CN106187203A - A kind of based on aluminium carbide method preparing aluminium nitride powder and products thereof - Google Patents
A kind of based on aluminium carbide method preparing aluminium nitride powder and products thereof Download PDFInfo
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Abstract
The invention belongs to inorganic non-metallic raw powder's production technology field, and disclose a kind of based on aluminium carbide method preparing aluminium nitride powder and products thereof, including: appropriate micron aluminium powder and micrometer carbon powder are uniformly mixed by (a), it is placed in inert atmosphere and is heated to predetermined temperature, insulation a period of time, it is allowed to reaction and generates aluminium carbide；B aluminium carbide is heated to predetermined temperature and is incubated a period of time in the ammonia or nitrogen of flowing by (), aluminium carbide reacts with ammonia or nitrogen in high temperature environments, generates aluminium nitride.Pass through the present invention, aluminium nitride powder can be prepared at relatively low temperature, prepared powder purity is high, particle diameter is little and even particle size distribution, and thermal conductivity is high and has excellent thermal property and mechanical performance, can be in field large-scale application such as the substrate materials of integrated circuit.
Description
Technical field
The invention belongs to inorganic non-metallic raw powder's production technology field, more particularly, to one based on carbonization aluminum
Method of standby aluminium nitride powder and products thereof.
Background technology
The wider substrate material of current industrial application is mainly aluminium oxide ceramics, beryllium oxide ceramics and aluminium nitride ceramics.
Aluminium oxide ceramics dielectric loss is low, mechanical strength is high, chemical stability is good, but its high heat conductance is only 30W/ (m K), far
The development of electronics industry can not be met.Although the theoretical thermal conductivity up to 350W/ (m K) of niberlox, but price is held high
Expensive, complicated process of preparation and have severe toxicity, is tapered off use.And aluminium nitride has high thermal conductivity, its theoretical thermal conductance
Rate may be up to 320W/ (m K), and aluminium nitride have reliable electrical insulating property, high temperature resistant, corrosion-resistant, low dielectric constant with
And and the linear expansion coefficient that matches of silicon.Additionally, aluminium nitride also has and most nonwettable feature of non-ferrous metal, available
Make high grade refractory, protecting tube etc..For high-heat conductivity aluminium nitride ceramics, the increase of oxygen content can cause aluminium nitride
Pottery thermal conductivity drastically declines.In order to prepare the aluminium nitride ceramics of high conduction, high-quality, it is necessary for preparing purity height, nitrogen
Content is high, oxygen content is low, granule is tiny, even-grained aluminium nitride powder.Therefore the preparation technology of aluminium nitride powder is to closing weight
Want.
The common preparation method of aluminium nitride powder mainly has: aluminium powder direct nitridation method, alumina carbon thermal reduction, self-propagating
High-temperature synthesis, chemical vapour deposition technique and plasma method.Aluminium powder direct nitridation method advantage is with low cost, raw material sources
Extensively, equipment cost is low and technique simple, but nitridation reaction process is wayward, and the Nitrogen in Products content of preparation is low, product quality
Poor, the product of generation is easily reunited, and follow-up palpus increases ball-milling technology, thus extends the production cycle, improves cost；Alumina carbon heat
Reducing process synthetic product nitrogen content is high, powder size is evenly distributed, be difficult to reunite, and has a good sintering character simultaneously, but carbon
The reaction temperature of thermal reduction is higher, the response time is longer；Self-propagating high-temperature synthesis reacts institute mainly by aluminum and nitrogen
The high chemical reaction heat produced makes that reaction is spontaneous to be carried out, it is not necessary to external heat source, and less energy consumption, production efficiency are high, but the method must be
Carry out under high pressure, equipment performance is required height, and spontaneous reaction process is difficult to control to；Chemical vapour deposition technique is according to aluminum source and nitrogen
Source issues biochemical reaction at gaseous condition, deposits aluminium nitride from gas, and the aluminium nitride purity that the method is prepared is high, but
The by-product of reaction has infringement to equipment, relatively costly during employing organo-aluminium source, expensive；Plasma chemistry synthetic method energy
Effectively shorten response time, synthesis fine size, specific surface is big, have the aluminium nitride powder of good sintering activity, but reaction can
Control property is poor, and aluminium nitride conversion ratio is the highest, need to carry out secondary nitridation.
