CN1435371A - Method for preparing aluminium nitride powder - Google Patents
Method for preparing aluminium nitride powder Download PDFInfo
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- CN1435371A CN1435371A CN03119584A CN03119584A CN1435371A CN 1435371 A CN1435371 A CN 1435371A CN 03119584 A CN03119584 A CN 03119584A CN 03119584 A CN03119584 A CN 03119584A CN 1435371 A CN1435371 A CN 1435371A
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Abstract
A process for preparing superfine aluminium nitride powder includes proportioning aluminium nitrate as Al source, urea, and water-soluble organic carbon source (glucose, cane sugar, citric acid, or soluble starch), mixing, preparing solution of mixture, thermal drying at 100-400 deg.C to obtain powder, reductive nitrifying reaction at 1200-1600 deg.C in N2 for 1-24 hr, and calcining at 600-700 deg.C for 1-7 hr.
Description
Technical field
The invention belongs to the low-temperature burning synthesis technical field, a kind of method for preparing superfine aluminium nitride powder about the low temperature carbothermic method particularly is provided.
Background technology
The sintered compact of aluminium nitride makes it both applicable to as ceramic material (as the substrate and the encapsulation of unicircuit) owing to have high heat conductivity, insulation, low thermal expansivity and good a series of good characteristics such as chemical stability, applicablely again is structured material (as being used for the member that high temperature and/or corrosive atmosphere use).Aluminium nitride ceramics has become one of research focus of modern field of new.
Aluminium nitride powder is the raw material of preparation aluminium nitride ceramics, and the sintering of stupalith and thermal conductivity depend on the purity of aluminium nitride powder and the granularity and the pattern of powder.
At present, the PREPARATION OF ALUMINUM NITRIDE POWDER method mainly contains following several:
1, the metallic aluminium powder heats the method for nitrogenize in nitrogen and/or ammonia.Because the reaction of the direct nitrogenize of aluminium powder is a strong exothermal reaction, reaction process is wayward, a large amount of heats of emitting easily make aluminium formation melting piece, hinder the diffusion of nitrogen, cause reaction not exclusively, reaction product often needs pulverization process, unavoidably can bring impurity into, so this method is difficult to synthesis of high purity, fine-grained product.
2, the method for volatility aluminum compound and nitrogen and/or ammonia nitrogenize in gas phase.Though this method can be produced the high quality aluminium nitride powder, the raw materials cost height, and can't form large-scale production, still can not be widely used at present.
3, the method for the mixture of alumina powder and carbon dust reacting by heating in nitrogen and/or ammonia.This method can be passed through controlled oxidation aluminium and the quality synthesizing fine-granularity of carbon dust and the aluminium nitride powder of even particle size distribution, but because the difference of aluminum oxide and carbon black polarity and proportion, raw material is difficult to mix; Because the aluminum oxide reactive behavior is relatively poor, needing at high temperature usually, (usually above 1600 ℃) long-time (usually greater than 3h) just can finish building-up reactions in addition.
Prepare Al by chemical process
2O
3+ C mixture can improve aluminum oxide and carbon dust and be difficult to the blended shortcoming, and it is more even to make that raw mix mixes, and can reduce the granularity of raw material simultaneously, makes two kinds of direct contact reactss of subparticle, thereby improves reactive behavior, reduces temperature of reaction.In addition, by the granularity of aluminium source and carbon source in the change raw material, might prepare ultra-fine even nano level aluminium nitride powder, thereby improve the sintering character of pottery.
United States Patent (USP) NO.4,643,859 adopt chemical process to prepare Al
2O
3+ C mixture is dispersed in carbon dust in a kind of suspension of alcohol in advance, and hydrolysis is also carried out with ammonia precipitation aluminium alcoholates salt then.
Summary of the invention
The object of the present invention is to provide a kind of method that adopts the synthetic precursor of low-temperature burning to prepare aluminium nitride powder.Simplified and produced Al
2O
3The technology of+C mixture.
