CN102502539B - Method for preparing yttrium-doped nano aluminum nitride powder - Google Patents
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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 prepares nano aluminum nitride powder as auxiliary agent method of adding, belong to materials science field.
Background technology
The characteristics such as the linear expansivity that aluminium nitride ceramics (AlN) has high thermal conductivity, be complementary with silicon, low specific inductivity, good electrical insulation capability, corrosion-resistant and environment-protecting asepsis, instead of alumina and beryllium oxide become the preferred material of present super large-scale integration substrate, are widely used at high-technology fields such as hyundai electronics and microelectronics.But because aluminium nitride 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 by 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 with the form of liquid phase sintering again; Another kind is by 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 alkaline-earth metal and fluorochemical were the sintering aids of commonly using.Such as " 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, the densification temperature of aluminium nitride ceramics can be reduced to 1650-1750 ℃; Qiao Liang etc. " material engineering, 2003,1:10-13 " are with CaF
2-YF
3As sintering aid, obtain the aluminium nitride ceramics of dense structure at 1750 ℃ of insulation 4 h, its thermal conductivity is 172 W/ (mK).With respect to other sintering aid, Y
2O
3Because the 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.Such as " Powder Techn., 2005,159:155-157 " such as Hiroya with Y
2O
3As sintering aid, at 1800 ℃ of insulation 3 h, aluminium nitride ceramics namely obtains theoretical sintered density, and thermal conductivity is 169 W/ (mK); " the J. Mater. Sci. such as Hirano, 1993,28 (17): 4725-4730 " when not adding any sintering aid the AlN powder is incubated 8 h at 1900 ℃, the thermal conductivity that sintering obtains the AlN pottery only is 114 W/ (mK), and adopts 4% Y
2O
3As sintering aid, the thermal conductivity of preparing the AlN pottery under identical sintering condition 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 are present main synthetic methods in conjunction with carbothermic method.With respect to front two kinds of preparation methods, wet-chemical is in conjunction with carbothermic reduction law technology comparative maturity, and technological process is easy, is suitable for suitability for industrialized production and uses.At present, pass through wet chemical method, such as sol-gel method, coprecipitation method etc., realize aluminium source and carbon source in the even mixing of molecular level level with the solution form, and then by 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 " adopt sol-gel technology to obtain presoma take aluminum isopropylate, sucrose, urea as raw material, then obtain particle diameter 23 nm, specific surface area 70 m 1500 ℃ of nitrogenize
2The aluminium nitride powder of/g; Chowdhury etc. " J. Cryst. Growth, 2004,263:12-20 " as raw material, obtain presoma by coprecipitation method with aluminum nitrate and carbon black, then by the synthetic aluminium nitride powder that obtains median size 100 nm of carbothermic method; Qin etc. " Mater. Res. Bull., 2008,43:2954-2960 " adopt nitrate-organism low-temperature burning technique to obtain presoma take aluminum nitrate, glucose and urea as raw material, have obtained nano level aluminium nitride powder 1550 ℃ of nitrogenize.
From domestic and international in the research aspect the dense sintering aluminium nitride ceramics at present, adding sintering aid and be the simplest also is one of the most effective way, but also there are some inevitable defectives simultaneously, all are micron-sized powders such as present used sintering aid and aluminium nitride powder, be difficult to realize the even 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 nano aluminum nitride powder, add sintering aid, the also even distribution of difficult realization auxiliary agent in aluminium nitride ceramics.
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 mentioned solution (1) is mixed with solution (2), forms the mixing solutions in aluminium source and yttrium source;
(4) citric acid is dissolved in the ethylene glycol, the mol ratio of citric acid and ethylene glycol is 1:4～1:8;
(5) press the mol ratio 1:1 of citric acid and aluminium element～4:1, 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, mentioned solution (6) is joined in the solution (5) mixing and stirring; Then be warmed up to 125～135 ℃ of insulations 2～4 hours, continue to be warmed up to 180～220 ℃ of insulations 2～4 hours, obtain fluffy brownish black material;
(8) above-mentioned fluffy brownish black material is calcined under 800～1200 ℃ vacuum or nitrogen atmosphere, obtained mixed uniformly Al
2O
3, C and Y
2O
3Grind after the cooling, put into again crucible and place under the mobile nitrogen atmosphere, 1450～1550 ℃ of insulations 1～5 hour, obtain the grey black powder;
(9) place 700～800 ℃ air to be incubated 1～4 hour above-mentioned grey black powder and carry out decarburization, obtain 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 dehydrated alcohol, acetone and the deionized water; Described carbon source can be one or more in glucose, sucrose, methylcellulose gum, ethyl cellulose, polyacrylic acid and the polyacrylamide.
