CN110015648A - A kind of high-purity aluminium nitride powder and aluminium nitride powder method of purification - Google Patents
A kind of high-purity aluminium nitride powder and aluminium nitride powder method of purification Download PDFInfo
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- CN110015648A CN110015648A CN201910243035.0A CN201910243035A CN110015648A CN 110015648 A CN110015648 A CN 110015648A CN 201910243035 A CN201910243035 A CN 201910243035A CN 110015648 A CN110015648 A CN 110015648A
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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
- C01B21/0722—Preparation by direct nitridation of aluminium
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- C—CHEMISTRY; METALLURGY
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- 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
Abstract
The present invention relates to a kind of high-purity aluminium nitride powder and aluminium nitride powder methods of purification.The processing of high temperature air purge is carried out to the synthetic cavity where the mixed powder of Al powder and AlN powder using reducing gas, for removing the oxygen in the synthetic cavity；Under vacuum state, at a temperature of the first purification, the hydroxide in the mixed powder impurity is removed, at a temperature of the second purification, the carbon in the mixed powder impurity is removed, at a temperature of third purification, utilizes the aluminium oxide in mixed powder impurity described in the Al vapour removal.Method of purification is simple, pass through the rational design of impurity removal sequence and corresponding purification step, in addition the addition of Al powder, effectively inhibit the decomposition of AlN powder in purification process, reduce the loss of raw material, as High frequency combustion infrared-adsorption method and noble gas pulsed infrared thermal conductivity method test it is of the invention obtained by aluminium nitride powder carbon content be 42PPM, oxygen content 220PPM, purity is high.
Description
Technical field
The present invention relates to aluminium nitride preparations, are specifically related to a kind of high-purity aluminium nitride powder and aluminium nitride powder purification side
Method.
Background technique
Semiconductor material and synthetic technology are the foundation stones of modern information technologies development, and 20th century are with silicon (Si) and GaAs
(GaAs) fast development of electronics and photoelectric technology, in the 21st century, have been pushed for the first and second generation semiconductor material of representative
With the requirements at the higher level to material property, with aluminium nitride (AlN), silicon carbide (SiC), the third generation that gallium nitride (GaN) is representative
Semiconductor material compensates for the first and second generation material intrinsic performance deficiency, is greatly promoted the development of semicon industry.
AlN has direct band gap 6.2eV, and band is roomy, and luminescence band can be important indigo plant as deep as 200nm
Light, purple light luminescent material；Fusing point is high, and 2800 DEG C of calculated value；In addition chemical stability is good, high disruptive field intensity 11.7MV/
Cm, dielectric constant is low, more excellent heat-conductive characteristic, can be widely applied to the electricity of high temperature, high pressure, high-frequency high-power electric appliance
Sub- material, table 1 provide the comparison of one or two three generations's semiconductor material performances.
Table 1: semiconductor material performance comparison
More importantly AlN is growth group III-nitride epitaxial layer and device architecture compared with Si, sapphire, SiC
Ideal substrate, advantage have: there was only 2.4% lattice mismatch with GaN, thermal mismatching is almost 0；Crystal structure is identical, is not in
Faulted layer；Chemical stabilization and without other elements exist to contamination of substrate it is few.Table 2 provides part semiconductor and the matching feelings of GaN
Condition.
Table 2: the lattice and thermally matched situation of semiconductor and GaN
| As GaN substrate | Si | Al2O3 | SiC | AlN |
| Lattice mismatch ratio | 17% | 13.8% | 3.4% | 2.4% |
| Thermal mismatching ratio | 56% | 33.9% | 25% | 0 |
At present there are mainly two types of the methods of synthesis aluminium nitride, one kind is gas phase physical transfer (PVT), and another kind is hydride
Vapour phase epitaxy (HVPE), according to the difference of composition principle, HVPE method synthesis temperature is low, but the speed of growth is slow, is suitble to film raw
It is long；PVT method is the disadvantage is that synthesis temperature is high, but aggregate velocity is fast, therefore this method is suitble to body crystals growth.PVT method grows crystal
The process in low-temperature space crystal growth, and powder bring carbon, oxygen in growth course are decomposed in high-temperature region distillation by AlN powder
Impurity element influences the performance of crystal, such as to ultraviolet permeability, heating conduction, high voltage performance or even a large amount of impurity elements
Aggregation the problems such as will lead to crystal cleavage, need to handle material powder removal of impurities to solve this problem, current powder is except living together
Reason method is powder to be put into high-temperature crucible then to handle by high-temperature calcination, excludes impurity substances in powder, has cleaned
It is even crystallized at rear powder at irregular roundness cylindricality and ceramic, and cylindrical-shaped structure is unfavorable for the exclusion of bulk inner impurity,
And the high rigidity of ceramic brings great difficulty during later period crushing grinding, causes powder transition loss, it is broken using machinery
It is broken, and easily cause the secondary pollution of raw material.The above problem is badly in need of solving.
