CN105836717B - The preparation method of aluminium nitride electronic ceramic powder - Google Patents
The preparation method of aluminium nitride electronic ceramic powder Download PDFInfo
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- CN105836717B CN105836717B CN201610156386.4A CN201610156386A CN105836717B CN 105836717 B CN105836717 B CN 105836717B CN 201610156386 A CN201610156386 A CN 201610156386A CN 105836717 B CN105836717 B CN 105836717B
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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
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
Abstract
A kind of preparation method of aluminium nitride electronic ceramic powder, the method comprising the steps of：S1, raw material mixing, alumina powder and metallic aluminium powder are mutually mixed；S2, inert environments sintering, mixed-powder is sintered；S3, the multiple oxide powder of aluminum oxide mixed with carbon dust, is sintered；S4, except carbon operate, by primary aluminium nitride powder carry out except carbon operation aluminium nitride electronic ceramic powder is made.Multiple oxide in alumina powder to be present in the present invention, reaction activity can be reduced in carbothermic reduction reaction, by changing aluminum ions chemical valence, the aluminium ion of high price is changed into the aluminium ion of low price, reach and improved the activity of aluminum oxide, reduce carbon thermal reduction temperature and the purpose of recovery time, because reduction temperature declines, the recovery time reduces, solve the problems, such as that aluminium nitride is existing into production high energy consumption in the prior art.
Description
Technical field
The present invention relates to technical field of integrated circuits, more specifically, more particularly to a kind of aluminium nitride electronic ceramic powder
Preparation method.
Background technology
Aluminium nitride electronic ceramics is a kind of new function ceramic material, has good heat-conductive characteristic, reliable electricity absolutely
Edge, low dielectric loss and dielectric constant, adaptable is to be processed as large-scale integrated circuit substrate by the tape casting,
Can also be as high grade refractory and optics, wear resistant appliance.
The substrate of integrated circuit mainly has aluminium oxide ceramics (Al in the market2O3), cubic boron nitride (BN), beryllium oxide
(BeO).The advantages of aluminium oxide ceramics, is the features such as low dielectric loss, high mechanical strength, chemical stability are good.But aoxidize
The lower thermal conductivity of aluminium ceramics limits semiconductor element to high density, the development in high-performance direction.Cubic boron nitride (BN) conduct
Highly thermally conductive material is better than aluminium oxide ceramics as semiconductor-based piece performance, at present preliminary market, but BN preparation technologies
Complexity is expensive to be unfavorable for promoting.Beryllium oxide (BeO) ceramic heat-dissipating function admirable, but because beryllium oxide powder has severe toxicity, make
Its preparation technology is complicated, cost increase, limits its popularization and use.
The aluminium nitride ceramics (AIN) that developed recently gets up have thermal conductivity is high, thermal coefficient of expansion is low, electrical insulating property is stable,
The advantages that dielectric properties are excellent, good mechanical performance, it is considered to be the rationality material of ceramic substrate of new generation.Carbothermic method
It is very high at 1600~1700 DEG C to prepare temperature needed for aluminium nitride powder, soaking time needs 10~12h, so that aluminium nitride
The problem of energy consumption is higher be present in preparation.
The content of the invention
(1) technical problem
How to solve the problems, such as that energy consumption existing for aluminium carbide preparation is higher in conventional art.
(2) technical scheme
The invention provides a kind of preparation method of aluminium nitride electronic ceramic powder, the method comprising the steps of：
S1, raw material mixing, by alumina powder of the purity not less than 99.99% and metallic aluminium of the purity not less than 99.99%
Powder, which is mutually mixed, is uniformly made mixed-powder, wherein, alumina powder content is 90~100wt%, metallic aluminium powder content is 0~
10wt%；
S2, inert environments sintering, the mixed-powder are carried out in an inert atmosphere normal pressure-sintered, its sintering temperature is
900 DEG C~1100 DEG C, 4h~5h insulation is then carried out, the multiple oxide powder of aluminum oxide is made after cooling with stove；
S3, nitrogen environment sintering, the multiple oxide powder of the aluminum oxide and carbon dust of the purity not less than 99.99% are pressed
Mixed according to mass ratio for 1.5~2.5: 1, be blended with the multiple oxide powder of the aluminum oxide of carbon dust in nitrogen environment
It is lower carry out it is normal pressure-sintered primary aluminium nitride powder is made, its sintering temperature is 1400 DEG C~1500 DEG C, sintering time be 5h~6h,
Nitrogen flow is 0.4m3/h~1.0m3/h；
S4, except carbon operate, by the primary aluminium nitride powder carry out except carbon operation aluminium nitride electronic ceramic powder is made, its
Except carbon temperature is 600 DEG C~700 DEG C, except the carbon time is 4h~6h.
