CN106966715A - 一种高抗热震性骨质瓷的制备方法 - Google Patents
一种高抗热震性骨质瓷的制备方法 Download PDFInfo
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Abstract
本发明涉及一种高抗热震性骨质瓷的制备方法，属于骨质瓷技术领域。本发明针对目前传统骨质瓷虽然具有瓷质洁白、透光度高、光泽柔和等优点，但是其抗热震性较差，限制了骨质瓷的使用的问题，本发明提供了一种利用碳酸钙及磷酸钙作为钙源，在三聚磷酸钠及磷酸钠的环境下，获得自制骨粉，自制骨粉中负载钴离子，增加热稳定性，同时获得自制骨粉具有良好的空间结构和晶型，提高了可缩性，降低了收缩率，随后通过煅烧后，与蒙脱土、长石等混合物，获得原料，通过添加白硼钙石补充钙，同时增加了硼及氧化锂，进一步提高了物料的热稳定性，最后通过压制、烧结，获得高抗热震性骨质瓷，本发明制备的高抗热震性骨质瓷具有高的抗热震性，良好的力学性能。
Description
技术领域
本发明属于瓷制品领域，具体涉及一种高抗热震性骨质瓷的制备方法。
背景技术
骨质瓷原称骨灰瓷，通常也简称为骨瓷，是采用动物骨灰经过脱脂漂洗、高温煅烧以及许多特殊工艺制备而成的。骨瓷属软质瓷，所使用的动物骨灰多为上等牛骨，因而骨瓷瓷质细腻、釉面光润、光泽柔和，有如脂似玉之感，极显雍容华贵，并具有较高的透明度和一定的机械强度。在日用陶瓷中，骨质瓷的应用非常广泛。
骨质瓷的性能与其物相组成密切相关，传统的骨质瓷瓷坯物相组成主要是磷酸三钙、钙长石及一定含量的磷酸盐玻璃相。具有瓷质洁白、透光度高、光泽柔和等优点，同时存在着抗热震性较差的不足，提高骨质瓷的抗热震性是提高骨质瓷质量的关键技术问题。
近年来，研究人员外骨质瓷进行了比较细致的研究分析，找出了骨质瓷显微结构组成特性与物理性能的关系，取得了一些研究成果，为提高骨质瓷的抗热震性地研究提供了一定的理论依据。但在解决骨质瓷抗热震性方面仍未有大的突破，而且传统骨质瓷由于受其配方特点的制约，其抗热震性差是影响骨质瓷质量的主要问题，也是限制骨质瓷使用的主要原因，此问题是多年来许多科研人员致力解决的技术难题。
发明内容
本发明所要解决的技术问题：针对目前传统骨质瓷虽然具有瓷质洁白、透光度高、光泽柔和等优点，但是其抗热震性较差，限制了骨质瓷的使用的问题，提供了一种高抗热震性骨质瓷的制备方法。
为解决上述技术问题，本发明采用如下所述的技术方案是：
一种高抗热震性骨质瓷的制备方法，具体制备步骤为：
（1）坯料原料：按重量份数计，取60～65份自制骨炭、32～34份蒙脱土、25～29份长石、13～16份白硼钙石、11～13份石英砂、3～6份氧化锂及2～7份腐植酸钠，混合均匀，得坯料原料；
（2）坯体制备：将步骤（1）中的坯料原料放入球磨机中，按料、球和水质量比1:3:1，向球磨机中加入钢球和水，进行球磨，得球磨混合物，再对球磨混合物进行磁选除铁，将磁选除铁后的球磨混合物过200目筛，得筛下物，在室温下陈腐，再将陈腐后的筛下物放入压滤机中进行压滤，得到滤饼，并把滤饼放入模具中压制成型，脱模，收集脱模物，得坯体；
（3）高抗热震性骨质瓷的制备：将步骤（2）中的坯体放入烧结炉中进行烧结，再进行抛光、吹尘，即可得高抗热震性骨质瓷。
所述步骤（1）中自制骨炭的制备方法为：
a、按重量份数计，取55～60份醋酸溶液、33～39份磷酸氢钙、12～15份碳酸钙、11～14份三聚磷酸钠、10～13份羟乙基纤维素及1～3份氯化钴，放入反应釜中，设定温度为90～95℃，搅拌30～40min，再向反应釜中加入羟乙基纤维素等质量的磷酸钠，升温至110～130℃，搅拌2～4h；
b、在上述搅拌结束后出料，得出料物，将出料物置于2～4℃下静置结晶，再进行过滤，得滤渣，并将滤渣置于105℃干燥箱中干燥，得干燥物，将干燥物进行粉碎，对粉碎物过200目筛，收集过筛颗粒，得自制骨粉；
