CN106747468A - 用于气雾化钛及钛合金粉末的导液管材料及其制备方法 - Google Patents

用于气雾化钛及钛合金粉末的导液管材料及其制备方法 Download PDF

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CN106747468A
CN106747468A CN201611027625.2A CN201611027625A CN106747468A CN 106747468 A CN106747468 A CN 106747468A CN 201611027625 A CN201611027625 A CN 201611027625A CN 106747468 A CN106747468 A CN 106747468A
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titanium
powder
aerosolization
titanium alloy
drain tube
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CN106747468B (zh
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王鹏
李军
林崇智
朱阮利
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
Chengdu Advanced Metal Materials Industry Technology Research Institute Co Ltd
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Abstract

本发明公开了一种用于气雾化制备钛及钛合金粉末装置中的导液管材料及其制备方法。本发明的导液管材料为氧化钇(Y2O3)/六方氮化硼(hBN)陶瓷复合材料。以高纯Y2O3和hBN粉末为原料，与助熔剂、粘结剂、分散剂和去离子水制成预混液，充分研磨制得均匀、分散性好的浆料。浆料经造粒，干燥后得到粒径分布均匀、填充性能好的粉体，对造粒后的粉体经超声波辅助模压成形得到初坯，低温脱脂除去添加剂后进行冷等静压得到成分均匀、致密度高的素坯。最后，将素坯在氮气(N2)气氛下常压烧结得到Y2O3/hBN复合陶瓷导液管成品。本发明工艺简单，便于产业化，能够制备出与钛及钛合金化学反应活性低、热导率低、强度高、耐熔融钛及钛合金合金侵蚀的导液管。

