CN107698259A - A kind of method of iron and impurity levels in reduction aluminium nitride powder - Google Patents
A kind of method of iron and impurity levels in reduction aluminium nitride powder Download PDFInfo
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Abstract
The present invention relates to a kind of method for reducing trace iron, silicone content in aluminium nitride powder, belong to the preparation field of aluminium nitride powder.Methods described, which includes handling aluminium nitride powder by vacuum high-temperature, makes iron contained by it, silicon impurities volatilize, so as to improve the thermal conductivity of the purity of aluminium nitride powder and corresponding sintered body.
Description
Technical field
The present invention relates to aluminium nitride powder preparing technical field, and in particular to one kind reduces iron and sila in aluminium nitride powder
The method of matter content.
Background technology
With the development of the high power semiconductor device of the applications such as LED illumination, electric locomotive, hybrid vehicle, height is led
Tropical resources aluminium ceramic substrate gradually obtains market accreditation, as part substitution resin and the radiating material of aluminium oxide ceramic substrate
Material starts to use on a large scale.The theoretical thermal conductivity of aluminium nitride is 320W/mK, but the thermal conductivity of aluminium nitride ceramics material, highest
Reported values in 270W/mK or so, and the aluminum nitride ceramic substrate in actually using, its thermal conductivity is generally in 120-190W/mK
Between.
Making for aluminum nitride ceramic substrate, generally aluminium nitride powder is mixed with corresponding sintering aid first
It is even, tabular is then made by dry-pressing or wet moulding (curtain coating, slip casting, gel pouring etc.) technique, then by dumping, sintering etc.
Technique obtains ceramic of compact substrate.Each process procedure can impact to the thermal conductivity of final products, and this is also aluminium nitride
Ceramic substrate thermal conductivity is far below the reason for its theoretical value.
In the link of these influence thermal conductivities, as most basic aluminium nitride powder, its performance is to follow-up production ring
The thermal conductivity of section and final products has conclusive influence.AlN powder characteristics index includes its particle diameter, than surface, crystal grain
Shape, metals content impurity and surface oxygen content etc..Many researchs show, in addition to oxygen, the metal impurities in AlN powders,
Mainly iron and silicon, because these impurity can be dissolved into aluminium nitride lattice and cause defect in sintering process, influence phonon
Propagate, so as to thermal conductivity be caused to reduce.Therefore try to reduce the iron in AlN powders, the metals content impurity such as silicon just turns into and carried
The important channel of high AlN powder characteristics.
The preparation process of aluminium nitride powder is broadly divided into two kinds of technology paths, and one kind is carbon heat reducing nitriding, this method
Raw material is done using alumina powder and powdered carbon, nitrogen is passed through under high temperature, by reaction equation 1, obtains aluminium nitride powder；Another technology
Route is aluminium powder nitriding, i.e., using metallic aluminium powder (aluminium liquid) and nitrogen, at a certain temperature, by reaction equation 2, is nitrogenized
Aluminium powder body.
2Al2O3+3C+2N2=4AlN+3CO2 (1)
2Al+N2=2AlN (2)
In the specific implementation, aluminium powder nitriding technology path is divided into burning synthesis method (external heat), self- propagating again
Burning synthesis method (does not heat outside), aluminium liquid nitriding method etc..
Both technology paths can all be related to that raw material is self-contained or mixing/crushing process in the metal impurities that introduce, it is special
It is not aluminium powder nitriding, its AlN head product synthesized is generally harder, it is necessary to which prolonged crushing process, is finally obtained
Fe, Si impurity possibly even reach hundreds of ppm in AlN powders, have a strong impact on the thermal conductivity of sintered body.
Method for reducing Fe, Si content in ceramic powder at present, mainly there are pickling and magnetic force to go from what outside was carried out
Except two classes.Acid washing method has the application more than comparison, but this method pollution environment in SiC powder purification, and for easy water
The aluminium nitride powder of solution is not appropriate for.High-strength magnetic field can remove magnetic with iron tramp existing for form of iron oxide but right
Still it is difficult to carry out in Fe existing for iron micro hundreds of ppm or other non magnetic forms, such as simple substance Fe, this method.So
In order to reduce Fe, Si impurity in aluminium nitride, can only be reduced as far as possible during material purity and follow-up powder handling by improving
The method that Fe, Si are introduced passively is implemented.And raw material and use aluminium nitride mill Jie's ball of high-purity etc. carries out aluminium nitride powder
Crushing grinding, be a huge challenge for production cost.
New etc. mention of Chen Ke is handled raw material aluminium powder with the method for pickling, but does not refer to the change of Fe, Si content
(China Patent Publication No. CN1321621A).The it is proposeds such as Wu Liang use the method (China Patent Publication No. of high temperature purification
CN106757322A), but only refer only to reduce Al (OH)3Content.Guo great Wei etc., which is mentioned, prepares hypoxemia low iron content aluminum nitride powder
The method (China Patent Publication No. CN105399065A) of body, but the method simply reaches out for loose aluminium nitride powder, keeps away
Exempt from excessive grinding and introduce impurity.
