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 PDF

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Publication number
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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substrate
crystal
brilliant
growth
aluminum nitride
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程章勇
杨丽雯
刘欣宇
杨雷雷
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BEIJING HUAJIN CHUANGWEI ELECTRONICS Co Ltd
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BEIJING HUAJIN CHUANGWEI ELECTRONICS Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/40AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C30B29/403AIII-nitrides
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B23/00Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02Epitaxial-layer growth
    • C30B23/025Epitaxial-layer growth characterised by the substrate

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

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

A kind of aluminum nitride crystal growth is prepared with homo-substrate and expanding growing method
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.
CN201711454088.4A 2017-12-28 2017-12-28 A kind of aluminum nitride crystal growth is prepared with homo-substrate and expanding growing method Pending CN108085745A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007204309A (en) * 2006-02-01 2007-08-16 Matsushita Electric Ind Co Ltd Single crystal growth device and single crystal growth method
CN101484617A (en) * 2006-07-04 2009-07-15 住友电气工业株式会社 Process for producing substrate of AlN crystal, method of growing AlN crystal, and substrate of AlN crystal
CN101535533A (en) * 2006-11-17 2009-09-16 住友电气工业株式会社 Process for producing group iii element nitride crystal
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
CN107059116A (en) * 2007-01-17 2017-08-18 晶体公司 Defect in the aluminum nitride crystal growth of seeding is reduced
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

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007204309A (en) * 2006-02-01 2007-08-16 Matsushita Electric Ind Co Ltd Single crystal growth device and single crystal growth method
CN101484617A (en) * 2006-07-04 2009-07-15 住友电气工业株式会社 Process for producing substrate of AlN crystal, method of growing AlN crystal, and substrate of AlN crystal
CN101535533A (en) * 2006-11-17 2009-09-16 住友电气工业株式会社 Process for producing group iii element nitride crystal
CN107059116A (en) * 2007-01-17 2017-08-18 晶体公司 Defect in the aluminum nitride crystal growth of seeding is reduced
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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Application publication date: 20180529