CN111138173A - 一种快速成型制备低温烧结陶瓷复合材料的方法 - Google Patents

一种快速成型制备低温烧结陶瓷复合材料的方法 Download PDF

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CN111138173A
CN111138173A CN202010161277.8A CN202010161277A CN111138173A CN 111138173 A CN111138173 A CN 111138173A CN 202010161277 A CN202010161277 A CN 202010161277A CN 111138173 A CN111138173 A CN 111138173A
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张小立
郭颖
段佳玮
王熠柔
成小哲
刘�英
刘磊
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Zhongyuan University of Technology
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Abstract

本发明提供了一种快速成型制备低温烧结陶瓷复合材料的方法，本发明使用檬酸铵和聚丙烯酸铵作分散剂，氨水和盐酸调节剂pH值，柠檬酸钙做固化剂，使用二氧化钛作为活化烧结助剂，得到了快速成型的氧化铝氧化锆复合材料，并低温烧结致密。该方法可连续生产，并适用于工业规模。

Description

一种快速成型制备低温烧结陶瓷复合材料的方法
技术领域
本发明涉及陶瓷制备领域，具体涉及一种快速成型制备低温烧结陶瓷复合材料的方法。
背景技术
氧化锆的熔点高达2700℃，耐热性、耐蚀性优良，热导率在常见的陶瓷材料中最低（λ=16.8W•m-1•K-1），热膨胀系数又最大（10-6K-1），与金属材料较为接近，完全稳定化氧化锆（FSZ）易产生较高的热应力，但部分稳定氧化锆（PSZ）具有强度高，脆性低，较高的断裂韧性，被认为是发动机上最有前途的陶瓷材料。
氧化铝（Al2O3）在不添加其他助剂的条件下，高温条件下达到约2054℃时开始融化，达到2980℃呈沸腾状态，在高温情况下不易与其他物质发生反应的现象说明热稳定性和化学稳定性较好。氧化铝业作为一种高硬度化合物，普遍运用在陶瓷、化工及电子等行业，是目前氧化物陶瓷中用处最广的陶瓷材料。
氧化铝和氧化锆在高温下能共熔，并且氧化铝颗粒的存在还有助于氧化锆四方相的保留，对其增韧有促进作用。氧化锆/氧化铝复合材料，因具有优良的力学性能和热力学性能，近年来受到普遍重视。
从增韧机理来分析，氧化锆的相变增韧作用和氧化铝的弥散增韧可以叠加。氧化铝对裂纹的钉扎，弥补了微裂纹对强度的消极作用，因而使得复合陶瓷的抗弯强度和断裂韧性的极值逐渐出现在同一烧成温度。
再者，由于氧化铝的热膨胀系数约为8*10-6℃-1，小于氧化锆热膨胀系数，所以氧化锆在氧化铝基体中分布时，氧化铝晶体处于压应力状态，氧化铝和氧化锆在晶界处结合良好，具有良好的晶界强度，使裂纹不易在氧化铝和氧化锆晶界形成，因此，氧化铝和氧化锆的混合，使晶界得到强化，从而使复合陶瓷的抗弯强度、断裂韧性得到显著提高。
目前，氧化锆和氧化铝复合材料作为高温涂层得到广泛应用。对于块材，通常要进行高温烧结。
发明内容
本发明提出了一种快速成型制备低温烧结陶瓷复合材料的方法，解决了现有复合材料需要高温烧结的问题。
实现本发明的技术方案是：
一种快速成型制备低温烧结陶瓷复合材料的方法，以氧化铝及氧化锆作为陶瓷粉体，柠檬酸铵和聚丙烯酸铵作分散剂，氨水和盐酸调节剂pH值，柠檬酸钙做固化剂，使用二氧化钛作为活化烧结助剂，得到快速成型的低温烧结陶瓷复合材料。
所述的快速成型制备低温烧结陶瓷复合材料的方法，具体步骤如下：
（1）将陶瓷粉体氧化铝、氧化锆、聚丙烯酸铵、柠檬酸铵和二氧化钛放入研磨钵中，使用研磨棒研磨30-60min，混料均匀，得到陶瓷悬浮体；
（2）调节步骤（1）陶瓷悬浮体的pH值；
（3）向步骤（2）得到的陶瓷悬浮体中加入固化剂柠檬酸钙，搅拌均匀注入锡纸模具中，室温静置8-10h至样品固化；
（4）将步骤（3）固化样品置于马弗炉中烧结获得低温烧结陶瓷复合材料。
所述步骤（1）中氧化铝、氧化锆、聚丙烯酸铵、柠檬酸铵和二氧化钛的重量份分别是：60-90份、10-40份、2-4份、1-3份、0.5-2份，步骤（3）固化剂柠檬酸钙的重量份是0.5-2份。
所述步骤（2）中利用1-2 mol/L的盐酸和氨水调节pH值为8-9。
所述步骤（4）中烧结温度为1200-1450℃，烧结时间为200-400min。
本发明的有益效果是：本发明使用檬酸铵和聚丙烯酸铵作分散剂，氨水和盐酸调节剂PH值，柠檬酸钙做固化剂，使用二氧化钛作为活化烧结助剂，得到了快速成型的氧化铝氧化锆复合材料，并低温烧结致密。该方法可连续生产，并适用于工业规模。
具体实施方式
下面将结合本发明实施例，对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有付出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种快速成型制备低温烧结陶瓷复合材料的方法，步骤如下：
称取氧化铝18.001g，柠檬酸铵0.127g，氧化锆2.007g，聚丙烯酸铵0.170g，二氧化钛0.847g，放入研磨钵中，使用研磨棒使其混料均匀，研磨时间约为60min，接着采用2 mol/L的盐酸和氨水调节陶瓷悬浮体的pH值。将制备好的陶瓷悬浮体添加固化剂柠檬酸钙0.848g搅拌至均匀状态，注入40×5×5mm锡纸模具中。在室温静置10h至样品固化完成，每组配料需要制备6个样品，防止后续实验中出现样品损坏。
以上样品放入1450℃马弗炉中烧结获得致密复合材料。
实施例2
一种快速成型制备低温烧结陶瓷复合材料的方法，步骤如下：
称取氧化铝15.000g，柠檬酸铵0.127g，氧化锆5.002g，聚丙烯酸铵0.169g，二氧化钛0.847g。放入研磨钵中，使用研磨棒使其混料均匀，研磨时间约为60min，接着采用 2 mol/L的盐酸和氨水调节陶瓷悬浮体的 pH 值。将制备好的陶瓷悬浮体添加柠檬酸钙0.848g搅拌至均匀状态，注入40×5×5mm锡纸模具中。在室温静置10h至样品固化完成，每组配料需要制备6个样品，防止后续实验中出现样品损坏。
以上样品放入1400℃马弗炉中烧结200min获得致密复合材料。
实施例3
一种快速成型制备低温烧结陶瓷复合材料的方法，步骤如下：
称取氧化铝15g，柠檬酸铵0.25g，氧化锆2.5g，聚丙烯酸铵0.5g，二氧化钛0.1255g，放入研磨钵中，使用研磨棒使其混料均匀，研磨时间约为30min；
接着采用1mol/L的盐酸和氨水调节陶瓷悬浮体的 pH 值为8；
将制备好的陶瓷悬浮体添加固化剂柠檬酸钙0.125g搅拌至均匀状态，注入40×5×5mm锡纸模具中。在室温静置8h至样品固化完成，每组配料需要制备6个样品，防止后续实验中出现样品损坏。
以上样品放入1200℃马弗炉中烧结400min获得致密复合材料。
实施例4
一种快速成型制备低温烧结陶瓷复合材料的方法，步骤如下：
称取氧化铝22.5g，柠檬酸铵0.75g，氧化锆10g，聚丙烯酸铵1g，二氧化钛0.5g，放入研磨钵中，使用研磨棒使其混料均匀，研磨时间约为45min；
接着采用1.5 mol/L的盐酸和氨水调节陶瓷悬浮体的 pH值为9；
将制备好的陶瓷悬浮体添加柠檬酸钙0.5g搅拌至均匀状态，注入40×5×5mm锡纸模具中。在室温静置9h至样品固化完成，每组配料需要制备6个样品，防止后续实验中出现样品损坏。
以上样品放入1300℃马弗炉中烧结350min获得致密复合材料。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (5)

