CN107954715A - 一种致密块体陶瓷材料的制备方法 - Google Patents
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Abstract
本发明属于材料制备技术领域,具体涉及一种通过添加亚稳相促进陶瓷粉体烧结,制备致密块体陶瓷材料方法。致密块体陶瓷材料,是在稳定相陶瓷粉体中加入少量其亚稳相的粉体,在溶剂中均匀分散后,搅拌蒸干,过筛制得前驱体粉末;所述前驱体粉末在保护气氛下施加压力经高温烧结后得到所述致密块体陶瓷材料。所述亚稳相粉体采用一种或多种粒径的粉体制备,在高温下发生相变为次生稳定相,次生稳定相均匀分布在原稳定相的孔隙中,得到致密块体陶瓷材料。本发明所制备的致密块体陶瓷材料具有高的致密度,高的强度和良好的使用性能。
Description
技术领域
本发明属于材料制备技术领域,具体涉及一种致密块体陶瓷材料的制备方法。
背景技术
陶瓷材料因其具有高硬度、高强度,高化学稳定性等优异的性能,广泛应用在结构材料和功能材料中。但由于陶瓷材料烧结较为困难,一定程度上限制了陶瓷材料的应用领域,其核心问题是陶瓷材料的致密化问题。因此,研究致密块体陶瓷材料的制备成为我国的迫切课题。本发明的致密块体陶瓷材料制备方法是在稳定相陶瓷粉体中加入少量亚稳相粉体,在溶剂中均匀分散后,搅拌蒸干制得前驱体粉末,在保护气氛下施加压力经高温烧结后得到所述致密块体陶瓷材料。本发明所制备的致密块体陶瓷材料具有高的致密度,高的强度和良好的使用性能。
发明内容
为了克服现有技术的不足,攻克由固相烧结法制备高致密度高强度的致密块体陶瓷材料难题,本发明提供了一种通过固相反应烧结得到的致密块体陶瓷材料的制备方法。本发明以稳定相陶瓷粉体为原料,添加少量亚稳相粉体进行热压烧结,制得高致密度高强度的致密块体陶瓷材料。
本发明采用的具体技术方案是:
一种致密块体陶瓷材料的制备方法,是先制得前驱体粉体,再经过加压烧结转化为致密块体陶瓷材料。
进一步的,所述前驱体是采用稳定相陶瓷粉体,采用一种或多种粒径的亚稳相制备,在无水乙醇中经超声分散,搅拌蒸干,干燥后过筛制得。
进一步的,所述前驱体粉末的制备过程包括以下步骤:
(1)致密块体陶瓷材料前驱体粉体的制备:称取粒径为1~2μm的稳定相陶瓷粉体3.48~4.00g,称取粒径50~400nm的亚稳相粉体0.20~0.50g,研磨混合;将研磨后的混合粉体加入50ml无水乙醇,超声分散20~30min;加热搅拌使溶剂蒸发至溶液成糊状,再进行烘干;取出物料放入研钵中,滴入几滴无水乙醇并研磨至干燥,重复该步骤多次;将所得粉体用不锈钢标准筛过筛,制得致密块体陶瓷材料的前驱体粉末;
(2)致密块体陶瓷材料的制备:称取前驱体粉末置于模具中,在保护气体气氛下烧结;在600~900℃时开始对模具加压,施加的压力为40~80MPa;达到最高烧结温度时,保温2~10min,泄压冷却至室温。高温时,亚稳相转变为次生稳定相,次生稳定相均匀分布在原稳定相的孔隙中,得到致密的块体陶瓷材料。
所述步骤(1)中,稳定相陶瓷粉体的粒度应为亚微米级,亚稳相粉体的粒度应为纳米级。
所述步骤(1)中,所述的溶剂为无水乙醇。
所述步骤(2)中,所述保护气氛为氩气。
所述步骤(2)中,烧结方式为放电等离子体烧结时;升温速率为100~150℃/min。
所述步骤(2)中,烧结方式为热压烧结或热等静压烧结时;升温速率为5~10℃/min。
本发明与现有技术相比所具有的有益效果是:
本发明以稳定相陶瓷粉体和亚稳相粉体为主要原料,在高温下亚稳相经相转变,其原子历经较高的势能位置,活跃度大,相比现有的技术大都是采用各种中间相,本发明非常有利于烧结和提高产品的致密度。高温时,亚稳相转变为由次生稳定相,次生稳定相均匀分布在原稳定相孔隙中。该致密块体陶瓷材料具有高的致密度和良好的使用性能。
