CN102618930A - Method for preparing AlN crystal - Google Patents
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- CN102618930A CN102618930A CN2012100932223A CN201210093222A CN102618930A CN 102618930 A CN102618930 A CN 102618930A CN 2012100932223 A CN2012100932223 A CN 2012100932223A CN 201210093222 A CN201210093222 A CN 201210093222A CN 102618930 A CN102618930 A CN 102618930A
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Abstract
The invention discloses a method for preparing an AlN crystal, which relates to a method for preparing a crystal and solves the problems of large lattice mismatch between a heterogeneous seed crystal and the AlN crystal and high defect density of the AlN crystal in a method for preparing an AlN single crystal by a physical vapor transport (PVT) method in the prior art. The method comprises the following steps of: 1, putting AlN powder into a crucible, fixing a seed crystal on the top of the crucible, raising the temperature to 1,800-2,000 DEG C in the presence of nitrogen, and preserving the heat for 1 to 5 hours; and 2, heating to raise the temperature of the pre-sintered AlN powder to 2,150-2,300 DEG C in the presence of the nitrogen, preserving the heat, reacting for 8 to 20 hours, and reducing to room temperature. A zero micro tube SiC is used as the heterogeneous seed crystal, so that the defect density of the AlN crystal can be reduced; and simultaneously, an angle-deviated SiC seed crystal is deviated from a surface at a certain angel, so that the inheriting probability of defects is remarkably reduced, and negative influences of the defects on the performance of a device are reduced finally. The AlN crystal is used for a semiconductor device.
Description
Technical field
The present invention relates to a kind of crystalline preparation method.
Background technology
The AlN crystal is one of typical case's representative of third generation semiconductor material; Have broad-band gap (6.2eV), high heat conductance (330W/mK), high resistivity, good ultraviolet permeability, the saturated mobility of high electronics and higher capability of resistance to radiation; Thereby be more suitable for being used to make high temperature, high frequency, radioprotective and high power device, such as high energy efficiency opto-electronic device, high power electronic device, solid-state laser detector, high-density SSD or the like.
At present, growing AIN crystalline method mainly comprises: hydride vapour phase epitaxy method (HVPE), molecular beam epitaxy (MBE), gas phase epitaxy of metal organic compound method (MOCVD) and physical vapor transmission method (PVT) etc.HVPE method growth velocity higher (reaching as high as 100 μ m/h) has impurity automatically cleaning effect, can prepare the bigger AlN film of thickness; MBE method growth velocity is (being about 1 μ m/h) slowly, and process of growth is convenient to control, utilizes this technology can prepare the AlN monocrystal thin films of tens atomic shells; The mocvd method depositing temperature is low, and growth temperature range is wide, and suitable batch production utilizes this method can prepare the AlN film; In the PVT method, raw material evaporates in the high-temperature zone, utilizes the diffusion of steam and transporting of gas phase, is grown to crystal at cold zone.Use this method crystal raw material spontaneous nucleation growth capable of using to go out monocrystalline, seed crystal also capable of using makes the crystal raw material distillation afterwards on seed crystal, deposit and grow monocrystalline.The PVT method has advantages such as growth velocity is fast, crystalline perfection is good, and big quantity research proves, the PVT method is one of effective way of preparation large size AlN crystalline.
In general, PVT method growing AIN crystal need be selected suitable seed crystal, this just should consider seed crystal and AlN crystalline lattice match (wurtzite structure:
), heat coupling (thermalexpansioncoefficient
a=4.15x10
-6/ K, α
c=5.27 * 10
-6/ factor such as K).Obviously, adopt AlN to come the growing AIN monocrystalline will reach very good effect, owing to do not have lattice mismatch and thermal mismatching between the two as the homogeneity seed crystal.Yet both at home and abroad associated mechanisms still is in the laboratory exploratory stage for the research of AlN monocrystalline, and having only minority mechanisms such as U.S. Crystal IS company, Russian N-Crystals company can prepare diameter is 2 inches AlN monocrystalline.Therefore, it is necessary adopting heterogeneous seeded growth AlN crystal.Big quantity research proves, uses silicon single crystal, sapphire, silit as substrate or seed crystal, can prepare AlN film or AlN body monocrystalline.Wherein, silicon single crystal belongs to diamond lattic structure, and is bigger with the AlN lattice mismatch, thermal expansivity (α=2.59 * 10
-6K) also differ bigger with AlN; Sapphire has wurtzite structure
Thermal expansivity (α
a=8.5x10
-6/ K, α
c=7.3 * 10
-6/ K) there are bigger lattice mismatch and thermal mismatching equally with AlN; The unit cell parameters of silit (6H-SiC)
Thermal expansivity (α
a=4.3 * 10
-6/ K, α
c=4.7 * 10
-6/ K) all comparatively approaching with AlN.Comparatively speaking, SiC more helps the growth of AlN crystalline, and can be used as PVT method growing AIN crystalline seed crystal material.
