CN113443915A - 一种制备三元稀土二硼二碳陶瓷粉体的方法 - Google Patents

一种制备三元稀土二硼二碳陶瓷粉体的方法 Download PDF

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CN113443915A
CN113443915A CN202010227236.4A CN202010227236A CN113443915A CN 113443915 A CN113443915 A CN 113443915A CN 202010227236 A CN202010227236 A CN 202010227236A CN 113443915 A CN113443915 A CN 113443915A
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陈继新
李治辉
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Abstract

本发明涉及高性能陶瓷领域，具体为一种制备三元稀土二硼二碳陶瓷粉体的方法。采用硼/碳热还原法，原料为硼酸稀土粉、碳化硼粉和石墨粉；其中，硼酸稀土粉、碳化硼粉和石墨粉的摩尔比为(3.5～4.5):(0.8～1.5):(17.5～20.5)。首先，将硼酸稀土粉、碳化硼粉和石墨粉按配比称重，经物理机械方法混合6～12小时；然后，在通有高纯氩气的烧结炉内进行烧结，升温速率为5～20℃/分钟，烧结温度为1800～2200℃，烧结时间为0.5～5小时。本发明方法工艺简单，能制备出高纯度的三元稀土二硼二碳陶瓷粉体。

Description

一种制备三元稀土二硼二碳陶瓷粉体的方法
技术领域
本发明涉及结构陶瓷领域，具体为一种制备三元稀土二硼二碳陶瓷粉体的方法。
背景技术
三元稀土二硼二碳陶瓷材料即REB2C2(Re包括但不限于Sc,Y,La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu)，是三元稀土硼碳化合物庞大家族中的一大类别。REB2C2材料具有层状晶体结构，可以描述为RE片层与B2C2片层在c轴方向上交替堆垛而成。
目前，对REB2C2材料的制备方法主要有：电弧熔炼法、两步法、原位热压法和硼/碳热还原法。文献1：Journal of Inorganic and Nuclear Chemistry 1967,29:375-382中Smith P.K.等人用“电弧熔炼法”制备了GdB2C2材料，该方法可描述为：以纯的稀土RE(屑或块体)、B(块体或粉体)和C粉为原料，首先压制成块体，然后经过多次电弧熔炼制得GdB2C2材料。文献2：Journal of Physics:Conference Series 2009,150:052160中Michor H.等人用“两步法”制备了YB2C2材料，该方法可描述为：以纯的Y粉、B和C粉为原料，首先将Y粉和C粉混合烧制成YC2，然后加入B粉烧制得YB2C2材料。文献3：Scripta Materialia 2016,124:86-89中Zhao G.R.等人用“原位热压法”制备了YB2C2材料，该方法可描述为：以纯的YH2粉、B4C和C粉为原料，在1600℃下原位烧结制得YB2C2材料。专利1：公开号CN107814570A中，陈继新等人用“硼/碳热还原法”制备了REB2C2粉体，该方法可描述为：以纯的稀土氧化物粉、碳化硼粉和石墨粉为原料，高温烧结制得REB2C2粉体。
REB2C2材料在航空航天、核材料、燃料电池、电子信息、超高温结构件等高新技术领域都有着广泛的应用前景。因此，发展一种简单高效制备高纯度三元稀土二硼二碳陶瓷粉体的方法，对研究其性能及推广其应用具有重要的意义。
发明内容
本发明的目的在于提供一种制备三元稀土二硼二碳陶瓷粉体的方法，以“硼/碳热还原法”为基础，原料采用硼酸稀土粉、碳化硼粉和石墨粉，该方法工艺简单，能制备出高纯三元稀土二硼二碳陶瓷粉体。
本发明的技术方案是：
一种制备三元稀土二硼二碳陶瓷粉体的方法，采用硼/碳热还原法，原料为硼酸稀土粉、碳化硼粉和石墨粉；其中，硼酸稀土粉、碳化硼粉和石墨粉的摩尔比为(3.5～4.5):(0.8～1.5):(17.5～20.5)。
所述的制备三元稀土二硼二碳陶瓷粉体的方法，三元稀土二硼二碳陶瓷材料中的“稀土”是指“钪、钇、镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱和镥”之一或两种以上。
所述的制备三元稀土二硼二碳陶瓷粉体的方法，首先，将硼酸稀土粉、碳化硼粉和石墨粉按配比称重，经物理机械方法混合6～12小时；然后，在通有高纯氩气的烧结炉内进行烧结，升温速率为5～20℃/分钟，烧结温度为1800～2200℃，烧结时间为0.5～5小时。
