CN114685168B - 一种B4C-TiB2导电复相陶瓷及其制备方法 - Google Patents

一种B4C-TiB2导电复相陶瓷及其制备方法 Download PDF

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CN114685168B
CN114685168B CN202210485924.XA CN202210485924A CN114685168B CN 114685168 B CN114685168 B CN 114685168B CN 202210485924 A CN202210485924 A CN 202210485924A CN 114685168 B CN114685168 B CN 114685168B
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complex phase
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CN114685168A (zh
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冉松林
赵峻
金星
王东
丁祥
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Anhui University of Technology AHUT
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Abstract

本发明公开了一种B4C‑TiB2导电复相陶瓷及其制备方法，属于陶瓷材料领域。该导电复相陶瓷具有包覆型显微结构的，其中TiB2的体积含量为10‑30％。该导电复相陶瓷制备原料为：B4C、TiC和无定形B粉体，其制备步骤是：按照成分设计配比分别称取原料粉体；混合均匀后充分干燥；使用放电等离子烧结炉在真空气氛中烧结制备复相陶瓷，烧结温度为2000℃，压力为50MPa，保温时间为5‑20min。本发明构筑了TiB2小晶粒包覆B4C大晶粒的包覆型显微结构，有利导电网络的形成和完善。在相同TiB2含量下，本发明制备的B4C‑TiB2复相陶瓷具有更高的电导率。本发明制备过程简单，无需任何其它特殊复杂方法。与传统方法相比，本发明所制备的B4C‑TiB2复相陶瓷的力学性能相当或更优。