Simultaneously, because SiC seed crystal and AlN exist certain lattice mismatch and thermal mismatching,, can alleviate this unfavorable factor greatly through epitaxy one deck AlN impact plies on the SiC substrate.The compound seed crystal of SiC/AlN is exactly that epitaxy AlN impact plies is prepared from the SiC substrate through metal-organic chemical vapor deposition equipment method (MOCVD).
Summary of the invention
The objective of the invention is to prepare in the method for AlN monocrystalline in order to solve the existing physical vapor transmission method (PVT) that adopts; When adopting heterogeneous seed crystal; Heterogeneous seed crystal and AlN crystalline lattice mismatch are bigger; The high problem of AlN defect concentrations in crystals that obtains the invention provides a kind of AlN crystalline preparation method.
The present invention adopts the physical vapor transmission method to prepare the AlN monocrystalline, and the AlN crystalline is the preparation method realize through following steps:
One, the AlN powder is placed crucible, then seed crystal is fixed on the crucible top, the distance of seed crystal and AlN powder is not more than 10mm; Be put into crucible in the monocrystal growing furnace again, in crucible, feed nitrogen, under 1 atmospheric nitrogen atmosphere; Temperature rise rate with 50 ℃/h～200 ℃/h; Heat temperature raising to 1800 ℃～2000 ℃, and be incubated 1～5 hour, accomplish the presintering of AlN powder;
Two, with the AlN powder after the presintering in the crucible under 1 atmospheric high pure nitrogen atmosphere; Temperature rise rate with 50 ℃/h～200 ℃/h; Heat temperature raising to 2150 ℃～2500 ℃ carried out insulation reaction 8～20 hours, again with the rate of temperature fall of 50 ℃/h～200 ℃/h; Reduce to room temperature, obtain the AlN crystal;
Seed crystal described in the step 1 is zero microtubule drift angle degree SiC seed crystal or the compound seed crystal of SiC/AlN; Wherein the crystal formation of zero microtubule drift angle degree SiC seed crystal is 6H-, and the drift angle degree is meant that SiC departs from the angle of 0 °～8 ° in
face.
Physical vapor transmission method described in the AlN crystalline preparation method of the present invention is those skilled in the art's a common practise.Employing well known to a person skilled in the art that crystal growing furnace gets final product.
AlN crystalline preparation method of the present invention adopts the physical vapor transmission method to prepare the AlN crystal, through the AlN powder is placed crucible bottom, seed crystal is placed the crucible top; The impurity of AlN powder is removed in the presintering that at first progressively heats up, and uses afterwards through the AlN of presintering powder as starting raw material; Under the nitrogen atmosphere of certain pressure; Elevated temperature, through the distillation of AlN powder and transporting of gas phase, depositing Al N crystal on seed crystal.The AlN crystal of preparing has excellent specific properties such as defect concentration is low, the diameter span is big, and said AlN crystal is applied to various types of semiconducter device.
SiC is one of the most sophisticated third generation semiconductor material, and the SiC crystal of large size (2,3,4 inches), defect concentration low (zero microtubule) has been realized suitability for industrialized production.Use zero microtubule drift angle degree SiC seed crystal or the compound seeded growth AlN of SiC/AlN crystal, will help obtaining high-quality AlN crystal, this shows: 1. micropipe defects is a SiC crystalline typical defect; In the AlN crystal growing process that with SiC is seed crystal; Exist the SiC seed crystal of micropipe defects can cause the AlN crystal lattice defects such as dislocation, fault to occur, have a strong impact on the AlN crystal mass, therefore; If select zero microtubule SiC as seed crystal, can reduce AlN crystalline defect concentration effectively.2. use zero microtubule SiC seed crystal; At
face growing AIN crystal; The existing defective of SiC seed crystal (like dislocation, fault etc.) largely upper edge aufwuchsplate entails the AlN crystal; If the SiC seed crystal departs from
face certain angle (scope is between 0-8 °); The probability of defective heredity will significantly reduce, thereby AlN crystalline quality is further enhanced.3. the compound seed crystal of being prepared by the SiC seed crystal of zero microtubule, drift angle degree of SiC/AlN, its AlN impact plies will effectively be alleviated thermal mismatching and the lattice mismatch of SiC and AlN, help reducing AlN crystalline defect concentration.
