CN106187203B - A kind of method and products thereof that aluminium nitride powder is prepared based on aluminium carbide - Google Patents
A kind of method and products thereof that aluminium nitride powder is prepared based on aluminium carbide Download PDFInfo
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Abstract
The invention belongs to inorganic non-metallic raw powder's production technology fields, and disclose a kind of method and products thereof that aluminium nitride powder is prepared based on aluminium carbide, it include: that (a) uniformly mixes appropriate micron aluminium powder and micrometer carbon powder, it is placed in inert atmosphere and is heated to predetermined temperature, heat preservation a period of time is allowed to reaction and generates aluminium carbide；(b) aluminium carbide is heated to predetermined temperature in the ammonia or nitrogen of flowing and keeps the temperature a period of time, aluminium carbide is reacted with ammonia or nitrogen under high temperature environment, generates aluminium nitride.Through the invention, aluminium nitride powder can be prepared at relatively low temperature, prepared powder purity is high, partial size is small and even particle size distribution, and thermal conductivity is high and has excellent thermal property and mechanical performance, can be in the fields such as substrate material of integrated circuit large-scale application.
Description
Technical field
The invention belongs to inorganic non-metallic raw powder's production technology fields, more particularly, to one kind based on carbonization aluminum
The method and products thereof of standby aluminium nitride powder.
Background technique
Industrially the wider substrate material of application is mainly aluminium oxide ceramics, beryllium oxide ceramics and aluminium nitride ceramics at present.
Aluminium oxide ceramics dielectric loss is low, high mechanical strength, chemical stability are good, but its highest thermal conductivity is only 30W/ (mK), far
It is not able to satisfy the development of electronics industry.Although the theoretical thermal conductivity up to 350W/ (mK) of niberlox, price is high
It is expensive, preparation process is complicated and has severe toxicity, tapered off use.And aluminium nitride has high thermal conductivity, theoretical thermal conductivity
Rate may be up to 320W/ (mK), and aluminium nitride have reliable electrical insulating property, high temperature resistant, corrosion-resistant, low dielectric constant with
And the linear expansion coefficient to match with silicon.In addition, aluminium nitride also has the characteristics that and most non-ferrous metals are nonwettable, can use
Make high grade refractory, protecting tube etc..For high-heat conductivity aluminium nitride ceramics, the increase of oxygen content will lead to aluminium nitride
Ceramic thermal conductivity sharply declines.In order to prepare the aluminium nitride ceramics of high conduction, high-quality, purity is high, nitrogen must be just prepared
Content is high, oxygen content is low, particle is tiny, even-grained aluminium nitride powder.Therefore the preparation process of aluminium nitride powder is to Guan Chong
It wants.
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 low in cost, raw material sources
Extensively, equipment cost is low and simple process, but nitridation reaction process is not easy to control, and the product nitrogen content of preparation is low, product quality
The product of difference, generation is easy to reunite, subsequent to increase ball-milling technology, to extend the production cycle, improves cost；Alumina carbon heat
Reduction method synthetic product nitrogen content is high, powder size is evenly distributed, is not easy to reunite, while having good sintering character, but carbon
The reaction temperature of thermal reduction is higher, the reaction time is longer；Self-propagating high-temperature synthesis mainly utilizes aluminium and nitrogen to react institute
The high chemical reaction heat generated makes to react spontaneous progress, and being not necessarily to external heat source, less energy consumption, high production efficiency, but this method must be
It is carried out under high pressure, height is required to equipment performance, and spontaneous reaction process is difficult to control；Chemical vapour deposition technique is according to silicon source and nitrogen
Source issues biochemical reaction in gaseous condition, and aluminium nitride is deposited from gas, the aluminium nitride purity is high that this method is prepared, but
The by-product of reaction has damage to equipment, expensive using higher cost when organic silicon source；Plasma chemistry synthetic method energy
Effectively shorten that reaction time, synthesis fine size, specific surface be big, the aluminium nitride powder with good sintering activity, but reacting can
Control property is poor, and aluminium nitride conversion ratio is not high, need to carry out secondary nitridation.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides one kind prepares aluminium nitride based on aluminium carbide
Method of powder and products thereof, wherein being studied and being set by each ingredient in specific steps to preparation method and products thereof
Thus meter solves the technical problems such as reaction temperature is high, and low output and particle diameter distribution are uneven.
To achieve the above object, according to one aspect of the present invention, it provides one kind and aluminum nitride powder is prepared based on aluminium carbide
The method of body, which is characterized in that this method includes the following steps:
(a) aluminium powder and carbon dust are mixed and is placed in inert gas, then heating reaction, generates among 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
It is set as 1h~8h between seasonable；
(b) intermediate product aluminium carbide is placed in nitrogen source, then heating reaction, is thus made required aluminium nitride powder,
Wherein reaction temperature is set as 600 DEG C~1500 DEG C, and the reaction time is set as 1h~10h；By generating intermediate product aluminium carbide
It avoids aluminum particle from melting reunion at high temperature, by this method, realizes that nitrogen to the infiltration inside aluminium carbide, generates aluminium nitride.
