A kind of preparation method of superfine aluminum nitride powder
An ultra-fine aluminum nitride and powder technology, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve problems such as uneven mixing of aluminum sources and carbon sources, avoid segregation of sucrose, and widen the process window. , the effect of simple preparation process
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[0018] As mentioned above, the present invention provides a kind of preparation method of ultrafine aluminum nitride powder, and described preparation method comprises the following steps:
[0019] (1) prepare alumina ethanol suspension, heat to temperature T1, keep warm and continue to stir, and add the soluble carbon source aqueous solution heated to temperature T1 while stirring, keep the mixed aqueous solution of gained stirring and cool down to temperature T2, Wherein said temperature T1 is higher than said temperature T2;
[0020] (2) subjecting the mixed aqueous solution to solid-liquid separation treatment to obtain a semi-dry precursor containing alumina, soluble carbon source, ethanol and water;
[0021] (3) drying the semi-dry precursor to obtain a reaction precursor containing alumina and a soluble carbon source;
[0022] (4) Calcining the reaction precursor in sequence in a nitrogen atmosphere and an air atmosphere to obtain ultrafine aluminum nitride powder.
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Embodiment 1
[0034] (1) Use alumina powder with a purity of 99.99% and a particle size of 40nm and 51g of absolute ethanol to prepare an ethanol suspension of alumina (molecular weight is about 101.96), heat it to 90°C (T1), and then Keep warm and keep stirring, wherein the amount of aluminum element substance is 1mol.
[0035] (2) The solubility of sucrose at 90°C (T1) is 421.9g, and the solubility of sucrose at 10°C (T2) is 191.1g. Use deionized water heated to 90°C (T1) to prepare a saturated aqueous solution of sucrose, and the carbon atoms in the sucrose The amount is 2.5 times the amount of the aluminum element substance, and the mass of sucrose is 130.4g, and the mass of water is 30.9g.
[0036] (3) Pour the sucrose aqueous solution into the alumina ethanol suspension liquid in a heat-retaining and stirring state, keep stirring and cool down to 10° C. (T2).
[0037] (4) The mixed liquid is subjected to solid-liquid separation by suction filtration to obtain a mixture containing alu...
Embodiment 2
[0041] Change the temperature T1 in Example 1 to 80°C, and the sucrose solubility at 80°C (T1) is 370.2g, then weigh 147.7g of sucrose and 39.9g of water, and the other operations are the same as in Example 1 to obtain the product as Example 1.
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