The AlN crystal of the present invention's preparation is applied to various types of semiconducter device.
Description of drawings
Fig. 1 is the used testing apparatus schematic diagram of the present invention, and wherein 1 is reacting outdoor wall, the 2nd, and ruhmkorff coil, the 3rd, lagging material, the 4th, crucible, the 5th, ALN powder, the 6th, seed crystal.
Embodiment
Technical scheme of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: this embodiment AlN crystalline is the preparation method realize through following steps:
One, the AlN powder is placed crucible, then seed crystal is fixed on the crucible top, the distance of seed crystal and AlN powder is not more than 10mm; Be put into crucible in the monocrystal growing furnace again, in crucible, feed nitrogen, under 1 atmospheric nitrogen atmosphere; Temperature rise rate with 50 ℃/h～200 ℃/h; Heat temperature raising to 1800 ℃～2000 ℃, and be incubated 1～5 hour, accomplish the presintering of AlN powder;
Two, with the AlN powder after the presintering in the crucible under 1 atmospheric high pure nitrogen atmosphere; Temperature rise rate with 50 ℃/h～200 ℃/h; Heat temperature raising to 2150 ℃～2500 ℃ carried out insulation reaction 8～20 hours, again with the rate of temperature fall of 50 ℃/h～200 ℃/h; Reduce to room temperature, obtain the AlN crystal;
Seed crystal described in the step 1 is zero microtubule drift angle degree SiC seed crystal or the compound seed crystal of SiC/AlN; Wherein the crystal formation of zero microtubule drift angle degree SiC seed crystal is 6H-, and the drift angle degree is meant that SiC departs from the angle of 0 °～8 ° in
face.
SiC is one of the most sophisticated third generation semiconductor material, and the SiC crystal of large size (2,3,4 inches), defect concentration low (zero microtubule) has been realized suitability for industrialized production.In this embodiment, use zero microtubule drift angle degree SiC seed crystal or the compound seeded growth AlN of SiC/AlN crystal, will help obtaining high-quality AlN crystal; To help obtaining high-quality AlN crystal; This shows: 1. micropipe defects is a SiC crystalline typical defect, in the AlN crystal growing process that with SiC is seed crystal, exists the SiC seed crystal of micropipe defects can cause the AlN crystal lattice defects such as dislocation, fault to occur; Have a strong impact on the AlN crystal mass; Therefore, if select zero microtubule SiC, can reduce AlN crystalline defect concentration effectively as seed crystal.2. use zero microtubule SiC seed crystal; At
face growing AIN crystal; The existing defective of SiC seed crystal (like dislocation, fault etc.) largely upper edge aufwuchsplate entails the AlN crystal; If the SiC seed crystal departs from
face certain angle (scope is between 0-8 °); The probability of defective heredity will significantly reduce, thereby AlN crystalline quality is further enhanced.3. the compound seed crystal of being prepared by the SiC seed crystal of zero microtubule, drift angle degree of SiC/AlN, its AlN impact plies will effectively be alleviated thermal mismatching and the lattice mismatch of SiC and AlN, help reducing AlN crystalline defect concentration.
Embodiment two: what this embodiment and embodiment one were different is: the distance of control seed crystal and AlN powder is 5～9mm in the step 1.Other are different with embodiment one.
Embodiment three: what this embodiment was different with embodiment one or two is: the compound seed crystal of SiC/AlN is through the metal-organic chemical vapor deposition equipment method in the step 1, and epitaxy AlN impact plies is prepared from zero microtubule drift angle degree SiC substrate.Other is identical with embodiment one or two.
Embodiment four: what this embodiment was different with one of embodiment one to three is: the diameter of seed crystal described in the step 1 is 1 inch, 2 inches or 3 inches.Other is identical with one of embodiment one to three.
Embodiment five: what this embodiment was different with one of embodiment one to four is: the drift angle degree of zero microtubule drift angle degree SiC is meant that SiC departs from the angle of
described in the step 1.Other is identical with one of embodiment one to four.
Embodiment six: what this embodiment was different with one of embodiment one to five is: the drift angle degree of zero microtubule drift angle degree SiC is meant that SiC departs from the angle of
described in the step 1.Other is identical with one of embodiment one to five.
