CN108275664A - A kind of high temperature sintering method of purification for aluminium nitride - Google Patents
A kind of high temperature sintering method of purification for aluminium nitride Download PDFInfo
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- CN108275664A CN108275664A CN201711481757.7A CN201711481757A CN108275664A CN 108275664 A CN108275664 A CN 108275664A CN 201711481757 A CN201711481757 A CN 201711481757A CN 108275664 A CN108275664 A CN 108275664A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
- C01B21/0728—After-treatment, e.g. grinding, purification
-
- 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
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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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/89—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by mass-spectroscopy
Abstract
The invention discloses a kind of high temperature sintering methods of purification for aluminium nitride can effectively remove the impurity in aluminium nitride powder by multiple multisection type heating and thermal insulation, and repeatedly sintering can be further reduced the impurity in aluminium nitride powder;During heating and thermal insulation, it is passed through the high pure nitrogen of flowing, can efficiently take away the impurity in aluminium nitride powder;By the way that the temperature of sintering is increased to long brilliant temperature, removal impurity that can be more efficient;The aluminium nitride polycrystal of obtained surface irregularity is crushed into dusting cover, high temperature sintering cleans again, and controls temperature under long brilliant temperature, with obtain relatively low impurity content, surfacing, regular shape aluminum nitride sintered body.
Description
Technical field
The present invention relates to aluminum-nitride single crystal Material growth technical fields, more particularly to a kind of high temperature sintering for aluminium nitride
Method of purification.
Background technology
Aluminium nitride (AlN) is one of third generation semiconductor material with wide forbidden band, has broad-band gap, high-melting-point, high critical breakdown
Field strength, high high-temp stability and the excellent properties such as resistant to chemical etching, are mainly used in light emitting diode (LED), laser diode
(LD), in the devices such as second harmonic transmitter and surface acoustic wave.AlN crystal is typical direct band-gap semicondictor, AlN under room temperature
Theoretical energy gap Eg=6.2eV of crystal.Since AlN crystal has the band gap of 6.2eV, theoretically highly crystalline quality
AlN crystal has very high transmissivity in ultraviolet band, is the ideal substrate of ultrashort wavelength (200-270nm) LED or LD devices
Material, currently, the transmission band of AlN crystal at ultraviolet end up to 200nm.
The theoretical calculation fusing point of material is 2800 DEG C, dissociation pressure 20MPa, and therefore, it is difficult to use melt vertical pulling method or temperature
The technology of gradient freeze method carries out crystal growth.The growing method of AlN monocrystalline is identical as the growing method of SiC single crystal, is to pass through
Physical vapor transport(PVT)Growth.Using containing high concentration in the AlN powders used in PVT method growing AIN monocrystalline
The impurity such as oxygen, carbon, these impurity can seriously affect nucleation, two-dimensional growth and the crystal quality of AlN monocrystalline in growth course, because
This must carry out high temperature purification to AlN raw materials first before crystal growth, fully remove the impurity such as oxygen and carbon therein, improve former
The purity of material.
Aluminium nitride crystallizes during high temperature purification in order to prevent, all controls the purification temperature of aln raw material at present
Under crystallization temperature, and temperature is higher, and the efficiency of removal of impurities is also higher.
Invention content
The object of the present invention is to provide a kind of high temperature sintering method of purification for aluminium nitride, it can be sintered to obtain impurity and contain
Measure lower aluminum nitride sintered body.
