CN106082149B - The preparation method of aluminium nitride powder - Google Patents
The preparation method of aluminium nitride powder Download PDFInfo
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- CN106082149B CN106082149B CN201610421672.9A CN201610421672A CN106082149B CN 106082149 B CN106082149 B CN 106082149B CN 201610421672 A CN201610421672 A CN 201610421672A CN 106082149 B CN106082149 B CN 106082149B
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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
- C01B21/0726—Preparation by carboreductive nitridation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention relates to a kind of preparation methods of aluminium nitride powder.The preparation method of the aluminium nitride powder includes the following steps：Boehmite gel, inorganic carbon source, Water Soluble Organic Carbon source and sintering aid are mixed, mixture is obtained；Under the atmosphere of nitrogen, mixture is nitrogenized in 1250~1700 DEG C, obtains reduzate；Under aerobic conditions, reduzate is calcined 3~10 hours under conditions of 600~720 DEG C, obtains aluminium nitride powder.The purity of aluminium nitride powder prepared by this method is higher.
Description
Technical field
The present invention relates to ceramic material field more particularly to a kind of preparation methods of aluminium nitride powder.
Background technology
Aluminium nitride ceramics material have high heat conductance, excellent electric property, more excellent mechanical property and with silicon phase
Matched coefficient of thermal expansion, while there is excellent anti-oxidant, thermal shock resistance, it is high power density integrated circuit, Gao Gong
Rate LED and the ideal cooling encapsulation material of IGBT module.
The preparation method of current aluminum nitride powder includes mainly：Carbothermic method, aluminium powder nitriding, self-propagating high-temperature method,
Sol-gal process, vapor phase method etc., wherein carbothermic method and aluminium powder nitriding are two kinds of sides of suitable scale of mass production at present
Method.
Carbothermic method mainly uniformly mixes silicon source and carbon source, is nitrogenized in a nitrogen atmosphere, in reaction process
A small amount of reaction promoter, such as rare earth oxide, weak base oxide are usually added, reaction rate is improved and reduces nitriding temperature.
However usually carbothermic method is to use aluminium oxide as silicon source, due to the proportion and surface property differences of alumina powder and carbon source
It is too big, it is more difficult to be uniformly mixed so that reaction is incomplete, causes the purity of powder relatively low.Aluminium powder nitriding is that aluminium powder is passed through height
Temperature heats Direct-Nitridation in a nitrogen atmosphere, generates aluminum nitride powder, since aluminium powder easily lumps in nitridation process or formed melting
Aluminium, it is incomplete to also result in nitridation, influences powder purity.
Invention content
Based on this, it is necessary to provide a kind of preparation side for the aluminium nitride powder that can prepare the powder with higher degree
Method.
A kind of preparation method of aluminium nitride powder, includes the following steps：
Boehmite gel, inorganic carbon source, Water Soluble Organic Carbon and sintering aid are mixed, mixture is obtained；
Under the atmosphere of nitrogen, the mixture is nitrogenized at 1400~1700 DEG C, obtains reduzate；
Under aerobic conditions, the reduzate is calcined 3~10 hours under conditions of 600~720 DEG C, is nitrogenized
Aluminium powder body.
The one kind of the inorganic carbon source in carbon black, coke, graphite powder and charcoal etc. in one of the embodiments,.
The one kind of the Water Soluble Organic Carbon in sucrose, glucose and sugared chaff in one of the embodiments,.
In one of the embodiments, the sintering aid in calcium oxide, calcium oxide, barium monoxide and yttrium oxide at least
It is a kind of.The sum of mole of carbon in the inorganic carbon source and the Water Soluble Organic Carbon and institute in one of the embodiments,
The ratio for stating the mole of the aluminium in boehmite gel is 1.5~6:1.
The inorganic carbon source, the Water Soluble Organic Carbon and the boehmite gel in one of the embodiments,
The ratio of quality of quality sum and the sintering aid be 100:0.1~1.5.