Description

用于气雾化钛及钛合金粉末的导液管材料及其制备方法
技术领域
本发明涉及一种用于气雾化钛及钛合金粉末的导液管材料及其制备方法，属于耐火材料领域。
背景技术
随着钛及钛合金3D打印等新兴粉末成形技术的飞速发展，市场对钛及钛合金粉末的需要越来越多，而高端粒径窄的球形钛及钛合金粉末则是供不应求。当前，高端钛及钛合金粉末主要通过气雾化的方法制备。因气雾化装置中关键部件及材料尚未取得突破，造成了当前气雾化制备钛及钛合金粉末的成本高、产量低、稳定性差。
在气雾化制备钛及钛合金粉末技术中，除了喷嘴的结构设计以外，导液管材料是制约气雾化制备钛及钛合金粉末技术发展的瓶颈。导液管位于气雾化喷嘴的中心，是气雾化制备钛及钛合金粉末装置中的核心部件，钛及钛合金熔液经导液管到达喷嘴前端，经喷嘴高速气流的作用破碎成小液滴，小液滴在表面张力及快速冷却的作用下凝结成小球。因而，导液管是影响钛及钛合金粉体的重要因素。导液管的直径、与钛及钛合金熔液的润湿性、热强度、冲刷损耗等因素对钛及钛合金的粉体的粒径分布、球形度以及整个气雾化过程的稳定性等都具有重要的影响。
另一方面，导液管是熔融钛及合金从熔炼室进去雾化室的通道，因而它需要经受熔融钛及合金的物理侵蚀和化学反应。而钛是一种高化学活性元素，在高温熔融状态，它几乎能和目前常用的各种耐火材料发生反应，使得气雾化钛及钛合金的母材受到污染，制得的粉体内在质量降低。
因此，导液管材料是气雾化制备高端钛粉的关键。开发高性能导液管材料是当前迫切需要的，具有重大的现实意义。
本发明人发现因六方氮化硼(hBN)化学性质稳定，对大多数金属没有润湿性，不发生反应。将hBN与Y2O3进行复合形成的陶瓷复合材料可以满足导液管对材料的苛刻要求。
发明内容
本发明所要解决的技术问题是提供用于气雾化钛及钛合金粉末的导液管材料。
用于气雾化钛及钛合金粉末的导液管材料，该材料由如下组分制备而成：预活化hBN粉体、Y2O3粉体、助熔剂、粘结剂和分散剂；其中Y2O3粉体与预活化hBN粉体重量比为5:995～2:3，助熔剂加入量为Y2O3粉体与预活化hBN粉体总重量的0.02～8％，粘结剂加入量为Y2O3粉体与预活化hBN粉体总重量的0.01～5％，分散剂加入量为Y2O3粉体与预活化hBN粉体总重量的0.01～3％；
其中，所述的预活化hBN粉体是由hBN粉体在1500～2100℃氮气气氛中烧结0.5～6h，冷却，再将冷却后的hBN粉体研磨2～12h制得。
优选的，所述hBN粉体纯度大于99％，过300目筛；Y2O3粉体纯度大于99％，过300目筛。
其中，所述助溶剂为Al2O3、B2O3、CaF2中的一种或几种，粘结剂为聚乙烯醇、聚丙烯酸中的一种或两种，分散剂为聚丙烯酸铵、三乙醇胺、十六烷基三甲溴化铵中的一种或几种。
本发明制备用于气雾化钛及钛合金粉末的导液管材料的方法，包括以下步骤：
a、按照上述的用于气雾化钛及钛合金粉末的导液管材料的组分比例称取各原料，混合，得到混合物；
b、将上述a的混合物加去离子水研磨，得到浆料；
c、将上述浆料用离心喷雾干燥机造粒，得到前驱体粉体；
d、用超声波振动辅助压制前驱体粉体，在60～300MPa压力下模压成形得到初坯；
e、将初坯脱脂，进行冷等静压得到素坯；
f、将制备好的素坯置于N2气氛下常压烧结，N2流速为20～200ml/min，得到导液管材料。
优选的，步骤b中，混合物加去离子水用搅拌磨研磨3～12小时。
优选的，步骤c中，用离心喷雾干燥机造粒，干燥温度150～250℃，雾化器频率5000～20000r/min。
优选的，步骤d中，用超声波辅助模具压制，超声波振动功率为0.5～5KW。
优选的，步骤e中，脱脂在脱脂炉中进行，炉中温度为300～700℃，保温时间2～7小时，冷等静压压力为100～350MPa。
优选的，步骤f中，N2流速为20～30ml/min，升温速率为500～1000℃/h，温度保持在1600～2100℃，时间为10～36小时。
其中一种用于气雾化钛及钛合金粉末的导液管，用用于气雾化钛及钛合金粉末的导液管材料制得。
本发明的有益效果：
本发明通过hBN预活化处理、造粒和超声波辅助压制提高了用于气雾化钛及钛合金粉末的导液管材料的致密度和均匀性。
其中，导液管初坯模压成形过程中引入了超声波振动，缓解了压制过程中粉体颗粒间的拱桥效应，进一步提高了初坯的均匀性和致密度，最大密度差降低了0.09g/cm3，得到初坯致密度可达53％。
经脱脂、冷等静压得到成分均匀、形状完好的素坯，素坯的致密度可达63％。
制备好的素坯置于N2气氛下常压烧结，烧结后成品成分均匀、无裂纹，致密度可达到99.5％。
本发明工艺简单，便于产业化，过程易于控制、生产成本较低，能够制备出与钛及钛合金化学反应活性低、热导率低、强度高、耐熔融钛及合金侵蚀的导液管。
本发明制得的用于气雾化钛及钛合金粉末的导液管材料，还可以作为用于钛及钛合金精密铸造的壳模材料。
