CN101113095A - Synthetic preparation method of A1N ceramic powder - Google Patents
Synthetic preparation method of A1N ceramic powder Download PDFInfo
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- CN101113095A CN101113095A CNA2007100845224A CN200710084522A CN101113095A CN 101113095 A CN101113095 A CN 101113095A CN A2007100845224 A CNA2007100845224 A CN A2007100845224A CN 200710084522 A CN200710084522 A CN 200710084522A CN 101113095 A CN101113095 A CN 101113095A
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Abstract
The invention pertains to a field of ceramic material, and particularly relates to a synthesis preparation method of AIN ceramic powder. The producing method is listed as following: the producing of aluminum ammonia carbonate gel; wet mixing the batch; the producing of powder block, and the nitriding of reaction synthesis under high temperature. The aluminum ammonia carbonate gel is made of Al(NO3) 3.9H2O and (NH4)2CO3. Through wet mixing, Al (NO3) 3.9H2O and (NH4) 2CO3 are mixed with carbon and additive, and then the mixture is dried to obtain powder block A. Through wet mixing, nanometer Al (OH) 3 or nanometer Al2O3 is mixed with carbon and the mixture then is dried to obtain powder block B. Powder AIN is made by carbon-thermal reduction and nitridating reaction to the powder A or the powder B in nitrogen under high temperature. Temperature needed in the synthesis reaction is 1400-1600 DEG C. Heat preservation time needed is 2-6 hours. The purity of the obtained AIN is more than 60 percent of AIN ceramic powder. The invention is the preparation method for ceramic powder AIN by adopting nanometer particle synthesis.
Description
[technical field]
The invention belongs to the stupalith field, be specifically related to a kind of synthesis and preparation process method of AlN ceramic powder.
[background technology]
Because the AlN pottery has good performances such as high temperature resistant, anticorrosive, high heat conductance, low thermal coefficient of expansion, heat shock resistance, simultaneously very high electrical insulating property is arranged again, thereby become integrated circuit substrate material, the packaged material of electronic component and the novel high-heat resistance shock resistant ceramic structure material of withstand high temperatures of the excellence that development in recent years gets up.
The key of preparation AlN pottery is synthetic AlN content height, the aluminium nitride powder material that crystallization property is good prepared, and the method for synthetic AlN mainly contains at present: direct nitridation method, carbothermic method, arc melting method, gas-phase reaction method, gas ions method, cracking process, microwave process for synthesizing, self propagating high temperature synthesis method and high-energy ball milling method etc.Wherein, the method that can realize suitability for industrialized production mainly contains direct nitridation method and carbothermic method.
Direct nitridation method is to be raw material with the aluminium powder, at high temperature feeds nitrogen, and directly chemical combination generates the AlN method, and temperature of reaction is generally 800-1200 ℃.Because nitrogenizing reaction is strong thermopositive reaction, reaction process is difficult to control, unstable product quality, and the AlN powder that makes often has from sintering phenomenon, and the AlN layer that forms of aluminium powder nitrided surface can hinder the carrying out of reaction, needs just can react completely for a long time.Prepare the AlN powder with direct nitridation method, for obtaining highly purified AlN, just need to use highly purified raw material, corresponding cost also just increases, and this is the principal element that the restriction direct nitridation method is promoted.
Carbothermic method is the method that the AlN powder is produced in another commercialization.Usually it is with α-Al
2O
3Or γ-Al
2O
3Mix with carbon black, generally need 1600-1800 ℃ of insulation 12h to synthesize preparation AlN powder under the condition of nitrogen gas.This method can make the size homogeneous and almost not have the AlN powder of reuniting.But, adopt α-Al
2O
3Or γ-Al
2O
3The synthetic preparation of carbothermic method AlN powder needs higher temperature of reaction and soaking time.
At the deficiency of above-mentioned direct nitridation method or the synthetic preparation of carbothermic method AlN powder, problem demanding prompt solution is to make the building-up process of AlN stablize and reduce synthetic preparation temperature and reduce soaking time.Principal character of the present invention is to be used for synthetic AlN ceramic powder with lower synthesis temperature and less soaking time.
[summary of the invention]
The objective of the invention is provides a kind of synthesis preparation method of AlN ceramic powder in order to overcome deficiency of the prior art.
Technical scheme of the present invention:
A kind of synthesis preparation method of AlN ceramic powder is characterized in that may further comprise the steps: the preparation of aluminium carbonate ammonia gel, admixtion wet-mixed, the preparation of powder material piece and high-temperature ammonolysis reaction are synthetic.