Further include the preparation process of boehmite gel in one of the embodiments,：
Aluminium hydroxide and sodium hydroxide are reacted in water, obtain the aqueous solution of sodium metaaluminate；
Carbon dioxide reaction is passed through to the aqueous solution of the sodium metaaluminate, it is solidifying to obtain boehmite.
The step of in one of the embodiments, reacting the aluminium hydroxide and the sodium hydroxide in water be：It presses
It it is 10 milliliters according to volume mass ratio:2 grams~6 grams, the hydrogen-oxygen that mass percentage concentration is 10~40% is added in the aluminium hydroxide
In the aqueous solution for changing sodium, it is stirred to react at 90~110 DEG C, obtains the aqueous solution of sodium metaaluminate.
In one of the embodiments, in the step of nitrogenizing the mixture, the flow of the nitrogen is 20 liters/min
Clock~50 liter/min.
The mass percentage of boehmite described in the boehmite gel is in one of the embodiments,
5~30%.
The preparation method of above-mentioned aluminium nitride powder is by using boehmite gel, inorganic carbon source and Water Soluble Organic Carbon
As raw material, and boehmite gel itself has preferable dispersibility in water, and water-soluble carbon source, which is added, uniformly to mix
It closes, can realize the uniform mixing of raw material, be conducive to the complete of subsequent nitridation reaction, improve the purity of aluminium nitride powder；Pass through
Addition sintering aid promotes the progress of nitridation reaction, improves reaction rate, reduces nitriding temperature, shortens the reaction time, by that will go back
It originates in object and calcines 3~10 hours under conditions of 600~720 DEG C to remove the carbon in reduzate, improve the purity of aluminium nitride,
To obtain the higher aluminium nitride powder of purity.
Description of the drawings
Fig. 1 is the flow chart of the preparation method of the aluminium nitride powder of an embodiment；
Fig. 2 is the flow chart of the preparation method of the boehmite gel of an embodiment.
Specific implementation mode
To facilitate the understanding of the present invention, below with reference to relevant drawings to invention is more fully described.In attached drawing
Give the preferred embodiment of the present invention.But the present invention can realize in many different forms, however it is not limited to herein
Described embodiment.Keep the understanding to the disclosure more saturating on the contrary, purpose of providing these embodiments is
It is thorough comprehensive.
Unless otherwise defined, all of technologies and scientific terms used here by the article and belong to the technical field of the present invention
The normally understood meaning of technical staff is identical.Used term is intended merely to description tool in the description of the invention herein
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term " and or " used herein includes one or more phases
Any and all combinations of the Listed Items of pass.
As shown in Figure 1, the preparation method of the aluminium nitride powder of an embodiment, includes the following steps：
Step S110：Boehmite gel, inorganic carbon source, Water Soluble Organic Carbon source and sintering aid are mixed, mixed
Close object.
Wherein, the mass percentage of boehmite gel is 5~30%.Boehmite gel can be purchased by market
It can buy, it can also be by being prepared.As shown in Fig. 2, the preparation method of boehmite gel is as follows：
Step S210：Aluminium hydroxide and sodium hydroxide are reacted in water, obtain the aqueous solution of sodium metaaluminate.
The step of aluminium hydroxide and sodium hydroxide are reacted in water be：It it is 10 milliliters according to volume mass ratio:2 grams~6
Gram, aluminium hydroxide is added in the aqueous solution for the sodium hydroxide that mass percentage concentration is 10~40%, is stirred at 90~110 DEG C
Reaction, obtains the aqueous solution of sodium metaaluminate.I.e. mass percentage concentration be 10~40% sodium hydroxide aqueous solution volume with
The ratio of the quality of aluminium hydroxide is 10 milliliters:2 grams~6 grams.
Step S220：Carbon dioxide is passed through to the aqueous solution of sodium metaaluminate, obtains boehmite gel.