As it is further preferred that the average grain diameter of aluminium powder be added is less than 15 microns, and its is pure in step (a)
Degree is greater than 98%.
As it is further preferred that it is characterized in that, the average grain diameter of aluminium powder is 12 microns, and purity is in step (a)
99%.
As it is further preferred that when the average grain diameter of carbon dust be added is less than 30 microns, and its purity is greater than 99%.
As it is further preferred that it is characterized in that, the average grain diameter of carbon dust is 20 microns, and purity is in step (b)
99%.
As it is further preferred that reaction temperature is further configured to 1000 DEG C~1300 DEG C in step (a).
As it is further preferred that it is characterized in that, reaction temperature is further configured to 1000 DEG C in step (b).
As it is further preferred that reaction temperature is further configured to 1000 DEG C~1300 DEG C in step (b).
As it is further preferred that it is characterized in that, reaction temperature is further configured to 1200 DEG C in step (b).
Other side according to the invention is additionally provided and is produced according to aluminium nitride powder obtained by the preparation method
Product.
Another aspect according to the invention additionally provides aluminium nitride powder product in integrated circuit substrate material, crucible
Purposes in terms of material and electronic device.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, by that can obtain following
The utility model has the advantages that
1, the present invention prepares aluminium nitride as intermediate product using aluminium carbide, since the fusing point of aluminium carbide is 2100 DEG C,
The setting of temperature is below the temperature in reaction process, effectively aluminum particle is avoided to melt at high temperature, hinders due to nitrogen
The diffusion in source and caused by reaction not exclusively, the effective content for improving aluminium nitride in final product；
2, by the specific restriction to mixed powder reaction temperature in the present invention, and shown by more comparison test
Reaction can be improved the production quantity of aluminium carbide within this temperature range, and when too high or too low for temperature, aluminium powder is reacted 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
Solution, the temperature being thus effectively controlled in the reaction process in reaction process cause reaction temperature too high, the reaction time
It will not be too long；
3, it uses the higher ammonia of activity as nitrogen source in the present invention, reaction temperature can be significantly reduced；And synthetic product is pure
Degree is high, and the byproduct of reaction does not damage equipment, while without carrying out secondary nitridation, and the aluminium nitride powder partial size point generated
Cloth is uniform, granularity is tiny, without carrying out pulverization process, so as to shorten the generation period, reduces production cost；
4, preparation method provided by the invention is divided into two steps, and integrated artistic is simple, low in cost, and reaction process is just
It is controlled in quality, obtained aluminium nitride powder product purity is high, and impurity oxygen content is low, significantly improves the thermal conductivity of product, fits
For large batch of industrialized production.
Detailed description of the invention
Fig. 1 is the process flow chart that aluminium nitride is prepared constructed by the present invention；
Fig. 2 is the device structure schematic diagram that aluminium nitride is prepared constructed by the present invention；
Fig. 3 is X-ray diffraction (XRD) map according to aluminium carbide powder obtained by the embodiment of the present invention 1；
Fig. 4 is the X-ray diffraction XRD spectrum according to aluminium nitride powder obtained by the embodiment of the present invention 1.
In all the appended drawings, identical appended drawing reference is used to denote the same element or structure, in which:
4,5,6- spinner flowmeter 7- tube furnace 8- vent gas treatment bottle of 1- argon bottle 2- batch-type furnace 3- ammonia bottle
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
Fig. 1 is the process flow chart that aluminium nitride is prepared constructed by the present invention, and Fig. 2 is according to constructed by the present invention
Prepare the device structure schematic diagram of aluminium nitride.As depicted in figs. 1 and 2, step (a) passes through complete in argon bottle 1 and batch-type furnace 2
At, step (b) by ammonia bottle 3, spinner flowmeter 4,5 and 6, tube furnace 7 is completed in vent gas treatment bottle 8.1 conduct of argon bottle
It protects gas gas source that argon gas is housed, quantitative aluminium powder is uniformly mixed with carbon dust and is fitted into batch-type furnace 2 and heats up, after heat preservation, continue
It is passed through argon gas and protective atmosphere is provided, aluminium powder is prevented to be oxidized.The aluminium carbide generated in batch-type furnace is uniformly layered on reaction utensil
Interior, the thickness of powder is not easy blocked up, prevents the carbonization aluminium powder of inner layer from can not come into full contact with ammonia, causes nitridation incomplete.