Summary of the invention
For disadvantages described above or the Improvement requirement of prior art, the invention provides one and prepare aluminium nitride based on aluminium carbide
Method of powder body and products thereof, wherein by composition each in concrete steps of its preparation method and products thereof is studied and set
Meter, thus solves reaction temperature high, yields poorly and the technical problem such as particle diameter skewness.
For achieving the above object, according to one aspect of the present invention, it is provided that one prepares aluminum nitride powder based on aluminium carbide
The method of body, it is characterised in that the method comprises the following steps:
A aluminium powder and carbon dust mixing are placed in noble gas by (), then reacting by heating, in the middle of raw Powdered aluminium carbide
Product, wherein the mass ratio of carbon dust and aluminium powder is set as 2.25～3:1～2, and reaction temperature is set as 600 DEG C～1300 DEG C, instead
1h～8h it is set as between Ying Shi；
B intermediate product aluminium carbide is placed in nitrogen source by (), then reacting by heating, thus prepares required aluminium nitride powder,
Wherein reaction temperature is set as 600 DEG C～1500 DEG C, and the response time is set as 1h～10h；By generating intermediate product aluminium carbide
Aluminum particle is avoided at high temperature to melt reunion, in this way, it is achieved nitrogen, to alumina particles internal penetration, generates aluminium nitride.
As it is further preferred that in step (a), the mean diameter of added aluminium powder is less than 15 microns, and it is pure
Degree is more than 98%.
As it is further preferred that it is characterized in that, in step (a), the mean diameter of aluminium powder is 12 microns, and purity is
99%.
As it is further preferred that when added carbon dust mean diameter be less than 30 microns, and its purity be more than 99%.
As it is further preferred that it is characterized in that, in step (b), the mean diameter of carbon dust is 20 microns, and purity is
99%.
As it is further preferred that in step (a), reaction temperature is further configured to 1000 DEG C～1300 DEG C.
As it is further preferred that it is characterized in that, in step (b), the response time is further configured to 1000 DEG C.
As it is further preferred that in step (b), reaction temperature is further configured to 1000 DEG C～1300 DEG C.
As it is further preferred that it is characterized in that, in step (b), the response time is further configured to 1200 DEG C.
According to another aspect of the present invention, additionally provide and produce according to the aluminium nitride powder obtained by described preparation method
Product.
According to an additional aspect of the present invention, additionally provide aluminium nitride powder product at integrated circuit substrate material, crucible
The purposes of the aspect such as material and electronic device.
In general, by the contemplated above technical scheme of the present invention compared with prior art, by, it is possible to obtain following
Beneficial effect:
1, the present invention uses aluminium carbide as intermediate product to prepare aluminium nitride, owing to the fusing point of aluminium carbide is 2100 DEG C,
In course of reaction, the setting of temperature is below this temperature, effectively avoids aluminum particle at high temperature to melt, hinders due to nitrogen
The diffusion in source and the reaction that causes is incomplete, effective improve the content of aluminium nitride in end product；
2, by the concrete restriction to mixed powder reaction temperature in the present invention, and shown by more comparison test,
In this temperature range, reaction can improve the growing amount of aluminium carbide, and when time too high or too low for temperature, aluminium powder reacts with carbon dust
Slowly or to the formation of aluminium carbide play inhibition, and aluminium carbide can occur point under conditions of temperature is higher than 1300 DEG C
Solve, the temperature being thus effectively controlled in the course of reaction in course of reaction, cause the reaction temperature will not be the highest, the response time
Will not be oversize；
3, the present invention uses active higher ammonia as nitrogen source, reaction temperature can be significantly reduced；And synthetic product is pure
Degree height, equipment is not damaged by the side-product of reaction, and simultaneously without carrying out secondary nitridation, and the aluminium nitride powder particle diameter generated divides
Cloth is uniform, granularity is tiny, it is not necessary to carries out pulverization process, thus shortens the generation cycle, reduces production cost；
4, the preparation method that the present invention provides is divided into two steps, and integrated artistic is simple, with low cost, and course of reaction is just
In quality control, obtained aluminium nitride powder product purity is high, and impurity oxygen content is low, significantly improves the thermal conductivity of product, suitable
For large batch of industrialized production.