1.一种快速成型制备低温烧结陶瓷复合材料的方法，其特征在于：以氧化铝及氧化锆作为陶瓷粉体，柠檬酸铵和聚丙烯酸铵作分散剂，氨水和盐酸调节剂pH值，柠檬酸钙做固化剂，使用二氧化钛作为活化烧结助剂，得到快速成型的低温烧结陶瓷复合材料。
2.根据权利要求1所述的快速成型制备低温烧结陶瓷复合材料的方法，其特征在于具体步骤如下：
（1）将陶瓷粉体氧化铝、氧化锆、聚丙烯酸铵、柠檬酸铵和二氧化钛放入研磨钵中，使用研磨棒研磨30-60min，混料均匀，得到陶瓷悬浮体；
（2）调节步骤（1）陶瓷悬浮体的pH值；
（3）向步骤（2）得到的陶瓷悬浮体中加入固化剂柠檬酸钙，搅拌均匀注入锡纸模具中，室温静置8-10h至样品固化；
（4）将步骤（3）固化样品置于马弗炉中烧结获得低温烧结陶瓷复合材料。
3.根据权利要求2所述的快速成型制备低温烧结陶瓷复合材料的方法，其特征在于：所述步骤（1）中氧化铝、氧化锆、聚丙烯酸铵、柠檬酸铵和二氧化钛的重量份分别是：60-90份、10-40份、2-4份、1-3份、0.5-2份，步骤（3）中固化剂柠檬酸钙的重量份是0.5-2份。
4.根据权利要求2所述的快速成型制备低温烧结陶瓷复合材料的方法，其特征在于：所述步骤（2）中利用1-2 mol/L的盐酸和氨水调节pH值为8-9。
5.根据权利要求2所述的快速成型制备低温烧结陶瓷复合材料的方法，其特征在于：所述步骤（4）中烧结温度为1200-1450℃，烧结时间为200-400min。
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