The preparation of aluminium carbonate ammonia gel is with analytical pure Al (NO
3)
39H
2O and (NH
4)
2CO
3Being mixed with concentration respectively with deionized water is 0.5mol.L
-1And 2.5mol.L
-1Solution; Under (35 ± 4) ℃ constant temperature and continuous agitation condition, by (NH
4)
2CO
3: Al (NO
3)
3The ratio of=2.5: 1 molar weight is with Al (NO
3)
3Solution at the uniform velocity is added drop-wise to (NH
4)
2CO
3In the solution; After dropwising, continue to stir 30min, use deionized water wash again 3 times, can make aluminium carbonate ammonium (NH
4AlO (OH) HCO
3) gel.
One of admixtion wet-mixed method is that the aluminium carbonate ammonium gel adding proper amount of deionized water that will make is diluted, and makes aluminium carbonate ammonium gel diluted slurry; Then carbon materials and additive are joined in the aluminium carbonate ammonia gel diluted slurry and carry out wet-mixed, mixing time 1～3h obtains mixed slurry A; The grain of carbon materials and additive is through equal＜5 μ m; Carbon materials is carbon black or coke or graphite, and the add-on of carbon materials is the 100-120% of aluminium carbonate ammonium molar weight; Additive is SrCO
3Or CaF
2-SrCO
3Or CaF
2, the add-on of additive is the 2.5-3.5% of aluminium carbonate ammonium weight.
Two of admixtion wet-mixed method is with nanometer Al (OH)
3Or nanometer Al
2O
3Carry out wet-mixed with the admixtion of carbon materials, mixing time 1～3h obtains mixed slurry B; Carbon materials is carbon black or coke or graphite, the carbon materials particle diameter all＜5 μ m; Nanometer Al (OH)
3Or nanometer Al
2O
3Particle diameter all＜0.1 μ m, nanometer Al (OH)
3Add-on be the 75-80% of carbon materials molar weight, nanometer Al
2O
3Add-on be the 145-160% of carbon materials molar weight.
The preparation of material piece is that above-mentioned mixed slurry A or mixed slurry B are placed dry 24h under 110 ℃ of conditions respectively, obtains to be used for powder material piece A or the powder material piece B of synthetic AlN.
The high temperature that above-mentioned powder material piece A or powder material piece B is carried out the AlN powder respectively is synthetic, and the atmosphere of the synthetic AlN powder of pyrocarbon thermal reduction and nitrogenizing reaction is nitrogen atmosphere, and synthesis temperature is controlled to be 1400-1600 ℃, and soaking time is 2h-6h.
Major technique feature of the present invention is to adopt nano material technology to be used for the synthetic of AlN powder, and the synthetic raw materials used technical requirements of AlN powder of the present invention is shown in table 1, and the physicals detected result of synthetic AlN powder is shown in table 2.The microstructure of AlN powder and thing are shown in accompanying drawing 1 and accompanying drawing 2 mutually respectively.By table 1, table 2, accompanying drawing 1, accompanying drawing 2 and embodiment as can be known, the present invention is a kind of preparation method who adopts the synthetic AlN powder of nano particle technology to have practicality.
Table 1 synthesizes the raw materials used technical requirements of AlN powder
| Material name | Chemical constitution | Specification |
| Aluminum nitrate carbonic acid ammonia aluminium hydroxide alumina carbon black stone China ink coke Strontium carbonate powder Calcium Fluoride (Fluorspan) | Al(NO 3) 3·9H 2O＞99％ (NH 4) 2CO 3＞99％ Al(OH) 3＞99％ Al 2O 3＞99％ C＞99％ C＞98％ C＞95％ SrCO 3＞99％ CaF 2＞99％ | ＜5μm ＜5μm ＜0.1μm ＜0.1μm ＜5μm ＜5μm ＜5μm ＜5μm ＜5μm |
The physicals detected result of the synthetic AlN powder of table 2
| Sample | The aluminium source | Carbon source | Additive | Temperature/℃ | True density g/cm 3 | AlN content % |
| AN-1 AN-2 AN-3 AN-4 AN-5 | NH 4AlO(OH)HCO 3 Al 2O 3 NH 4AlO(OH)HCO 3 Al 2O 3 Al(OH) 3 | Carbon black carbon black graphite coke graphite | SrCO 3 SrCO 3 CaF 2 CaF 2、SrCO 3 CaF 2 | 1500 1600 1500 1600 1600 | 3.38 3.52 3.42 3.47 3.36 | 75.3 51.2 69.5 66.1 75.2 |
[description of drawings]
Fig. 1 is the AlN crystallization shape SEM photo of AN-1 powder sample of the present invention
Fig. 2 is the XRD graphic representation of AN-1 powder sample thing phase of the present invention
[embodiment]
With analytical pure Al (NO
3)
39H
2O and (NH
4)
2CO
3Being mixed with concentration respectively with deionized water is 0.5mol.L
-1And 2.5mol.L
-1Solution; Under (35 ± 4) ℃ constant temperature and continuous agitation condition, by (NH
4)
2CO
3: Al (NO
3)
3The ratio of=2.5: 1 molar weight is with Al (NO
3)
3Solution at the uniform velocity is added drop-wise to (NH
4)
2CO
3In the solution; After dropwising, continue to stir 30min, use deionized water wash again 3 times, obtain aluminium carbonate ammonium (NH
4AlO (OH) HCO
3) gel.