In order to achieve the above objectives, the technical solution adopted by the present invention is:
A kind of high temperature sintering method of purification for aluminium nitride includes the steps that carrying out successively(a)And step(b);Wherein, step
(a)At least cycle carries out primary, and in step(b)It carries out before;
Step(a):
(1)Aluminium nitride powder is put into shoe, and the shoe is placed in furnace body, and the furnace body is taken out true
It is empty;
(2)Heating the shoe makes the temperature of aluminium nitride powder reach 900-1200 DEG C, and keeps 4-8h, by following anti-
It answers, takes away partial impurities:
2Al(OH)3=Al2O3+3H2O(g);
2Al(OOH)=Al2O3+H2O(g);
Aluminium nitride powder is sintered into aluminum nitride sintered body in the shoe;
(3)The high pure nitrogen of 50-90Kpa is passed through into the furnace body, while heating the shoe to make aluminum nitride sintered body
Temperature reach 1400-1600 DEG C, and keep 4-8h, by reacting as follows, take away partial impurities:
Al2O3(s)+3C+N2(g)=2AlN(g)+3CO(g);
Circulation status of the high pure nitrogen in the furnace body is kept, takes the foreign gas that reaction generates out of the furnace body;
(4)The high pure nitrogen of 50-90Kpa is passed through into the furnace body, while heating the shoe to make aluminum nitride sintered body
Temperature reach 2000-2300 DEG C, and keep 6-10h, by reacting as follows, take away partial impurities:
Al2O3+4Al(g)=3Al2O(g);
Circulation status of the high pure nitrogen in the furnace body is kept, takes the foreign gas that reaction generates out of the furnace body;
(5)Cool down to the shoe, the temperature of aluminum nitride sintered body is made to be down to 100 DEG C;
(6)Aluminum nitride sintered body is cooled to room temperature, takes out and crushes aluminum nitride sintered body, be carried out at the same time dusting cover, nitrogenized
Aluminium powder;
Step(b):
(7)The aluminium nitride powder obtained after dusting cover is put into the shoe, and the shoe is placed in the stove
In body;
(8)Heating the shoe makes the temperature of aluminium nitride powder reach 900-1200 DEG C, and keeps 2-4h, by following anti-
It answers, takes away partial impurities:
2Al(OH)3=Al2O3+3H2O(g);
2Al(OOH)=Al2O3+H2O(g);
Aluminium nitride powder is sintered into aluminum nitride sintered body in the shoe;
(9)The high pure nitrogen of 50-90Kpa is passed through into the furnace body, while heating the shoe to make aluminum nitride sintered body
Temperature reach 1400-1600 DEG C, and keep 2-4h, by reacting as follows, take away partial impurities:
Al2O3(s)+3C+N2(g)=2AlN(g)+3CO(g);
Circulation status of the high pure nitrogen in the furnace body is kept, takes the foreign gas that reaction generates out of the furnace body;
(10)The high pure nitrogen of 50-90Kpa is passed through into the furnace body, while heating the shoe to make aluminum nitride sintered body
Temperature reach 1800-2000 DEG C, and keep 4-8h, by reacting as follows, take away partial impurities:
Al2O3+4Al(g)=3Al2O(g);
Circulation status of the high pure nitrogen in the furnace body is kept, takes the foreign gas that reaction generates out of the furnace body.
Preferably, in step(6)In, pass sequentially through the sieve of 50 mesh, the sieve of 100 mesh, the sieve of 200 mesh, 500 purposes
Sieve carries out dusting cover to the aluminum nitride sintered body after crushing, to obtain aluminium nitride powder.
Preferably, in step(5)In, rate of temperature fall is 5-10 DEG C/min.
Preferably, in step(3)In, the high pure nitrogen of 60-80Kpa is passed through into the furnace body.
Preferably, in step(4)In, the high pure nitrogen of 60-80Kpa is passed through into the furnace body.
Preferably, in step(9)In, the high pure nitrogen of 60-80Kpa is passed through into the furnace body.
Preferably, in step(10)In, the high pure nitrogen of 60-80Kpa is passed through into the furnace body.
Due to the application of the above technical scheme, the present invention has following advantages compared with prior art:A kind of use of the present invention
In the high temperature sintering method of purification of aluminium nitride, multisection type heating and thermal insulation can effectively remove the impurity in aluminium nitride powder, more
Secondary sintering can be further reduced the impurity in aluminium nitride powder;It, being capable of higher by the way that the temperature of sintering is increased to long brilliant temperature
The removal impurity of effect;The aluminium nitride polycrystal of obtained surface irregularity is crushed into dusting cover, high temperature sintering cleans again, and
And control temperature is under long brilliant temperature, with obtain relatively low impurity content, surfacing, regular shape aluminum nitride sintered body.
Specific implementation mode
Technical scheme of the present invention is further elaborated with reference to specific embodiment.