所述的制备三元稀土二硼二碳陶瓷粉体的方法，硼酸稀土粉粒度为0.5～10微米，碳化硼粉和石墨粉的粒度范围为200～400目。
所述的制备三元稀土二硼二碳陶瓷粉体的方法，物理机械方法混合采用在氮化硅球磨罐中以无水乙醇为介质湿法球磨。
所述的制备三元稀土二硼二碳陶瓷粉体的方法，烧结方式为常压烧结。
本发明的设计思想是：基于专利公开号CN107814570A中“硼/碳热还原法”和氧化稀土粉制备REB2C2粉体的中间产物为硼酸稀土粉，本发明采用硼酸稀土粉代替氧化稀土粉。
本发明的优点及有益效果是：
1.本发明使用的原料简单，以硼酸稀土粉、碳化硼粉和石墨粉机械混合后的混合粉末作为原料。
2.工艺简单，成本低。本发明通过一步简单的常压烧结即可制得三元稀土二硼二碳陶瓷粉体。
3.与专利公开号CN107814570A的“硼/碳热还原法”和氧化稀土粉制备REB2C2粉体相比，本发明的所用的原料“硼酸稀土粉”不仅是氧化稀土粉制备REB2C2粉体的过渡产物，还是REB2C2水解产物。使用“硼酸稀土粉”不仅能制备出较纯的REB2C2粉，同时还能实现废物循环利用。
附图说明
图1为YbB2C2粉体的XRD衍射图。
图2为YbB2C2粉体扫描电镜图片。
图3为YB2C2粉体的XRD衍射图。
图4为YB2C2粉体扫描电镜图片。
具体实施方式
在具体实施过程中，本发明以硼酸稀土(REBO3)粉、碳化硼(B4C)粉和石墨(C)粉为原料制备REB2C2粉体，将适量配比的原料粉经物理机械方法混合6～12小时(h)，烘干、过筛后装入石墨坩埚，然后放入通有高纯氩气(Ar)的烧结炉内进行烧结，升温速率为5～20℃/分钟，烧结温度为1800～2200℃，烧结时间为0.5～5小时，获得三元稀土二硼二碳陶瓷粉体粒度为10～50微米。其在常压烧结过程中发生的化学反应为：
4REBO3+B4C+19C→4REB2C2+12CO
其中，REB2C2材料中的“稀土”(RE)是指：钪(Sc)、钇(Y)、镧(La)、铈(Ce)、镨(Pr)、钕(Nd)、钷(Pm)、钐(Sm)、铕(Eu)、钆(Gd)、铽(Tb)、镝(Dy)、钬(Ho)、铒(Er)、铥(Tm)、镱(Yb)和镥(Lu)等17种元素之一。
下面，通过实施例进一步详述本发明。
实施例1
本实施例中，YbBO3、B4C和C的摩尔比为4.0:1.3:18.2，制备过程为：将粒度为0.5微米的YbBO3粉45.81g、200目的B4C粉3.49g和200目的C粉10.70g装入氮化硅球磨罐中以无水乙醇为介质球磨6h，60℃烘干24h，过100目筛；随后装入石墨坩埚中，将石墨坩埚烧结炉中进行烧结，升温速率为20℃/分钟，升温至1800℃时保温5h，整个烧结过程在高纯氩气(氩气体积纯度在99.999％以上)保护下进行。如图1所示，将获得的反应产物进行XRD分析，可以发现制备材料为YbB2C2相。如图2所示，从扫描电镜照片可以发现，制备的粉体具有典型的片层结构，粉体粒度约10微米。
实施例2
本实施例中，YBO3、B4C和C的摩尔比为4.5:1.5:20.5，制备过程为：将粒度为10微米的YBO3粉40.14g、400目的B4C粉5.00g和400目的C粉14.86g装入氮化硅球磨罐中以无水乙醇为介质球磨12h，60℃烘干24h，过100目筛；随后装入石墨坩埚中，将石墨坩埚烧结炉中进行烧结，升温速率为5℃/分钟，升温至2200℃时保温0.5h，整个烧结过程在高纯氩气(氩气体积纯度在99.999％以上)保护下进行。如图3所示，将获得的反应产物进行XRD分析，可以发现制备材料为YB2C2相、少量石墨(C，Graphite)和少量未知相(unknown phase)，YB2C2相的质量分数约95％。如图4所示，从扫描电镜照片可以发现，制备的粉体具有典型的片层结构，粉体粒度约50微米。
实施例3
本实施例中，LaBO3、B4C和C的摩尔比为3.5:0.8:17.5，制备过程为：将粒度为5微米的LaBO3粉43.88g、300目的B4C粉2.80g和300目的C粉13.32g装入氮化硅球磨罐中以无水乙醇为介质球磨9h，60℃烘干24h，过100目筛，随后装入石墨坩埚中，将石墨坩埚烧结炉中进行烧结，升温速率为12℃/分钟，升温至2000℃时保温3h，整个烧结过程在高纯氩气(氩气体积纯度在99.999％以上)保护下进行，可获得LaB2C2粉体。制备的LaB2C2粉体具有典型的片层结构，粒度约30微米。
实施例结果表明，采用本发明方法能够实现制备三元稀土二硼二碳陶瓷粉体。采用本发明方法制备的材料具有较高的纯度(质量分数≥95％)，典型的片层结构，粉体粒度10～50微米。因此，该类材料在航空航天、核材料、燃料电池、电子信息、超高温结构件等高新技术领域都有着广泛的应用前景。

