CN107759226A - 一种陶瓷粉体制备方法 - Google Patents
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Abstract
本发明涉及陶瓷制作技术领域,尤其是一种陶瓷粉体制备方法,经过将α‑三氧化二铝和γ‑三氧化二铝进行配制,制备成混合粉;将硫酸铝与氯化铵溶液混合制备混合液,并将混合粉与混合液混合,加入添加剂,并经过200‑300℃干燥,600‑800℃处理,1200‑1300℃保温短时间处理,使得制备的陶瓷粉体中AIN的含量达到了83.12~92.13%,提高了陶瓷粉体的品质;使得用于制备AIN陶瓷后,陶瓷性能较优。
Description
技术领域
本发明涉及陶瓷制作技术领域,尤其是一种陶瓷粉体制备方法。
背景技术
AIN陶瓷具有耐高温、抗腐蚀、高热导率、低膨胀系数、耐热冲击等良好的性能,并且具有很高的电绝缘性能,使得其成为近年来发展的优异集成电路基片材料、电子元件的封装材料以及耐受高温的新型高抗热震性陶瓷结构材料。
制备AIN陶瓷关键在于AIN含量高、结晶特性良好的氮化铝粉体材料的制备,而现有技术中,能够实现工业化生产氮化铝粉体的方法主要有直接氮化法和碳热还原法。
直接氮化法是以铝粉为原料,在高温下通入氮气,直接化合生产AIN,反应温度一般为800-1200℃;但由于反应过程为放热反应,导致温度那一控制,使得产品质量不稳定,往往出现自烧结现象,并且,铝粉氮化比愛哦面形成的AIN层会阻碍反应的进行,需要长时间才能反应完全,而对于AIN纯度越高,导致制备成本越高,使得该法难以被广泛推广应用。
碳热还原法是采用γ-三氧化二铝或α-三氧化二铝与碳黑混合,氮气条件下,在1600-1800℃下,保温12h合成,得到的粉体几乎无团聚,但是其温度和保温时间均较高。
鉴于此,有研究者针对上述缺陷进行了研究,使得AIN陶瓷粉体合成时间较短、成本低、过程稳定、温度低、保温时间短;如专利号为200710084522.4的AIN陶瓷粉体的合成制备方法,经过碳酸铝氨凝胶的制备、配合料湿法混合、制备粉体料块、在温度为1400-1600℃下保温2-6h,可见,在合成过程中,其温度依然较高,并且也需要在较高温度下保温2-6h,能耗依然较大。
基于此,本研究者针对AIN陶瓷粉体的制备方法进行研究,为AIN陶瓷粉体提供一种新的制备思路。
发明内容
为了解决现有技术中存在的上述技术问题,本发明提供一种陶瓷粉体制备方法。
具体是通过以下技术方案得以实现的:
陶瓷粉体制备方法,包括以下步骤:
(1)将α-Al2O3与γ-Al2O3按照质量比为1:0.3~0.5混合,并研磨,过1000-3000目筛,得到混合粉;
(2)将硫酸铝与氯化铵溶液按照摩尔比为1:0.2~0.4滴加混合,并在40℃恒温搅拌,直至滴加完毕,继续搅拌30min,得到混合液;
(3)将混合液与混合粉按照质量比为1:1混合,并加入添加剂,添加剂加入量为占混合粉质量的0.003-0.007%,搅拌混合时间为1-3h,获得料浆;
(4)将料浆置于温度为200-300℃下干燥至成固体,并置于碳管炉中,在氮气气氛下,控制温度为600-800℃处理3-5h,再在温度为1200-1300℃下保温0.5h,获得。
优选,所述的硫酸铝是摩尔浓度为1.3mol/L的溶液。
优选,所述的氯化铵溶液摩尔浓度为0.8mol/L。
优选,所述的添加剂是活性炭负载贵金属的复合物。
优选,所述的活性炭负载贵金属为铂炭、钯炭、钌炭、铑炭中的一种或者几种的任意质量比混合。
本发明的目的还提供上述的制备方法制备的陶瓷粉体。
与现有技术相比,本发明创造的技术效果体现在:
经过将α-三氧化二铝和γ-三氧化二铝进行配制,制备成混合粉;将硫酸铝与氯化铵溶液混合制备混合液,并将混合粉与混合液混合,加入添加剂,并经过200-300℃干燥,600-800℃处理,1200-1300℃保温短时间处理,使得制备的陶瓷粉体中AIN的含量达到了83.12~92.13%,提高了陶瓷粉体的品质;使得用于制备AIN陶瓷后,陶瓷性能较优。
具体实施方式
下面结合具体的实施方式来对本发明的技术方案做进一步的限定,但要求保护的范围不仅局限于所作的描述。
实施例1
陶瓷粉体制备方法,包括以下步骤:
(1)将α-Al2O3与γ-Al2O3按照质量比为1:0.3混合,并研磨,过3000目筛,得到混合粉;
(2)将硫酸铝与氯化铵溶液按照摩尔比为1:0.2滴加混合,并在40℃恒温搅拌,直至滴加完毕,继续搅拌30min,得到混合液;
(3)将混合液与混合粉按照质量比为1:1混合,并加入添加剂,添加剂加入量为占混合粉质量的0.003%,搅拌混合时间为1h,获得料浆;
