CN102502539A - Method for preparing yttrium-doped nano aluminum nitride powder - Google Patents
Method for preparing yttrium-doped nano aluminum nitride powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 62
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title abstract description 19
- 238000000034 method Methods 0.000 title abstract description 19
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 46
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 27
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- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 5
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- 239000005720 sucrose Substances 0.000 claims description 5
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 4
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- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical compound [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 claims description 4
- DUSUCKWNBGMKRV-UHFFFAOYSA-N acetic acid;yttrium Chemical compound [Y].CC(O)=O DUSUCKWNBGMKRV-UHFFFAOYSA-N 0.000 claims description 3
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 claims description 2
- 238000005261 decarburization Methods 0.000 claims description 2
- 229920000609 methyl cellulose Polymers 0.000 claims description 2
- 239000001923 methylcellulose Substances 0.000 claims description 2
- NREVZTYRXVBFAQ-UHFFFAOYSA-N propan-2-ol;yttrium Chemical compound [Y].CC(C)O.CC(C)O.CC(C)O NREVZTYRXVBFAQ-UHFFFAOYSA-N 0.000 claims description 2
- PCMOZDDGXKIOLL-UHFFFAOYSA-K yttrium chloride Chemical compound [Cl-].[Cl-].[Cl-].[Y+3] PCMOZDDGXKIOLL-UHFFFAOYSA-K 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 34
- 239000000919 ceramic Substances 0.000 abstract description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
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- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
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- 230000000536 complexating effect Effects 0.000 abstract description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 abstract 6
- 239000011259 mixed solution Substances 0.000 abstract 2
- 238000000227 grinding Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
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- -1 yttrium ions Chemical class 0.000 abstract 1
- 238000005303 weighing Methods 0.000 description 12
- PSNPEOOEWZZFPJ-UHFFFAOYSA-N alumane;yttrium Chemical compound [AlH3].[Y] PSNPEOOEWZZFPJ-UHFFFAOYSA-N 0.000 description 9
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- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical class [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical class [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for preparing yttrium-doped nano aluminum nitride powder. The method comprises the following steps of: dissolving an aluminum source, a carbon source and an yttrium source into a solvent, and then mixing the solvent and an ethylene glycol solution of citric acid; and preserving the heat of the mixed solution for 2 to 4 hours at the temperature of between 125 and 135 DEG C, continuously heating the mixed solution to the temperature of between 180 and 220 DEG C, preserving the heat for 2 to 4 hours, calcining the obtained substance at the temperature of between 800 and 1,200 DEG C in vacuum or nitrogen, cooling, grinding, performing carbothermic reduction reaction at the temperature of between 1,450 and 1,550 DEG C, and thus obtaining the yttrium-doped nano aluminum nitride powder. By using the complexing effect of the citric acid and the steric hindrance effect of the ethylene glycol, the aluminum and yttrium ions are uniformly distributed in the carbon source, and the yttrium-doped nano aluminum nitride powder with small particle diameter and uniform components is finally obtained; and the yttrium-doped nano aluminum nitride powder can effectively reduce the sintering temperature of aluminum nitride ceramic and improve the heat conductivity of the aluminum nitride ceramic, and has an important application prospect in electronic substrates and power devices.
Description
Technical field
The present invention relates to a kind of yttrium that adds and prepare the method for nano aluminum nitride powder, belong to materials science field as auxiliary agent.
Background technology
Characteristics such as the linear expansivity that aluminium nitride ceramics (AlN) has high thermal conductivity, be complementary with silicon, low specific inductivity, excellent electric insulation performance, corrosion-resistant and environment-protecting asepsis; Instead of alumina and beryllium oxide become the preferred material of present VLSI substrate, and high-technology field such as electronics and microelectronics has obtained using widely in modern times.But because aluminium nitride AlN belongs to covalent compound, self-diffusion coefficient is little, causes being difficult to densified sintering product, even if sintering does not reach 90% of theoretical density yet under the high temperature more than 1900 ℃, the aluminium nitride ceramics thermal conductivity that obtains simultaneously is also far below theoretical value.For under relatively low temperature, realizing the dense sintering of stupalith; Thereby improve its thermal conductivity; Researcher is mainly realized through following two approach both at home and abroad at present: one is to select suitable sintering aid; Utilize the fusing of sintering aid in sintering process, perhaps sintering aid and ceramic matrix react the generation eutectic mixture at low temperatures, promote the densification of pottery again with the form of liquid phase sintering; Another kind is through the synthesis of nano ceramic powder, utilizes the high-ratio surface of nano-powder can promote ceramic densification process.
