CN107814570B - 硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法 - Google Patents
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Abstract
本发明涉及结构陶瓷领域，具体为一种硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法。采用稀土氧化物粉、碳化硼粉和石墨粉为原料，进行机械混合后，在加热炉内反应，升温速率为10～50℃/分钟，反应温度为1900～2100℃，反应时间为30分钟～2小时。采用本发明方法能够实现合成高纯三元稀土二硼二碳陶瓷粉体，具有原料成本低、操作简单、对工艺条件要求低的优点，并且为工业化生产奠定了良好的基础。
Description
技术领域
本发明涉及结构陶瓷领域，具体为一种硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法。
背景技术
三元稀土硼碳陶瓷材料即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。其晶体结构可以描述为RE片层与B2C2在c轴方向上交替堆垛而成(文献1J.Bauer等，Coordin.Chem.Rev.178(1998)723-753)。这一点与目前广泛研究的MAX相陶瓷极为相似，因此这类材料极有可能具有一些和MAX相陶瓷非常相似的性能，如：抗损伤、抗热震、可加工等(文献2，M.W.Barsoum,Prog.Solid State Chem.28(2000)201-81)。最近文献3(G.R.Zhao等Scripta Materialia,2016,124:86-89.)报道了REB2C2家族中的YB2C2具有优异的损伤容限及可加工性能。另外，文献4(A.Goldstein等J.Euro.Ceram.Soc.27(2007)695-700)报道，YB2C2在2180℃热处理条件下仍然可以稳定存在，说明这类材料有可能具有很好的耐超高温性能。因此，REB2C2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广泛的应用前景。
然而，目前关于此类材料合成及性能的报道非常少见，可能是由于其制备非常困难。通过分析目前很少的关于此类材料的文献可以发现，制备此类材料的方法主要为电弧熔炼和热压反应。对电弧熔炼而言，其以稀土金属粉，硼粉和石墨粉为原料，需要经过多次电弧熔炼，而后在2000℃长时间保温，成本昂贵、极其及耗时而且难以制备大尺寸、高纯度、高致密、均匀的块体材料。与电弧熔炼相比，热压反应可显著降低材料的制备成本，然而其制备过程中仍需使用稀土金属粉末，价格昂贵，不利于大规模的生产，极大地限制了对此类材料的研究及应用。
与稀土金属粉末相比，稀土氧化物粉具有价格低廉，来源广泛，易于保存等优点。因此，发展一种简单高效的利用硼/碳热还原法制备高纯度三元稀土二硼二碳陶瓷粉体的方法，对降低其生产成本，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硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法，能够实现廉价简单高效合成高纯三元稀土二硼二碳陶瓷粉体。
本发明的技术方案是：
一种硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法，具体步骤如下：
(1)原料组成及成分范围：
原料由稀土氧化物粉RE2O3、碳化硼粉B4C和石墨粉C组成，其中RE2O3：B4C：C的摩尔比为(0.9～1.1)：(0.9～1.1):(5.5～6.5)；
(2)制备工艺：
首先将稀土氧化物粉、碳化硼粉和石墨粉按配比称重，经物理机械方法混合8～24小时；在通有保护气氛的加热炉内进行原位反应，升温速率为10～50℃/分钟，反应温度为1900～2100℃，反应时间为30分钟～2小时，合成的材料为单相的稀土二硼二碳REB2C2陶瓷粉体。
所述的硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法，原位发生的化学反应为：
RE2O3+B4C+6C→2REB2C2+3CO。
所述的硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法，RE为稀土元素，包括但不限于周期表中原子序数从57到71号的稀土金属元素La,Ce,Pr,Nd,Sm,Eu,Gd,Dy,Ho,Er,Tm,Yb或Lu，或原子序数分别为21和39的稀土金属元素Sc和Y中的一种。
所述的硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法，稀土氧化物粉的粒度范围为50纳米～10微米，碳化硼粉的粒度范围为200～400目，石墨粉的粒度范围为200～400目。
所述的硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法，原位反应的保护气氛为氩气或氦气。
所述的硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法，物理机械方法混合为在聚氨酯球磨罐中干混或在酒精介质中球磨。
本发明的优点及有益效果是：
本发明方法以稀土氧化物粉，碳化硼粉和石墨粉为原料，合成了高纯的三元稀土二硼二碳陶瓷粉体，具有原料成本低、操作简单、对工艺条件要求低的优点，其工艺简单、效率高，为工业化生产奠定了良好的基础。
附图说明
