carried out preparatory processing, according to vertical
Equidistantly cut in (0001) crystal orientation direction, select suitable fixture by the crystal pro cessing after cutting into cylinder rotary body 23,
24、25；The end face of crystal is finally respectively labeled as (0001) and (000-1) face.
It is prepared by substrate：The dirt on 21 surface of seed crystal support is first subjected to clean processing；With aluminium nitride adhesive special equably
Be applied on seed crystal support 21, first 24 be bonded in the member crystalline substance being relatively large in diameter on seed crystal support 21, at the same ensure the axle center of first crystalline substance 24 with
The axle center of seed crystal support 21 is consistent.First crystalline substance 25 is gradually bonded on seed crystal support 21 in an orderly manner again, at the same ensure between first crystalline substance 25 and with
It is tangent between first crystalline substance 24；First crystalline substance 23 and member crystalline substance 24,25 are tangentially inserted in gap again, are prepared into substrate blank；In bonding process
In, first Jingjing face in same substrate face must be consistent, while first whisker in substrate surface is in same level, crystal orientation deviation
0~1 ° of value, 0 ° of optimum error value；It is operated during more than whole operation under constant temperature, temperature is 65 DEG C.Blank is served as a contrast
Bottom curing process；It is brilliant in the relative position on seed crystal support surface and the relative position of first intergranular with firm member, first with dead ring 22
Confine, ensure that crystal orientation deviation occurs in first intergranular in fastener cycle, once there is crystal orientation deviation, then stop fastening, to first brilliant crystalline substance
To being corrected in time, it is ensured that after each member intergranular crystal orientation deviation is in 0~1 ° of zone of reasonableness, blank substrate is placed in frock
It is sintered curing, places regular shape weight 15kg during sintering curing in frock, furnace chamber pressure 1000Pa is made with argon gas
For protective gas, 950 DEG C of temperature, constant temperature time 8h.
Blank substrate removes dead ring 22 after curing, and to handling its surface ease glue is clean, while it is fixed again
To it is 0 ゜ to determine that member Jingjing finely controls first intergranular deviation to deviation in zone of reasonableness, present case.If crystal orientation deviation is more than 1
゜ then carries out crystal orientation correction by force, if the crystal orientation deviation of first intergranular is big, quantity is excessive, is determined as defective work, must glue again
Knot and curing.After determining the crystal orientation deviation of member intergranular in the reasonable scope, then blank substrate is processed to epi-ready,
The final substrate template obtained suitable for aluminum nitride crystal growth.
Crystal growth：It is placed in aluminium nitride substrate template and aluminium nitride growth material source in same crucible, first serves as a contrast aluminium nitride
End template is in high-temperature position, and high temperature pretreatment is carried out to aluminium nitride substrate, and treatment temperature is 2000~2600 DEG C, the time for 5~
300min, furnace pressure are 10~120KPa, 10~500sccm of nitrogen or argon stream rate.It is adjusted by the stretching structure of stove
The position relationship of substrate and material source realizes that material source is in high-temperature position, and substrate is located at deposition growing position, the wherein brilliant group mould of aluminium nitride member
Plate growth conditions is 2220 DEG C, furnace pressure 60KPa, nitrogen 500sccm.
It is described above simply to illustrate that of the invention, it is understood that the invention is not limited in above example, meet
The various variants of inventive concept are within protection scope of the present invention.
Claims (5)
1. a kind of aluminum nitride crystal growth is prepared with homo-substrate and expanding growing method, which is characterized in that the described method includes
Following steps：
1) member is brilliant prepares：It is processed using physical vapour deposition (PVD) growing aluminum nitride crystal, and to it, is prepared into equidistant cylinder
Structural elements are brilliant, and the wherein brilliant end face of aluminium nitride member is { 0001 } family of crystal planes；
2) prepared by substrate：It bonds member crystalline substance in order with aluminium nitride adhesive special on clean seed crystal support, is advised according to brilliant bond of member
It draws and is equably bonded in diameter different member crystalline substance on seed crystal support by order, form blank substrate；Blank substrate is burnt again
Knot cures；Then crystal orientation deviation measuring and calculating is carried out, determines again to add crystal progress epi-ready after the brilliant crystal orientation deviation of each member is reasonable
Work；
3) crystal growth：Aluminium nitride substrate template and aluminium nitride growth material source are placed in same crucible, first make aluminium nitride substrate
Template is in high-temperature position, and high temperature pretreatment is carried out to aluminium nitride substrate；Substrate and material source are adjusted by the stretching structure of stove
Position relationship realizes that material source is in high-temperature position, and substrate is located at deposition growing position and carries out aluminum nitride crystal growth.