On the aluminium nitride ceramics sintering aid was selected, the oxide compound of rare earth metal and earth alkali metal and fluorochemical were the sintering aids of using always.Like " J. Eur. Ceram. Soc., 2002,22:1051-1053 " such as Terao with La
2O
3As sintering aid, be 3.27 g/cm 1850 ℃ of normal pressure-sintered density that obtain of insulation 2 h
-3Aluminium nitride ceramics, its thermal conductivity is 101 W/ (mK); Eirik etc. " J. Am. Ceram. Soc., 2002,85 (12): 2971-2976 " utilize CaO and Al
2O
3Product C a
12Al
14O
33As sintering aid, can the densification temperature of aluminium nitride ceramics be reduced to 1650-1750 ℃; Qiao Liang etc. " material engineering, 2003,1:10-13 " are with CaF
2-YF
3As sintering aid, be incubated the aluminium nitride ceramics that 4 h obtain dense structure at 1750 ℃, its thermal conductivity is 172 W/ (mK).With respect to other sintering aid, Y
2O
3Because advantage such as have that the oxygen of driving ability is strong, good stability and products obtained therefrom performance are good, become aluminium nitride ceramics the most frequently used also be one of the most effective sintering aid.Like " Powder Techn., 2005,159:155-157 " such as Hiroya with Y
2O
3As sintering aid, at 1800 ℃ of insulation 3 h, aluminium nitride ceramics promptly obtains theoretical sintered density, and thermal conductivity is 169 W/ (mK); Hirano etc. " J. Mater. Sci., 1993,28 (17): 4725-4730 " are incubated 8 h to the AlN powder at 1900 ℃ when not adding any sintering aid, the thermal conductivity that sintering obtains the AlN pottery is merely 114 W/ (mK), and adopts 4% Y
2O
3As sintering aid, the thermal conductivity of under identical sintering condition, preparing the AlN pottery is increased to 218 W/ (mK).
In the preparation process of nano aluminum nitride powder, plasma chemical synthesis method, chemical Vapor deposition process and wet-chemical combined carbon hot reducing method are present main compound methods.With respect to preceding two kinds of preparing methods, wet-chemical combined carbon hot reducing method technology comparative maturity, technological process is easy, is suitable for suitability for industrialized production and uses.At present; Pass through wet chemical method; Like sol-gel method, coprecipitation method etc., realize aluminium source and carbon source uniform mixing with the solution form in the molecular level level, and then through carbothermic method prepare even particle distribution, nano aluminum nitride powder that particle diameter is tiny has obtained broad research.Song Yang etc. " Rare Metals Materials and engineering, 2005,34 (z1): 147-151 " are raw material with aluminum isopropylate, sucrose, urea, adopt sol-gel technology to obtain presoma, obtain particle diameter 23 nm, specific surface area 70 m 1500 ℃ of nitrogenize then
2The aluminium nitride powder of/g; Chowdhury etc. " J. Cryst. Growth, 2004,263:12-20 " as raw material, obtain presoma through coprecipitation method with aluminum nitrate and carbon black, then through the synthetic aluminium nitride powder that obtains median size 100 nm of carbothermic method; Qin etc. " Mater. Res. Bull., 2008,43:2954-2960 " are raw material with aluminum nitrate, glucose and urea, adopt nitrate salt-organism low-temperature burning technology to obtain presoma, have obtained nano level aluminium nitride powder 1550 ℃ of nitrogenize.
Domestic and international from present in the research aspect the dense sintering aluminium nitride ceramics; Adding sintering aid and being simply the most also is the most effective one of way; But also having some inevitable defectives simultaneously, all is micron-sized powders like present used sintering aid and aluminium nitride powder, is difficult to realize the uniform mixing of auxiliary agent and body material; Cause sintering aid content to increase, thereby reduced the thermal conductivity of aluminium nitride ceramics; And adopt simple nano aluminum nitride powder limited aspect the effect that reduces the aluminium nitride ceramics sintering temperature; Even if in the nano aluminum nitride powder, add sintering aid, the also difficult uniform distribution of auxiliary agent in aluminium nitride ceramics of realizing.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of yttrium dopen Nano aluminium nitride powder; The sintering aid yttrium is uniformly distributed in the nano aluminum nitride powder; Thereby realize the combination that sintering aid effect and nano particle high-ratio surface can act on, for the aluminium nitride ceramics that obtains a small amount of sintering aid doping, high-compactness, high heat conductance is established material foundation.