(4)将料浆置于温度为200℃下干燥至成固体,并置于碳管炉中,在氮气气氛下,控制温度为600℃处理3h,再在温度为1200℃下保温0.5h,获得。
所述的硫酸铝是摩尔浓度为1.3mol/L的溶液。
所述的氯化铵溶液摩尔浓度为0.8mol/L。
所述的添加剂为铂炭。
本实施例合成的陶瓷粉体中的AIN含量为88.65%。
实施例2
陶瓷粉体制备方法,包括以下步骤:
(1)将α-Al2O3与γ-Al2O3按照质量比为1:0.5混合,并研磨,过1000目筛,得到混合粉;
(2)将硫酸铝与氯化铵溶液按照摩尔比为1:0.4滴加混合,并在40℃恒温搅拌,直至滴加完毕,继续搅拌30min,得到混合液;
(3)将混合液与混合粉按照质量比为1:1混合,并加入添加剂,添加剂加入量为占混合粉质量的0.007%,搅拌混合时间为3h,获得料浆;
(4)将料浆置于温度为300℃下干燥至成固体,并置于碳管炉中,在氮气气氛下,控制温度为800℃处理5h,再在温度为1300℃下保温0.5h,获得。
所述的硫酸铝是摩尔浓度为1.3mol/L的溶液。
所述的氯化铵溶液摩尔浓度为0.8mol/L。
所述的添加剂为钯炭、钌炭等质量比混合。
本实施例合成的陶瓷粉体中的AIN含量为92.13%。
实施例3
陶瓷粉体制备方法,包括以下步骤:
(1)将α-Al2O3与γ-Al2O3按照质量比为1:0.4混合,并研磨,过2000目筛,得到混合粉;
(2)将硫酸铝与氯化铵溶液按照摩尔比为1:0.3滴加混合,并在40℃恒温搅拌,直至滴加完毕,继续搅拌30min,得到混合液;
(3)将混合液与混合粉按照质量比为1:1混合,并加入添加剂,添加剂加入量为占混合粉质量的0.005%,搅拌混合时间为2h,获得料浆;
(4)将料浆置于温度为250℃下干燥至成固体,并置于碳管炉中,在氮气气氛下,控制温度为700℃处理4h,再在温度为1250℃下保温0.5h,获得。
所述的硫酸铝是摩尔浓度为1.3mol/L的溶液。
所述的氯化铵溶液摩尔浓度为0.8mol/L。
所述的添加剂为铂炭、钯炭、铑炭等质量比混合。
本实施例合成的陶瓷粉体中的AIN含量为83.12%。
实施例4
陶瓷粉体制备方法,包括以下步骤:
(1)将α-Al2O3与γ-Al2O3按照质量比为1:0.5混合,并研磨,过1000目筛,得到混合粉;
(2)将硫酸铝与氯化铵溶液按照摩尔比为1:0.2滴加混合,并在40℃恒温搅拌,直至滴加完毕,继续搅拌30min,得到混合液;
(3)将混合液与混合粉按照质量比为1:1混合,并加入添加剂,添加剂加入量为占混合粉质量的0.004%,搅拌混合时间为3h,获得料浆;
(4)将料浆置于温度为200℃下干燥至成固体,并置于碳管炉中,在氮气气氛下,控制温度为600℃处理4h,再在温度为1300℃下保温0.5h,获得。
所述的硫酸铝是摩尔浓度为1.3mol/L的溶液。
所述的氯化铵溶液摩尔浓度为0.8mol/L。
所述的添加剂为铂炭、钯炭、钌炭、铑炭等质量比混合。
本实施例合成的陶瓷粉体中的AIN含量为86.19%。
Claims (7)
1.一种陶瓷粉体制备方法,其特征在于,包括以下步骤:
(1)将α-Al2O3与γ-Al2O3按照质量比为1:0.3~0.5混合,并研磨,过1000-3000目筛,得到混合粉;
(2)将硫酸铝与氯化铵溶液按照摩尔比为1:0.2~0.4滴加混合,并在40℃恒温搅拌,直至滴加完毕,继续搅拌30min,得到混合液;
(3)将混合液与混合粉按照质量比为1:1混合,并加入添加剂,添加剂加入量为占混合粉质量的0.003-0.007%,搅拌混合时间为1-3h,获得料浆;
(4)将料浆置于温度为200-300℃下干燥至成固体,并置于碳管炉中,在氮气气氛下,控制温度为600-800℃处理3-5h,再在温度为1200-1300℃下保温0.5h,获得。
2.如权利要求1所述的陶瓷粉体制备方法,其特征在于,所述的硫酸铝是摩尔浓度为1.3mol/L的溶液。
3.如权利要求1所述的陶瓷粉体制备方法,其特征在于,所述的氯化铵溶液摩尔浓度为0.8mol/L。
4.如权利要求1所述的陶瓷粉体制备方法,其特征在于,所述的添加剂是活性炭负载贵金属的复合物。
5.如权利要求4所述的陶瓷粉体制备方法,其特征在于,所述的活性炭负载贵金属为铂炭、钯炭、钌炭、铑炭中的一种或者几种的任意质量比混合。
6.如权利要求1-5任一项所述的制备方法制备的陶瓷粉体。
7.如权利要求6所述的陶瓷粉体用于制备AIN陶瓷。
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