Reaction utensil is placed in tube furnace 7, ammonia is passed through before the reaction and drains air in quartz ampoule, end cap 5 and 6 has good sealing
Effect, can prevent during the reaction air enter in quartz ampoule.Tube furnace 7 is heated, is then kept the temperature, is answered in the whole process
Be continually fed into ammonia until powder be cooled to room temperature, prevent air return from powder being caused to be oxidized, and ammonia flow should not be too large,
Ammonia flow of the present invention is set as 3L/h, if ammonia flow is excessive, will lead to the reduction of tubular type in-furnace temperature, causes nitridation reaction
It carries out slowly or cannot nitrogenize completely.
The present invention is further elaborated with below with reference to the process flow of Fig. 1, and in conjunction with following multiple embodiments.
Embodiment 1
The micron aluminium powder of 0.9g is uniformly mixed with the carbon dust of 0.3g, the average grain diameter of aluminium powder is 10 microns, and purity is
98.5%, the average grain diameter of carbon dust is 20 microns, purity 99.2%, it is placed in batch-type furnace, is passed through argon gas and is used as protection gas,
Argon flow is 3L/h, and batch-type furnace is warming up to 1000 DEG C, keeps the temperature 3h.By the carbonization aluminium powder of generation after reacting and being cooled to room temperature
Last be uniformly layered in reaction utensil is placed in tube furnace, is passed through ammonia, and tube furnace is warming up to 1200 DEG C by ammonia flow 3L/h,
6h is kept the temperature, until reaction is cooled to room temperature, purity is high thus is made, the high-quality aluminum nitride powder that partial size is tiny, impurity oxygen content is low
Body product.
Embodiment 2
The micron aluminium powder of 0.9g is uniformly mixed with the carbon dust of 0.6g, the average grain diameter of aluminium powder is 15 microns, and purity is
98%, the average grain diameter of carbon dust is 30 microns, purity 99%, it is placed in batch-type furnace, is passed through argon gas as protection gas, argon gas
Flow is 3L/h, and batch-type furnace is warming up to 600 DEG C, keeps the temperature 8h.It is after reacting and being cooled to room temperature that the carbonization aluminium powder of generation is equal
Even be layered in reaction utensil is placed in tube furnace, is passed through ammonia, and tube furnace is warming up to 1500 DEG C, heat preservation by ammonia flow 3L/h
Thus until reaction is cooled to room temperature purity is high is made, the high-quality aluminium nitride powder that partial size is tiny, impurity oxygen content is low produces in 1h
Product.
Embodiment 3
The micron aluminium powder of 0.9g is uniformly mixed with the carbon dust of 0.4g, the average grain diameter of aluminium powder is 12 microns, and purity is
98.4%, the average grain diameter of carbon dust is 25 microns, purity 99.5%, it is placed in batch-type furnace, is passed through argon gas and is used as protection gas,
Argon flow is 3L/h, and batch-type furnace is warming up to 1300 DEG C, keeps the temperature 1h.By the carbonization aluminium powder of generation after reacting and being cooled to room temperature
Last be uniformly layered in reaction utensil is placed in tube furnace, is passed through ammonia, and tube furnace is warming up to 600 DEG C, protected by ammonia flow 3L/h
Thus until reaction is cooled to room temperature purity is high is made, the high-quality aluminium nitride powder that partial size is tiny, impurity oxygen content is low in warm 10h
Product.
Embodiment 4
The micron aluminium powder of 0.9g is uniformly mixed with the carbon dust of 0.3g, the average grain diameter of aluminium powder is 10 microns, and purity is
98.4%, the average grain diameter of carbon dust is 25 microns, purity 99.5%, it is placed in batch-type furnace, is passed through argon gas and is used as protection gas,
Argon flow is 3L/h, and batch-type furnace is warming up to 1000 DEG C, keeps the temperature 5h.By the carbonization aluminium powder of generation after reacting and being cooled to room temperature
Last be uniformly layered in reaction utensil is placed in tube furnace, is passed through ammonia, and tube furnace is warming up to 1000 DEG C by ammonia flow 3L/h,
6h is kept the temperature, until reaction is cooled to room temperature, purity is high thus is made, the high-quality aluminum nitride powder that partial size is tiny, impurity oxygen content is low
Body product.
Embodiment 5
The micron aluminium powder of 0.9g is uniformly mixed with the carbon dust of 0.4g, the average grain diameter of aluminium powder is 14 microns, and purity is
98.4%, the average grain diameter of carbon dust is 25 microns, purity 99.5%, it is placed in batch-type furnace, is passed through argon gas and is used as protection gas,
Argon flow is 3L/h, and batch-type furnace is warming up to 1200 DEG C, keeps the temperature 6h.By the carbonization aluminium powder of generation after reacting and being cooled to room temperature
Last be uniformly layered in reaction utensil is placed in tube furnace, is passed through ammonia, and tube furnace is warming up to 1200 DEG C by ammonia flow 3L/h,
4h is kept the temperature, until reaction is cooled to room temperature, purity is high thus is made, the high-quality aluminum nitride powder that partial size is tiny, impurity oxygen content is low
Body product.