The preparation method of yttrium dopen Nano aluminium nitride powder of the present invention may further comprise the steps:
(1) the aluminium source is dissolved in the solvent, forms the aluminium source solution of 0.4～2.0 mol/L;
(2) the yttrium source is dissolved in the solvent, forms the yttrium source solution of 0.4～2.0 mol/L;
(3) mol ratio by yttrium and aluminium element is 0.5:100～5:100, and above-mentioned solution (1) is mixed with solution (2), forms the mixing solutions in aluminium source and yttrium source;
(4) Hydrocerol A is dissolved in the terepthaloyl moietie, the mol ratio of Hydrocerol A and terepthaloyl moietie is 1:4～1:8;
(5) press the mol ratio 1:1～4:1 of Hydrocerol A and aluminium element, above-mentioned solution (3) is mixed with solution (4), and stir;
(6) carbon source is dissolved in the solvent, forms the carbon source solution of 0.4～2.0 mol/L;
(7) mol ratio by carbon and aluminium element is 2:1～10:1, above-mentioned solution (6) is joined in the solution (5) mixing and stirring; Be warmed up to 125～135 ℃ of insulations 2～4 hours then, continue to be warmed up to 180～220 ℃ of insulations 2～4 hours, obtain fluffy brownish black material;
(8) with the calcining under 800～1200 ℃ vacuum or nitrogen atmosphere of above-mentioned fluffy brownish black material, obtain mixed uniformly Al
2O
3, C and Y
2O
3Grind the cooling back, puts into crucible again and place under the flowing nitrogen atmosphere, 1450～1550 ℃ of insulations 1～5 hour, obtains the grey black powder;
(9) placing 700～800 ℃ air to be incubated 1～4 hour above-mentioned grey black powder carries out decarburization, obtains yttrium dopen Nano aluminium nitride powder.
Among the present invention, described aluminium source can be one or more in aluminum nitrate, Burow Solution, aluminum isopropylate, aluminum chloride and the aluminium colloidal sol; Described yttrium source can be one or more in Yttrium trinitrate, acetic acid yttrium, yttrium isopropoxide and the Yttrium trichloride; Described solvent can be one or more in absolute ethyl alcohol, acetone and the deionized water; Described carbon source can be one or more in glucose, sucrose, methylcellulose gum, TKK 021, ROHM and the SEPIGEL 305.
The present invention utilizes the complexing action of Hydrocerol A and the sterically hindered effect of terepthaloyl moietie, and aluminium, ruthenium ion are evenly distributed in the carbon source, thereby obtains finally that particle diameter is tiny, the uniform yttrium dopen Nano of component aluminium nitride powder.Compared with prior art; The yttrium dopen Nano aluminium nitride powder that the present invention prepares; In the ceramic post sintering process, both can reduce the sintering temperature of aluminium nitride ceramics through the effect of yttrium auxiliary agent; And because auxiliary agent uniform distribution in powder can effectively overcome the disadvantageous effect of auxiliary agent skewness to ceramic performance; The nano effect of superfine powder capable of using promotes the dense sintering of aluminium nitride ceramics simultaneously, thereby is that the aluminium nitride ceramics for preparing a small amount of sintering aid doping, high-compactness, high heat conductance is established material foundation.Product of the present invention has important application prospects on electric substrate, power device.
Description of drawings
Fig. 1 is the different embodiment material phase analysis of the yttrium dopen Nano aluminium nitride powder of preparation down;
Fig. 2 is the electron scanning micrograph of the yttrium dopen Nano aluminium nitride powder of embodiment 1 preparation;
Fig. 3 is the electron scanning micrograph of the yttrium dopen Nano aluminium nitride powder of embodiment 2 preparations;
Fig. 4 is the electron scanning micrograph of the yttrium dopen Nano aluminium nitride powder of embodiment 3 preparations.
Embodiment
Below in conjunction with instance the present invention is further described.