Summary of the invention
In order to solve the above-mentioned technical problem, the purpose of the present invention is to provide a kind of high-purity aluminium nitride powder and aluminium nitride
Powder method of purification.
According to an aspect of the invention, there is provided a kind of aluminium nitride powder method of purification, comprising the following steps:
The processing of high temperature air purge is carried out to the synthetic cavity where the mixed powder of Al powder and AlN powder using reducing gas, is used
Oxygen in the removal synthetic cavity；
Under vacuum state, aluminium nitride powder purification processes are carried out to the mixed powder, wherein
At a temperature of the first purification, the hydroxide in the mixed powder impurity is removed,
At a temperature of the second purification, the carbon in the mixed powder impurity is removed,
At a temperature of third purification, it is filled with high pure nitrogen, Al powder in the mixed powder forms Al steam, using described
Aluminium oxide in mixed powder impurity described in Al vapour removal, then cools down, through crushing grinding under high purity inert gas protection
It handles up to high-purity aluminium nitride powder.
Further, the molar ratio of Al powder and AlN powder is 0.1-0.5:1.A small amount of high-purity Al is added in AlN powder
Powder can effectively reduce transition of the AlN powder in high temperature purification and decompose, improve the decomposition rate of impurity substances in powder.The two ratio
For example by lot of experiment validation when the molar ratio of Al powder and AlN powder is 0.1-0.5:1, Al powder function and effect described above are best.
The mixed powder carries out cold moudling under high purity inert gas protection, is subsequently placed in synthetic cavity.It is described
Mixed powder is tubular by mold cold moudling, can make to calcine uniformly when powder high-temperature calcination, be conducive to hand breaking and grind,
It reduces Mechanical Crushing and grinds bring secondary pollution.
The reducing gas is that the synthetic cavity is under vacuum state, the filling in the synthetic cavity.
The vacuum degree < 1 × 10 of the vacuum state-4Pa。
The reducing gas is the mixed gas of hydrogen and nitrogen, wherein hydrogen 0.5%-5% of the total volume.
The temperature of high temperature air purge processing is 200-400 DEG C.
The first purification temperature is 800-1000 DEG C, and the second purification temperature is 1700-1800 DEG C, and third purification temperature is
1900-2200℃。
In third purification phase, after being filled with high pure nitrogen, pressure 80-120KPa, with the cooling speed lower than 10 DEG C/min
Degree is down to 1000 DEG C, then vacuumizes and is evacuated to 1 × 10-4Pa is hereinafter, until be cooled to room temperature.
According to another aspect of the present invention, a kind of high-purity aluminium nitride powder is provided, according to nitridation described above
Aluminium powder body method of purification is made.
Compared with prior art, the invention has the following advantages:
Exemplary high-purity aluminium nitride powder of the invention and corresponding aluminium nitride powder method of purification, method of purification is simple,
By the rational design of impurity removal sequence and corresponding purification step, the addition of Al powder, is effectively inhibited in purification process in addition
The decomposition of AlN powder reduces the loss of raw material, is tested by High frequency combustion infrared-adsorption method and noble gas pulsed infrared thermal conductivity method
The carbon content of gained aluminium nitride powder of the invention is 42PPM, oxygen content 220PPM, purity is high.
Specific embodiment
In order to be better understood by technical solution of the present invention, the present invention is made into one below with reference to specification specific embodiment
Walk explanation.