Therefore the content of the impurity such as iron in aluminium nitride powder, silicon how is reduced, so as to improve AlN powder characteristics to obtain height
The aluminum nitride ceramic substrate of thermal conductivity, just turn into AlN power productions enterprise and the important subject of researcher.
The content of the invention
In order to solve the above technical problems, it is an object of the invention to provide a kind of easy to operate, inexpensive reduction nitridation
The method of iron and impurity levels in aluminium powder body.The inventive method is utilized under high temperature, and iron, silicon and its compound, which have, melts what is volatilized
Feature, the aln raw material containing micro Fe, Si impurity is handled by high temperature high vacuum condition, prepares the nitridation powder of high-purity
Body.
Therefore, one aspect of the present invention proposes a kind of method of iron and impurity levels in reduction aluminium nitride powder, institute
The method of stating includes：The iron tramp included in the aluminium nitride powder and silicon impurities are made to wave by the high-temperature process under vacuum condition
Hair, so as to improve the purity of aluminium nitride powder.
Further, the average grain diameter of the aluminium nitride powder is 0.5-30 microns；Specific surface area is 1-30m2/g；Iron is miscellaneous
Matter content is in more than 30ppm, and impurity levels are in more than 30ppm.Wherein, the iron tramp content is preferably 30-200ppm, silicon
Impurity content is preferably 30-200ppm.For the AlN powders of above-mentioned performance indications, can be obtained by processing method of the present invention
Maximum treatment effect/cost ratio.
Further, the iron tramp and silicon impurities exist in the aluminium nitride powder with compound or simple substance form.
In a specific embodiment, the compound is oxide.Wherein, the oxide of iron and silicon is above-mentioned in aluminium nitride powder
Impurity is most common and the most form of content.
Further, the high-temperature process under the vacuum condition, treatment temperature is at 1400-1750 DEG C, vacuum<10Pa,
Processing time is 1-10h, and the preferred process time is 2-5h.In addition, preferred 1600-1750 DEG C of the treatment temperature.
Alternatively, methods described is in vacuum<The nitrogen and/or argon gas of flowing can also be passed through after 10Pa.It is passed through lazy
Property gas nitrogen and/or argon gas can be poor with balanced reaction container external and internal pressure, play protection consersion unit, extension device uses the longevity
The effect of life.Nitrogenized in addition, being passed through nitrogen and a small amount of unreacted aluminium powder can also be made in aluminium nitride powder further to react
Aluminium, so as to further improve the purity of AlN powders.It is therefore preferable that it is passed through the mixed gas of nitrogen and nitrogen and argon gas.It is more excellent
The mixed gas into nitrogen and argon gas is gated, to be advantageous to relax the severe degree of reaction.
Further, methods described comprises the following steps：
(1) raw material aluminium nitride powder is put into high purity graphite crucible or aluminium nitride ceramics crucible, is then placed into carbon
In pipe furnace, below 5Pa is slowly evacuated to, design temperature is heated under 10 DEG C/min programming rates, is incubated 1h-10h；
(2) aluminium nitride powder handled well is sieved through 55 eye mesh screens, that is, obtains high purity silicon nitride aluminium powder body.The Fe of the powder
With Si impurity contents more than 30% is reduced compared with before processing.
Wherein, the high purity graphite crucible can be that the isostatic pressing formed graphite of 10ppm purity is made.
Further, the preparation method also includes：
(3) by the high purity silicon nitride aluminium powder body, the Y with 5wt%2O3, it is scattered to be put into nylon ball milling bucket using absolute ethyl alcohol
Medium, Si3N4Ball is mill Jie's ball, ball milling 12h, after taking out slurry drying, is sieved through 50 eye mesh screens, the mixed powder obtained is i.e.
It can be sintered.
The mixed powder can pressureless sintering be fine and close between 1780-1950 DEG C, and the density of its 1850 DEG C of sintered samples is
3.31g/cm3, thermal conductivity 185W/mK.
In one embodiment, handled by the method for the present invention, the total content of iron and silicon in aluminium nitride powder
25ppm can be reduced to from original 180ppm；The thermal conductivity of its sintered body can bring up to 185W/ from original 149W/mK
mK。
The inventive method has the following advantages that：
(1) it is obvious for the micro Fe in aluminium nitride powder, Si impurity, refining effect；Being handled by high-temperature vacuum makes it
Gasification volatilization, reach reduce Fe, Si content, lifted aluminium nitride purity purpose, by processing make impurity content reduce by 30% with
On, so as to improve the thermal conductivity of AlN Products.