Embodiment 6
The micron aluminium powder of 0.45g is uniformly mixed with the carbon dust of 0.4g, the average grain diameter of aluminium powder is 12 microns, and purity is
98.2%, the average grain diameter of carbon dust is 28 microns, purity 99.6%, it is placed in batch-type furnace, is passed through argon gas and is used as protection gas,
Argon flow is 3L/h, and batch-type furnace is warming up to 1300 DEG C, keeps the temperature 8h.By the carbonization aluminium powder of generation after reacting and being cooled to room temperature
Last be uniformly layered in reaction utensil is placed in tube furnace, is passed through ammonia, and tube furnace is warming up to 1200 DEG C by ammonia flow 3L/h,
8h is kept the temperature, until reaction is cooled to room temperature, purity is high thus is made, the high-quality aluminum nitride powder that partial size is tiny, impurity oxygen content is low
Body product.
Embodiment 7
The micron aluminium powder of 0.9g is uniformly mixed with the carbon dust of 0.3g, the average grain diameter of aluminium powder is 12 microns, and purity is
98.2%, the average grain diameter of carbon dust is 28 microns, purity 99.6%, it is placed in batch-type furnace, is passed through argon gas and is used as protection gas,
Argon flow is 3L/h, and batch-type furnace is warming up to 1000 DEG C, keeps the temperature 4h.By the carbonization aluminium powder of generation after reacting and being cooled to room temperature
Last be uniformly layered in reaction utensil is placed in tube furnace, is passed through nitrogen, and tube furnace is warming up to 1500 DEG C by nitrogen flow 3L/h,
2h is kept the temperature, until reaction is cooled to room temperature, purity is high thus is made, the high-quality aluminum nitride powder that partial size is tiny, impurity oxygen content is low
Body product.
Fig. 3 is X-ray diffraction (XRD) map according to aluminium carbide powder obtained by the embodiment of the present invention 1, Fig. 4 be by
According to X-ray diffraction (XRD) map of 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
Based on diffraction maximum, the nitridation aluminium content for illustrating that embodiment according to the invention is prepared is high.
Aluminium nitride powder prepared by above 7 specific implementations case is analyzed by testing detection, the results showed that
The purity for the aluminium nitride powder prepared is up to 95%-100%, and powder diameter distribution is 1-10 microns.Compared to such as carbon
The purity of 70% or so aluminium nitride of other preparation methods such as thermal reduction, aluminium nitride powder purity prepared by the present invention are aobvious
It writes and improves, and is uniform particle sizes, tiny.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (6)
1. a kind of method for preparing aluminium nitride powder based on aluminium carbide, which is characterized in that this method includes the following steps:
(a) aluminium powder and carbon dust are mixed and is placed in inert gas, then heating reaction, generated and produced among powdered aluminium carbide
Object, 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, then heating reaction, is thus made required aluminium nitride powder, wherein
Reaction temperature is set as 600 DEG C~1300 DEG C, and the reaction time is set as 1h~10h, realizes nitrogen to intermediate product carbon by this method
Change the infiltration inside aluminium, ultimately generates required aluminium nitride；It can avoid aluminum particle in this way to melt at high temperature, hinder due to nitrogen
The diffusion in source and caused by reaction not exclusively, and effectively improve the content of aluminium nitride in final product.
2. preparation method as described in claim 1, which is characterized in that in step (a), the average grain diameter of aluminium powder be added is small
In 15 microns, and its purity is greater than 98%.
3. preparation method as claimed in claim 1 or 2, which is characterized in that when the average grain diameter of carbon dust be added is micro- less than 30
Rice, and its purity is greater than 99%.
4. preparation method as described in claim 1, which is characterized in that in step (a), reaction temperature is further configured to
1000 DEG C~1300 DEG C.
5. preparation method as described in claim 1, which is characterized in that in step (b), reaction temperature is further configured to
1000 DEG C~1300 DEG C.
6. preparation method as described in claim 1, which is characterized in that in step (b), reaction temperature is further configured to
1200℃。
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| Title |
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| 氮化铝和氮化铝陶瓷;周文钊;《现代化工》;19951231;第44页左栏制法及基本化学性质 |
| 氮化铝粉末的制备;黄莉萍 等;《硅酸盐学报》;19860930;第14卷(第3期);第333页实验和结果部分 |
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