Embodiment one
The aluminium nitride powder purification process of the present embodiment are as follows:
S1, by high-purity Al powder (99.99%) and AlN powder according to molar ratio 0.1-0.5:1, carry out uniformly mixed, then root
According to the dimension scale (crucible internal diameter is Φ 60mm, height 60mm) of high-temperature calcination crucible design, tungsten is used in inertia glove box
Matter mold (or aluminum) carries out cold moudling to mixed powder, by the preferable powder packed of mobility to tungsten matter metal die cavity,
Briquetting pressure is in 0.5-4MPa, by carrying out cold pressing tubular design to powder, so that subsequent powder high-temperature calcination is uniform, thus sharp
It is ground in hand breaking, reduces Mechanical Crushing and grind bring secondary pollution.Molding outside diameter of cylinder < 60mm, internal diameter >
20mm, the ratio between internal-and external diameter are greater than 1/3, height 50-60mm (according to calcining crucible size).
S2, molding powder is put into tungsten crucible, covers crucible cover, the high pure nitrogen filled in crucible at this time.Then
Crucible is put into high temperature furnace, is evacuated to 1 × 10-4Pa is hereinafter, be subsequently filled hydrogen and nitrogen mixed gas, wherein hydrogen accounts for
Total volume is 0.5%-5%, and temperature is increased to 200-400 DEG C, and gas keeps recurrent state, is kept for 1-2 hours, by being filled with hydrogen
Gas and nitrogen mixing reducing gas, exclude oxygen in synthetic cavity under 200-400 DEG C of high temperature, pairing as water vapor
Forming apparatus chamber carries out the processing of high temperature air purge, reaction process this moment are as follows:
H2(g)+O2(g)=H2O(g)
S3, it is evacuated to 1 × 10-4After Pa is hereinafter, temperature drops to room temperature, ultra-high vacuum state is kept, temperature rises to 800-
1000 DEG C, 6-10 hours are kept the temperature, easily quickly generates hydroxide film (main component AlOOH) since AlN powder is contacted with air,
It needs to formulate corresponding process flow according to the reaction of AlOOH at high temperature, reaction process this moment are as follows:
2AlOOH (s)=Al2O3(s)+H2O(g)
S4, high vacuum state is kept, temperature rises to 1700-1800 DEG C, keeps the temperature 6-10 hours, this moment reaction process are as follows:
Al2O3(s)+3C (s)=2Al (g)+3CO (g)
Al2O3(s)+3C (s)=Al2(g)+3CO(g)
Al2O3(s)+C (s)=Al2O(g)+2CO(g)
Al2O3(s)+C (s)=2AlO (g)+CO (g)
S5, temperature are increased to 1900-2200 DEG C, are filled with high pure nitrogen, and pressure 80-120KPa keeps the temperature 6-10 hours, this
The decomposition that high pressure inhibits AlN is carved, powder loss is reduced, while metal Al forms Al steam and oxidation reactive aluminum under high temperature, this moment
Reaction process are as follows:
Al2O3(s)+4Al (g)=3Al2O(g)
S6, after the reaction was completed is down to 1000 DEG C with the cooling rate lower than 10 DEG C/min, then vacuumizes and be evacuated to 1 × 10- 4Pa is subsequently filled the high pure nitrogen of 1atm hereinafter, up to being cooled to room temperature, and crucible taking-up is put into inertia glove box and is carried out
Crushing grinding processing, is detected after the completion of processing.
Embodiment two
The aluminium nitride powder purification process of the present embodiment are as follows:
S1, by high-purity Al powder (99.99%) and AlN powder according to molar ratio 0.1:1, carry out it is uniformly mixed, then according to height
The dimension scale (crucible internal diameter is Φ 60mm, height 60mm) of warm calcining crucible design, uses tungsten matter mould in inertia glove box
Have (or aluminum) and cold moudling is carried out to mixed powder, by the preferable powder packed of mobility to tungsten matter metal die cavity, forms
Pressure is in 0.5-4MPa, by carrying out cold pressing tubular design to powder, so that subsequent powder high-temperature calcination is uniform, to be conducive to people
Work crushing grinding reduces Mechanical Crushing and grinds bring secondary pollution.Molding outside diameter of cylinder < 60mm, internal diameter > 20mm, it is interior
The ratio between outer diameter is greater than 1/3, height 50-60mm (according to calcining crucible size).