Description

一种B4C-TiB2导电复相陶瓷及其制备方法
技术领域
本发明属于陶瓷材料技术领域，具体涉及一种B4C-TiB2导电复相陶瓷及其制备方法。
背景技术
B4C具有高硬度、低密度、良好的化学稳定性和较大的中子吸收截面等特性，广泛应用于防弹装甲、耐磨器件、航空航天及核工业等领域。由于B4C的共价键组成，其烧结性能差，很难实现致密化。同时，较低的断裂韧性也使单相B4C陶瓷的加工效率、精度和成本很难满足工业应用的需求。
在B4C基体中引入第二相TiB2形成B4C-TiB2复相陶瓷，不仅可以显著改善 B4C陶瓷的烧结性能和力学性能，还可大幅度降低陶瓷的电阻率，使其满足电火花加工技术(EDM)的要求。一般说来，材料的电阻率越低，其EDM加工性能就越好。因此，降低B4C-TiB2复相陶瓷的电阻率是提高其EDM加工性能的关键。提高复相陶瓷中导电相的含量是降低其电阻率最有效的方法。但是，对于B4C-TiB2复相陶瓷而言，增加导电TiB2相的含量会带来三个问题：(1)增加了复相陶瓷的密度(TiB2密度约为B4C的1.8倍)；(2)降低了复相陶瓷的硬度(TiB2硬度比B4C低)；(3)增加原料成本。以上问题都限制了B4C-TiB2复相陶瓷在轻质装甲领域的应用。可以看出，常规方法降低B4C-TiB2复相陶瓷的电阻率都是以牺牲材料其它性能或增加制备成本为代价实现的。
发明内容
为克服现有技术的不足，本发明所要解决的问题是：提供一种具有包覆型显微结构的B4C-TiB2导电复相陶瓷及其制备方法，以期在低TiB2含量下实现复相陶瓷的高导电性。
本发明是通过以下技术方案予以实现的。
本发明一种B4C-TiB2导电复相陶瓷，其具有包覆型显微结构，即TiB2小晶粒包覆在B4C大晶粒周围；该导电复相陶瓷中TiB2的体积含量为10-30％。
本发明同时提供了上述B4C-TiB2导电复相陶瓷的制备方法，具体包括如下步骤：
(1)按照成分设计分别称取B4C、TiC和无定形B粉体；
(2)将称量好的粉体混合均匀并充分干燥；
(3)将干燥后的粉体装入石墨模具，并置于放电等离子体烧结炉内在真空气氛中进行烧结。
作为一种优化，在步骤(1)中，所述B4C粉体的粒径为3.0-20.0μm，所述TiC粉体的粒径为0.05-3.0μm，所述无定形B粉体的粒径为0.5-1.0μm。
作为一种优化，在步骤(3)中，所述放电等离子体烧结炉内：烧结温度为2000℃，压力为50MPa，保温时间为5-20min。
与现有技术相比，本发明具有以下技术效果：
(1)构筑了TiB2小晶粒包覆B4C大晶粒的包覆型显微结构，有利导电网络的形成和完善。
(2)使用放电等离子技术，可有效阻止TiB2晶粒长大，这有利于B4C-TiB2 复相陶瓷电学性能的提升。
(3)相同TiB2含量下，本发明制备的B4C-TiB2复相陶瓷具有更高的电导率。
(4)B4C-TiB2复相陶瓷的电阻率相同时，本发明所需的TiB2含量更少。
(5)B4C粒径越大，所制备电阻率复相陶瓷的电导率越高，有助降低原料成本。
(6)与传统方法相比，本发明所制备的B4C-TiB2复相陶瓷的力学性能相当或更优。
(7)本发明制备过程简单，无需任何其它特殊复杂方法。
附图说明
图1为本发明的原理示意图；
如图所示，本发明具体过程为：(a)原料B4C、TiC与B粉体混合后；(b) 在烧结过程中，TiC与B首先发生原位反应生成B4C-TiB2超细复合粉体；(c)原料B4C大颗粒选择性吸收B4C-TiB2复合粉体中的超细B4C颗粒，发生晶粒长大； (d)TiB2小晶粒分布在B4C大晶粒周围形成一种包覆型显微结构。
图2为本发明实施例1所制备B4C-TiB2复相陶瓷抛光面的显微结构变化图；
如图所示，(a)在保温初期，原料B4C大颗粒原位反应生成的B4C-TiB2超细复合粉体共存；(b)随着保温时间的延长，原料B4C大颗粒选择性吸收B4C-TiB2复合粉体中的超细B4C颗粒，发生晶粒长大；(c)保温一定时间后，B4C-TiB2复合粉体中的超细B4C颗粒全部被原料B4C大颗粒吸收，TiB2小晶粒分布在B4C大晶粒周围形成一种包覆型显微结构。在此过程中，TiB2也发生了晶粒长大，但由于初始晶粒尺寸较小，其尺寸增长有效，相对于B4C晶粒而言，仍属于小晶粒。
图3为本发明实施例1所制备B4C-TiB2复相陶瓷断裂面的显微结构图；
如图所示，TiB2小晶粒分布在B4C大晶粒周围。
具体实施方式
为了进一步了解本发明的技术内容，以下结合具体实施例详述本发明，但本发明不局限于下述实施例。
实施例1
分别称量粒径为10.3μm的B4C粉体5.03g，粒径为0.05μm的TiC粉体1.83g，粒径为0.9μm的无定形B粉体2.19g。将称量好的粉体混合均匀并充分干燥。将干燥后的粉体装入石墨模具，并置于放电等离子体烧结炉内在真空气氛中进行烧结，烧结温度为2000℃，压力为50MPa，保温时间为16min。自然冷却后即可获得B4C-15vol％TiB2导电复相陶瓷。经测试，所制备B4C-15vol％TiB2复相陶瓷的相对密度为98.7％，三点弯曲强度为676MPa，维氏硬度为29.0GPa，断裂韧性为5.3MPa·m1/2，电导率为2.8×104S/m。
作为对比，以10.3μm的B4C粉体和2.5μm的TiB2粉体为原料，采用相同的混合和烧结方法制备B4C-15vol％TiB2复相陶瓷，其相对密度为95.3％,三点弯曲强度为552MPa，维氏硬度为27.5GPa，断裂韧性为4.4MPa·m1/2，电导率为4.3×103S/m。
实施例2
分别称量粒径为3.1μm的B4C粉体5.99g，粒径为0.8μm的TiC粉体 1.22g，粒径为0.9μm的无定形B粉体1.46g。将称量好的粉体混合均匀并充分干燥。将干燥后的粉体装入石墨模具，并置于放电等离子体烧结炉内在真空气氛中进行烧结，烧结温度为2000℃，压力为50MPa，保温时间为16 min。自然冷却后即可获得B4C-15vol％TiB2导电复相陶瓷。经测试，所制备 B4C-15vol％TiB2复相陶瓷的相对密度为99.5％，三点弯曲强度为780MPa，维氏硬度为31.8GPa，断裂韧性为5.8MPa·m1/2，电导率为3.3×103S/m。
作为对比，以3.1μm的B4C粉体和2.5μm的TiB2粉体为原料，采用相同的混合和烧结方法制备B4C-15vol％TiB2复相陶瓷，其相对密度为98.65％,三点弯曲强度为638MPa，维氏硬度为29.2GPa，断裂韧性为4.9MPa·m1/2，电导率为2.1×103S/m。
实施例3
分别称量粒径为10.3μm的B4C粉体4.07g，粒径为0.8μm的TiC粉体 2.45g，粒径为0.9μm的无定形B粉体2.91g。将称量好的粉体混合均匀并充分干燥。将干燥后的粉体装入石墨模具，并置于放电等离子体烧结炉内在真空气氛中进行烧结，烧结温度为2000℃，压力为50MPa，保温时间为16 min。自然冷却后即可获得B4C-20vol％TiB2导电复相陶瓷。经测试，所制备 B4C-20vol％TiB2复相陶瓷的相对密度为98.1％，三点弯曲强度为701MPa，维氏硬度为28.5GPa，断裂韧性为6.2MPa·m1/2，电导率为6.9×104S/m。
作为对比，以10.3μm的B4C粉体和2.50μm的TiB2粉体为原料，采用相同的混合和烧结方法制备B4C-20vol％TiB2复相陶瓷，其相对密度为93.5％,三点弯曲强度为587MPa，维氏硬度为27.6GPa，断裂韧性为5.1MPa·m1/2，电导率为1.6×104S/m。

Claims (2)

1.一种B4C-TiB2导电复相陶瓷，其特征在于，所述导电复相陶瓷具有包覆型显微结构，即TiB2小晶粒包覆在B4C大晶粒周围；所述导电复相陶瓷中TiB2的体积含量为10-30 %；
所述的B4C-TiB2导电复相陶瓷的制备包括如下步骤：
按照成分设计分别称取B4C、TiC和无定形B粉体；
所述B4C粉体的粒径为3.0-20.0 µm，所述TiC粉体的粒径为0.05-3.0 µm，所述无定形B粉体的粒径为0.5-1.0 µm；
（2）将步骤（1）称量好的粉体混合均匀并充分干燥；
（3）将步骤（2）干燥后的粉体装入石墨模具，并置于放电等离子体烧结炉内在真空气氛中进行烧结。
2.如权利要求1所述的B4C-TiB2导电复相陶瓷，其特征在于，在步骤（3）中，所述放电等离子体烧结炉内：烧结温度为2000℃ ，压力为50 MPa，保温时间为5-20 min。
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