具体实施方式
用于气雾化钛及钛合金粉末的导液管材料，该材料由如下组分制备而成：预活化hBN粉体、Y2O3粉体、助熔剂、粘结剂和分散剂；其中Y2O3粉体与预活化hBN粉体重量比为5:995～2:3，助熔剂加入量为Y2O3粉体与预活化hBN粉体总重量的0.02～8％，粘结剂加入量为Y2O3粉体与预活化hBN粉体总重量的0.01～5％，分散剂加入量为Y2O3粉体与预活化hBN粉体总重量的0.01～3％；
其中，为了进一步的显著改善hBN颗粒的表面特性与形貌，增加了hBN颗粒的流动性，所述的预活化hBN粉体是由hBN粉体在1500～2100℃氮气气氛中烧结0.5～6h，冷却，再将冷却后的hBN粉体研磨2～12h制得。烧结可以在氮气气氛炉中进行。
优选的，所述hBN粉体纯度大于99％，过300目筛；Y2O3粉体纯度大于99％，过300目筛。
其中，所述助溶剂为Al2O3、B2O3、CaF2中的一种或几种，粘结剂为聚乙烯醇、聚丙烯酸中的一种或两种，分散剂为聚丙烯酸铵、三乙醇胺、十六烷基三甲溴化铵中的一种或几种。
本发明制备用于气雾化钛及钛合金粉末的导液管材料的方法，包括以下步骤：
a、按照上述的用于气雾化钛及钛合金粉末的导液管材料的组分比例称取各原料，混合，得到混合物；
b、将上述a的混合物加去离子水研磨，得到浆料；
c、将上述浆料用离心喷雾干燥机造粒，得到前驱体粉体；
d、用超声波振动辅助压制前驱体粉体，在60～300MPa压力下模压成形得到初坯；
e、将初坯脱脂，进行冷等静压得到素坯；
f、将制备好的素坯置于N2气氛下常压烧结，N2流速为20～200ml/min，得到导液管材料。
优选的，为了得到均匀、分散性好的浆料，步骤b中，混合物加去离子水用搅拌磨研磨3～12小时。
优选的，步骤c中，为了使前驱体粉体成球率高、表面光滑、粒径分布均匀、填充性能更好，用离心喷雾干燥机造粒，干燥温度150～250℃，雾化器频率5000～20000r/min。
优选的，为了能有效改善初坯的致密度和均匀性，降低最大密度差，步骤d中，用超声波辅助模具压制，超声波振动功率为0.5～5KW。其中，可以根据需要，选择不同的模具压制，比如用模具压制成导液管或者壳膜材料。
优选的，为了进一步去除初坯中的粘结剂和分散剂，得到成分均匀、致密度高的素坯，步骤e中，脱脂在脱脂炉中进行，炉中温度为300～700℃，保温时间2～7小时，冷等静压压力为100～350MPa。
优选的，为了得到无裂纹致密度高的成品，步骤f中，N2流速为20～30ml/min，升温速率为500～1000℃/h，温度保持在1600～2100℃，时间为10～36小时。
其中一种用于气雾化钛及钛合金粉末的导液管，用用于气雾化钛及钛合金粉末的导液管材料制得。
下面结合实施例对本发明的具体实施方式做进一步的描述，并不因此将本发明限制在所述的实施例范围之中。
实施例1 用于气雾化钛及钛合金粉末的导液管的制备
将纯度大于99％的hBN粉末和Y2O3粉末分别过300目筛。然后将hBN在1600℃的N2气氛炉中烧结3小时，冷却，再将冷却后的hBN在高能球磨机中湿磨6小时，取出干燥后得到预活化hBN粉体。将预活化hBN粉体与Y2O3粉体按92:8的重量比混合得到混合粉体，加入混合粉体总质量1.5％的Al2O3助熔剂、1％的聚乙烯醇、0.5％的聚丙烯酸铵和一定量的去离子水，用搅拌磨搅拌6小时得到浆料。浆料在离心喷雾干燥机中造粒(干燥温度为170℃，雾化器频率为12000r/min)，得到前驱体粉体。前驱体粉体在110MPa压力和1.5kW超声波振动功率下模压成形，然后在脱脂炉中600℃脱脂6小时后经350MPa冷等静压得到素坯，素坯的致密度62％，将素坯置于氮气气氛炉中，氮气流速为30ml/min，以600℃/h升温速率升高到1850℃保温22小时得到无裂纹的用于气雾化钛及钛合金粉末的导液管。
实施例2 用于气雾化钛及钛合金粉末的导液管的制备
将纯度大于99％的hBN粉末和Y2O3粉末分别过300目筛。再将hBN在1800℃的N2气氛炉中烧结1小时，冷却，再将冷却后的hBN在高能球磨机中湿磨2小时，取出干燥后得到预活化hBN粉体。将预活化hBN粉体与Y2O3粉体按96:4的重量比混合得到混合粉体，加入混合粉体总质量0.1％的B2O3助熔剂、0.1％的聚乙烯醇、0.5％的聚丙烯酸铵和一定量的去离子水。用搅拌磨搅拌3小时得到浆料。浆料在离心喷雾干燥机中造粒(干燥温度为150℃，雾化器频率15000r/min)，得到前驱体粉体。前驱体粉体在190MPa压力和0.8kW超声波振动功率下模压成形，然后在脱脂炉中350℃脱脂2小时后经250MPa冷等静压得到素坯，将素坯置于氮气气氛炉中，氮气流速为20ml/min，以800℃/h升温速率升高到2000℃保温10小时得到无裂纹的用于气雾化钛及钛合金粉末的导液管。