S2, molding powder is put into tungsten crucible, covers crucible cover, the high pure nitrogen filled in crucible at this time.Then
Crucible is put into high temperature furnace, is evacuated to 1 × 10-4Pa is hereinafter, be subsequently filled hydrogen and nitrogen mixed gas, wherein hydrogen accounts for
Total volume is 0.5%, and temperature is increased to 400 DEG C, and gas keeps recurrent state, is kept for 1-2 hours, by being filled with hydrogen and nitrogen
Mix reducing gas, oxygen in synthetic cavity is excluded as water vapor under 400 DEG C of high temperature, to synthesis device chamber into
The processing of row high temperature air purge, reaction process this moment are as follows:
H2(g)+O2(g)=H2O(g)
S3, it is evacuated to 1 × 10-4After Pa is hereinafter, temperature drops to room temperature, ultra-high vacuum state is kept, temperature rises to 800
DEG C, 10 hours are kept the temperature, easily hydroxide film (main component AlOOH) is quickly generated since AlN powder is contacted with air, needs root
Corresponding process flow is formulated according to the reaction of AlOOH at high temperature, reaction process this moment are as follows:
2AlOOH (s)=Al2O3(s)+H2O(g)
S4, high vacuum state is kept, temperature rises to 1700 DEG C, keeps the temperature 10 hours, this moment reaction process are as follows:
Al2O3(s)+3C (s)=2Al (g)+3CO (g)
Al2O3(s)+3C (s)=Al2(g)+3CO(g)
Al2O3(s)+C (s)=Al2O(g)+2CO(g)
Al2O3(s)+C (s)=2AlO (g)+CO (g)
S5, temperature are increased to 1900 DEG C, are filled with high pure nitrogen, and pressure 80-120KPa keeps the temperature 10 hours, this moment high pressure
Inhibit the decomposition of AlN, reduce powder loss, while metal Al forms Al steam and oxidation reactive aluminum, reaction this moment under high temperature
Process are as follows:
Al2O3(s)+4Al (g)=3Al2O(g)
S6, after the reaction was completed is down to 1000 DEG C with the cooling rate lower than 10 DEG C/min, then vacuumizes and be evacuated to 1 × 10- 4Pa is subsequently filled the high pure nitrogen of 1atm hereinafter, up to being cooled to room temperature, and crucible taking-up is put into inertia glove box and is carried out
Crushing grinding processing, is detected after the completion of processing.
Embodiment three
The aluminium nitride powder purification process of the present embodiment are as follows:
S1, by high-purity Al powder (99.99%) and AlN powder according to molar ratio 0.5:1, carry out it is uniformly mixed, then according to height
The dimension scale (crucible internal diameter is Φ 60mm, height 60mm) of warm calcining crucible design, uses tungsten matter mould in inertia glove box
Have (or aluminum) and cold moudling is carried out to mixed powder, by the preferable powder packed of mobility to tungsten matter metal die cavity, forms
Pressure is in 0.5-4MPa, by carrying out cold pressing tubular design to powder, so that subsequent powder high-temperature calcination is uniform, to be conducive to people
Work crushing grinding reduces Mechanical Crushing and grinds bring secondary pollution.Molding outside diameter of cylinder < 60mm, internal diameter > 20mm, it is interior
The ratio between outer diameter is greater than 1/3, height 50-60mm (according to calcining crucible size).
S2, molding powder is put into tungsten crucible, covers crucible cover, the high pure nitrogen filled in crucible at this time.Then
Crucible is put into high temperature furnace, is evacuated to 1 × 10-4Pa is hereinafter, be subsequently filled hydrogen and nitrogen mixed gas, wherein hydrogen accounts for
Total volume is 5%, and temperature is increased to 300 DEG C, and gas keeps recurrent state, is kept for 1-2 hours, mixed by being filled with hydrogen and nitrogen
Reducing gas is closed, excludes oxygen in synthetic cavity as water vapor under 300 DEG C of high temperature, synthesis device chamber is carried out
The processing of high temperature air purge, reaction process this moment are as follows:
H2(g)+O2(g)=H2O(g)
S3, it is evacuated to 1 × 10-4After Pa is hereinafter, temperature drops to room temperature, ultra-high vacuum state is kept, temperature rises to 900
DEG C, 8 hours are kept the temperature, easily hydroxide film (main component AlOOH) is quickly generated since AlN powder is contacted with air, needs root
Corresponding process flow is formulated according to the reaction of AlOOH at high temperature, reaction process this moment are as follows:
2AlOOH (s)=Al2O3(s)+H2O(g)
S4, high vacuum state is kept, temperature rises to 1800 DEG C, keeps the temperature 6 hours, this moment reaction process are as follows:
Al2O3(s)+3C (s)=2Al (g)+3CO (g)
Al2O3(s)+3C (s)=Al2(g)+3CO(g)
Al2O3(s)+C (s)=Al2O(g)+2CO(g)
Al2O3(s)+C (s)=2AlO (g)+CO (g)
S5, temperature are increased to 2200 DEG C, are filled with high pure nitrogen, and pressure 80-90KPa keeps the temperature 6 hours, this moment high to constrain
The decomposition of AlN processed reduces powder loss, while metal Al forms Al steam and oxidation reactive aluminum, reaction this moment under high temperature
Journey are as follows:
Al2O3(s)+4Al (g)=3Al2O(g)
S6, after the reaction was completed is down to 1000 DEG C with the cooling rate lower than 10 DEG C/min, then vacuumizes and be evacuated to 1 × 10- 4Pa is subsequently filled the high pure nitrogen of 1atm hereinafter, up to being cooled to room temperature, and crucible taking-up is put into inertia glove box and is carried out
Crushing grinding processing, is detected after the completion of processing.