Embodiment seven: what this embodiment was different with one of embodiment one to six is: heat temperature raising to 2200 ℃ in the step 2～2450 ℃, carried out insulation reaction 8～20 hours.Other is identical with one of embodiment one to six.
Embodiment eight: what this embodiment was different with one of embodiment one to seven is: heat temperature raising to 2250 ℃ in the step 2～2400 ℃ carried out insulation reaction 8～20 hours.Other is identical with one of embodiment one to seven.
Embodiment nine: what this embodiment was different with one of embodiment one to eight is: heat temperature raising to 2300 ℃ in the step 2, carried out insulation reaction 8～20 hours.Other is identical with one of embodiment one to eight.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment one:
Present embodiment AlN crystalline is the preparation method realize through following steps:
One, 200g AlN powder 5 is placed the bottom of crucible 4, utilize epoxy AB glue that seed crystal 6 is fixed on crucible 4 tops, the distance of seed crystal and AlN powder is 5mm; Be put into crucible 4 in the monocrystal growing furnace again, in crucible 4, feed high pure nitrogen, under 1 atmospheric nitrogen atmosphere; Temperature rise rate with 100 ℃/h; Heat temperature raising to 1800 ℃, and be incubated 2 hours, accomplish the presintering of AlN powder; Seed crystal described in the step 1 is that diameter is 2 inches a zero microtubule 6H-SiC seed crystal, and SiC departs from 1 ° in
face;
Two, with the AlN powder after the presintering in the crucible under 1 atmospheric high pure nitrogen atmosphere, with the temperature rise rate of 100 ℃/h, heat temperature raising to 2200 ℃ carried out insulation reaction 10 hours, with the rate of temperature fall of 100 ℃/h, reduced to room temperature again, obtained the AlN crystal.
The volume percent purity of high pure nitrogen is 99.999% in the present embodiment, the raw materials used commercially available prod that is.
Embodiment two:
Present embodiment AlN crystalline is the preparation method realize through following steps:
One, 200g AlN powder 5 is placed the bottom of crucible 4, utilize epoxy AB glue that seed crystal 6 is fixed on crucible 4 tops, the distance of seed crystal and AlN powder is 8mm; Be put into crucible 4 in the monocrystal growing furnace again, in crucible 4, feed high pure nitrogen, under 1 atmospheric nitrogen atmosphere; Temperature rise rate with 50 ℃/h; Heat temperature raising to 1900 ℃, and be incubated 2 hours, accomplish the presintering of AlN powder; Seed crystal described in the step 1 is that diameter is 2 inches a zero microtubule 6H-SiC seed crystal, and SiC departs from 1 ° in
face;
Two, with the AlN powder after the presintering in the crucible under 1 atmospheric high pure nitrogen atmosphere, with the temperature rise rate of 50 ℃/h, heat temperature raising to 2250 ℃ carried out insulation reaction 8 hours, with the rate of temperature fall of 50 ℃/h, reduced to room temperature again, obtained the AlN crystal.
The volume percent purity of high pure nitrogen is 99.999% in the present embodiment, the raw materials used commercially available prod that is.
Embodiment three:
Present embodiment AlN crystalline is the preparation method realize through following steps:
One, 200g AlN powder 5 is placed the bottom of crucible 4, utilize epoxy AB glue that seed crystal 6 is fixed on crucible 4 tops, the distance of seed crystal and AlN powder is 5mm; Be put into crucible 4 in the monocrystal growing furnace again, in crucible 4, feed high pure nitrogen, under 1 atmospheric nitrogen atmosphere; Temperature rise rate with 150 ℃/h; Heat temperature raising to 2000 ℃, and be incubated 1 hour, accomplish the presintering of AlN powder; Seed crystal described in the step 1 is that diameter is 2 inches a zero microtubule 6H-SiC seed crystal, and SiC departs from 1 ° in
face;
Two, with the AlN powder after the presintering in the crucible under 1 atmospheric high pure nitrogen atmosphere, with the temperature rise rate of 150 ℃/h, heat temperature raising to 2500 ℃ carried out insulation reaction 8 hours, with the rate of temperature fall of 150 ℃/h, reduced to room temperature again, obtained the AlN crystal.
The volume percent purity of high pure nitrogen is 99.999% in the present embodiment, the raw materials used commercially available prod that is.