Aluminium carbonate ammonium gel is added proper amount of deionized water dilute, add the carbon black of the particle diameter＜5 μ m that press aluminium carbonate ammonium molar weight 100% and the SrCO that presses the particle diameter＜5 μ m of aluminium carbonate ammonium weight 3.0% then
3Wet method mixes 1h, obtains mixed slurry; Mixed slurry is placed dry 24h under 110 ℃ of conditions, obtain to be used for the powder material piece of synthetic AlN; With the synthetic AlN of powder material piece high temperature under nitrogen atmosphere, synthesis temperature is 1500 ℃, and soaking time is 5h.
AlN content in the synthetic AlN powder of present embodiment is 75.3%
With analytical pure Al (NO
3)
39H
2O and (NH
4)
2CO
3Being mixed with concentration respectively with deionized water is 0.5mol.L
-1And 2.5mol.L
-1Solution; Under (35 ± 4) ℃ constant temperature and continuous agitation condition, by (NH
4)
2CO
3: Al (NO
3)
3The ratio of=2.5: 1 molar weight is with Al (NO
3)
3Solution at the uniform velocity is added drop-wise to (NH
4)
2CO
3In the solution; After dropwising, continue to stir 30min, use deionized water wash again 3 times, obtain aluminium carbonate ammonium (NH
4AlO (OH) HCO
3) gel.
Aluminium carbonate ammonium gel is added proper amount of deionized water dilute, add the graphite of the particle diameter＜5 μ m that press aluminium carbonate ammonium molar weight 120% and the CaF that presses the particle diameter＜5 μ m of aluminium carbonate ammonium weight 3.0% then
2Wet method mixes 2h, obtains mixed slurry; Mixed slurry is placed dry 24h under 110 ℃ of conditions, obtain to be used for the powder material piece of synthetic AlN; With the synthetic AlN of powder material piece high temperature under nitrogen atmosphere, synthesis temperature is 1500 ℃, and soaking time is 6h.
AlN content in the synthetic AlN powder of present embodiment is 69.5%
Embodiment 3
With particle diameter＜coke of 5 μ m, the Al of particle diameter＜70nm
2O
3The SrCO of (add-on be coke molar weight 150%), particle diameter＜5 μ m
3(add-on is Al
2O
3Weight 1.0%) and the CaF of particle diameter＜5 μ m
2(add-on is Al
2O
3Weight 2.0%) wet-mixed, mixing time 3h obtains mixed slurry; Mixed slurry is placed dry 24h under 110 ℃ of conditions, obtain to be used for the powder material piece of synthetic AlN; With the synthetic AlN of powder material piece high temperature under nitrogen atmosphere, synthesis temperature is 1600 ℃, and soaking time is 6h.
AlN content in the synthetic AlN powder of present embodiment is 66.1%
Claims (10)
1. the synthesis preparation method of an AlN ceramic powder is characterized in that may further comprise the steps: the preparation of aluminium carbonate ammonia gel, admixtion wet-mixed, the preparation of powder material piece and high-temperature ammonolysis reaction are synthetic.
2. material preparation method as claimed in claim 1 is characterized in that the (NO with analytical pure Al
3)
39H
2O and (NH
4)
2CO
3Being mixed with concentration respectively with deionized water is 0.5mol.L
-1And 2.5mol.L
-1Solution; Under (35 ± 4) ℃ constant temperature and continuous agitation condition, by (NH
4)
2CO
3: Al (NO
3)
3The ratio of=2.5: 1 molar weight is with Al (NO
3)
3Solution at the uniform velocity is added drop-wise to (NH
4)
2CO
3In the solution; After dropwising, continue to stir 30min, use deionized water wash again 3 times, can make aluminium carbonate ammonium (NH
4AlO (OH) HCO
3) gel.
3. material preparation method as claimed in claim 1 is characterized in that the aluminium carbonate ammonium gel that will make adds proper amount of deionized water and dilutes, and makes aluminium carbonate ammonium gel diluted slurry; Then carbon materials and additive are joined in the aluminium carbonate ammonia gel diluted slurry and carry out wet-mixed, mixing time 1～3h obtains mixed slurry A.