(2) the inventive method efficiency high, simple to operate, big, pollution-free, the suitable industrialized production of yield.
Brief description of the drawings
Fig. 1 is the pattern of AlN raw materials powder used in comparative example 2 and embodiment 3-5.
The XRD spectrum of AlN raw materials powder used in Fig. 2 comparative examples 2 and embodiment 3-5.
Embodiment
The principle and feature of the present invention are described further by following examples.It should be understood that following examples are only
For explaining the present invention, and it is not limited to the scope of the present invention.
Comparative example 1
The block aluminium nitride obtained by aluminium powder nitriding, after crushed, obtain the powder that median (d50) is 3.8 μm
End.Iron, silicone content in the AlN powder is as shown in table 1, Fe the and Si contents in powder are respectively 150ppm and 200ppm.
Embodiment 1
Aluminium nitride powder 100g in comparative example 1 is weighed, is put into D=140mm high purity graphite crucible, is then placed in carbon pipe
In stove.After being evacuated to 5Pa, in the case where keeping vacuum state, 1600 DEG C are heated to, and be incubated 4 hours.Treat that furnace temperature is down to 100 DEG C
After below, graphite crucible is taken out in blow-on, analyzes Fe the and Si contents in powder, is down to 90ppm and 120ppm respectively.
Embodiment 2
Aluminium nitride powder 100g in comparative example 1 is weighed, is put into D=140mm high purity graphite crucible, is then placed in carbon pipe
In stove.After being evacuated to 5Pa, in the case where keeping vacuum state, 1700 DEG C are heated to, and be incubated 4 hours.Treat that furnace temperature is down to 100 DEG C
After below, graphite crucible is taken out in blow-on, analyzes Fe the and Si contents in powder, is down to 30ppm and 30ppm respectively.
Comparative example 2
The block aluminium nitride obtained by aluminium powder nitriding, after crushed, obtain the powder that median (d50) is 0.9 μm
End.Iron, silicone content in the AlN powder is as shown in table 1.Fe and Si contents in powder are respectively 80ppm and 100ppm.
The powder adds 5wt% Y2O3As sintering aid, after 1850 DEG C are incubated 2h, the thermal conductivity for obtaining sintered body is
149W/mK。
Embodiment 3
Aluminium nitride powder 100g in comparative example 2 is weighed, is put into D=140mm high purity graphite crucible, is then placed in carbon pipe
In stove.After being evacuated to 5Pa, in the case where keeping vacuum state, 1600 DEG C are heated to, and be incubated 4 hours.Treat that furnace temperature is down to 100 degree
After below, graphite crucible is taken out in blow-on, analyzes Fe the and Si contents in powder, is down to 30ppm and 35ppm respectively.
Embodiment 4
Aluminium nitride powder 100g in comparative example 2 is weighed, is put into D=140mm high purity graphite crucible, is then placed in carbon pipe
In stove.After being evacuated to 5Pa, in the case where keeping vacuum state, 1700 DEG C are heated to, and be incubated 4 hours.Treat that furnace temperature is down to 100 DEG C
After below, graphite crucible is taken out in blow-on, analyzes Fe the and Si contents in powder, is down to 10ppm and 15ppm respectively.
The powder adds 5wt% Y2O3As sintering aid, after 1850 DEG C are incubated 2h, the thermal conductivity for obtaining sintered body is
183W/mK。
Embodiment 5
Aluminium nitride powder 100g in comparative example 2 is weighed, is put into D=140mm high purity graphite crucible, is then placed in carbon pipe
In stove.After being evacuated to 5Pa, in the case where keeping vacuum state, 1800 DEG C are heated to, and be incubated 4 hours.Treat that furnace temperature is down to 100 DEG C
After below, graphite crucible is taken out in blow-on, analyzes Fe the and Si contents in powder, is down to 9ppm and 15ppm respectively.But the powder
Particle has agglomeration, and initial state can not be returned to without ball mill crushing.
Comparative example 3
Business aluminium nitride powder, median (d50) are 2.3 μm, and iron, silicone content are as shown in table 1.Fe and Si in powder
Content is respectively 100ppm and 120ppm.
Embodiment 6
Aluminium nitride powder 100g in comparative example 3 is weighed, is put into D=140mm high purity graphite crucible, is then placed in carbon pipe
In stove.After being evacuated to 5Pa, in the case where keeping vacuum state, 1700 DEG C are heated to, and be incubated 4 hours.Treat that furnace temperature is down to 100 DEG C
After below, graphite crucible is taken out in blow-on, analyzes Fe the and Si contents in powder, is down to 18ppm and 21ppm respectively.