Example IV
The aluminium nitride powder purification process of the present embodiment are as follows:
S1, by high-purity Al powder (99.99%) and AlN powder according to molar ratio 0.1-0.5:1, carry out uniformly mixed, then root
According to the dimension scale (crucible internal diameter is Φ 60mm, height 60mm) of high-temperature calcination crucible design, tungsten is used in inertia glove box
Matter mold (or aluminum) carries out cold moudling to mixed powder, by the preferable powder packed of mobility to tungsten matter metal die cavity,
Briquetting pressure is in 0.5-4MPa, by carrying out cold pressing tubular design to powder, so that subsequent powder high-temperature calcination is uniform, thus sharp
It is ground in hand breaking, reduces Mechanical Crushing and grind bring secondary pollution.Molding outside diameter of cylinder < 60mm, internal diameter >
20mm, the ratio between internal-and external diameter are greater than 1/3, height 55mm (according to calcining crucible size).
S2, molding powder is put into tungsten crucible, covers crucible cover, the high pure nitrogen filled in crucible at this time.Then
Crucible is put into high temperature furnace, is evacuated to 1 × 10-4Pa is hereinafter, be subsequently filled hydrogen and nitrogen mixed gas, wherein hydrogen accounts for
Total volume is 3%, and temperature is increased to 250 DEG C, and gas keeps recurrent state, is kept for 2 hours, is mixed by being filled with hydrogen with nitrogen
Reducing gas excludes oxygen in synthetic cavity under 250 DEG C of high temperature as water vapor, carries out to synthesis device chamber high
Wet washes processing, reaction process this moment are as follows:
H2(g)+O2(g)=H2O(g)
S3, it is evacuated to 1 × 10-4After Pa is hereinafter, temperature drops to room temperature, ultra-high vacuum state is kept, temperature rises to 800
DEG C, 10 hours are kept the temperature, easily hydroxide film (main component AlOOH) is quickly generated since AlN powder is contacted with air, needs root
Corresponding process flow is formulated according to the reaction of AlOOH at high temperature, reaction process this moment are as follows:
2AlOOH (s)=Al2O3(s)+H2O(g)
S4, high vacuum state is kept, temperature rises to 1700-1800 DEG C, keeps the temperature 6-10 hours, this moment reaction process are as follows:
Al2O3(s)+3C (s)=2Al (g)+3CO (g)
Al2O3(s)+3C (s)=Al2(g)+3CO(g)
Al2O3(s)+C (s)=Al2O(g)+2CO(g)
Al2O3(s)+C (s)=2AlO (g)+CO (g)
S5, temperature are increased to 2000-2200 DEG C, are filled with high pure nitrogen, and pressure 110-120KPa keeps the temperature 7 hours, this moment
High pressure inhibits the decomposition of AlN, reduces powder loss, while metal Al forms Al steam and oxidation reactive aluminum under high temperature, this moment
Reaction process are as follows:
Al2O3(s)+4Al (g)=3Al2O(g)
S6, after the reaction was completed is down to 1000 DEG C with the cooling rate lower than 10 DEG C/min, then vacuumizes and be evacuated to 1 × 10- 4Pa is subsequently filled the high pure nitrogen of 1atm hereinafter, up to being cooled to room temperature, and crucible taking-up is put into inertia glove box and is carried out
Crushing grinding processing, is detected after the completion of processing.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.Those skilled in the art
Member is it should be appreciated that invention scope involved in the application, however it is not limited to technology made of the specific combination of above-mentioned technical characteristic
Scheme, while should also cover in the case where not departing from the inventive concept, it is carried out by above-mentioned technical characteristic or its equivalent feature
Any combination and the other technical solutions formed.Such as features described above has similar function with (but being not limited to) disclosed herein
Can technical characteristic replaced mutually and the technical solution that is formed.
