CN107021741A - 一种烧制陶瓷的方法 - Google Patents
一种烧制陶瓷的方法 Download PDFInfo
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Abstract
本发明公开一种烧制陶瓷的方法，属于烧制陶瓷技术领域。本发明所述方法采用镓作为陶瓷烧结时的承载体，即将镓盛在氧化锆坩埚中，再将生坯放在其上，然后放入炉子进行烧结。本发明所述方法可以极大改善传统烧制方法带来的不足。镓的熔点为29.8℃，沸点为2204℃，密度为5.904g/cm3，当生坯烧结时镓会熔化为液体，而陶瓷的密度一般小于5.904g/cm3，所以生坯会漂浮其上，进而改善了炉膛温场不均的问题，使陶瓷受热更加均匀，烧制出的陶瓷致密度好，尺寸变化不大，基本达到近终成型，而且烧制时液体会给生坯提供浮力，有效的改善了样品的坍塌问题。
Description
技术领域
本发明涉及一种烧制陶瓷的方法，属于烧制陶瓷技术领域。
背景技术
陶瓷是最古老的一种材料，是人类在征服自然中获得的经化学变化而制成的产品，是人类文明的象征之一。它和金属材料、高分子材料并列为当代固体三大材料。 由于陶瓷的原子结合方式是键能较大的离子键、共价键或者离子－共价混合键，所以其具有耐高温、耐腐蚀、耐磨损、耐热冲击、高强度、硬质、高刚性、低膨胀、隔热以及不吸收外来物质等许多优良性质。陶瓷材料的应用范围很广，在日用、卫生、建筑、化工、电气、航天、汽车、生物医学等领域均有重要应用。不仅如此，陶瓷材料潜在的应用对经济也会有很大影响。
传统方法在陶瓷烧制过程中，受热不均匀，容易使陶瓷破裂及坍塌，陶瓷烧结后尺寸变化较大，不能近终成型，有些领域要求陶瓷尺寸误差小，传统的烧结方法不能满足，因此也制约了陶瓷在很多领域的发展。
发明内容
本发明的目的在于提供一种烧制陶瓷的方法，具体包括以下步骤：
（1）制样：将粉体原料按比例称量，加入粘结剂，球磨、干燥、过筛、造粒后制成生坯；
（2）烧结：将镓盛在氧化锆坩埚中，再将生坯放在其上，烧结后随炉冷却得到所需陶瓷。
本发明所述方法适用于烧结温度小于2100℃且密度小于5.904g/cm3的陶瓷，因为镓的沸点为2204℃，温度过高会使镓沸腾，从而影响烧结，而如果密度大于镓的密度，即大于5.904g/cm3，生坯会沉入镓液体中，从而影响烧结效果。
本发明步骤（1）粘结剂为陶瓷制备过程中的常规粘结剂，例如聚乙烯醇（ PVA ） 、聚乙二醇、甲基纤维素等，粘结剂质量分数为5%~10%，添加量为粉体质量的6%~10%。
本发明步骤（1）球磨过程为常规方法，优选的，球磨过程中球磨机的转速为300 r/min~500 r/min，球磨时间为12~24 h。
优选的，本发明步骤（1）干燥后过100目筛。
优选的，本发明步骤（1）成型方式为冷等静压成型，成型压力为180~200 MPa，压力作用时间为1~4 min。
优选的，本发明步骤（1）中干燥的条件为：干燥温度为100℃，干燥时间10~22 h。
优选的，本发明步骤（2）所述烧结温度为1400~2100℃，烧结温度保温时间为1~3h。
本发明的原理为：本发明采用镓作为陶瓷烧结时的承载体，即将镓盛在氧化锆坩埚中，再将生坯放在其上进行烧结，烧结时镓会熔化为液体，生坯会漂浮其上，从而改善了炉膛温场不均的问题，使陶瓷受热更加均匀，烧制出的陶瓷致密度好，尺寸变化不大，基本达到近终成型，而且烧制时液体会给生坯提供浮力，有效的改善了样品的坍塌问题。
本发明的有益效果为：
（1）采用镓作为陶瓷烧结时的承载体，烧制出的陶瓷更加致密。
（2）采用镓作为陶瓷烧结时的承载体，烧制出的陶瓷近终成型。
（3）采用镓作为陶瓷烧结时的承载体，烧制出的陶瓷硬度更高。
（4）采用镓作为陶瓷烧结时的承载体，烧制出的陶瓷抗弯强度更高。
综上所述，本发明操作简单，对实验条件要求低，效果明显，而且对比传统烧制方法烧制出的陶瓷，优点明显，此发明不仅可以提高陶瓷的致密性、硬度、抗弯强度，而且使陶瓷近终成型，是陶瓷烧结方法的一个重大突破。
附图说明
图1为实施例1未用镓作为载体烧制陶瓷的SEM图；
图2为实施例1用镓作为载体烧制陶瓷的SEM图；
图3为实施例5未用镓作为载体烧制陶瓷的SEM图；
图4为实施例5用镓作为载体烧制陶瓷的SEM图。
具体实施方式
下面通过具体实施方式对本发明作进一步说明，但本发明的保护范围并不限于以下内容。
实施例1
（1）称取Al2O3粉99.0 g，MgO粉0.4 g，SiO2粉0.6 g，加入8 g质量分数为7%的PVA水溶液，在无水乙醇中混合后，置于转速为350 r/min的行星式球磨机中球磨16 h，将球磨好的混合物在100℃下干燥18 h后过100目筛，造粒，然后在200MPa的冷等静压下保压时间为4min，压制成型。