附图说明
图1是本发明制备一种致密块体陶瓷材料的简要流程图。
具体实施方式
以下通过对实施例的描述,对本发明的具体实施方式作进一步的详细说明。
实施例1:
如附图1中所示流程,致密块体石墨材料的制备方法,包括前驱体的制备、致密块体石墨材料的烧结,具体步骤如下:
(1)致密块体石墨材料前驱体粉体的制备:
称取粒径为1~2μm的石墨粉体3.78g,称取粒径100nm的金刚石粉体0.20g,放入研钵混合,研磨10min,将研磨后的粉体放入到100ml的烧杯中,向其烧杯中滴加30ml无水乙醇,将烧杯放入超声清洗仪中,采用120w功率超声分散20min;放在恒温磁力搅拌器上,在60℃下缓慢搅拌使溶剂蒸发至溶液成糊状,再将其放入干燥箱中60℃烘干;取出物料放入研钵中,滴入几滴无水乙醇并研磨至干燥,重复该步骤5次;最后将所得粉体用100目不锈钢标准筛过筛,制得的前驱体粉末。
(2)前驱体粉末的烧结:
称取0.9g(1)中制得的前驱体粉末,置于内径为15mm的石墨模具中,在氩气保护下,采用放电等离子体烧结,烧结时升温速率为150℃/min,烧结温度为1700℃,轴向压力为80MPa。高温时,金刚石相转变为次生石墨,次生石墨均匀地分布在原石墨的孔隙中,得到致密块体石墨材料。
实施例2:
一种致密块体石墨材料的制备方法,包括前驱体的制备、致密块体石墨材料的烧结,具体步骤如下:
(1)致密块体石墨材料前驱体粉体的制备:
称取粒径为1~2μm的石墨粉体3.58g,分别称取粒径200nm和100nm的金刚石粉体0.30g和0.10g,放入研钵混合,研磨10min,将研磨后的粉体放入到100ml的烧杯中,向其烧杯中滴加30ml无水乙醇,将烧杯放入超声清洗仪中,采用120w功率超声分散20min;放在恒温磁力搅拌器上,在60℃下缓慢搅拌使溶剂蒸发至溶液成糊状,再将其放入干燥箱中70℃烘干;取出物料放入研钵中,滴入几滴无水乙醇并研磨至干燥,重复该步骤4次;最后将所得粉体用100目不锈钢标准筛过筛,制得的前驱体粉末。
(2)前驱体粉末的烧结:
称取0.9g(1)中制得的前驱体粉末,置于内径为15mm的石英玻璃套中,在氩气保护下,采用热等静压进行烧结,烧结时升温速率为5℃/min,烧结温度为1600℃,施加压力为40MPa。高温时,金刚石相转变为次生石墨,次生石墨均匀地分布在原石墨的孔隙中,得到致密块体石墨材料。
实施例3:
如附图1中所示流程,致密块体六方氮化硼材料的制备方法,包括前驱体的制备、致密块体六方氮化硼材料的烧结,具体步骤如下:
(1)致密块体六方氮化硼材料前驱体粉体的制备:
称取粒径为1~2μm的六方氮化硼粉体3.48g,分别称取粒径400nm和200nm的立方氮化硼粉体0.37g和0.12g,放入研钵混合,研磨10min,将研磨后的粉体放入到100ml的烧杯中,向其烧杯中滴加30ml无水乙醇,将烧杯放入超声清洗仪中,采用120w功率超声分散20min;放在恒温磁力搅拌器上,在70℃下缓慢搅拌使溶剂蒸发至溶液成糊状,再将其放入干燥箱中60℃烘干;取出物料放入研钵中,滴入几滴无水乙醇并研磨至干燥,重复该步骤5次;最后将所得粉体用100目不锈钢标准筛过筛,制得的前驱体粉末。
(2)前驱体粉末的烧结:
称取0.9g(1)中制得的前驱体粉末,置于内径为15mm的石墨模具中,在氩气保护下,采用放电等离子体烧结,烧结时升温速率为100℃/min,烧结温度为1600℃,轴向压力为70MPa。高温时,立方氮化硼相转变为次生六方氮化硼,次生六方氮化硼均匀地分布在原六方氮化硼的孔隙中,得到致密块体六方氮化硼材料。