Embodiment 1:
Take by weighing 1.0 mol aluminum nitrates and be dissolved in the aluminium source solution that forms 0.5 mol/L in the 2.0 L deionized waters; Take by weighing 0.0076 mol Yttrium trinitrate and be dissolved in the yttrium source solution that forms 0.5 mol/L in the 0.0152 L deionized water; Above-mentioned aluminium source solution and yttrium source solution are mixed, form aluminium-yttrium mixing solutions.Take by weighing 1.0 mol Hydrocerol As and be dissolved in the 5.0 mol terepthaloyl moietie, add to after the mixing and stirring in above-mentioned aluminium-yttrium mixing solutions.Take by weighing 0.83 mol glucose and be dissolved in the carbon source solution that forms 0.5 mol/L in the 1.66 L deionized waters, add to after the mixing and stirring in above-mentioned aluminium-yttrium mixing solutions.Above-mentioned mixing solutions is stirred, be warming up to 130 ℃ of insulation 2 h then, continue to be warmed up to 200 ℃ of insulation 2 h, obtain fluffy brownish black powder after the cooling.Above-mentioned fluffy brownish black powder is calcined 1 h, the carbothermic reduction presoma that obtains mixing in 1000 ℃ of nitrogen atmospheres; Grind cooling back, places then under the nitrogen atmosphere of circulation in 1450 ℃ of insulation 2 h, obtains the grey black powder.With above-mentioned grey black powder under air atmosphere in 700 ℃ the insulation 3 h, remove unnecessary carbon, finally obtain the equally distributed nano aluminum nitride powder of yttrium.The yttrium uniform distribution nano aluminum nitride powder that obtains is tested through XRD analysis, obtains its thing and is AlN and Y mutually
2O
3The coexistence (see figure 1); Through the sem analysis test, the median size of powder is in 40-60 nm (see figure 2).
Embodiment 2:
Take by weighing 1.0 mol Burow Solutions and be dissolved in the aluminium source solution that forms 1.0 mol/L in the 1.0 L absolute ethyl alcohols; Take by weighing 0.023 mol Yttrium trinitrate and be dissolved in the yttrium source solution that forms 1.0 mol/L in the 0.023 L absolute ethyl alcohol; Above-mentioned aluminium source solution and yttrium source solution are mixed, form aluminium-yttrium mixing solutions.Take by weighing 2.0 mol Hydrocerol As and be dissolved in the 8.0 mol terepthaloyl moietie, add to after the mixing and stirring in above-mentioned aluminium-yttrium mixing solutions.Take by weighing 0.8 mol sucrose and be dissolved in the carbon source solution that forms 1.0 mol/L in the 0.8 L absolute ethyl alcohol, add to after the mixing and stirring in above-mentioned aluminium-yttrium mixing solutions.Above-mentioned mixing solutions is stirred, be warming up to 125 ℃ of insulation 3 h then, continue to be warmed up to 180 ℃ of insulation 4 h, obtain fluffy brownish black powder after the cooling.Above-mentioned fluffy brownish black powder is calcined 1 h, the carbothermic reduction presoma that obtains mixing in 900 ℃ of nitrogen atmospheres; Grind cooling back, places then under the nitrogen atmosphere of circulation in 1500 ℃ of insulation 2 h, obtains the grey black powder.With above-mentioned grey black powder under air atmosphere in 750 ℃ the insulation 2 h, remove unnecessary carbon, finally obtain the equally distributed nano aluminum nitride powder of yttrium.The yttrium uniform distribution nano aluminum nitride powder that obtains is tested through XRD analysis, and its thing is AlN and Y mutually
2O
3The coexistence (see figure 1); Through the sem analysis test, the median size of powder is in 60-80 nm (see figure 3).