Claims (6)

1.一种制备三元稀土二硼二碳陶瓷粉体的方法，其特征在于，采用硼/碳热还原法，原料为硼酸稀土粉、碳化硼粉和石墨粉；其中，硼酸稀土粉、碳化硼粉和石墨粉的摩尔比为(3.5～4.5):(0.8～1.5):(17.5～20.5)。
2.按照权利要求1所述的制备三元稀土二硼二碳陶瓷粉体的方法，其特征在于，三元稀土二硼二碳陶瓷材料中的“稀土”是指“钪、钇、镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱和镥”之一或两种以上。
3.按照权利要求1所述的制备三元稀土二硼二碳陶瓷粉体的方法，其特征在于，首先，将硼酸稀土粉、碳化硼粉和石墨粉按配比称重，经物理机械方法混合6～12小时；然后，在通有高纯氩气的烧结炉内进行烧结，升温速率为5～20℃/分钟，烧结温度为1800～2200℃，烧结时间为0.5～5小时。
4.按照权利要求1或3所述的制备三元稀土二硼二碳陶瓷粉体的方法，其特征在于，硼酸稀土粉粒度为0.5～10微米，碳化硼粉和石墨粉的粒度范围为200～400目。
5.按照权利要求3所述的制备三元稀土二硼二碳陶瓷粉体的方法，其特征在于，物理机械方法混合采用在氮化硅球磨罐中以无水乙醇为介质湿法球磨。
6.按照权利要求3所述的制备三元稀土二硼二碳陶瓷粉体的方法，其特征在于，烧结方式为常压烧结。
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