Accompanying drawing explanation
Fig. 1 is according to the process chart preparing aluminium nitride constructed by the present invention；
Fig. 2 is according to the device structure schematic diagram preparing aluminium nitride constructed by the present invention；
Fig. 3 is X-ray diffraction (XRD) collection of illustrative plates according to the aluminium carbide powder body obtained by the embodiment of the present invention 1；
Fig. 4 is to compose according to the X-ray diffraction XRD figure of the aluminium nitride powder obtained by the embodiment of the present invention 1.
In all of the figs, identical reference is used for representing identical element or structure, wherein:
1-argon bottle 2-batch-type furnace 3-ammonia bottle 4,5,6-spinner flowmeter 7-tube furnace 8-vent gas treatment bottle
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, right
The present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, and
It is not used in the restriction present invention.If additionally, technical characteristic involved in each embodiment of invention described below
The conflict of not constituting each other just can be mutually combined.
Fig. 1 is that Fig. 2 is according to constructed by the present invention according to the process chart preparing aluminium nitride constructed by the present invention
Prepare the device structure schematic diagram of aluminium nitride.As depicted in figs. 1 and 2, step (a) is by complete in argon bottle 1 and batch-type furnace 2
Becoming, step (b) passes through ammonia bottle 3, spinner flowmeter 4,5 and 6, tube furnace 7, completes in vent gas treatment bottle 8.Argon bottle 1 conduct
Quantitative aluminium powder, equipped with argon, is mixed homogeneously with carbon dust and is loaded in batch-type furnace 2 and heat up by protection gas source of the gas, after insulation, continues
It is passed through argon and protective atmosphere is provided, prevent aluminium powder oxidized.The aluminium carbide generated in batch-type furnace is layered on reaction utensil uniformly
In, the thickness of powder is difficult to blocked up, prevents the aluminium carbide powder of nexine cannot be fully contacted with ammonia, causes nitridation not exclusively.
Being placed in by reaction utensil in tube furnace 7, be passed through the air that ammonia drains in quartz ampoule before the reaction, end cap 5 and 6 has good sealing
Effect, can prevent in course of reaction air to enter in quartz ampoule.Tube furnace 7 is heated, is then incubated, should during whole
It is continually fed into ammonia until powder is cooled to room temperature, prevents air return from causing powder oxidized, and ammonia flow is unsuitable excessive,
Ammonia flow of the present invention is set as 3L/h, if ammonia flow is excessive, then tubular type in-furnace temperature can be caused to reduce, cause nitridation reaction
Carry out slowly or can not nitrogenize completely.
Below with reference to the technological process of Fig. 1, and the following multiple embodiments of combination are further elaborated with the present invention.
Embodiment 1
Being mixed homogeneously with the carbon dust of 0.3g by the micron aluminium powder of 0.9g, the mean diameter of aluminium powder is 10 microns, and purity is
98.5%, the mean diameter of carbon dust is 20 microns, and purity is 99.2%, be placed in batch-type furnace, be passed through argon as protection gas,
Argon flow amount is 3L/h, and batch-type furnace is warming up to 1000 DEG C, is incubated 3h.The carbonization aluminium powder that question response will generate after being cooled to room temperature
End uniform spreading is placed in tube furnace in reaction utensil, is passed through ammonia, and ammonia flow is 3L/h, and tube furnace is warming up to 1200 DEG C,
Insulation 6h, is cooled to room temperature to reaction, thus prepares the high-quality aluminum nitride powder that purity is high, particle diameter is tiny, impurity oxygen content is low
Body product.
Embodiment 2
Being mixed homogeneously with the carbon dust of 0.6g by the micron aluminium powder of 0.9g, the mean diameter of aluminium powder is 15 microns, and purity is
98%, the mean diameter of carbon dust is 30 microns, and purity is 99%, it is placed in batch-type furnace, is passed through argon as protection gas, argon
Flow is 3L/h, and batch-type furnace is warming up to 600 DEG C, is incubated 8h.Question response is cooled to equal for the aluminium carbide powder that generates after room temperature
Even being layered in reaction utensil is placed in tube furnace, is passed through ammonia, and ammonia flow is 3L/h, and tube furnace is warming up to 1500 DEG C, insulation
1h, is cooled to room temperature to reaction, thus prepares the high-quality aluminium nitride powder that purity is high, particle diameter is tiny, impurity oxygen content is low and produces
Product.