4. as carbon materials and additive in the mixed slurry preparation as described in the claim 3, the grain that it is characterized in that carbon materials and additive is through equal＜5 μ m, the add-on of carbon materials is the 100-120% of aluminium carbonate ammonium molar weight, and the add-on of additive is the 2.5-3.5% of aluminium carbonate ammonium weight.
5. material preparation method as claimed in claim 1 is characterized in that with nanometer Al (OH)
3Or nanometer Al
2O
3Carry out wet-mixed with the admixtion of carbon materials, mixing time 1～3h obtains mixed slurry B.
6. as carbon materials and additive in the mixed slurry preparation as described in the claim 3, it is characterized in that carbon materials is carbon black or coke or graphite, additive is SrCO
3Or CaF
2-SrCO
3Or CaF
2
7. as carbon materials and nanometer Al (OH) in the mixed slurry preparation as described in the claim 5
3Or nanometer Al
2O
3, it is characterized in that carbon materials is carbon black or coke or graphite, the carbon materials particle diameter all＜5 μ m; Nanometer Al (OH)
3Or nanometer Al
2O
3Particle diameter all＜0.1 μ m; Nanometer Al (OH)
3Add-on be the 75-80% of carbon materials molar weight, nanometer Al
2O
3Add-on be the 145-160% of carbon materials molar weight.
8. material preparation method as claimed in claim 1 is characterized in that described mixed slurry A of claim 3 or the described mixed slurry B of claim 5 are placed dry 24h under 110 ℃ of conditions respectively, obtains to be used for powder material piece A or the powder material piece B of synthetic AlN.
9. material preparation method as claimed in claim 1 is characterized in that the atmosphere of the synthetic AlN powder of pyrocarbon thermal reduction and nitrogenizing reaction is nitrogen atmosphere.
10. material preparation method as claimed in claim 1 is characterized in that the temperature of synthetic AlN powder is controlled to be 1400-1600 ℃, and soaking time is 2h-6h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100845224A CN100457684C (en) | 2007-02-12 | 2007-02-12 | Synthetic preparation method of A1N ceramic powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100845224A CN100457684C (en) | 2007-02-12 | 2007-02-12 | Synthetic preparation method of A1N ceramic powder |
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| Publication Number | Publication Date |
|---|---|
| CN101113095A true CN101113095A (en) | 2008-01-30 |
| CN100457684C CN100457684C (en) | 2009-02-04 |
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ID=39021652
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100845224A Expired - Fee Related CN100457684C (en) | 2007-02-12 | 2007-02-12 | Synthetic preparation method of A1N ceramic powder |
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| Country | Link |
|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107840668A (en) * | 2017-10-29 | 2018-03-27 | 贵州喜文化艺术有限责任公司 | A kind of ceramic composition and preparation method thereof |
| CN110015900A (en) * | 2019-02-22 | 2019-07-16 | 福建臻璟新材料科技有限公司 | Composite Nano aluminium nitride powder and preparation method thereof with low-temperature sintering performance |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4988646A (en) * | 1988-05-12 | 1991-01-29 | International Business Machines | Method for producing a ceramic |
| US5279808A (en) * | 1992-12-17 | 1994-01-18 | United Technologies Corporation | Metal nitride powders |
-
2007
- 2007-02-12 CN CNB2007100845224A patent/CN100457684C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107840668A (en) * | 2017-10-29 | 2018-03-27 | 贵州喜文化艺术有限责任公司 | A kind of ceramic composition and preparation method thereof |
| CN110015900A (en) * | 2019-02-22 | 2019-07-16 | 福建臻璟新材料科技有限公司 | Composite Nano aluminium nitride powder and preparation method thereof with low-temperature sintering performance |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100457684C (en) | 2009-02-04 |
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Inventor after: Bo Jinglong Inventor after: Wang Ronglin Inventor after: Wang Zhifa Inventor after: Jia Cui Inventor after: Hu Chunfang Inventor after: Zhang Jian Inventor after: Wang Xibei Inventor before: Bo Jinglong Inventor before: Wang Ronglin Inventor before: Wang Zhifa Inventor before: Jia Cui Inventor before: Hu Chunfang Inventor before: Zhang Jian |
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| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: BU JINGLONG WANG RONGLIN WANG ZHIFA JIA CUI HU CHUNFANG ZHANG JIAN TO: BU JINGLONG WANG RONGLIN WANG ZHIFA JIA CUI HU CHUNFANG ZHANG JIAN WANG XIBEI |
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Granted publication date: 20090204 Termination date: 20120212 |