Embodiment four:
Present embodiment AlN crystalline is the preparation method realize through following steps:
One, 200g AlN powder 5 is placed the bottom of crucible 4, utilize epoxy AB glue that seed crystal 6 is fixed on crucible 4 tops, the distance of seed crystal and AlN powder is 6mm; Be put into crucible 4 in the monocrystal growing furnace again, in crucible 4, feed high pure nitrogen, under 1 atmospheric nitrogen atmosphere; Temperature rise rate with 150 ℃/h; Heat temperature raising to 2000 ℃, and be incubated 2 hours, accomplish the presintering of AlN powder; Seed crystal described in the step 1 is that diameter is 2 inches a zero microtubule 6H-SiC seed crystal, and SiC departs from 2 ° in
face;
Two, with the AlN powder after the presintering in the crucible under 1 atmospheric high pure nitrogen atmosphere, with the temperature rise rate of 150 ℃/h, heat temperature raising to 2400 ℃ carried out insulation reaction 8 hours, with the rate of temperature fall of 150 ℃/h, reduced to room temperature again, obtained the AlN crystal.
The volume percent purity of high pure nitrogen is 99.999% in the present embodiment, the raw materials used commercially available prod that is.
Embodiment five:
Present embodiment AlN crystalline is the preparation method realize through following steps:
One, 200g AlN powder 5 is placed the bottom of crucible 4, utilize epoxy AB glue that seed crystal 6 is fixed on crucible 4 tops, the distance of seed crystal and AlN powder is 3mm; Be put into crucible 4 in the monocrystal growing furnace again, in crucible 4, feed high pure nitrogen, under 1 atmospheric nitrogen atmosphere; With the temperature rise rate of 150 ℃/h, heat temperature raising to 1900 ℃, and be incubated 2 hours; Accomplish the presintering of AlN powder, the distance of wherein controlling seed crystal and AlN powder is 0～10mm; Seed crystal described in the step 1 is that diameter is 2 inches a zero microtubule 6H-SiC seed crystal, and SiC departs from 3.4 ° in
face;
Two, with the AlN powder after the presintering in the crucible under 1 atmospheric high pure nitrogen atmosphere, with the temperature rise rate of 150 ℃/h, heat temperature raising to 2300 ℃ carried out insulation reaction 12 hours, with the rate of temperature fall of 150 ℃/h, reduced to room temperature again, obtained the AlN crystal.
The volume percent purity of high pure nitrogen is 99.999% in the present embodiment, the raw materials used commercially available prod that is.
Embodiment six:
The difference of present embodiment and embodiment five is: seed crystal described in the step 1 is that diameter is 2 inches a zero microtubule 6H-SiC seed crystal; SiC departs from 3.5 ° in
face, and other is identical with embodiment five.
Embodiment seven:
The difference of present embodiment and embodiment five is: seed crystal described in the step 1 is that diameter is 2 inches a zero microtubule 6H-SiC seed crystal; SiC departs from 4 ° in
face, and other is identical with embodiment five.
Embodiment eight:
The difference of present embodiment and embodiment five is: seed crystal described in the step 1 is that diameter is 2 inches a zero microtubule 6H-SiC seed crystal; SiC departs from 6.5 ° in
face, and other is identical with embodiment five.
Embodiment nine:
The difference of present embodiment and embodiment five is: seed crystal described in the step 1 is that diameter is 2 inches a zero microtubule 6H-SiC seed crystal; SiC departs from 8 ° in
face, and other is identical with embodiment five.
In the foregoing description, use zero microtubule drift angle degree SiC seeded growth AlN crystal, will help obtaining high-quality AlN crystal; This shows: 1. micropipe defects is a SiC crystalline typical defect, in the AlN crystal growing process that with SiC is seed crystal, exists the SiC seed crystal of micropipe defects can cause the AlN crystal lattice defects such as dislocation, fault to occur; Have a strong impact on the AlN crystal mass; Therefore, if select zero microtubule SiC, can reduce AlN crystalline defect concentration effectively as seed crystal.2. use zero microtubule SiC seed crystal; At
face growing AIN crystal; The existing defective of SiC seed crystal (like dislocation, fault etc.) largely upper edge aufwuchsplate entails the AlN crystal; If the SiC seed crystal departs from
face certain angle (scope is between 0-8 °); The probability of defective heredity will significantly reduce, thereby AlN crystalline quality is further enhanced.
Embodiment ten:
The difference of present embodiment and embodiment five is: seed crystal described in the step 1 is that diameter is 1 inch the compound seed crystal of zero microtubule 6H-SiC/AlN; SiC departs from 4 ° in
face; The zero compound seed crystal of microtubule 6H-SiC/AlN is through metal-organic chemical vapor deposition equipment method (MOCVD) in the present embodiment, and epitaxy AlN impact plies is prepared from zero microtubule 6H-SiC substrate.Other is identical with embodiment five.