（2）将生坯放在盛有镓的氧化锆坩埚中，以5℃/min升温至550℃，保温1 h，然后以10℃/min升温至1600℃，保温2 h，随炉冷却至40℃。
表1为本实施例各项数据对比
本实施例制得的陶瓷致密度更好，增加了0.6%，硬度更好，增加了1.5 GPa，抗弯强度更好，增加了13.5MPa，而且尺寸收缩小，近终成型。
本实施例制备得到的陶瓷SEM图如图2所示，未用镓作为载体烧制陶瓷的SEM图如图1所示，对比以后可以看出本实施例制得的陶瓷致密度更好。
实施例2
（1）称取Al2O3粉99.0 g，TiO2粉0.8 g，La2O3粉0.2 g，加入6 g质量分数为9%的甲基纤维素水溶液，在无水乙醇中混合后，置于转速为400 r/min的行星式球磨机中球磨12 h，将球磨好的混合物在100℃下干燥22 h后过100目筛，造粒，然后在190 MPa的冷等静压下保压时间为2 min，压制成型。
（2）将生坯放在盛有镓的氧化锆坩埚中，以5℃/min升温至550℃，保温1 h，然后以10℃/min升温至1400℃，保温3 h，随炉冷却至40℃。
表2为本实施例各项数据对比
本实施例制得的陶瓷致密度好，力学性能良好，而且尺寸收缩小，基本近终成型。
实施例3
（1）称取Al2O3粉4.8 g，B4C粉86.2 g，TiC粉9.0 g，加入7 g质量分数为8%的聚乙二醇水溶液，在无水乙醇中混合后，置于转速为500 r/min的行星式球磨机中球磨24 h，将球磨好的混合物在100℃下干燥10 h后过100目筛，造粒，然后在200 MPa的冷等静压下保压时间为1 min，压制成型。
（2）将生坯放在盛有镓的氧化锆坩埚中，以5℃/min升温至550℃，保温1 h，然后以10℃/min升温至1900℃，保温1 h，随炉冷却至40℃。
表3为本实施例各项数据对比
本实施例制得的陶瓷致密度更好，增加了0.7%，硬度更好，增加了3.3GPa，抗弯强度更好，增加了16.1MPa，而且尺寸收缩小，近终成型。
实施例4
（1）称取SiC粉97.0 g，B4C粉3.0 g，加入10 g质量分数为5%的聚乙二醇水溶液，在无水乙醇中混合后，置于转速为300 r/min的行星式球磨机中球磨20 h，将球磨好的混合物在100℃下干燥18 h后过100目筛，造粒，然后在200 MPa的冷等静压下保压时间为3 min，压制成型。
（2）将生坯放在盛有镓的氧化锆坩埚中，以5℃/min升温至550℃，保温1 h，然后以10℃/min升温至2100℃，保温2h，随炉冷却至40℃。
表4为本实施例各项数据对比
本实施例制得的陶瓷致密度更好，增加了0.6%，硬度更好，增加了1.3GPa，抗弯强度更好，增加了20.0MPa，而且尺寸收缩小，近终成型。
实施例5
（1）称取Al2O3粉99.0 g，MgO粉0.75 g，La2O3粉0.25 g，加入8 g质量分数为10 %的PVA水溶液，在无水乙醇中混合后，置于转速为450 r/min的行星式球磨机中球磨18 h，将球磨好的混合物在100℃下干燥14 h后过100目筛，造粒，然后在180 MPa的冷等静压下保压时间为3 min，压制成型。
（2）将生坯放在盛有镓的氧化锆坩埚中，以5℃/min升温至550℃，保温1 h，然后以10℃/min升温至1700℃，保温1 h，随炉冷却至40℃。
表5为本实施例各项数据对比
本实施例制得的陶瓷致密度更好，增加了0.8%，硬度更好，增加了1.9GPa，抗弯强度更好，增加了15.6MPa，而且尺寸收缩小，近终成型。
本实施例制备得到的陶瓷SEM图如图3所示，未用镓作为载体烧制陶瓷的SEM图如图4所示，对比以后可以看出本实施例制得的陶瓷致密度更好。
Claims (3)
1.一种烧制陶瓷的方法，其特征在于，具体包括以下步骤：
（1）制样：将粉体原料按比例称量，加入粘结剂，球磨、干燥、过筛、造粒后制成生坯；
（2）烧结：将镓盛在氧化锆坩埚中，再将生坯放在其上，烧结后随炉冷却得到所需陶瓷。
2.根据权利要求1所述烧制陶瓷的方法，其特征在于：步骤（2）所述烧结温度为1400~2100℃，烧结温度保温时间为1~3 h。
3.根据权利要求1所述烧制陶瓷的方法，其特征在于：步骤（1）中成型方式为冷等静压成型，成型压力为180~200 MPa，压力作用时间为1~4 min。
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