Specifically, the aqueous solution to sodium metaaluminate is specially the step of being passed through carbon dioxide：In 25 DEG C~60 DEG C of condition
Under, it is passed through carbon dioxide 50~120 minutes to the aqueous solution of sodium metaaluminate, is subsequently added into ammonium hydroxide, until pH value is 10~12, after
It is continuous to be passed through carbon dioxide until pH value is 8.5~9.5, obtain boehmite gel.Wherein, the flow of carbon dioxide be 2~
12Nm3/h。
Wherein, the mass percentage concentration of ammonium hydroxide is 5~15%.And ammonium hydroxide is added by the way of being added dropwise；Drop rate is 3
It drips within~5 minutes 1.
Wherein, the one kind of inorganic carbon source in carbon black, coke, charcoal and graphite powder.
Wherein, the one kind of Water Soluble Organic Carbon source in sucrose, glucose and sugared chaff.
Wherein, the sum of mole of carbon in inorganic carbon source and Water Soluble Organic Carbon source and the aluminium in boehmite gel
Mole ratio be 1.5~6:1.
Wherein, the molar ratio of carbon is 1~3 in inorganic carbon source and Water Soluble Organic Carbon source:1.
Wherein, sintering aid is selected from least one of calcium oxide, barium monoxide and yttrium oxide.It is appreciated that sintering aid may be used also
Think other rare earth oxides other than yttrium oxide.
Wherein, inorganic carbon source, the quality of the quality sum in Water Soluble Organic Carbon source and boehmite gel and sintering aid
Than being 100:0.1~1.5.
Step S120：Under the atmosphere of nitrogen, mixture is nitrogenized in 1400~1700 DEG C, obtains reduzate.
Wherein, in step S120, the flow of nitrogen is 20 liters/min~50 liters/min.
Wherein, time mixture nitrogenized in 1400~1700 DEG C is 5~10 hours.I.e. nitridation time is shorter, drop
Low energy consumption, advantageously reduces the manufacturing cost of aluminium nitride powder.
Step S130：Under conditions of aerobic, reduzate is calcined 3~10 hours under conditions of 600~720 DEG C,
Obtain aluminium nitride powder.
Wherein, reduzate is calcined to 3~10 hours under conditions of 600~720 DEG C to remove the carbon in reduzate,
Improve the purity of powder.
Wherein, the device that the step of reduzate being calcined 3~10 hours under conditions of 600~720 DEG C uses is back
Converter, batch-type furnace or steel belt furnace.
The preparation method of above-mentioned aluminium nitride powder is by using boehmite gel, inorganic carbon source and Water Soluble Organic Carbon
As raw material, and boehmite gel itself has preferable dispersibility in water, and water-soluble carbon source, which is added, uniformly to mix
It closes, can realize the uniform mixing of raw material, be conducive to the complete of subsequent nitridation reaction, improve the purity of aluminium nitride powder；Pass through
Addition sintering aid promotes the progress of nitridation reaction, improves reaction rate, reduces nitriding temperature, shortens the reaction time, by that will go back
It originates in object and calcines 3~10 hours under conditions of 600~720 DEG C to remove the carbon in reduzate, improve the purity of aluminium nitride,
To obtain the higher aluminium nitride powder of purity.
And simultaneously because the raw material that above-mentioned preparation method uses can be mixed uniformly, while nitrogen can fully connect with raw material
It touches, advantageously reduces the oxygen content of aluminium nitride powder.