The present invention is the aluminium source with the inorganic aluminate aluminum nitrate, and water soluble organic substances such as glucose, sucrose, citric acid, Zulkovsky starch are carbon source, and adds amount of urea, and key step is as follows:
1, with the water-soluble mixing solutions that is mixed with of aluminum nitrate, urea and water-soluble organic carbon source;
2, with the temperature range internal heating drying of above-mentioned solution, and constantly stir, obtain a kind of fluffy powder after reacting in the solution, as precursor mixture at 100～400 ℃;
3, in 1200～1600 ℃ temperature range step 2 synthetic precursor is carried out reduction nitridation reaction in the flowing nitrogen atmosphere of 1～10L/h, the time is 1～24 hour;
4, in oxygen-containing atmosphere, the reduction nitridation reaction product was calcined in 600～700 ℃ temperature range 1～7 hour, remove carbon unnecessary in the reaction product, obtain aluminium nitride powder.
The aluminium source of being adopted is the inorganic aluminate aluminum nitrate, and the carbon source that is adopted is water soluble organic substances such as glucose, sucrose, citric acid, Zulkovsky starch, therefore, can utilize liquid phase with aluminium source and carbon source uniform mixing on molecular level.
The adding of urea is necessary, and the proportioning of urea and aluminum nitrate has material impact to reaction, and the proportioning of urea and aluminum nitrate is 0.5～2.5 mol ratio, and best proportioning is 0.5～1.5 mol ratio.
The proportioning of aluminium source and carbon source has considerable influence to the performance of speed of response and synthetic powder in the raw material, and aluminium source and carbon source are 4/1～14/1 batching by the C/Al atomic ratio in the raw material, and best proportioning is 6/1～10/1.
The drying temperature scope of the mixing solutions of raw material is 100 ℃～400 ℃.
The invention has the advantages that: the technology of synthetic precursor is simple and direct, convenient, can in several minutes, finish, adopting the synthetic precursor is that raw material carries out reduction-nitridation, not only can realize complete nitrogenize under the lesser temps between 1400～1550 ℃ and within 3 hours, and can prepare high purity, ultra-fine granularity even nano level aluminium nitride powder.
Embodiment
Take by weighing 75g aluminum nitrate and 12g urea and place the beaker of 1000ml, add water 100ml, slowly heating and constantly stirring is till obtaining colourless transparent solution.Is that 16/2 amount is dissolved in the above-mentioned solution with glucose by the C/Al atomic ratio.
To adopt the solution of aforesaid method preparation to place on the temperature controllable electric furnace, under 200 ℃ temperature, heat while stirring, after being heated to certain phase, can observe bubbling takes place in the solution, smolder, a series of phenomenons such as burning, obtain a kind of very fluffy powder at last, as precursor, its weight is 26g.
The resulting powder of 10g is placed plumbago crucible, in 1500 ℃ stove, be incubated 3 hours then.During heating, keeping nitrogen flow in the reaction chamber is 4L/h.
In air, under 600～700 ℃, superfluous carbon was removed in the powder oxidation that nitrogenizing reaction generated in 2 hours.
The X-ray diffraction analytical results shows that the gained powder is an aluminium nitride, and chemical analysis shows that the nitrogen content of this product is 32.56%, and oxygen level is 1.69%, and the specific surface area of measuring powder is 17.4m
2/ g utilizes scanning electron microscope (SEM) to observe aluminium nitride powder, finds that the synthetic aluminium nitride powder is the spheroidal particle of regular shape, the even particle size distribution of powder, and mean particle size is about 0.1m, the particle of not growing up unusually, particles dispersed is good.
Table 1 is listed the different material material phase analysis result of reaction product at various temperatures
According to C/Al atomic ratio 3/1 respectively with α-Al
2O
3, aluminium hydroxide and specific surface area be 126m
2The carbon black wet ball grinding of/g 4 hours, mixed evenly back be as raw material, and and last routine synthetic precursor between 1200～1700 ℃, reacted respectively 3 hours respectively, nitrogen flow is identical with last example.Utilize X-ray diffraction to analyze the crystalline phase of reaction product under the differing temps, the result is as follows:
Table 1 different material is the material phase analysis temperature oc-Al as a result of reaction product at various temperatures
2O
31200 ℃ of α-Al of aluminium hydroxide prepared precursor of the present invention
2O
3Incomplete α-the Al of crystallization
2O
3γ-Al
2O
31300 ℃ of α-Al
2O
3AlN, α-Al
2O
3AlN, γ-Al
2O
31400 ℃ of AlN, α-Al
2O
3AlN, α-Al
2O
3AlN1500 ℃ of AlN, α-Al
2O
3AlN, α-Al
2O
3AlN1600 ℃ of AlN, α-Al
2O
3AlN AlN1700 ℃ of AlN AlN AlN
Table 2 is listed urea and aluminum nitrate proportioning to effects of phase transition in the precursor nitrogenizing reaction process.