Claims (10)
1. a kind of aluminium nitride powder method of purification, characterized in that the following steps are included:
The processing of high temperature air purge is carried out to the synthetic cavity where the mixed powder of Al powder and AlN powder using reducing gas, for going
Except the oxygen in the synthetic cavity；
Under vacuum state, aluminium nitride powder purification processes are carried out to the mixed powder, wherein
At a temperature of the first purification, the hydroxide in the mixed powder impurity is removed,
At a temperature of the second purification, the carbon in the mixed powder impurity is removed,
At a temperature of third purification, it is filled with high pure nitrogen, the Al powder in the mixed powder forms Al steam, steams using the Al
Vapour removes the aluminium oxide in the mixed powder impurity, then cools down, and handles under high purity inert gas protection through crushing grinding
Up to high-purity aluminium nitride powder.
2. aluminium nitride powder method of purification according to claim 1, characterized in that Al powder and the molar ratio of AlN powder are
0.1-0.5:1。
3. aluminium nitride powder method of purification according to claim 1, characterized in that the mixed powder is in high-purity indifferent gas
Body protection is lower to carry out cold moudling, is subsequently placed in synthetic cavity.
4. aluminium nitride powder method of purification according to claim 1, characterized in that the reducing gas is the synthesis chamber
Body is under vacuum state, the filling in the synthetic cavity.
5. aluminium nitride powder method of purification according to claim 1 to 4, characterized in that the vacuum degree < of vacuum state
1×10-4Pa。
6. aluminium nitride powder method of purification according to claim 1, characterized in that reducing gas is the mixed of hydrogen and nitrogen
Gas is closed, wherein hydrogen 0.5%-5% of the total volume.
7. aluminium nitride powder method of purification according to claim 1, characterized in that the temperature of high temperature air purge processing is 200-
400℃。
8. aluminium nitride powder method of purification according to claim 1, characterized in that the first purification temperature is 800-
1000 DEG C, the second purification temperature is 1700-1800 DEG C, and it is 1900-2200 DEG C that third, which purifies temperature,.
9. aluminium nitride powder method of purification according to claim 8, characterized in that in third purification phase, be filled with high-purity
After nitrogen, pressure 80-120KPa, to be down to 1000 DEG C lower than the cooling rate of 10 DEG C/min, then vacuumize and be evacuated to 1 ×
10-4Pa is hereinafter, until be cooled to room temperature.
10. a kind of high-purity aluminium nitride powder, characterized in that -9 any aluminium nitride powder purification according to claim 1
Method is made.
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| CN112062108A (en) * | 2020-08-07 | 2020-12-11 | 福建臻璟新材料科技有限公司 | Aluminum nitride powder purification method |
| CN115353082A (en) * | 2022-08-29 | 2022-11-18 | 山东大学 | Method for sintering high-quality aluminum nitride raw material in one step |
| CN115745623A (en) * | 2022-11-23 | 2023-03-07 | 郑州大学 | Aluminum nitride composite material, preparation method and application thereof |
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| CN115353082A (en) * | 2022-08-29 | 2022-11-18 | 山东大学 | Method for sintering high-quality aluminum nitride raw material in one step |
| CN115353082B (en) * | 2022-08-29 | 2023-10-24 | 山东大学 | Method for sintering high-quality aluminum nitride raw material in one step |
| CN115745623A (en) * | 2022-11-23 | 2023-03-07 | 郑州大学 | Aluminum nitride composite material, preparation method and application thereof |
| CN115745623B (en) * | 2022-11-23 | 2024-02-06 | 郑州大学 | Aluminum nitride composite material, preparation method and application thereof |
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