Claims (10)

1.用于气雾化钛及钛合金粉末的导液管材料，其特征在于该材料由如下组分制备而成：预活化hBN粉体、Y2O3粉体、助熔剂、粘结剂和分散剂；其中Y2O3粉体与预活化hBN粉体重量比为5:995～2:3，助熔剂加入量为Y2O3粉体与预活化hBN粉体总重量的0.02～8％，粘结剂加入量为Y2O3粉体与预活化hBN粉体总重量的0.01～5％，分散剂加入量为Y2O3粉体与预活化hBN粉体总重量的0.01～3％；
其中，所述的预活化hBN粉体是由hBN粉体在1500～2100℃氮气气氛中烧结0.5～6h，冷却，再将冷却后的hBN粉体研磨2～12h制得。
2.根据权利要求1所述的用于气雾化钛及钛合金粉末的导液管材料，其特征在于所述hBN粉体纯度大于99％，过300目筛；Y2O3粉体纯度大于99％，过300目筛。
3.根据权利要求1所述的用于气雾化钛及钛合金粉末的导液管材料，其特征在于所述助溶剂为Al2O3、B2O3、CaF2中的一种或几种，粘结剂为聚乙烯醇、聚丙烯酸中的一种或两种，分散剂为聚丙烯酸铵、三乙醇胺、十六烷基三甲溴化铵中的一种或几种。
4.制备权利要求1～3任一项所述的用于气雾化钛及钛合金粉末的导液管材料的方法，其特征在于，包括以下步骤：
a、按照权利要求1～3任一项所述的用于气雾化钛及钛合金粉末的导液管材料的组分比例称取各原料，混合，得到混合物；
b、将上述a的混合物加去离子水研磨，得到浆料；
c、将上述浆料用离心喷雾干燥机造粒，得到前驱体粉体；
d、用超声波振动辅助压制前驱体粉体，在60～300MPa压力下模压成形得到初坯；
e、将初坯脱脂，进行冷等静压得到素坯；
f、将制备好的素坯置于N2气氛下常压烧结，N2流速为20～200ml/min，得到导液管材料。
5.根据权利要求4所述的制备用于气雾化钛及钛合金粉末的导液管材料的方法，其特征在于步骤b中，混合物加去离子水用搅拌磨研磨3～12小时。
6.根据权利要求4～5任一项所述的制备用于气雾化钛及钛合金粉末的导液管材料的方法，其特征在于步骤c中用离心喷雾干燥机造粒，干燥温度150～250℃，雾化器频率5000～20000r/min。
7.根据权利要求4～6任一项所述的制备用于气雾化钛及钛合金粉末的导液管材料的方法，其特征在于步骤d中，用超声波辅助模具压制，超声波振动功率为0.5～5KW。
8.根据权利要求4～7任一项所述的制备用于气雾化钛及钛合金粉末的导液管材料的方法，其特征在于步骤e中，脱脂在脱脂炉中进行，炉中温度为300～700℃，保温时间2～7小时，冷等静压压力为100～350MPa。
9.根据权利要求4～8任一项所述的制备用于气雾化钛及钛合金粉末的导液管材料的方法，其特征在于步骤f中，N2流速为20～30ml/min，升温速率为500～1000℃/h，温度保持在1600～2100℃，时间为10～36小时。
10.一种用于气雾化钛及钛合金粉末的导液管，其特征在于由权利要求1～3所述用于气雾化钛及钛合金粉末的导液管材料制得。
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