2. aluminum nitride crystal growth according to claim 1 is prepared with homo-substrate and expanding growing method, feature exist
In the method for the brilliant preparation of member is specially in step 1)：Using physical vapour deposition (PVD) growing aluminum nitride monocrystal, by aluminium nitride column
Crystal prepares end face and rotates volume elements for the cylinder of { 0001 } sets of crystal planes by equidistantly being cut perpendicular to (0001) crystal orientation direction
Crystalline substance, and to each end face mark (0001) and (000-1) face；And it is divided into different brackets by the difference of first brilliant diameter.
3. aluminum nitride crystal growth according to claim 1 is prepared with homo-substrate and expanding growing method, feature exist
In the brilliant process of member is bonded in step 2) is specially：One layer of aluminium nitride adhesive special is uniformly applied on the seed crystal support of crystallization, it will
The brilliant demand according to technique of member of different-diameter is successively bonded on seed crystal support in order, forms blank substrate；In bonding process
In, first Jingjing face in same substrate face must be consistent, while first whisker in substrate surface is in same level, crystal orientation deviation
0~1 ° of value；More than whole operation process operates under constant temperature, and temperature is 25~85 DEG C.
4. aluminum nitride crystal growth according to claim 1 is prepared with homo-substrate and expanding growing method, feature exist
In, it is firm to first brilliant group using dead ring in step 2) substrate preparation process, while ensure each first intergranular crystal orientation deviation at 0~1 °
Zone of reasonableness；The blank substrate consolidated is placed in seed crystal again to fire in frock, is placed it in high temperature furnace, is fired in seed crystal
The regular weight of 2~200kg, furnace chamber pressure 10 are suppressed in frock-1~106Pa, using nitrogen or argon gas as protective gas, temperature
200~1500 DEG C, 0.5~50h of constant temperature time；The dead ring on blank material source, and clean processing are removed afterwards, are oriented again,
Determine member Jingjing to deviation in 0~1 ゜ zone of reasonableness；If crystal orientation deviation is excessive, crystal orientation correction is carried out by force, if crystal orientation deviation
It is excessive, quantity is excessive, then failed sample, must bond and cure again；Blank substrate epi-ready ranks are processed, are obtained
Aluminium nitride substrate template.
5. aluminum nitride crystal growth according to claim 1 is prepared with homo-substrate and expanding growing method, feature exist
In the process of step 3) crystal growth is specially：Substrate template is placed in growth material source in same growth room, first makes substrate template
It being pre-processed in high-temperature position, treatment temperature is 2000~2600 DEG C, and the time is 5~300min, and furnace pressure is 10~120KPa,
10~500sccm of nitrogen or argon stream rate；Again by adjusting crucible and the position relationship of coil, realize that material source is in high temperature
Position, substrate are located at deposition growing position, wherein the brilliant group template growth condition of aluminium nitride member be 1800~2260 DEG C, furnace pressure 20~
120KPa, 10~1000sccm of nitrogen.
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| CN102618930A (en) * | 2012-03-31 | 2012-08-01 | 哈尔滨工业大学 | Method for preparing AlN crystal |
| CN103474331A (en) * | 2013-10-08 | 2013-12-25 | 中国电子科技集团公司第四十四研究所 | Method for growing epitaxy AlN template on sapphire substrate |
| CN107338477A (en) * | 2016-05-02 | 2017-11-10 | 国立大学法人大阪大学 | The manufacture method and crystalline growth substrate of crystal of nitride substrate |
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