CN109336572A - 一种制备氧化物陶瓷的冷压烧结方法 - Google Patents
一种制备氧化物陶瓷的冷压烧结方法 Download PDFInfo
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Abstract
本发明提供一种制备氧化物陶瓷的冷压烧结方法,包括以下步骤：制备氧化物纳米粉体；将氧化物纳米粉体进行表面同质包覆；将包覆后的氧化物纳米粉体加入介质进行研磨；将研磨后的混合物放进模具中，对模具施加300MPa‑2GPa的压力，并在100‑300℃下烧结形成固相陶瓷。通过本发明所得到的氧化物陶瓷的相对密度可以超过90％，且性能优异。此外，本发明还能使大部分氧化物陶瓷烧结温度降低到300℃以下，缩短了陶瓷制备周期，降低了生产能耗，减少生产成本。
Description
技术领域
本发明属于陶瓷材料制备技术领域，具体涉及一种制备氧化物陶瓷的冷压烧结方法。
背景技术
陶瓷的烧结是粉体成型后在高温下烧成具有一定强度的致密体，是生产陶瓷工艺过程的一部分，在此过程中晶粒和气孔的尺寸及外形发生很大的变化。颗粒重排及晶界滑移，引起流动传质，物质通过扩散，填充到颗粒点接触的颈部和气孔，从而使颈部长大，气孔减小，最终使坯体致密化。粉体坯体烧成陶瓷是系统由介稳态向稳态转变的过程，但其不能自发的进行，是因为其本身还具有难以克服的能量壁垒，因此需要在特定的温度下才能进行。传统的陶瓷烧结温度一般为陶瓷材料熔融温度的50％-75％。对于大部分氧化物而言，烧结温度一般在1000℃以上，消耗了巨大的能量。因此降低陶瓷烧结温度不仅是解决能源问题的需要，也是降低成本、增加经济效益、适应特殊工艺要求的需要。
近年来，陶瓷的低温烧结技术飞速发展，例如微波辅助烧结、等离子体烧结、快速烧结、高压烧结等，但是烧结温度仍然在400℃以上。目前，由宾夕法尼亚州立大学Randall课题组提出的冷压烧结技术，在粉体中加入少量液体，在加压和加热的情况下，粉体表面发生部分溶解和重排，液体在压力下迅速渗透到颗粒孔隙当中，随着温度的升高，液体蒸发，颗粒表面发生溶解-重结晶过程，从而使陶瓷致密化。这一冷压烧结技术大大的降低了陶瓷烧结温度，但是对于难溶的氧化物或者是非均匀溶解的多元氧化物来说，溶解-重结晶过程进行困难，为了解决这一问题，必需提出新的技术。
发明内容
针对现有技术存在的问题，本发明提供一种制备氧化物陶瓷的冷压烧结方法，通过在氧化物纳米粉体的表面包覆一层同质活性层，在冷压烧结过程中促进溶解-重结晶过程，进而使陶瓷致密化。
本发明的技术方案为：
一种制备氧化物陶瓷的冷压烧结方法，包括以下步骤：制备氧化物纳米粉体；将氧化物纳米粉体进行表面同质包覆；将包覆后的氧化物纳米粉体加入介质进行研磨；将研磨后的混合物放进模具中，对模具施加300MPa-2GPa的压力，并在100-300℃下烧结形成固相陶瓷。
进一步地，所述氧化物包括氧化硅、氧化锆、氧化锌、钛酸钡、钛酸铋、钛酸铅、锆钛酸钡、锆钛酸铅。
进一步地，所述制备氧化物纳米粉体的方法包括水热法、溶胶-凝胶法。
进一步地，所述表面同质包覆的方法包括沉淀法、溶胶-凝胶法。
进一步地，所述介质包括水、乙酸或氨水。
进一步地，所述烧结过程的温度为180～300℃，时间为30min～3h。
进一步地，所述固相陶瓷的相对密度为85～99％。
本发明的有益效果在于：本发明采用表面包覆的方法，有效的增加了冷压烧结陶瓷的密度，且适应面广，适用于大部分氧化物陶瓷，得到的氧化物陶瓷的相对密度可以超过90％，且性能优异。此外，本发明减少了后续烧结工艺，工艺步骤简单，可操作性强，能使大部分氧化物陶瓷烧结温度降低到300℃以下，缩短了陶瓷制备周期，降低了生产能耗，减少生产成本。
附图说明
图1为本发明实施案例1中氧化物纳米粉体表面包覆的透射电镜照片。
图2为本发明实施案例2得到的氧化物陶瓷照片。