图1为实施例1中反应产物的XRD分析图谱。图中，横坐标2θ为衍射角(degrees)；纵坐标为Intensity为强度(arb.units)。
图2为实施例1中反应产物的扫描电镜照片。
图3为实施例2中反应产物的XRD分析图谱。图中，横坐标2θ为衍射角(degrees)；纵坐标为Intensity为强度(arb.units)。
图4为实施例2中反应产物的扫描电镜照片。
图5为实施例3中反应产物的XRD分析图谱。图中，横坐标2θ为衍射角(degrees)；纵坐标为Intensity为强度(arb.units)。
图6为实施例3中反应产物的扫描电镜照片。
具体实施方式
在具体实施过程中，本发明硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法，原料由稀土氧化物粉(RE2O3)、碳化硼粉(B4C)和石墨粉(C)，其中RE2O3：B4C：C的摩尔比为(0.9～1.1):(0.9～1.1):(5.5～6.5)组成，在制备过程中，首先将稀土氧化物粉、碳化硼粉和石墨粉按配比称重，经物理机械方法混合8～24小时；在通有保护气氛的加热炉内反应，升温速率为10～50℃/分钟，反应温度为1900～2100℃，反应时间为30分钟～2小时，合成的材料为接近单相的稀土二硼二碳REB2C2陶瓷粉体。
下面，通过实施例和附图进一步详述本发明。
实施例1
本实施例中，将粒度为50纳米的氧化钇粉66.12克、300目的碳化硼粉14.71克和粒度为200目的石墨粉19.17克在玛瑙球磨罐中球磨24小时，之后装入石墨坩埚中，将石墨坩埚放入以石墨为发热体的电阻炉中，升温速率为20℃/分钟，加热到2000℃保温90分钟进行反应。整个反应过程都是在氩气保护下进行。本实施例中，将获得的反应产物进行XRD分析(见图1)，可以发现制备材料为YB2C2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。
实施例2
本实施例中，将粒度为1微米的氧化镝粉72.89克、400目的碳化硼粉11.87克和粒度为400目的石墨粉12.54克在聚氨酯球磨罐中球磨16小时，之后装入石墨坩埚中，将石墨坩埚放入以石墨为发热体的电阻炉中，升温速率为50℃/分钟，加热到1900℃保温2小时进行反应。整个反应过程都是在氩气保护下进行。本实施例中，将获得的反应产物进行XRD分析(见图3)，可以发现制备材料由单相DyB2C2组成。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。
实施例3
本实施例中，将粒度为10微米的氧化镱粉74.52克、400目的碳化硼粉11.61克和粒度为400目的石墨粉13.87克在聚氨酯球磨罐中球磨16小时，之后装入石墨坩埚中，将石墨坩埚放入以石墨为发热体的电阻炉中，升温速率为10℃/分钟，加热到2100℃保温30分钟进行反应。整个反应过程都是在氩气保护下进行。本实施例中，将获得的反应产物进行XRD分析(见图5)，可以发现制备材料由单相YbB2C2组成。如图6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。
实施例结果表明，采用本发明方法能够实现三元稀土二硼二碳陶瓷粉体的合成。采用本发明方法制备的粉体具有非常高的纯度，同时原料成本大幅度的降低。本发明为三元稀土二硼二碳陶瓷的大规模制备开辟了道路，对研究其性能及推广其应用具有重要的意义。因此，在航空航天、核工业、超高温结构件等高新技术领域有着广泛的应用前景。
Claims (6)
1.一种硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法，其特征在于，具体步骤如下：
(1)原料组成及成分范围：
原料由稀土氧化物粉RE2O3、碳化硼粉B4C和石墨粉C组成，其中RE2O3：B4C：C的摩尔比为(0.9～1.1)：(0.9～1.1):(5.5～6.5)；
(2)制备工艺：
首先将稀土氧化物粉、碳化硼粉和石墨粉按配比称重，经物理机械方法混合8～24小时；在通有保护气氛的加热炉内进行原位反应，升温速率为10～50℃/分钟，反应温度为1900～2100℃，反应时间为30分钟～2小时，合成的材料为单相的稀土二硼二碳REB2C2陶瓷粉体。
2.按照权利要求1所述的硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法，其特征在于，原位发生的化学反应为：
RE2O3+B4C+6C→2REB2C2+3CO。
3.按照权利要求1所述的硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法，其特征在于，RE为稀土元素，采用周期表中原子序数从57到71号的稀土金属元素La,Ce,Pr,Nd,Sm,Eu,Gd,Dy,Ho,Er,Tm,Yb或Lu，或原子序数分别为21和39的稀土金属元素Sc和Y中的一种。
4.按照权利要求1所述的硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法，其特征在于，稀土氧化物粉的粒度范围为50纳米～10微米，碳化硼粉的粒度范围为200～400目，石墨粉的粒度范围为200～400目。
5.按照权利要求1所述的硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法，其特征在于，原位反应的保护气氛为氩气或氦气。
6.按照权利要求1所述的硼/碳热还原法制备三元稀土二硼二碳陶瓷粉体的方法，其特征在于：物理机械方法混合为在聚氨酯球磨罐中干混或在酒精介质中球磨。
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