Embodiment 7
Aluminium nitride powder 100g in comparative example 3 is weighed, is put into D=140mm high purity graphite crucible, is then placed in carbon pipe
In stove.After being evacuated to 5Pa, after being passed through high pure nitrogen (more than 99.99% purity) to 1 atmospheric pressure, 1700 DEG C are heated to, and
Insulation 4 hours.After furnace temperature is down to below 100 DEG C, graphite crucible is taken out in blow-on, analyzes Fe the and Si contents in powder, respectively
It is down to 21ppm and 19ppm.
Embodiment 8
Aluminium nitride powder 100g in comparative example 3 is weighed, is put into D=140mm high purity graphite crucible, is then placed in carbon pipe
In stove.After being evacuated to 5Pa, after being passed through high-purity argon gas (more than 99.99% purity) to 1 atmospheric pressure, 1700 DEG C are heated to, and
Insulation 4 hours.After furnace temperature is down to below 100 DEG C, graphite crucible is taken out in blow-on, analyzes Fe the and Si contents in powder, respectively
It is down to 28ppm and 22ppm.
The comparative example 1-3 of table 1 and embodiment 1-8 AlN powder characteristics parameter and processing bar
As shown in table 1, by the processing of the inventive method, compared to Fe the and Si impurity contents in comparative example 1-3, implement
Corresponding impurity content in example 1-8 declines to a great extent.As shown in comparative example 1-2 and embodiment 1-5, under identical vacuum,
With the raising for the treatment of temperature, impurity content has declined；In addition, as described in Example 5, although treatment temperature is 1800 DEG C
When obtained the impurity content more reduced, but start agglomeration occur.
In addition, as shown in comparative example 3 and embodiment 6-8, in identical vacuum and under identical treatment temperature, nitrogen is passed through
Gas and argon gas all achieve the impurity treatment effect suitable with not being passed through protective gas.Wherein, nitrogen is passed through to show than being passed through
The lower slightly impurity content of argon gas.
Although above with general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the scope of protection of present invention.
Claims (10)
1. a kind of method of iron and impurity levels in reduction aluminium nitride powder, it is characterised in that methods described includes：By true
High-temperature process under empty condition makes the iron tramp included in the aluminium nitride powder and silicon impurities volatilize, so as to improve aluminum nitride powder
The purity of body.
2. according to the method for claim 1, it is characterised in that the average grain diameter of the aluminium nitride powder is that 0.5-30 is micro-
Rice；Specific surface area is 1-30m2/g；Iron tramp content is in more than 30ppm, and impurity levels are in more than 30ppm.
3. according to the method for claim 2, it is characterised in that the iron tramp content is 30-200ppm, impurity levels
For 30-200ppm.
4. according to the method for claim 1, it is characterised in that the iron tramp and silicon impurities are in the aluminium nitride powder
Exist with oxide or simple substance form.
5. according to the method any one of claim 1-4, it is characterised in that the high-temperature process under the vacuum condition,
Treatment temperature is at 1400-1750 DEG C, vacuum<10Pa, processing time 1-10h.
6. according to the method for claim 5, it is characterised in that the processing time is 2-5h.
7. according to the method for claim 5, it is characterised in that methods described is in vacuum<Flowing is also passed through after 10Pa
Nitrogen and/or argon gas.
8. according to the method for claim 1, it is characterised in that methods described comprises the following steps：
(1) raw material aluminium nitride powder is put into high purity graphite crucible or aluminium nitride ceramics crucible, is then placed into carbon shirt-circuiting furnace
In, below 5Pa is slowly evacuated to, heats to design temperature, is incubated 1h-10h；
(2) aluminium nitride powder handled well is sieved through 55 eye mesh screens, that is, obtains high purity silicon nitride aluminium powder body, the Fe and Si of the powder
Impurity content reduces by more than 30% compared with before processing.
9. according to the method for claim 8, it is characterised in that methods described also includes：
(3) by the high purity silicon nitride aluminium powder body, the Y with 5wt%2O3, it is put into nylon ball milling bucket using absolute ethyl alcohol to be scattered and is situated between
Matter, Si3N4Ball is mill Jie's ball, ball milling 12h, after taking out slurry drying, is sieved through 50 eye mesh screens, the mixed powder obtained
It is sintered.
10. according to the method for claim 9, it is characterised in that the mixed powder burns between 1780-1950 DEG C without pressure
Knot is fine and close, and the density of its 1850 DEG C of sintered samples is 3.31g/cm3, thermal conductivity 185W/mK.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111364104A (en) * | 2020-04-23 | 2020-07-03 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Preparation method of high-purity raw material for aluminum nitride single crystal growth |
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| CN1199036A (en) * | 1998-04-24 | 1998-11-18 | 中国科学院上海硅酸盐研究所 | Process for preparation of transparent aluminium nitride ceramic |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111364104A (en) * | 2020-04-23 | 2020-07-03 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Preparation method of high-purity raw material for aluminum nitride single crystal growth |
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Application publication date: 20180216 |