Embodiment 11:
The difference of present embodiment and embodiment five is: seed crystal described in the step 1 is that diameter is 2 inches the compound seed crystal of zero microtubule 6H-SiC/AlN; SiC departs from 8 ° in
face; The zero compound seed crystal of microtubule 6H-SiC/AlN is through metal-organic chemical vapor deposition equipment method (MOCVD) in the present embodiment, and epitaxy AlN impact plies is prepared from zero microtubule 6H-SiC substrate.Other is identical with embodiment five.
Embodiment 12:
The difference of present embodiment and embodiment five is: seed crystal described in the step 1 is that diameter is 3 inches the compound seed crystal of zero microtubule 6H-SiC/AlN; SiC departs from 8 ° in
face; The zero compound seed crystal of microtubule 6H-SiC/AlN is through metal-organic chemical vapor deposition equipment method (MOCVD) in the present embodiment, and epitaxy AlN impact plies is prepared from zero microtubule 6H-SiC substrate.Other is identical with embodiment five.
In the foregoing description; Use the compound seeded growth AlN of SiC/AlN crystal; To help obtaining high-quality AlN crystal; By the compound seed crystal of SiC/AlN that the SiC seed crystal of zero microtubule, drift angle degree is prepared, its AlN impact plies will effectively be alleviated thermal mismatching and the lattice mismatch of SiC and AlN, help reducing AlN crystalline defect concentration.
Claims (9)
1. an AlN crystalline preparation method adopts the physical vapor transmission method to prepare the AlN monocrystalline, it is characterized in that AlN crystalline preparation method realizes through following steps:
One, the AlN powder is placed crucible, then seed crystal is fixed on the crucible top, the distance of seed crystal and AlN powder is not more than 10mm; Be put into crucible in the monocrystal growing furnace again, in crucible, feed nitrogen, under 1 atmospheric nitrogen atmosphere; Temperature rise rate with 50 ℃/h～200 ℃/h; Heat temperature raising to 1800 ℃～2000 ℃, and be incubated 1～5 hour, accomplish the presintering of AlN powder;
Two, with the AlN powder after the presintering in the crucible under 1 atmospheric high pure nitrogen atmosphere; Temperature rise rate with 50 ℃/h～200 ℃/h; Heat temperature raising to 2150 ℃～2500 ℃ carried out insulation reaction 8～20 hours, again with the rate of temperature fall of 50 ℃/h～200 ℃/h; Reduce to room temperature, obtain the AlN crystal;
Seed crystal described in the step 1 is zero microtubule drift angle degree SiC seed crystal or the compound seed crystal of SiC/AlN; Wherein the crystal formation of zero microtubule drift angle degree SiC seed crystal is 6H-, and the drift angle degree is meant that SiC departs from the angle of 0 °～8 ° in
face.
2. a kind of AlN crystalline preparation method according to claim 1 is characterized in that in the step 1 that the distance of control seed crystal and AlN powder is 5～9mm.
3. a kind of AlN crystalline preparation method according to claim 2 is characterized in that the compound seed crystal of SiC/AlN is through the metal-organic chemical vapor deposition equipment method in the step 1, and epitaxy AlN impact plies is prepared from zero microtubule drift angle degree SiC substrate.
4. a kind of AlN crystalline preparation method according to claim 3, the diameter that it is characterized in that seed crystal described in the step 1 is 1 inch, 2 inches or 3 inches.
5. a kind of AlN crystalline preparation method according to claim 1 is characterized in that the drift angle degree of zero microtubule drift angle degree SiC described in the step 1 is meant that SiC departs from the angle of
.
6. a kind of AlN crystalline preparation method according to claim 1 is characterized in that the drift angle degree of zero microtubule drift angle degree SiC described in the step 1 is meant that SiC departs from the angle of
.
7. a kind of AlN crystalline preparation method according to claim 1 and 2 is characterized in that in the step 2 heat temperature raising to 2200 ℃～2450 ℃ carrying out insulation reaction 8～20 hours.
8. a kind of AlN crystalline preparation method according to claim 1 and 2 is characterized in that in the step 2 that heat temperature raising to 2250 ℃～2400 ℃ carried out insulation reaction 8～20 hours.
9. a kind of AlN crystalline preparation method according to claim 1 and 2 is characterized in that in the step 2 heat temperature raising to 2300 ℃ carrying out insulation reaction 8～20 hours.
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