Embodiment 3
Being mixed homogeneously with the carbon dust of 0.4g by the micron aluminium powder of 0.9g, the mean diameter of aluminium powder is 12 microns, and purity is
98.4%, the mean diameter of carbon dust is 25 microns, and purity is 99.5%, be placed in batch-type furnace, be passed through argon as protection gas,
Argon flow amount is 3L/h, and batch-type furnace is warming up to 1300 DEG C, is incubated 1h.The carbonization aluminium powder that question response will generate after being cooled to room temperature
End uniform spreading is placed in tube furnace in reaction utensil, is passed through ammonia, and ammonia flow is 3L/h, and tube furnace is warming up to 600 DEG C, protects
Temperature 10h, is cooled to room temperature to reaction, thus prepares the high-quality aluminium nitride powder that purity is high, particle diameter is tiny, impurity oxygen content is low
Product.
Embodiment 4
Being mixed homogeneously with the carbon dust of 0.3g by the micron aluminium powder of 0.9g, the mean diameter of aluminium powder is 10 microns, and purity is
98.4%, the mean diameter of carbon dust is 25 microns, and purity is 99.5%, be placed in batch-type furnace, be passed through argon as protection gas,
Argon flow amount is 3L/h, and batch-type furnace is warming up to 1000 DEG C, is incubated 5h.The carbonization aluminium powder that question response will generate after being cooled to room temperature
End uniform spreading is placed in tube furnace in reaction utensil, is passed through ammonia, and ammonia flow is 3L/h, and tube furnace is warming up to 1000 DEG C,
Insulation 6h, is cooled to room temperature to reaction, thus prepares the high-quality aluminum nitride powder that purity is high, particle diameter is tiny, impurity oxygen content is low
Body product.
Embodiment 5
Being mixed homogeneously with the carbon dust of 0.4g by the micron aluminium powder of 0.9g, the mean diameter of aluminium powder is 14 microns, and purity is
98.4%, the mean diameter of carbon dust is 25 microns, and purity is 99.5%, be placed in batch-type furnace, be passed through argon as protection gas,
Argon flow amount is 3L/h, and batch-type furnace is warming up to 1200 DEG C, is incubated 6h.The carbonization aluminium powder that question response will generate after being cooled to room temperature
End uniform spreading is placed in tube furnace in reaction utensil, is passed through ammonia, and ammonia flow is 3L/h, and tube furnace is warming up to 1200 DEG C,
Insulation 4h, is cooled to room temperature to reaction, thus prepares the high-quality aluminum nitride powder that purity is high, particle diameter is tiny, impurity oxygen content is low
Body product.
Embodiment 6
Being mixed homogeneously with the carbon dust of 0.4g by the micron aluminium powder of 0.45g, the mean diameter of aluminium powder is 12 microns, and purity is
98.2%, the mean diameter of carbon dust is 28 microns, and purity is 99.6%, be placed in batch-type furnace, be passed through argon as protection gas,
Argon flow amount is 3L/h, and batch-type furnace is warming up to 1300 DEG C, is incubated 8h.The carbonization aluminium powder that question response will generate after being cooled to room temperature
End uniform spreading is placed in tube furnace in reaction utensil, is passed through ammonia, and ammonia flow is 3L/h, and tube furnace is warming up to 1200 DEG C,
Insulation 8h, is cooled to room temperature to reaction, thus prepares the high-quality aluminum nitride powder that purity is high, particle diameter is tiny, impurity oxygen content is low
Body product.
Embodiment 7
Being mixed homogeneously with the carbon dust of 0.3g by the micron aluminium powder of 0.9g, the mean diameter of aluminium powder is 12 microns, and purity is
98.2%, the mean diameter of carbon dust is 28 microns, and purity is 99.6%, be placed in batch-type furnace, be passed through argon as protection gas,
Argon flow amount is 3L/h, and batch-type furnace is warming up to 1000 DEG C, is incubated 4h.The carbonization aluminium powder that question response will generate after being cooled to room temperature
End uniform spreading is placed in tube furnace in reaction utensil, is passed through nitrogen, and nitrogen flow is 3L/h, and tube furnace is warming up to 1500 DEG C,
Insulation 2h, is cooled to room temperature to reaction, thus prepares the high-quality aluminum nitride powder that purity is high, particle diameter is tiny, impurity oxygen content is low
Body product.