c、将上述自制骨粉在1050～1100℃下，煅烧3～6h，收集煅烧物，得自制骨炭。
所述步骤（2）中陈腐时间为3～6天。
所述步骤（2）中压滤机的压力为20～23MPa。
所述步骤（2）中滤饼的含水量为12～18％。
所述步骤（3）中烧结温度为1170～1220℃，烧结时间为2～4h。
本发明有益技术效果是：
（1）本发明以碳酸钙及磷酸氢钙作为钙源，在三聚磷酸钠及磷酸钠的环境下形成羟基磷酸钙类物质，同时添加钴离子，结合钴离子，增加了自制骨粉的热稳定性，同时钴离子起到晶型调节物质的作用，使获得的自制骨粉具有良好的空间结构和晶型，通过煅烧获得自制骨炭，提高了可缩性，降低了收缩率，进而使制备的高抗热震性骨质瓷抗热震性能提高；
（2）本发明通过添加白硼钙石，作为钙源补充物，防止原料在制备过程中钙的损失，同时增加硼、锂等元素，进一步提高了物料的热稳定性，从而获得高抗热震性骨质瓷；
（3）本发明制得的高抗热震性骨质瓷在220℃至20℃热交换五次，无裂纹出现，吸水率为0.02～0.04％，白度为92.3～94.6％，抗弯曲强度达到130～132MPa。
具体实施方式
自制骨粉的制备：先按重量份数计，取55～60份质量分数为37％醋酸溶液、33～39份磷酸氢钙、12～15份碳酸钙、11～14份三聚磷酸钠、10～13份羟乙基纤维素及1～3份氯化钴，放入反应釜中，设定温度为90～95℃，以200r/min搅拌30～40min；再向反应釜中加入羟乙基纤维素等质量的磷酸钠，升温至110～130℃，搅拌2～4h，搅拌结束后，自然冷却至室温，进行出料，将出料物置于2～4℃冷藏室内静置40～50min，再进行过滤，得到滤渣，并将滤渣置于105℃干燥箱中，干燥7～9h，得干燥物，并放入粉碎机中进行粉碎，对粉碎物过200目筛，收集过筛颗粒，得自制骨粉。
自制骨炭的制备：将自制骨粉放入煅烧炉中，设定温度为1050～1100℃，煅烧3～6h，收集煅烧物，得自制骨炭。
高抗热震性骨质瓷的制备方法，按重量份数计，取如下原料，60～65份自制骨炭、32～34份蒙脱土、25～29份长石、13～16份白硼钙石、11～13份石英砂、3～6份氧化锂及2～7份腐植酸钠，放入球磨机中，按料、球和水质量比1:3:1，向球磨机中加入直径为60mm的钢球和水，以300r/min球磨6～9h，球磨结束后，将球磨机中的球磨混合物放入磁选机中磁选除铁3～5次，随后将除铁后的球磨混合物过200目筛，得到过筛物，并陈腐3～6天，再将陈腐后的过筛物放入压滤机中，以20～23MPa进行压滤，压至压滤物含水量至12～18％，得到滤饼，再将滤饼放入模具中，并将模具放入压机中压制成型，进行脱模，收集脱模物，得坯体，将坯体放入烧结炉中，设定温度为1170～1220℃，烧结2～4h，收集烧结物，进行抛光、吹尘，即可得高抗热震性骨质瓷。
实例1
按重量份数计，取如下原料，60份自制骨炭、32份蒙脱土、25份长石、13份白硼钙石、11份石英砂、3份氧化锂及2份腐植酸钠，放入球磨机中，按料、球和水质量比1:3:1，向球磨机中加入直径为60mm的钢球和水，以300r/min球磨6h，球磨结束后，将球磨机中的球磨混合物放入磁选机中磁选除铁3次，随后将除铁后的球磨混合物过200目筛，得到过筛物，并陈腐3天，再将陈腐后的过筛物放入压滤机中，以20MPa进行压滤，压至压滤物含水量至12％，得到滤饼，再将滤饼放入模具中，并将模具放入压机中压制成型，进行脱模，收集脱模物，得坯体，将坯体放入烧结炉中，设定温度为1170℃，烧结2h，收集烧结物，进行抛光、吹尘，即可得高抗热震性骨质瓷。
实例2