Preferably, in the step S2, mixed-powder is carried out using graphite crucible in an inert atmosphere normal pressure-sintered；
In the step S4, the primary aluminium nitride powder is carried out except carbon is grasped using alumina crucible for container in except carbon stove
Make.
Preferably, in the step S2, described inert environments are helium environment or ar gas environment.
Preferably, the average grain diameter of the alumina powder is not more than 1 micron；The average grain diameter of the metallic aluminium powder is not more than
1 micron.
(3) beneficial effect
In the preparation method of aluminium nitride electronic ceramic powder provided by the invention, aluminium nitride electronic ceramic powder is to utilize
Alumina powder and metallic aluminium powder are mutually mixed uniformly in proportion, are sintered what is be prepared at a certain temperature, by processing
Multiple oxide in the alumina powder obtained afterwards be present, reaction activity can be reduced in carbothermic reduction reaction, the technique phase
1400 DEG C applied of the invention are reduced to than being 1600 DEG C~1700 DEG C in untreated alumina powder nitriding temperature
~1500 DEG C, soaking time drops to 5h~6h by original 10h~12h, by changing aluminum ions chemical valence, by the aluminium of high price
Ion transit is the aluminium ion of low price, has reached and has improved the activity of aluminum oxide, reduces carbon thermal reduction temperature and the mesh of recovery time
, because reduction temperature declines, the recovery time reduces, solve existing the asking into production high energy consumption of aluminium nitride in the prior art
Topic.
Brief description of the drawings
Fig. 1 is the flow chart of the preparation method of aluminium nitride electronic ceramic powder in the embodiment of the present invention；
Fig. 2 is that the experiment of the embodiment of the present invention 1, embodiment 2 and comparative example detects chart.
Embodiment
Embodiments of the present invention are described in further detail with reference to the accompanying drawings and examples.Following examples are used for
Illustrate the present invention, but can not be used for limiting the scope of the present invention.
In the description of the invention, unless otherwise indicated, " multiple " are meant that two or more；Term " on ",
" under ", "left", "right", " interior ", " outer ", " front end ", " rear end ", " head ", the orientation of the instruction such as " afterbody " or position relationship be
Based on orientation shown in the drawings or position relationship, it is for only for ease of the description present invention and simplifies description, rather than instruction or dark
Show that the device of meaning or element there must be specific orientation, with specific azimuth configuration and operation, thus it is it is not intended that right
The limitation of the present invention.In addition, term " first ", " second ", " the 3rd " etc. be only used for describe purpose, and it is not intended that instruction or
Imply relative importance.
In the description of the invention, it is necessary to which explanation, unless otherwise clearly defined and limited, term " connected ", " connects
Connect " it should be interpreted broadly, for example, it may be being fixedly connected or being detachably connected, or it is integrally connected；It can be machine
Tool connects or electrical connection；Can be joined directly together, can also be indirectly connected by intermediary.For this area
For those of ordinary skill, the concrete meaning of above-mentioned term in the present invention can be understood with concrete condition.
Fig. 1 is refer to, Fig. 1 is the flow chart of the preparation method of aluminium nitride electronic ceramic powder in the embodiment of the present invention.