图3为本发明实施案例4得到的钛酸钡氧化物陶瓷的介电性能随温度的变化曲线。
具体实施方式
在本发明的描述中，需要说明的是，实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
下面结合附图和具体的实施例对本发明做进一步详细说明，所述是对本发明的解释而不是限定。
实施例1
本实施例提供一种制备二氧化硅陶瓷的冷压烧结方法，其中以溶胶-凝胶法制备二氧化硅纳米粉体，溶胶-凝胶法包覆，过程如下：
1、溶胶-凝胶法制备二氧化硅纳米粉体
将0.1mol正硅酸乙酯溶解于100ml乙醇中，搅拌10min后，以1滴/min的速度逐滴加入0.4mol去离子水，搅拌2小时，又以1滴/min的速度逐滴加入0.02mol氨水，搅拌3小时，随后静置一天陈化得到二氧化硅溶胶。二氧化硅溶胶在80℃下烘干24小时，得到的粉体400℃煅烧2小时得到二氧化硅纳米粉体。
2、溶胶-凝胶法包覆
将上述粉体分散在乙醇中，滴入5mol％上述二氧化硅溶胶，所得悬浊液90℃搅拌蒸发，然后120℃干燥12小时，所得粉体在400℃下煅烧2小时。
3、冷压烧结制备二氧化硅陶瓷
将包覆后的二氧化硅粉体放入干净研钵中，滴入30wt.％去离子水，并研磨1-2min，然后将研磨后的产物放入模具中，并套上加热套，固定在手动压片机上，使用手动压片机下施加压力400MPa，加热套加热至200℃，保持30min，然后停止加热，降温至室温，松压，取出的产物便是二氧化硅陶瓷。
包覆粉体效果如图1透射电镜照片所示，所得陶瓷密度如表1所示。
实施例2
本实施例提供一种制备氧化锆陶瓷的冷压烧结方法，其中以溶胶-凝胶法制备二氧化锆纳米粉体，沉淀法包覆，过程如下：
1、溶胶-凝胶法制备二氧化锆纳米粉体
以蒸馏水作为溶剂，称取定量氯氧化锆和硝酸钇(为稳定剂)，其中，硝酸钇质量按最终产物中氧化钇的掺杂量为3％(摩尔百分数)计算，配制0.5mol/L的氯氧化锆溶液。保持温度75℃左右，均匀缓慢滴加氨水，氨水的量按照n(Zr4+)∶n(NH3·H2O)＝1:2，氨水稍过量。逐步形成白色半透明溶胶，继续加热形成干凝胶，用蒸馏水洗涤干凝胶2次，再用无水乙醇洗涤后干燥，得到前驱体干凝胶，充分研磨后在650℃下煅烧2h，得到氧化锆粉体。
2、溶胶-凝胶法包覆
正丙醇锆、正丙醇、乙酰丙酮、去离子水摩尔比为1:50:0.5:10。先将正丙醇锆和乙酰丙酮分别溶于正丙醇中，分别超声振荡10分钟，然后将两种溶液混合搅拌60分钟，最后滴加去离子水，再搅拌60分钟，得到澄清透明二氧化锆溶胶。将氧化锆粉体分散于正丙醇中，滴加5mol％二氧化锆溶胶，所得悬浊液90℃搅拌蒸发，然后120℃干燥12小时，所得粉体在400℃下煅烧2小时。
3、冷压烧结制备氧化锆陶瓷
将上述包覆粉体放入干净研钵中，滴入30wt.％去离子水，并研磨1-2min，然后将研磨后的粉体放入模具中，并套上加热套，固定在手动压片机上，使用手动压片机下施加压力414MPa，加热套加热至200℃，保持1小时，然后停止加热，降温至室温，松压，取出的产物便是氧化锆陶瓷。
所得陶瓷照片如图2所示，密度如表1所示。
实施例3
本实施例提供一种制备钛酸钡陶瓷的冷压烧结方法，其中以水热法制备钛酸钡纳米粉体，沉淀法包覆，过程如下：
1、水热法制备钛酸钡纳米粉体
将0.01mol氢氧化钡在90℃下溶于25ml去离子水中，0.01mol钛酸四丁酯溶于25ml乙醇中，两种溶液混合，滴入氨水产生白色沉淀，将悬浊液倒入水热釜内胆中，填充率为60％，在200℃下反应24小时。反应完成后，将所得粉体清洗干燥。
2、沉淀法包覆
将醋酸钡和钛酸四丁酯溶于乙酸和乙二醇甲醚的混合溶剂中，配置0.2mol/LBaTiO3溶胶。将水热法制备的钛酸钡粉体分散在乙酸和乙二醇甲醚混合溶剂中，加入5mol％BaTiO3溶胶，然后滴入溶剂体积1.5倍的氨水，使溶胶沉淀，所得悬浊液90℃搅拌蒸发，然后120℃干燥12小时，所得粉体在600℃下煅烧2小时。