It is specific embodiment part below：
Embodiment 1
The preparation process of the aluminium nitride powder of the present embodiment is as follows：
(1) preparation of boehmite gel：It it is 10 milliliters according to volume mass ratio:4 grams, aluminium hydroxide is added to matter
It in the aqueous solution for measuring the sodium hydroxide that percentage concentration is 25%, and is stirred to react at 100 DEG C, obtains the aqueous solution of sodium metaaluminate；
Under conditions of 40 DEG C, carbon dioxide is passed through into the aqueous solution of sodium metaaluminate 50 minutes, it is 11 to be neutralized to pH value, according still further to 3
The ammonium hydroxide that mass percentage concentration is 5% is added dropwise in the rate of minute 1 drop, continues to be passed through carbon dioxide until pH value is 9, obtain quasi- thin
The boehmite gel that the mass percentage of diaspore is 25%, wherein the flow that is passed through of carbon dioxide is 8Nm3/h。
(2) by boehmite gel, inorganic carbon source, Water Soluble Organic Carbon source and sintering aid ball milling mixing, so that quasi- thin
Diaspore gel, inorganic carbon source, Water Soluble Organic Carbon source and sintering aid are uniformly mixed, and obtain mixture.Wherein, inorganic carbon source is
Carbon black；Water Soluble Organic Carbon source is the mixture of sucrose and glucose；Inorganic carbon source and the carbon in Water Soluble Organic Carbon source rub
The ratio of the sum of your amount and the mole of the aluminium in boehmite gel is 1.5:1；Inorganic carbon source and Water Soluble Organic Carbon source carbon
Molar ratio be 1:1, sintering aid is calcium oxide；The quality of inorganic carbon source, Water Soluble Organic Carbon source and boehmite gel it
With with the mass ratio of sintering aid be 100:0.8.
(3) under the atmosphere of nitrogen, mixture is nitrogenized 10 hours in nitriding furnace in 1600 DEG C, wherein the stream of nitrogen
Amount is 25 liters/min.
(4) under the atmosphere of air, reduzate is calcined 3 hours with removal under conditions of 660 DEG C in rotary furnace
Carbon in reduzate, obtains aluminium nitride powder, and aluminium nitride powder is vacuum-packed.
The aluminium nitride powder of the present embodiment is dry-pressing formed, then obtain substrate through 1600 DEG C of sintering.
The particle diameter distribution of the aluminium nitride powder of the present embodiment is tested using Malvern laser particle analyzer；Using LECO companies nitrogen
Oxygen tester tests the nitrogen content and oxygen content of the aluminium nitride powder of the present embodiment；Originally using the carbon sulphur tester test of LECO companies
The phosphorus content of the aluminium nitride powder of embodiment；The aluminium nitride powder for testing the present embodiment using resistance to laser heat conducting instrument of speeding prepares substrate
Thermal conductivity；Tested using the Material Testing Machine of Instro the present embodiment aluminium nitride powder prepare substrate three-point bending resistance it is strong
Degree.Wherein, the grain diameter of the aluminium nitride powder of the present embodiment, nitrogen content, oxygen content, phosphorus content, the thermal conductivity for preparing substrate
And intensity is shown in Table 1.
Embodiment 2
The preparation process of the aluminium nitride powder of the present embodiment is as follows：
(1) preparation of boehmite gel：It it is 10 milliliters according to volume mass ratio:2 grams, aluminium hydroxide is added to matter
It measures in the sodium hydrate aqueous solution that percentage concentration is 10%, is stirred to react at 90 DEG C, obtains the aqueous solution of sodium metaaluminate；At 25 DEG C
Under conditions of, carbon dioxide is passed through into the aqueous solution of sodium metaaluminate 120 minutes, it was 10 to be neutralized to pH value, according still further to 5 minutes 1
The ammonium hydroxide that mass percentage concentration is 5% is added dropwise in the rate of drop, continues to be passed through carbon dioxide until pH value is 8.5, obtains intending thin water
The boehmite gel that the mass percentage of aluminium stone is 5%, wherein the flow that is passed through of carbon dioxide is 2Nm3/h。
(2) it by boehmite gel, inorganic carbon source, Water Soluble Organic Carbon source and sintering aid ball milling mixing, is mixed
Object.Wherein, inorganic carbon source is coke；Water Soluble Organic Carbon source is glucose；Carbon in inorganic carbon source and Water Soluble Organic Carbon source
The sum of mole and the ratio of the mole of the aluminium in boehmite gel be 2:1；Inorganic carbon source and Water Soluble Organic Carbon source
Molar ratio be 1.5:1；Sintering aid is the mixture of calcium oxide and barium monoxide；Inorganic carbon source, Water Soluble Organic Carbon source and quasi- thin
The quality sum of diaspore gel and the mass ratio of sintering aid are 100:0.1.