The invention provides a kind of preparation method of aluminium nitride electronic ceramic powder, this method includes：
Step S1, it is alumina powder of the purity not less than 99.99% and purity is mutual not less than 99.99% metallic aluminium powder
It is well mixed that mixed-powder is made, wherein, alumina powder content is 90~100wt%, and metallic aluminium powder content is 0~10wt%；
Step S2, mixed-powder is carried out in an inert atmosphere it is normal pressure-sintered, its sintering temperature be 900 DEG C~1100 DEG C,
Then 4h~5h insulation is carried out, the multiple oxide powder of aluminum oxide is made after cooling with stove；
Step S3, it is 1.5 according to mass ratio by the carbon dust of the multiple oxide powder of aluminum oxide and purity not less than 99.99%
Mixed at~2.5: 1, and the multiple oxide powder of aluminum oxide for being blended with carbon dust carries out normal pressure-sintered system in a nitrogen environment
Into primary aluminium nitride powder, its sintering temperature is 1400 DEG C~1500 DEG C, sintering time is 5h~6h, nitrogen flow 0.4m3/
H~1.0m3/h；
Step S4, primary aluminium nitride powder is carried out except aluminium nitride electronic ceramic powder is made in carbon operation, it removes carbon temperature
For 600 DEG C~700 DEG C, except the carbon time is 4h~6h.
Specifically, in step s 2, mixed-powder is carried out using graphite crucible in an inert atmosphere normal pressure-sintered；In step
In rapid S4, primary aluminium nitride powder is carried out except carbon operates using alumina crucible for container in except carbon stove；In step s 2,
Inert environments be helium environment or ar gas environment.
Limit herein：The average grain diameter of alumina powder is not more than 1 micron；The average grain diameter of metallic aluminium powder is not more than 1 micron.
The present invention prepares aluminium nitride electronic ceramic powder, nitrogen prepared by the present invention using alumina powder using carbothermic method
It is hexagonal crystal shape to change aluminium electronic ceramic powder (AlN) crystal structure, and the oxygen content of aluminium nitride powder is below 0.9%, nitrogen content
More than 33%, particle is uniform, and primary particle size is 0.8~1.5um, and integrated circuit base can be done by flow casting molding
Plate.
AIN is aluminium nitride, and AlN is atomic crystal, belongs to DLC nitride, and highest can be stabilized to 2200 DEG C.Room temperature is strong
Degree is high, and intensity is slower with the rise decline of temperature.Thermal conductivity is good, and thermal coefficient of expansion is small, is good heat shock resistance material.It is anti-
The ability of molten metal attack is strong, is founding pure iron, the preferable crucible material of aluminum or aluminum alloy.Aluminium nitride or electrical insulator,
Dielectric properties are good, also get a good chance of as electric elements.
In specific implementation process, its preparation method is as follows：
(1) material mixes
Alumina powder of the purity not less than 99.99% is weighed to be mutually mixed with metallic aluminium powder of the purity not less than 99.99%
Uniformly, wherein：Alumina powder content is 90~100wt%, and metallic aluminium powder content is 0~10wt%.
(2) sinter
Gained mixture in above-mentioned steps is loaded into crucible, is put into sintering furnace, nothing is carried out under inertia or vacuum environment
Pressure sintering, wherein sintering temperature are 900~1100 DEG C；Soaking time is 4~5h.
(3) nitrogenize
Gained alumina powder in previous step step and carbon dust of the purity not less than 99.99% are mutually mixed uniformly, wherein：
The ratio of alumina powder and carbon dust is 2: 1.Well mixed material is loaded in crucible, carries out normal pressure burning in a nitrogen environment
Knot, wherein：Sintering temperature is 1400~1500 DEG C；Soaking time is 5~6h；Nitrogen flow is 0.4m3/h~1.0m3/h.