3、冷压烧结制备钛酸钡陶瓷
将上述包覆粉体放入干净研钵中，滴入30wt.％去离子水，并研磨1-2min，然后将研磨后的粉体放入模具中，并套上加热套，固定在手动压片机上，使用手动压片机下施加压力550MPa，加热套加热至230℃，保持3小时，然后停止加热，降温至室温，松压，取出的产物便是钛酸钡陶瓷，密度如表1所示。
实施例4
本实施例提供一种制备钛酸钡陶瓷的冷压烧结方法，其中以水热法制备钛酸钡纳米粉体，沉淀法包覆，过程同实施例3，区别在于：在冷压烧结制备钛酸钡陶瓷中，滴入30wt.％的氨水溶液，得到钛酸钡陶瓷，密度如表1所示。所得陶瓷的介电性能如图3所示，室温1kHz时，相对介电常数为1550。
实施例5
本实施例提供一种制备锆钛酸钡陶瓷的冷压烧结方法，其中以水热法制备锆钛酸钡纳米粉体，沉淀法包覆，过程如下：
1、水热法制备锆钛酸钡纳米粉体
将0.01mol氢氧化钡在90℃下溶于25ml去离子水中，0.002mol正丙醇锆和0.008mol钛酸四丁酯溶于25ml乙醇中，两种溶液混合，滴入氨水产生白色沉淀，将悬浊液倒入水热釜内胆中，填充率为60％，在200℃下反应24小时。反应完成后，将所得粉体清洗干燥。
2、沉淀法包覆
将一定比例的醋酸钡、正丙醇锆和钛酸四丁酯溶于乙酸和乙二醇甲醚的混合溶剂中，配置0.2mol/L BaZr0.2Ti0.8O3溶胶。将水热法制备的锆钛酸钡粉体分散在乙酸和乙二醇甲醚混合溶剂中，加入5mol％BaZr0.2Ti0.8O3溶胶，然后滴入溶剂体积1.5倍的氨水，使溶胶沉淀，所得悬浊液90℃搅拌蒸发，然后120℃干燥12小时，所得粉体在600℃下煅烧2小时。
3、冷压烧结制备锆钛酸钡陶瓷
将上述包覆粉体放入干净研钵中，滴入30wt.％去离子水，并研磨1-2min，然后将研磨后的粉体放入模具中，并套上加热套，固定在手动压片机上，使用手动压片机下施加压力550MPa，加热套加热至230℃，保持3小时，然后停止加热，降温至室温，松压，取出的产物便是钛酸锆钡陶瓷，密度如表1所示。
表1提供了所有实施例制备的陶瓷密度。
表1
综上，在本发明具体实施例中，通过在氧化物纳米粉体的表面包覆一层同质活性层，有效的提高了氧化物陶瓷的密度。
尽管上面已经示出和描述了本发明的实施例，可以理解的是，上述实施例是示例性的，不能理解为对本发明的限制，本领域的普通技术人员在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。
Claims (7)
1.一种制备氧化物陶瓷的冷压烧结方法，其特征在于，包括以下步骤：制备氧化物纳米粉体；将氧化物纳米粉体进行表面同质包覆；将包覆后的氧化物纳米粉体加入介质进行研磨；将研磨后的混合物放进模具中，对模具施加300MPa-2GPa的压力，并在100-300℃下烧结形成固相陶瓷。
2.根据权利要求1所述的一种制备氧化物陶瓷的冷压烧结方法，其特征在于，所述氧化物包括氧化硅、氧化锆、氧化锌、钛酸钡、钛酸铋、钛酸铅、锆钛酸钡、锆钛酸铅。
3.根据权利要求1所述的一种制备氧化物陶瓷的冷压烧结方法，其特征在于，所述制备氧化物纳米粉体的方法包括水热法、溶胶-凝胶法。
4.根据权利要求1所述的一种制备氧化物陶瓷的冷压烧结方法，其特征在于，所述表面同质包覆的方法包括沉淀法、溶胶-凝胶法。
5.根据权利要求1所述的一种制备氧化物陶瓷的冷压烧结方法，其特征在于，所述介质包括水、乙酸或氨水。
6.根据权利要求1所述的一种制备氧化物陶瓷的冷压烧结方法，其特征在于，所述烧结过程的温度为180～300℃，时间为30min～3h。
7.根据权利要求1所述的一种制备氧化物陶瓷的冷压烧结方法，其特征在于，所述固相陶瓷的相对密度为85～99％。
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