Above-mentioned a kind of high temperature sintering method of purification for aluminium nitride, for being sintered the aluminum nitride powder containing trace impurity
End, in the present embodiment, the purity of the aluminium nitride powder is 99%.Since aluminium nitride is during manufacture and preservation, meeting and air
In water and oxygen reaction, generate AlOOH, Al (OH)3、Al2O3Equal impurity, bring the impurity elements such as hydrogen, oxygen, carbon.
In aluminium nitride powder production process:
Al2O3(s)+3C(s)+N2(g)→2AlN(s)+3CO(g);
The reaction causes to contain C impurity and Al in the aluminium nitride powder produced2O3Impurity.
The aerial reaction of aluminium nitride powder:
AlN(s)+2H2O(g)→AlOOH(s)+NH3(g);
AlN(s)+3H2O(g)→Al(OH)3(s)+NH3(g);
AlN(s)+O2(g)→Al2O3(s)+N2(g);
The reaction causes to contain AlOOH impurity As l (OH) in aluminium nitride powder3Impurity, Al2O3Impurity.
Here is an a kind of specific embodiment of aln raw material high temperature purification method, and this method includes carrying out successively
Step(a)And step(b);Wherein, step(a)At least cycle carries out primary, and in step(b)It carries out before;In this implementation
In example, step(a)It only carries out primary.
Step(a):
(1)Aluminium nitride powder is put into shoe, and shoe is placed in furnace body, and furnace body is vacuumized;
(2)Heating shoe makes the temperature of aluminium nitride powder reach 900-1200 DEG C, and keeps 4-8h, by reacting as follows,
Take away partial impurities:
2Al(OH)3=Al2O3+3H2O(g);
2Al(OOH)=Al2O3+H2O(g);
Aluminium nitride powder is sintered into aluminum nitride sintered body in shoe;In the present embodiment, heating heating shoe
So that the temperature of aluminium nitride powder is reached 1000 DEG C, and keeps 6h;
(3)The high pure nitrogen of 50-90Kpa is passed through into furnace body, while heating shoe makes the temperature of aluminum nitride sintered body reach
To 1400-1600 DEG C, and 4-8h is kept, by reacting as follows, takes away partial impurities:
Al2O3(s)+3C+N2(g)=2AlN(g)+3CO(g);
Circulation status of the high pure nitrogen in furnace body is kept, takes the foreign gas that reaction generates out of furnace body;In the present embodiment,
The high pure nitrogen of 60-80Kpa is passed through into furnace body;Heating shoe makes the temperature of aluminum nitride sintered body reach 1500 DEG C, and
Keep 6h;
(4)The high pure nitrogen of 50-90Kpa is passed through into furnace body, while heating shoe makes the temperature of aluminum nitride sintered body reach
To 2000-2300 DEG C, and 6-10h is kept, by reacting as follows, takes away partial impurities:
Al2O3+4Al(g)=3Al2O(g);
Circulation status of the high pure nitrogen in furnace body is kept, takes the foreign gas that reaction generates out of furnace body;In the present embodiment,
The high pure nitrogen of 60-80Kpa is passed through into furnace body;Heating shoe makes the temperature of aluminum nitride sintered body reach 2200 DEG C, and
Keep 8h;
In step(4)In, since heating temperature has reached the long brilliant temperature of aluminium nitride, although temperature is higher, impurities removing efficiency it is higher and
Impurity-eliminating effect is preferable, but obtained aluminium nitride polycrystal surface irregularity, is not used to crystal growth;
(5)Cool down to shoe, the temperature of aluminum nitride sintered body is made to be down to 100 DEG C;In the present embodiment, rate of temperature fall
For 5-10 DEG C/min;
(6)Aluminum nitride sintered body is cooled to room temperature, takes out and crushes aluminum nitride sintered body, be carried out at the same time dusting cover, nitrogenized