The present invention utilizes the complexing action of citric acid and the sterically hindered effect of ethylene glycol, 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 by the effect of yttrium auxiliary agent the sintering temperature of aluminium nitride ceramics, and because auxiliary agent even distribution in powder can effectively overcome the auxiliary agent skewness to the disadvantageous effect of ceramic performance, can utilize simultaneously the nano effect of superfine powder to promote the dense sintering of aluminium nitride ceramics, thereby be 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 prospect at electric substrate, power device.
Description of drawings
Fig. 1 is the material phase analysis of the yttrium dopen Nano aluminium nitride powder for preparing under the different embodiment;
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
The invention will be further described below in conjunction with example.
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 citric acids and be dissolved in the 5.0 mol ethylene glycol, 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, then be warming up to 130 ℃ of insulation 2 h, 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 after the cooling, then place under the nitrogen atmosphere of circulation in 1450 ℃ of insulation 2 h, obtain 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 that the obtains nano aluminum nitride powder that evenly distributes is tested through XRD analysis, and obtaining its phase is AlN and Y
2O
3The coexistence (see figure 1); Through the sem analysis test, the median size of powder is seen Fig. 2 at 40-60 nm().
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 dehydrated 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 dehydrated alcohol, above-mentioned aluminium source solution and yttrium source solution are mixed, form aluminium-yttrium mixing solutions.Take by weighing 2.0 mol citric acids and be dissolved in the 8.0 mol ethylene glycol, 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 dehydrated alcohol, add to after the mixing and stirring in above-mentioned aluminium-yttrium mixing solutions.Above-mentioned mixing solutions is stirred, then be warming up to 125 ℃ of insulation 3 h, 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 after the cooling, then place under the nitrogen atmosphere of circulation in 1500 ℃ of insulation 2 h, obtain 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 that the obtains nano aluminum nitride powder that evenly distributes is tested through XRD analysis, and its phase is AlN and Y
2O
3The coexistence (see figure 1); Through the sem analysis test, the median size of powder is seen Fig. 3 at 60-80 nm().
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 citric acids and be dissolved in the 8.0 mol ethylene glycol, 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, then be warming up to 125 ℃ of insulation 2 h, 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 after the cooling, then place under the nitrogen atmosphere of circulation in 1450 ℃ of insulation 2 h, obtain 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 that the obtains nano aluminum nitride powder that evenly distributes is tested through XRD analysis, and obtaining its phase is AlN and Y
2O
3, Al
2Y
4O
9The coexistence (see figure 1); Through the sem analysis test, the median size of powder is seen Fig. 4 at 60-80 nm().
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 the solution that the solution that step (1) is obtained and step (2) obtain forms the mixing solutions in aluminium source and yttrium source;
(4) citric acid is dissolved in the ethylene glycol, the mol ratio of citric acid and ethylene glycol is 1:4～1:8;
(5) press the mol ratio 1:1 of citric acid and aluminium element～4:1, the solution that step (3) is obtained mixes with the solution that step (4) obtains, and stirs;
(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, and the solution that step (6) is obtained joins in the solution that step (5) obtains, mixing and stirring; Then be warmed up to 125～135 ℃ of insulations 2～4 hours, continue to be warmed up to 180～220 ℃ of insulations 2～4 hours, obtain fluffy brownish black material;
(8) above-mentioned fluffy brownish black material is calcined under 800～1200 ℃ vacuum or nitrogen atmosphere, obtained mixed uniformly Al
2O
3, C and Y
2O
3Grind after the cooling, put into again crucible and place under the mobile nitrogen atmosphere, 1450～1550 ℃ of insulations 1～5 hour, obtain the grey black powder;
(9) place 700～800 ℃ air to be incubated 1～4 hour above-mentioned grey black powder and carry out decarburization, obtain yttrium dopen Nano aluminium nitride powder.
2. the preparation method of yttrium dopen Nano aluminium nitride powder according to claim 1, it 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, it 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, it is characterized in that: described solvent is one or more in dehydrated alcohol, acetone and the deionized water.
5. the preparation method of yttrium dopen Nano aluminium nitride powder according to claim 1, it is characterized in that: described carbon source is one or more in glucose, sucrose, methylcellulose gum, ethyl cellulose, polyacrylic acid and the polyacrylamide.
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