Alpha-alumina material prepared from two-component nucleating agent, preparation method of alpha-alumina material and nucleating agent
A nucleating agent, alumina technology, applied in the preparation of alumina/hydroxide, chemical instruments and methods, aluminum compounds, etc., can solve the problems of prolonged crystallization time, increased steps, impure products, etc., to achieve particle size Narrow uniform distribution, lower phase transition temperature, and ease of mass production
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[0031]The disclosure relates to a preparation method of a two-component nucleating agent and α-Al prepared by using the nucleating agent 2 o 3 Material. The present disclosure utilizes α-phase Fe obtained by mixing and grinding nucleating agent precursors 2 o 3 and Al 2 o 3 The two kinds of nanoparticles constitute a composite nucleating agent, which is fully mixed with the aluminum sol, without significantly reducing the α-Al 2 o 3 Under the premise of material purity, provide more nucleation sites, reduce the phase transition temperature during sintering, and make the phase transition of aluminum sol easier to occur, so as to obtain α-Al with small grain size 2 o 3 Material. By adjusting the ratio and size of the composite nucleating agent, it is also possible to control the α-Al 2 o 3 The shape and size of the material. α-Al prepared in the present invention 2 o 3 The material has high purity and narrow particle size distribution, with the size between 50-150nm...
Embodiment 1
[0043] Using a mixture of deionized water and absolute ethanol as a solvent (volume ratio of 3:2), adding citric acid and ferrous sulfate with mass fractions of 8.3-9.2% and 1.1-1.5% respectively into the solvent, and dissolving the raw materials by magnetic stirring, Prepare the precursor, evaporate in a water bath at 80-85°C to obtain a wet gel, and dry at 130°C to obtain an iron-containing xerogel;
[0044] 100mL of 0.1mol·L -1 Al 2 (SO 4 ) 3 aqueous solution and 20mL of 2.5mmol·L -1 Add polyethyleneamine / ethanol solution to 0.5L reactor, Al 3+ The molar ratio to polyethyleneamine is 400:1. Then, add 280mL deionized water to make the liquid filling rate in the reactor reach 80%, add 1.64g urea, seal the reactor, place it at 150°C for 48 hours, cool to room temperature, filter, wash with deionized water and ethanol 3 times, drying at 60°C to obtain aluminum-containing xerogel;
[0045] Weigh 1 g of iron-containing gel and 9 g of aluminum-containing gel respectively, p...
Embodiment 2
[0049] 27g FeCl 3 ﹒ 6H 2 O was dissolved in 1L deionized water, and ammonia water was added to make Fe 3+ Precipitate completely, filter, wash with deionized water three times, and dry at 80°C;
[0050] 100mL 0.5mol / L Al 2 (SO 4 ) 3 Put the aqueous solution in a polytetrafluoroethylene-lined stainless steel autoclave, add 0.18g of urea to make the liquid filling rate to 80%, seal it, react at 190°C for 24h, naturally cool down, filter, and use deionized water and absolute ethanol respectively Wash 3 times. Vacuum drying at 60°C for later use;
[0051] Weigh 0.5g of iron-containing compound and 8g of aluminum-containing gel respectively, place them in a ball mill, and mill for 60 minutes to obtain a composite nucleating agent. The molar ratio of Fe / Al in the nucleating agent is 1 / 4, and the particle size of the nucleating agent is 20 -40nm;
[0052] Add the obtained composite nucleating agent into 200 g of aluminum sol with a solid content of 10%, stir and mix evenly t...
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