Embodiment 3:
Take by weighing 1.0 mol aluminum isopropylates and be dissolved in the aluminium source solution that forms 2.0 mol/L in the 0.5 L acetone; Take by weighing 0.03 mol acetic acid yttrium and be dissolved in the yttrium source solution that forms 1.0 mol/L in the 0.03 L acetone; Above-mentioned aluminium source solution and yttrium source solution are mixed, form aluminium-yttrium mixing solutions.Take by weighing 1.5 mol Hydrocerol As and be dissolved in the 8.0 mol terepthaloyl moietie, add to after the mixing and stirring in above-mentioned aluminium-yttrium mixing solutions.Take by weighing 0.3 mol glucose and 0.3 mol sucrose and be dissolved in the carbon source solution that forms 0.5 mol/L in the 1.2 L deionized waters, add to after the mixing and stirring in above-mentioned aluminium-yttrium mixing solutions.Above-mentioned mixing solutions is stirred, be warming up to 125 ℃ of insulation 2 h then, continue to be warmed up to 220 ℃ of insulation 2 h, obtain fluffy brownish black powder after the cooling.Above-mentioned fluffy brownish black powder is calcined 1 h, the carbothermic reduction presoma that obtains mixing in 800 ℃ of nitrogen atmospheres; Grind cooling back, places then under the nitrogen atmosphere of circulation in 1450 ℃ of insulation 2 h, obtains the grey black powder.With above-mentioned grey black powder under air atmosphere in 800 ℃ the insulation 1 h, remove unnecessary carbon, finally obtain the equally distributed nano aluminum nitride powder of yttrium.The yttrium uniform distribution nano aluminum nitride powder that obtains is tested through XRD analysis, obtains its thing and is AlN and Y mutually
2O
3, Al
2Y
4O
9The coexistence (see figure 1); Through the sem analysis test, the median size of powder is in 60-80 nm (see figure 4).
Claims (5)
1. the preparation method of a yttrium dopen Nano aluminium nitride powder may further comprise the steps:
(1) the aluminium source is dissolved in the solvent, forms the aluminium source solution of 0.4～2.0 mol/L;
(2) the yttrium source is dissolved in the solvent, forms the yttrium source solution of 0.4～2.0 mol/L;
(3) mol ratio by yttrium and aluminium element is 0.5:100～5:100, and above-mentioned solution (1) is mixed with solution (2), forms the mixing solutions in aluminium source and yttrium source;
(4) Hydrocerol A is dissolved in the terepthaloyl moietie, the mol ratio of Hydrocerol A and terepthaloyl moietie is 1:4～1:8;
(5) press the mol ratio 1:1～4:1 of Hydrocerol A and aluminium element, above-mentioned solution (3) is mixed with solution (4), and stir;
(6) carbon source is dissolved in the solvent, forms the carbon source solution of 0.4～2.0 mol/L;
(7) mol ratio by carbon and aluminium element is 2:1～10:1, above-mentioned solution (6) is joined in the solution (5) mixing and stirring; Be warmed up to 125～135 ℃ of insulations 2～4 hours then, continue to be warmed up to 180～220 ℃ of insulations 2～4 hours, obtain fluffy brownish black material;
(8) with the calcining under 800～1200 ℃ vacuum or nitrogen atmosphere of above-mentioned fluffy brownish black material, obtain mixed uniformly Al
2O
3, C and Y
2O
3Grind the cooling back, puts into crucible again and place under the flowing nitrogen atmosphere, 1450～1550 ℃ of insulations 1～5 hour, obtains the grey black powder;
(9) placing 700～800 ℃ air to be incubated 1～4 hour above-mentioned grey black powder carries out decarburization, obtains yttrium dopen Nano aluminium nitride powder.
2. the preparation method of yttrium dopen Nano aluminium nitride powder according to claim 1 is characterized in that: described aluminium source is one or more in aluminum nitrate, Burow Solution, aluminum isopropylate, aluminum chloride and the aluminium colloidal sol.
3. the preparation method of yttrium dopen Nano aluminium nitride powder according to claim 1 is characterized in that: described yttrium source is one or more in Yttrium trinitrate, acetic acid yttrium, yttrium isopropoxide and the Yttrium trichloride.
4. the preparation method of yttrium dopen Nano aluminium nitride powder according to claim 1 is characterized in that: described solvent is one or more in absolute ethyl alcohol, acetone and the deionized water.
5. the preparation method of yttrium dopen Nano aluminium nitride powder according to claim 1 is characterized in that: described carbon source is one or more in glucose, sucrose, methylcellulose gum, TKK 021, ROHM and the SEPIGEL 305.
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| CN102910598A (en) * | 2012-10-31 | 2013-02-06 | 吉林大学 | Yttrium-doped aluminum nitride diluted magnetic semiconductor quasi-array microtube and fabrication method of microtube |
| CN103320899A (en) * | 2013-07-01 | 2013-09-25 | 中国计量学院 | Preparation method of nanometer aluminum nitride fiber |
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| CN106220186A (en) * | 2016-08-05 | 2016-12-14 | 郭迎庆 | A kind of preparation method of ceramic base electronic substrate |
| CN106565246B (en) * | 2016-10-21 | 2019-10-29 | 浙江工业大学 | A method of preparing aluminium nitride/yttrium nitride composite powder |
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