(3) under the atmosphere of nitrogen, the time that mixture is nitrogenized in nitriding furnace in 1650 DEG C is 8 hours, wherein nitrogen
The flow of gas is 30 liters/min.
(4) under the atmosphere of air, reduzate is calcined 5 hours with removal under conditions of 620 DEG C in batch-type furnace
Carbon in reduzate, obtains aluminium nitride powder, and aluminium nitride powder is vacuum-packed.
The aluminium nitride powder of the present embodiment is dry-pressing formed, then obtain substrate through 1600 DEG C of sintering.
Using 1 identical test method of embodiment, obtain the grain diameter of the aluminium nitride powder of the present embodiment, nitrogen content and
Oxygen content, phosphorus content and prepare the thermal conductivity of substrate and intensity is shown in Table 1.
Embodiment 3
The preparation process of the aluminium nitride powder of the present embodiment is as follows：
(1) preparation of boehmite gel：It it is 10 milliliters according to volume mass ratio:6 grams, aluminium hydroxide is added to matter
It measures in the sodium hydrate aqueous solution that percentage concentration is 40%, is stirred to react at 110 DEG C, obtains the aqueous solution of sodium metaaluminate；60
Under conditions of DEG C, carbon dioxide is passed through into the aqueous solution of sodium metaaluminate 80 minutes, it was 12 to be neutralized to pH value, according still further to 3 minutes 1
The ammonium hydroxide that mass percentage concentration is 10% is added dropwise in the rate of drop, continues to be passed through carbon dioxide until pH value is 9.5, obtains intending thin water
The boehmite gel that the mass percentage of aluminium stone is 30%, wherein the flow that is passed through of carbon dioxide is 12Nm3/h。
(2) it by boehmite gel, inorganic carbon source, Water Soluble Organic Carbon source and sintering aid ball milling mixing, is mixed
Object.Wherein, inorganic carbon source is the mixture of charcoal and graphite powder；Water Soluble Organic Carbon source is the mixture of sucrose and sugared chaff；Nothing
The sum of mole of carbon in machine carbon source and Water Soluble Organic Carbon source and the ratio of the mole of the aluminium in boehmite gel are
3:1, the molar ratio in organic carbon source and Water Soluble Organic Carbon source is 6:1；Sintering aid is yttrium oxide；Inorganic carbon source, water solubility are organic
The mass ratio of the quality sum and sintering aid of carbon source and boehmite gel is 100:0.5.
(3) under the atmosphere of nitrogen, the time that mixture is nitrogenized in nitriding furnace in 1550 DEG C is 10 hours, wherein
The flow of nitrogen is 5 liters/min.
(4) reduzate in rotary furnace is calcined 3 hours 650 DEG C under conditions of under the atmosphere of air with removal also
The carbon in object is originated in, aluminium nitride powder is obtained, aluminium nitride powder is vacuum-packed.
The aluminium nitride powder of the present embodiment is dry-pressing formed, then obtain substrate through 1600 DEG C of sintering.
Using 1 identical test method of embodiment, obtain the grain diameter of the aluminium nitride powder of the present embodiment, nitrogen content and
Oxygen content, phosphorus content and prepare the thermal conductivity of substrate and intensity is shown in Table 1.