In the preparation method of aluminium nitride electronic ceramic powder provided by the invention, aluminium nitride electronic ceramic powder is to utilize
Alumina powder and metallic aluminium powder are mutually mixed uniformly in proportion, are sintered what is be prepared at a certain temperature, by processing
Multiple oxide in the alumina powder obtained afterwards be present, reaction activity can be reduced in carbothermic reduction reaction, the technique phase
1400 DEG C applied of the invention are reduced to than being 1600 DEG C~1700 DEG C in untreated alumina powder nitriding temperature
~1500 DEG C, soaking time drops to 5h~6h by original 10h~12h, by changing aluminum ions chemical valence, by the aluminium of high price
Ion transit is the aluminium ion of low price, has reached and has improved the activity of aluminum oxide, reduces carbon thermal reduction temperature and the mesh of recovery time
, because reduction temperature declines, the recovery time reduces, solve existing the asking into production high energy consumption of aluminium nitride in the prior art
Topic.
Fig. 2 is refer to, Fig. 2 is that the experiment of the embodiment of the present invention 1, embodiment 2 and comparative example detects chart.
The present invention is described further with reference to embodiments.
Embodiment 1
It is 99.99% to select purity, and average grain diameter is 1 micron of alumina powder, purity 99.99%, average grain diameter 1
The metallic aluminium powder of micron is aluminum oxide as raw material, percentage by weight: metallic aluminium 95: 5, is put into V-type batch mixer and mixes together
Material 15 minutes.
Mixed powder material is put into high purity graphite crucible；Graphite crucible is put into graphite sintering stove, in nitrogen gas
Under atmosphere, it is that in-furnace temperature is risen to 1000 DEG C by 10 DEG C/h according to heating rate, is incubated 4h.
By the mixed-powder after processing and purity it is 99.99% after cooling, the carbon dust that average grain diameter is 1 micron mixes, oxygen
The ratio for changing aluminium powder and carbon dust is 2: 1.
The raw material for mixing carbon dust is put into high purity graphite crucible；Graphite crucible is put into graphite sintering stove, in nitrogen gas
Under atmosphere, it is that in-furnace temperature is risen to 1450 DEG C by 10 DEG C/h according to heating rate, is incubated 6h.
Powder after nitridation is put into high purity aluminium oxide crucible, alumina crucible is put into except in carbon stove, according to heating speed
Rate is that in-furnace temperature is risen to 650 DEG C by 2 DEG C/h, is incubated 4h.
After furnace temperature cooling, aluminium nitride powder is taken out.
Embodiment 2
It is 99.99% to select purity, and average grain diameter is 1 micron of alumina powder, purity 99.99%, average grain diameter 1
The metallic aluminium powder of micron is aluminum oxide as raw material, percentage by weight: metallic aluminium=90: 10, it is put into V-type batch mixer and mixes together
Material 15 minutes.
Mixed powder material is put into high purity graphite crucible；Graphite crucible is put into graphite sintering stove, in nitrogen gas
Under atmosphere, it is that in-furnace temperature is risen to 1000 DEG C by 10 DEG C/h according to heating rate, is incubated 4h.
By the mixed-powder after processing and purity it is 99.99% after cooling, the carbon dust that average grain diameter is 1 micron mixes, oxygen
The ratio for changing aluminium powder and carbon dust is 2: 1.
The raw material for mixing carbon dust is put into high purity graphite crucible；Graphite crucible is put into graphite sintering stove, in nitrogen gas
Under atmosphere, it is that in-furnace temperature is risen to 1450 DEG C by 10 DEG C/h according to heating rate, is incubated 6h.
Powder after nitridation is put into high purity aluminium oxide crucible, alumina crucible is put into except in carbon stove, according to heating speed
Rate is that in-furnace temperature is risen to 650 DEG C by 2 DEG C/h, is incubated 4h.
After furnace temperature cooling, aluminium nitride powder is taken out.
Comparative example
It is 99.99% to select purity, and average grain diameter is 1 micron of alumina powder, purity 99.99%, average grain diameter 1
The carbon dust of micron is aluminum oxide as raw material, percentage by weight: carbon dust=2: 1, batch mixing 15 in V-type batch mixer is put into together to be divided
Clock.
The raw material for mixing carbon dust is put into high purity graphite crucible；Graphite crucible is put into graphite sintering stove, in nitrogen gas
Under atmosphere, it is that in-furnace temperature is risen to 1600 DEG C by 10 DEG C/h according to heating rate, is incubated 10h.