按重量份数计，取如下原料，63份自制骨炭、33份蒙脱土、27份长石、15份白硼钙石、12份石英砂、5份氧化锂及5份腐植酸钠，放入球磨机中，按料、球和水质量比1:3:1，向球磨机中加入直径为60mm的钢球和水，以300r/min球磨7h，球磨结束后，将球磨机中的球磨混合物放入磁选机中磁选除铁4次，随后将除铁后的球磨混合物过200目筛，得到过筛物，并陈腐5天，再将陈腐后的过筛物放入压滤机中，以21MPa进行压滤，压至压滤物含水量至15％，得到滤饼，再将滤饼放入模具中，并将模具放入压机中压制成型，进行脱模，收集脱模物，得坯体，将坯体放入烧结炉中，设定温度为1190℃，烧结3h，收集烧结物，进行抛光、吹尘，即可得高抗热震性骨质瓷。
实例3
按重量份数计，取如下原料，65份自制骨炭、34份蒙脱土、29份长石、16份白硼钙石、13份石英砂、6份氧化锂及7份腐植酸钠，放入球磨机中，按料、球和水质量比1:3:1，向球磨机中加入直径为60mm的钢球和水，以300r/min球磨9h，球磨结束后，将球磨机中的球磨混合物放入磁选机中磁选除铁5次，随后将除铁后的球磨混合物过200目筛，得到过筛物，并陈腐6天，再将陈腐后的过筛物放入压滤机中，以23MPa进行压滤，压至压滤物含水量至18％，得到滤饼，再将滤饼放入模具中，并将模具放入压机中压制成型，进行脱模，收集脱模物，得坯体，将坯体放入烧结炉中，设定温度为1220℃，烧结4h，收集烧结物，进行抛光、吹尘，即可得高抗热震性骨质瓷。
将上述实施例所得的高抗热震性骨质瓷进行检测，结果如表一所示。
检测仪器及方法为：白度检测仪，陶瓷吸水率检测仪（浸泡时间1～999h连续可调），用三点负荷法测定陶瓷材料室温抗弯强度。
表一：高抗热震性骨质瓷性能
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (6)
1.一种高抗热震性骨质瓷的制备方法，其特征在于具体制备步骤为：
（1）坯料原料：按重量份数计，取60～65份自制骨炭、32～34份蒙脱土、25～29份长石、13～16份白硼钙石、11～13份石英砂、3～6份氧化锂及2～7份腐植酸钠，混合均匀，得坯料原料；
（2）坯体制备：将步骤（1）中的坯料原料放入球磨机中，按料、球和水质量比1:3:1，向球磨机中加入钢球和水，进行球磨，得球磨混合物，再对球磨混合物进行磁选除铁，将磁选除铁后的球磨混合物过200目筛，得筛下物，在室温下陈腐，再将陈腐后的筛下物放入压滤机中进行压滤，得到滤饼，并把滤饼放入模具中压制成型，脱模，收集脱模物，得坯体；
（3）高抗热震性骨质瓷的制备：将步骤（2）中的坯体放入烧结炉中进行烧结，再进行抛光、吹尘，即可得高抗热震性骨质瓷。
2.根据权利要求1所述的一种高抗热震性骨质瓷的制备方法，其特征在于：所述步骤（1）中自制骨炭的制备方法为：
a、按重量份数计，取55～60份醋酸溶液、33～39份磷酸氢钙、12～15份碳酸钙、11～14份三聚磷酸钠、10～13份羟乙基纤维素及1～3份氯化钴，放入反应釜中，设定温度为90～95℃，搅拌30～40min，再向反应釜中加入羟乙基纤维素等质量的磷酸钠，升温至110～130℃，搅拌2～4h；
b、在上述搅拌结束后出料，得出料物，将出料物置于2～4℃下静置结晶，再进行过滤，得滤渣，并将滤渣置于105℃干燥箱中干燥，得干燥物，将干燥物进行粉碎，对粉碎物过200目筛，收集过筛颗粒，得自制骨粉；
c、将上述自制骨粉在1050～1100℃下，煅烧3～6h，收集煅烧物，得自制骨炭。
3.根据权利要求1所述的一种高抗热震性骨质瓷的制备方法，其特征在于：所述步骤（2）中陈腐时间为3～6天。
4.根据权利要求1所述的一种高抗热震性骨质瓷的制备方法，其特征在于：所述步骤（2）中压滤机的压力为20～23MPa。
5.根据权利要求1所述的一种高抗热震性骨质瓷的制备方法，其特征在于：所述步骤（2）中滤饼的含水量为12～18％。
6.根据权利要求1所述的一种高抗热震性骨质瓷的制备方法，其特征在于：所述步骤（3）中烧结温度为1170～1220℃，烧结时间为2～4h。
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