Fixedly the C/Al atomic ratio is 16/2 constant in the raw material, the proportioning that changes urea and aluminum nitrate is respectively 0 (not adding urea), 0.5,1,1.5,2.5, adopt prepared precursor of the present invention, the various precursors of being prepared were reacted respectively between 1200～1600 ℃ 3 hours, nitrogen flow is identical with more preceding example, utilizes X-ray diffraction to analyze the crystalline phase of reaction product under the differing temps, and the result is as follows:
Table 2 urea and aluminum nitrate proportioning are to 1200 ℃ 1300 ℃ 1400 ℃ 1500 ℃ 1600 ℃ of effects of phase transition proportionings in the precursor nitrogenizing reaction process
γ-Al
2O
3
γ-Al
2O
3 α-Al
2O
3 α-Al
2O
3 α-Al
2O
30 α-Al
2O
3 AlON AlON AlON AlN
AlON AlN AlN AlN
γ-Al
2O
3
γ-Al
2O
3 α-Al
2O
3 AlON AlN AlN
α-Al
2O
3 AlON AlN
AlON AlN
γ-Al
2O
31 γ-Al
2O
3 AlN AlN AlN AlN
γ-Al
2O
32 γ-Al
2O
3 AlN AlN AlN AlN2.5 γ-Al
2O
3 γ-Al
2O
3 AlN AlN AlN
AIN
At 1500 ℃ of reaction 3h, with measurement the specific area after the various reaction product process carbonization treatment of gained, table 3 is a measurement result with various precursors:
Table 3 urea and aluminum nitrate proportioning influence urea and aluminum nitrate proportioning 0 0.5 1 1.5 2.5 specific surface area (m to the reaction product specific surface area
2/ g) 1.17 23.63 17.40 18.56 23.94
Scanning electron microscope (SEM) analytical results shows, the precursor synthetic aluminium nitride powder that does not add urea is block hard agglomeration, and the various precursor synthetic aluminium nitride powders behind the interpolation urea are the spheroidal particle of regular shape, even particle size distribution, powder mean particle sizes is less than 0.2 μ m, and different along with urea and aluminum nitrate proportioning, and powder size is chap at first gradually, in proportioning is to reach maximum value at 1 o'clock, reduces gradually again subsequently.After urea and aluminum nitrate proportioning are greater than 2.5, though phase transformation in the synthetic precursor nitrogenizing reaction process and speed of reaction change little, but the specific surface area of synthetic aluminium nitride powder is excessive, powder surface oxygen impurities content raises, can influence the heat conductivility of the pottery prepared of subsequent technique, so bad.
Table 4 is listed the phase transformation in the different carbon source synthetic precursor nitrogenizing reaction processes.
The proportioning of urea and aluminum nitrate is 1/1 in the raw material, by the C/Al atomic ratio is 16/2 to be that carbon source is prepared burden with sucrose, Zulkovsky starch, citric acid and carbon black respectively, and the synthetic various precursors of the technology of utilizing embodiment of the present invention, the synthetic precursor reacted respectively between 1200～1600 ℃ 3 hours, and nitrogen flow is identical with more preceding example.Utilize X-ray diffraction to analyze the crystalline phase of reaction product under the differing temps, table 4 is an experimental result:
Utilize scanning electron microscope (SEM) to observe various precursor synthetic aluminium nitride powders, when discovery is carbon source with water soluble organic substances such as sucrose, Zulkovsky starch, citric acids, the synthetic aluminium nitride powder is the spheroidal particle of regular shape, the even particle size distribution of various aluminium nitride powders, mean particle size is between 0.1～0.2 μ m, the particle of not growing up unusually, and be raw material synthetic aluminium nitride powder with aluminum nitrate and carbon black, grain graininess is thicker, size-grade distribution is inhomogeneous, can observe the particle of growing up unusually in the powder.