Embodiment 4
The preparation process of the aluminium nitride powder of the present embodiment is as follows：
(1) preparation of boehmite gel：It it is 10 milliliters according to volume mass ratio:3 grams, aluminium hydroxide is added to matter
It measures in the sodium hydrate aqueous solution that percentage concentration is 20%, is stirred to react at 95 DEG C, obtains the aqueous solution of sodium metaaluminate；At 50 DEG C
Under conditions of, carbon dioxide is passed through into the aqueous solution of sodium metaaluminate 100 minutes, it is 11 to be neutralized to pH value, then is instilled thereto
The ammonium hydroxide that mass percentage concentration is 15% continues to be passed through carbon dioxide until pH value is 9, obtains the quality percentage of boehmite
The boehmite gel that content is 20%, wherein the flow that is passed through of carbon dioxide is 10Nm3/h。
(2) it by boehmite gel, inorganic carbon source, Water Soluble Organic Carbon source and sintering aid ball milling mixing, is mixed
Object.Wherein, inorganic carbon source is the mixture of carbon black, coke, charcoal and graphite powder；Water Soluble Organic Carbon source is glucose, sucrose
With the mixture of sugared chaff；The sum of mole of carbon in inorganic carbon source and Water Soluble Organic Carbon source in boehmite gel
The ratio of the mole of aluminium is 6:1；Inorganic carbon source and the molar ratio in Water Soluble Organic Carbon source are 3:1；Sintering aid is calcium oxide, oxidation
Yttrium and barium monoxide, mass ratio 1:1；The quality sum of inorganic carbon source, Water Soluble Organic Carbon source and boehmite gel and help burning
The mass ratio of agent is 100:1.5.
(3) under the atmosphere of nitrogen, the time that mixture is nitrogenized in nitriding furnace in 1500 DEG C is 12 hours, wherein
The flow of nitrogen is 50 liters/min.
(4) reduzate in rotary furnace is calcined 3 hours under conditions of 680 DEG C to remove the carbon in reduzate,
Aluminium nitride powder is obtained, aluminium nitride powder is vacuum-packed.
The aluminium nitride powder of the present embodiment is dry-pressing formed, then obtain substrate through 1600 DEG C of sintering.
Using 1 identical test method of embodiment, obtain the grain diameter of the aluminium nitride powder of the present embodiment, nitrogen content and
Oxygen content, phosphorus content and prepare the thermal conductivity of substrate and intensity is shown in Table 1.
Comparative example 1
The preparation process of the aluminium nitride powder of comparative example 1 is：
Under the atmosphere of nitrogen, metallic aluminium is calcined at 2000 DEG C, obtains the aluminium nitride powder that grain size is 2.4 microns.
The aluminium nitride powder of comparative example 1 is dry-pressing formed, then obtain substrate through 1600 DEG C of sintering.
Using 1 identical test method of embodiment, obtain the grain diameter of the aluminium nitride powder of comparative example 1, nitrogen content and
Oxygen content, phosphorus content and prepare the thermal conductivity of substrate and intensity is shown in Table 1.
Comparative example 2
The preparation process of the aluminium nitride powder of comparative example 2 is：
Aluminium hydroxide is mixed with fluoride, is calcined 3 hours at 900 DEG C, obtains porous activated alumina, it will be active
Aluminium oxide crushes, then the activated alumina after crushing is added to the water preparation as suspension, is then added in suspension
Aluminium chloride, carbon dust carry out gelation, and nitrogen is passed through after drying, crushing and restores to obtain the aluminium nitride powder that grain size is 2.2 microns.
The aluminium nitride powder of comparative example 2 is dry-pressing formed, then obtain substrate through 1600 DEG C of sintering.
Using 1 identical test method of embodiment, the particle of the aluminium nitride powder of the present embodiment of comparative example 2 is obtained
Diameter, nitrogen content, oxygen content, phosphorus content and prepare the thermal conductivity of substrate and intensity is shown in Table 1.
Be respectively in table 1 Examples 1 to 6, the grain diameter of aluminium nitride powder of comparative example 1 and comparative example 2, nitrogen content,
Oxygen content, phosphorus content and the thermal conductivity and intensity that prepare substrate.