Aluminium powder;In the present embodiment, the aluminum nitride sintered body that will be cooled to room temperature is wrapped up with high-purity aluminum foil multilayer, the nitrogen that will be wrapped
Change aluminum sinter body and is placed on punching press crushing in high rigidity press machine groove;
The sieve of the sieve of 50 mesh, the sieve of 100 mesh, the sieve of 200 mesh, 500 mesh is passed sequentially through to the aluminium nitride burning after crushing
Knot body carries out dusting cover, to obtain aluminium nitride powder;Aluminium nitride powder diameter after sieve screens is less than 25um, passes through sieve
Aluminium foil impurity is filtered out, ensures the high-purity of aluminium nitride powder;Aluminium nitride powder screening operates in glove box, leads in glove box
Enter high pure nitrogen, can avoid aluminium nitride powder and reacted with the vapor in air and oxygen, avoids introducing carbon, oxygen, hydrogen impurity;
Step(b):
(7)The aluminium nitride powder obtained after dusting cover is put into shoe, and shoe is placed in furnace body;
(8)Heating shoe makes the temperature of aluminium nitride powder reach 900-1200 DEG C, and keeps 2-4h, by reacting as follows,
Take away partial impurities:
2Al(OH)3=Al2O3+3H2O(g);
2Al(OOH)=Al2O3+H2O(g);
Aluminium nitride powder is sintered into aluminum nitride sintered body in shoe;In the present embodiment, heating shoe makes nitrogen
The temperature for changing aluminium powder reaches 1000 DEG C, and keeps 2h;
(9)The high pure nitrogen of 50-90Kpa is passed through into furnace body, while heating shoe makes the temperature of aluminum nitride sintered body reach
To 1400-1600 DEG C, and 2-4h is kept, by reacting as follows, takes away partial impurities:
Al2O3(s)+3C+N2(g)=2AlN(g)+3CO(g);
Circulation status of the high pure nitrogen in furnace body is kept, takes the foreign gas that reaction generates out of furnace body;In the present embodiment,
The high pure nitrogen of 60-80Kpa is passed through into furnace body;Heating shoe makes the temperature of aluminium nitride powder reach 1500 DEG C, and protects
Hold 2h;
(10)The high pure nitrogen of 50-90Kpa is passed through into furnace body, while heating shoe makes the temperature of aluminum nitride sintered body reach
To 1800-2000 DEG C, and 4-8h is kept, by reacting as follows, takes away partial impurities:
Al2O3+4Al(g)=3Al2O(g);
Circulation status of the high pure nitrogen in furnace body is kept, takes the foreign gas that reaction generates out of furnace body;In the present embodiment,
The high pure nitrogen of 60-80Kpa is passed through into furnace body;Heating shoe makes the temperature of aluminium nitride powder reach 1900 DEG C, and protects
Hold 4h.
Due to step(10)In temperature be not up to the long brilliant temperature of aluminium nitride, therefore step(10)After, aluminium nitride
The surfacing of sintered body disclosure satisfy that the needs of long crystalline substance.
By the above method, can obtain relatively low impurity content, surfacing, regular shape aluminum nitride sintered body.
In the present embodiment, twice(Three sections every time)High temperature sintering obtains aluminum nitride sintered body, passes through glow discharge spectrometry
(GDMS)Test, wherein oxygen content are 150ppm, and carbon content 100ppm, which is high purity silicon nitride aluminum sinter
Body.According to actual needs, suitably increase sintering number, to reach the purity of requirement.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar can understand present disclosure and be implemented, and it is not intended to limit the scope of the present invention, all according to the present invention
Equivalent change or modification made by Spirit Essence should all cover within the scope of the present invention.