1200 ℃ of 1300 ℃ of 1400 ℃ of 1500 ℃ of 1600 ℃ of sucrose γ-Al of phase transformation carbon source in the different carbon source synthetic of the table 4 precursor nitrogenizing reaction process
2O
3γ-Al
2O
3AlN AlN AlN
AlN Zulkovsky starch γ-Al
2O
3γ-Al
2O
3AlN AlN AlN
γ-Al
2O
3 γ-Al
2O
3 AlN AlN AlN
AlN carbon black α-Al
2O
3α-Al
2O
3α-Al
2O
3AlN AlN
AlN AlN
The performance of the various precursor nitrogenizing reaction of synthetic product when table 5 is listed different C/Al atomic ratio.
With aluminum nitrate, glucose and urea is raw material, the proportioning of urea and aluminum nitrate is 1/1 in the control raw material, the atomic ratio that changes C/Al in the raw material is respectively 4/1,6/1,8/1,10/1,12/1, utilize the synthetic various precursors of invention, the various precursors of being prepared were reacted respectively 3 hours at 1500 ℃, nitrogen flow is identical with more preceding example, after reaction finishes, after the various reaction product process carbonization treatment with gained, utilize the nitrogen content and the oxygen level of chemical gauging powder, utilize the BET method to measure the specific surface area of powder, analytical results is as follows:
Performance C/Al atomic ratio 4/1 6/1 8/1 1,0/1 12/1 nitrogen contents (%) 28.25 32.59 32.56 32.21 31.69 oxygen levels (%) the 5.78 1.67 1.69 1.98 2.66 specific surface area (m of the various precursor nitrogenizing reaction of synthetic product during the different C/Al atomic ratio of table 5
2/ g) 6.65 13.43 17.40 21.04 25.68
Utilize scanning electron microscope (SEM) to observe various precursor synthetic aluminium nitride powders, find that various precursor synthetic aluminium nitride powders are the spheroidal particle of regular shape, even particle size distribution is along with the increase of C/Al atomic ratio, the dispersiveness of powder particle increases, the powder particle particle size reduction.Continuing increases the C/Al atomic ratio, and speed of reaction slows down, and the surface oxygen content of synthetic powder increases, therefore bad.
Claims (2)
1, the synthetic precursor of a kind of low-temperature burning prepares the method for aluminium nitride powder, is the aluminium source with the inorganic aluminate aluminum nitrate, and water soluble organic substances such as glucose, sucrose, citric acid, Zulkovsky starch are carbon source, and adds urea; It is characterized in that: the technological process of preparation is:
A, with the water-soluble mixing solutions that is mixed with of aluminum nitrate, urea and water-soluble organic carbon source, the proportioning of urea and aluminum nitrate is 0.5～2.5 mol ratio, the C/Al atomic ratio is 4/1～14/1;
B, with the temperature range internal heating drying of above-mentioned solution at 100～400 ℃, and constantly stir, obtain a kind of fluffy powder after reacting in the solution, as precursor mixture;
C, in 1200～1600 ℃ temperature range precursor mixture is carried out reduction nitridation reaction in flowing nitrogen atmosphere, the time is 1～24 hour;
E, in oxygen-containing atmosphere, the reduction nitridation reaction product was calcined in 600～700 ℃ temperature range 1～7 hour, remove carbon unnecessary in the reaction product, obtain aluminium nitride powder.
2, prepare the method for aluminium nitride powder according to the synthetic precursor of the described low-temperature burning of claim 1, it is characterized in that: the best proportioning of urea and aluminum nitrate is 0.5～1.5 mol ratio; The best proportioning of C/Al atom is 6/1～10/1.
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| CN112897481A (en) * | 2020-12-30 | 2021-06-04 | 河北利福光电技术有限公司 | Aluminum nitride powder and preparation method thereof |
| CN114716250A (en) * | 2021-01-06 | 2022-07-08 | 中国科学院福建物质结构研究所 | Preparation method of AlON powder |
| CN113135759A (en) * | 2021-04-23 | 2021-07-20 | 北京科技大学 | Method for preparing high-purity high-light-transmittance AlON ceramic by solution combustion synthesis method |
| CN114314531A (en) * | 2022-01-04 | 2022-04-12 | 华东理工大学 | Method for preparing nano aluminum nitride powder by sol-gel foaming |
| CN116082043A (en) * | 2023-02-28 | 2023-05-09 | 福建华清电子材料科技有限公司 | Continuous preparation method for aluminum nitride powder by sintering |
| CN116082043B (en) * | 2023-02-28 | 2023-09-22 | 福建华清电子材料科技有限公司 | Continuous preparation method for aluminum nitride powder by sintering |
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