Table 1
From table 1 it follows that the D of the grain size of the aluminium nitride powder of Examples 1 to 450Maximum is only 2 microns, nitrogen content
At least 32%, oxygen content is only at most 1.1%, and thermal conductivity is at least 155w/mk, and three-point bending resistance intensity is at least
400Mpa, and the nitrogen content of the aluminium nitride powder of comparative example 1 and comparative example 2 is only 28%, and grain diameter is larger, thermal conductivity and
Three-point bending resistance intensity also be far below Examples 1 to 4, it is clear that the aluminum nitride powder of Examples 1 to 4 have smaller grain diameter, compared with
High nitrogen content, lower oxygen content, higher thermal conductivity and preferable intensity.
And it can also be seen that the phosphorus content of the aluminium nitride powder of comparative example 1 and 2 is 700ppm from table 1, and oxygen content
Respectively 1.5% and 1.4%, and the phosphorus content of the aluminium nitride powder of Examples 1 to 4 at most only 300ppm, and oxygen content
Up to 1.1%, well below comparative example 1 and comparative example 2 aluminium nitride powder phosphorus content and oxygen content, and phosphorus content and
Oxygen content is lower to illustrate that the purity of aluminium nitride powder is higher, it is clear that the aluminium nitride powder of Examples 1 to 4 has higher purity.
Each technical characteristic of embodiment described above can be combined arbitrarily, to keep description succinct, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, it is all considered to be the range of this specification record.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (1)
1. a kind of preparation method of aluminium nitride powder, which is characterized in that include the following steps：
It it is 10 milliliters according to volume mass ratio:4 grams, aluminium hydroxide is added to the sodium hydroxide that mass percentage concentration is 25%
It in aqueous solution, and is stirred to react at 100 DEG C, obtains the aqueous solution of sodium metaaluminate, under conditions of 40 DEG C, to the sodium metaaluminate
Aqueous solution in be passed through carbon dioxide 50 minutes, be neutralized to pH value be 11, according still further to 3 minutes 1 drop rate be added dropwise quality percentage
A concentration of 5% ammonium hydroxide continues to be passed through the carbon dioxide until pH value is 9, obtains the mass percentage of boehmite
For 25% boehmite gel, wherein the flow that is passed through of the carbon dioxide is 8Nm3/h；
By the boehmite gel, inorganic carbon source, Water Soluble Organic Carbon source and sintering aid ball milling mixing, so that described quasi- thin
Diaspore gel, inorganic carbon source, Water Soluble Organic Carbon source and sintering aid are uniformly mixed, and obtain mixture, wherein the inorganic carbon
Source is carbon black, and the Water Soluble Organic Carbon source is the mixture of sucrose and glucose, and the inorganic carbon source and the water solubility have
The ratio of the sum of mole of carbon in machine carbon source and the mole of the aluminium in the boehmite gel is 1.5:1, the nothing
Machine carbon source and the molar ratio of Water Soluble Organic Carbon source carbon are 1:1, the sintering aid is calcium oxide, the inorganic carbon source, institute
It is 100 to state Water Soluble Organic Carbon source and the quality sum of the boehmite gel and the mass ratio of the sintering aid:0.8；
Under the atmosphere of nitrogen, the mixture is nitrogenized 10 hours in nitriding furnace in 1600 DEG C, reduzate is obtained,
In, the flow of the nitrogen is 25 liters/min；
Under the atmosphere of air, the reduzate is calcined 3 hours to remove reduction under conditions of 660 DEG C in rotary furnace
Carbon in product, obtains aluminium nitride powder.
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| CN112897482A (en) * | 2021-01-14 | 2021-06-04 | 中氢能源科技发展(内蒙古)有限公司 | Method for preparing aluminum nitride by using aluminum alloy as raw material |
| CN113753867B (en) * | 2021-08-31 | 2023-09-12 | 湖南邦普循环科技有限公司 | Preparation method of aluminum nitride |
| CN115724450B (en) * | 2022-10-21 | 2024-01-19 | 黄山天之都环境科技发展有限公司 | Preparation method of alumina solid catalyst carrier |
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