实施例4:
一种致密块体六方氮化硼材料的制备方法,包括前驱体的制备、致密块体六方氮化硼材料的烧结,具体步骤如下:
(1)致密块体六方氮化硼材料前驱体粉体的制备:
称取粒径为1~2μm的六方氮化硼粉体3.58g,称取粒径200nm的立方氮化硼粉体0.40g,放入研钵混合,研磨10min,将研磨后的粉体放入到100ml的烧杯中,向其烧杯中滴加30ml无水乙醇,将烧杯放入超声清洗仪中,采用120w功率超声分散20min;放在恒温磁力搅拌器上,在60℃下缓慢搅拌使溶剂蒸发至溶液成糊状,再将其放入干燥箱中60℃烘干;取出物料放入研钵中,滴入几滴无水乙醇并研磨至干燥,重复该步骤6次;最后将所得粉体用100目不锈钢标准筛过筛,制得的前驱体粉末。
(2)前驱体粉末的烧结:
称取0.9g(1)中制得的前驱体粉末,置于内径为15mm的石英玻璃套中,在氩气保护下,采用热等静压进行烧结,烧结时升温速率为10℃/min,烧结温度为1700℃,施加压力为40MPa。高温时,立方氮化硼相转变为由次生六方氮化硼,次生六方氮化硼均匀地分布在原六方氮化硼的孔隙中,得到致密块体六方氮化硼材料。
以上描述只是本发明的具体实施方式,各举例说明不对本发明的实质内容构成限制,所属技术领域的技术人员对前述的具体实施方式做修改或变形,不背离本发明的实质。
Claims (8)
1.一种致密块体陶瓷材料,其特征在于:所述致密块体陶瓷材料的结构包括次生稳定相和原稳定相;所述次生稳定相是亚稳相粉体在高温条件下相变得到;次生稳定相均匀分布在原稳定相周围。
2.一种如权利要求1所述的致密块体陶瓷材料的制备方法,其特征在于:采用稳定相陶瓷粉体加入少量亚稳相粉体,在溶剂中均匀分散后,搅拌蒸干,过筛制得前驱体粉末;所述前驱体粉末在保护气氛下施加压力经高温烧结后得到所述致密块体陶瓷材料。
3.根据权利要求2所述的致密块体陶瓷材料的制备方法,其特征在于:所述亚稳相粉体采用一种或多种粒径的粉体制备。
4.根据权利要求2中任一条所述的致密块体陶瓷材料的制备方法,其特征在于:包括以下步骤:
(1)致密块体陶瓷材料前驱体粉体的制备:称取粒径为1~2μm的稳定相陶瓷粉体3.48~4.00g,称取粒径50~400nm的亚稳相粉体0.20~0.50g,研磨混合;将研磨后的混合粉体加入50ml无水乙醇,超声分散20~30min;加热搅拌使溶剂蒸发至溶液成糊状,再进行烘干;取出物料放入研钵中,滴入几滴无水乙醇并研磨至干燥,重复该步骤多次;将所得粉体用不锈钢标准筛过筛,制得致密块体陶瓷材料的前驱体粉末;
(2)致密块体陶瓷材料的制备:将制备好的前驱体粉末定量地放置到模具中,在保护气氛下施加压力经高温烧结后得到致密块体陶瓷材料。
5.根据权利要求4所述的致密块体陶瓷材料的制备方法,其特征在于:所述步骤(1)中,稳定相陶瓷粉体的粒度应为亚微米级,亚稳相粉体的粒度应为纳米级。
6.根据权利要求4所述的致密块体陶瓷材料的制备方法,其特征在于:所述步骤(2)中,所述烧结的具体过程为:在保护气氛下烧结,所述保护气氛为氩气;在600~900℃时开始对模具加压,施加的压力为40~80MPa;当达到最高烧结温度时,保温2~10min;然后泄压冷却至室温。
7.根据权利要求4所述的致密块体陶瓷材料的制备方法,其特征在于:所述烧结为放电等离子体烧结时,升温速率为100~150℃/min。
8.根据权利要求4所述的致密块体陶瓷材料的制备方法,其特征在于:所述烧结为热压烧结或热等静压烧结时,升温速率为5~10℃/min。
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