Powder after nitridation is put into high purity aluminium oxide crucible, alumina crucible is put into except in carbon stove, according to heating speed
Rate is that in-furnace temperature is risen to 650 DEG C by 2 DEG C/h, is incubated 4h.
After furnace temperature cooling, aluminium nitride powder is taken out.
Embodiments of the invention provide for the sake of example and description, and are not exhaustively or by this to send out
It is bright to be limited to disclosed form.Many modifications and variations are obvious for the ordinary skill in the art.Choosing
Select and describe embodiment and be to more preferably illustrate the principle and practical application of the present invention, and make one of ordinary skill in the art
It will be appreciated that the present invention is so as to designing the various embodiments with various modifications suitable for special-purpose.
Claims (4)
- A kind of 1. preparation method of aluminium nitride electronic ceramic powder, it is characterised in thatStep 1: alumina powder of the purity not less than 99.99% and metallic aluminium powder of the purity not less than 99.99% are mutually mixed Mixed-powder uniformly is made, wherein, alumina powder content be more than or equal to 90wt%, metallic aluminium powder content be less than or equal to 10wt%；Step 2: the mixed-powder is carried out in an inert atmosphere it is normal pressure-sintered, its sintering temperature be 900 DEG C~1100 DEG C, Then 4h~5h insulation is carried out, the multiple oxide powder of aluminum oxide is made after cooling with stove；Step 3: according to mass ratio it is 1.5 by the carbon dust of the multiple oxide powder of the aluminum oxide and purity not less than 99.99% Mixed at~2.5: 1, and the multiple oxide powder of the aluminum oxide for being blended with carbon dust carries out normal pressure burning in a nitrogen environment Primary aluminium nitride powder is made in knot, and its sintering temperature is 1400 DEG C~1500 DEG C, sintering time is 5h~6h, nitrogen flow is 0.4m3/h~1.0m3/h；Step 4: the primary aluminium nitride powder is carried out except aluminium nitride electronic ceramic powder is made in carbon operation, it removes carbon temperature For 600 DEG C~700 DEG C, except the carbon time is 4h~6h.
- 2. the preparation method of aluminium nitride electronic ceramic powder according to claim 1, it is characterised in thatIn the step 2, mixed-powder is carried out using graphite crucible in an inert atmosphere normal pressure-sintered；In the step 4, the primary aluminium nitride powder is carried out removing carbon for container using alumina crucible in except carbon stove Operation.
- 3. the preparation method of aluminium nitride electronic ceramic powder according to claim 2, it is characterised in thatIn the step 2, described inert environments are helium environment or ar gas environment.
- 4. the preparation method of the aluminium nitride electronic ceramic powder according to any one of claims 1 to 3, it is characterised in thatThe average grain diameter of the alumina powder is not more than 1 micron；The average grain diameter of the metallic aluminium powder is not more than 1 micron.
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| CN110577199A (en) * | 2018-06-07 | 2019-12-17 | 有研稀土新材料股份有限公司 | Method for removing carbon from nitride powder |
| CN110577403A (en) * | 2018-06-07 | 2019-12-17 | 有研稀土新材料股份有限公司 | high-purity aluminum nitride powder and preparation method thereof |
| CN110577198A (en) * | 2018-06-11 | 2019-12-17 | 河北高富氮化硅材料有限公司 | Method for removing crushed small particles in aluminum nitride powder |
| CN109763202B (en) * | 2019-01-03 | 2021-10-12 | 昆明理工大学 | Preparation method of aluminum nitride fiber |
| CN109650897B (en) * | 2019-02-20 | 2021-07-09 | 广东省新材料研究所 | Method for preparing aluminum nitride powder by APS plasma, aluminum nitride powder and application |
| CN110203893B (en) * | 2019-06-17 | 2021-04-27 | 邱瑞光 | Method for directly manufacturing spherical aluminum nitride from aluminum metal |
| CN111663185A (en) * | 2020-06-22 | 2020-09-15 | 哈尔滨化兴软控科技有限公司 | Device and method for preparing powder for PVT method aluminum nitride single crystal growth |
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