Fig. 3 is X-ray diffraction (XRD) collection of illustrative plates according to the aluminium carbide powder body obtained by the embodiment of the present invention 1, Fig. 4 be by
X-ray diffraction (XRD) collection of illustrative plates according to the aluminium nitride powder obtained by the embodiment of the present invention 1.As seen from Figure 3 according to the present invention
Powder prepared by the technique of embodiment 1 mainly occurs with the diffraction maximum of aluminium carbide, and the diffraction maximum in Fig. 4 is mainly with aluminium nitride
Diffraction maximum is main, illustrates that the aluminium nitride content prepared according to embodiments of the invention is high.
Being analyzed above 7 aluminium nitride powders being embodied as prepared by case by experiment detection, result shows
The high purity 95%-100% of the aluminium nitride powder prepared, powder diameter distribution is 1-10 micron.Compared to such as carbon
The purity of the aluminium nitride of about the 70% of other preparation method such as thermal reduction, the aluminium nitride powder purity prepared by the present invention shows
Write and improve, and uniform particle sizes, tiny.
As it will be easily appreciated by one skilled in the art that and the foregoing is only presently preferred embodiments of the present invention, not in order to
Limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, all should comprise
Within protection scope of the present invention.
Claims (8)
1. the method preparing aluminium nitride powder based on aluminium carbide, it is characterised in that the method comprises the following steps:
A aluminium powder and carbon dust mixing are placed in noble gas by (), then reacting by heating is produced in the middle of raw Powdered aluminium carbide
Thing, wherein the mass ratio of carbon dust and aluminium powder is set as 2.25～3:1～2, and reaction temperature is set as 600 DEG C～1300 DEG C, reaction
Time is set as 1h～8h；
B intermediate product aluminium carbide is placed in nitrogen source by (), then reacting by heating, thus prepares required aluminium nitride powder, wherein
Reaction temperature is set as 600 DEG C～1500 DEG C, and the response time is set as 1h～10h；Avoid by generating intermediate product aluminium carbide
Aluminum particle at high temperature melts reunion, in this way, it is achieved nitrogen, to alumina particles internal penetration, generates aluminium nitride.
2. preparation method as claimed in claim 1, it is characterised in that in step (a), the mean diameter of added aluminium powder is little
In 15 microns, and its purity is more than 98%.
3. preparation method as claimed in claim 1 or 2, it is characterised in that when the mean diameter of added carbon dust is micro-less than 30
Rice, and its purity is more than 99%.
4. the preparation method as described in any one of claim 1-3, it is characterised in that in step (a), reaction temperature is further
It is set as 1000 DEG C～1300 DEG C.
5. the preparation method as described in any one of claim 1-4, it is characterised in that in step (b), reaction temperature is further
It is set as 1000 DEG C～1300 DEG C.
6. the preparation method as described in any one of claim 1-5, it is characterised in that in step (b), the response time is further
It is set as 1200 DEG C.
7. the aluminium nitride powder product obtained by the preparation method utilized described in any one of claim 1-6.
8. aluminium nitride powder product as claimed in claim 7 is at integrated circuit substrate material, crucible material and electronic device etc.
The purposes of aspect.
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| CN106882773A (en) * | 2017-03-06 | 2017-06-23 | 昆明理工大学 | A kind of method for preparing aluminium nitride |
| CN113526960A (en) * | 2021-07-20 | 2021-10-22 | 宁波东联密封件有限公司 | Silicon carbide ceramic and hot isostatic pressing sintering process thereof |
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Cited By (3)
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| CN106882773A (en) * | 2017-03-06 | 2017-06-23 | 昆明理工大学 | A kind of method for preparing aluminium nitride |
| CN106882773B (en) * | 2017-03-06 | 2019-04-12 | 昆明理工大学 | A method of preparing aluminium nitride |
| CN113526960A (en) * | 2021-07-20 | 2021-10-22 | 宁波东联密封件有限公司 | Silicon carbide ceramic and hot isostatic pressing sintering process thereof |
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