Claims (7)
1. a kind of high temperature sintering method of purification for aluminium nitride, it is characterised in that:Include the steps that carrying out successively(a)And step
(b);Wherein, step(a)At least cycle carries out primary, and in step(b)It carries out before;
Step(a):
(1)Aluminium nitride powder is put into shoe, and the shoe is placed in furnace body, and the furnace body is taken out true
It is empty;
(2)Heating the shoe makes the temperature of aluminium nitride powder reach 900-1200 DEG C, and keeps 4-8h, by following anti-
It answers, takes away partial impurities:
2Al(OH)3=Al2O3+3H2O(g);
2Al(OOH)=Al2O3+H2O(g);
Aluminium nitride powder is sintered into aluminum nitride sintered body in the shoe;
(3)The high pure nitrogen of 50-90Kpa is passed through into the furnace body, while heating the shoe to make aluminum nitride sintered body
Temperature reach 1400-1600 DEG C, and keep 4-8h, by reacting as follows, take away partial impurities:
Al2O3(s)+3C+N2(g)=2AlN(g)+3CO(g);
Circulation status of the high pure nitrogen in the furnace body is kept, takes the foreign gas that reaction generates out of the furnace body;
(4)The high pure nitrogen of 50-90Kpa is passed through into the furnace body, while heating the shoe to make aluminum nitride sintered body
Temperature reach 2000-2300 DEG C, and keep 6-10h, by reacting as follows, take away partial impurities:
Al2O3+4Al(g)=3Al2O(g);
Circulation status of the high pure nitrogen in the furnace body is kept, takes the foreign gas that reaction generates out of the furnace body;
(5)Cool down to the shoe, the temperature of aluminum nitride sintered body is made to be down to 100 DEG C;
(6)Aluminum nitride sintered body is cooled to room temperature, takes out and crushes aluminum nitride sintered body, be carried out at the same time dusting cover, nitrogenized
Aluminium powder;
Step(b):
(7)The aluminium nitride powder obtained after dusting cover is put into the shoe, and the shoe is placed in the stove
In body;
(8)Heating the shoe makes the temperature of aluminium nitride powder reach 900-1200 DEG C, and keeps 2-4h, by following anti-
It answers, takes away partial impurities:
2Al(OH)3=Al2O3+3H2O(g);
2Al(OOH)=Al2O3+H2O(g);
Aluminium nitride powder is sintered into aluminum nitride sintered body in the shoe;
(9)The high pure nitrogen of 50-90Kpa is passed through into the furnace body, while heating the shoe to make aluminum nitride sintered body
Temperature reach 1400-1600 DEG C, and keep 2-4h, by reacting as follows, take away partial impurities:
Al2O3(s)+3C+N2(g)=2AlN(g)+3CO(g);
Circulation status of the high pure nitrogen in the furnace body is kept, takes the foreign gas that reaction generates out of the furnace body;
(10)The high pure nitrogen of 50-90Kpa is passed through into the furnace body, while heating the shoe to make aluminum nitride sintered body
Temperature reach 1800-2000 DEG C, and keep 4-8h, by reacting as follows, take away partial impurities:
Al2O3+4Al(g)=3Al2O(g);
Circulation status of the high pure nitrogen in the furnace body is kept, takes the foreign gas that reaction generates out of the furnace body.
2. a kind of high temperature sintering method of purification for aluminium nitride according to claim 1, it is characterised in that:In step
(6)In, the sieve of the sieve of 50 mesh, the sieve of 100 mesh, the sieve of 200 mesh, 500 mesh is passed sequentially through to the aluminium nitride after crushing
Sintered body carries out dusting cover, to obtain aluminium nitride powder.
3. a kind of high temperature sintering method of purification for aluminium nitride according to claim 1, it is characterised in that:In step
(5)In, rate of temperature fall is 5-10 DEG C/min.
4. a kind of high temperature sintering method of purification for aluminium nitride according to claim 1, it is characterised in that:In step
(3)In, the high pure nitrogen of 60-80Kpa is passed through into the furnace body.
5. a kind of high temperature sintering method of purification for aluminium nitride according to claim 1, it is characterised in that:In step
(4)In, the high pure nitrogen of 60-80Kpa is passed through into the furnace body.
6. a kind of high temperature sintering method of purification for aluminium nitride according to claim 1, it is characterised in that:In step
(9)In, the high pure nitrogen of 60-80Kpa is passed through into the furnace body.
7. a kind of high temperature sintering method of purification for aluminium nitride according to claim 1, it is characterised in that:In step
(10)In, the high pure nitrogen of 60-80Kpa is passed through into the furnace body.
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CN109576783A (en) * | 2019-01-23 | 2019-04-05 | 山东大学 | A kind of preprocessing method of raw materials for high quality aluminum nitride crystal growth |
CN110015648A (en) * | 2019-03-28 | 2019-07-16 | 北京中材人工晶体研究院有限公司 | A kind of high-purity aluminium nitride powder and aluminium nitride powder method of purification |
CN113789573A (en) * | 2021-11-16 | 2021-12-14 | 山西中科潞安紫外光电科技有限公司 | Method for preparing AlN crystal by spontaneous nucleation through PVT method |
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CN116143085A (en) * | 2022-12-26 | 2023-05-23 | 奥趋光电技术(杭州)有限公司 | Preparation method of high-purity aluminum nitride raw material |
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Cited By (7)
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