CN113387705B - 一种碳化硼陶瓷的制备方法 - Google Patents
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- 229910052580 B4C Inorganic materials 0.000 title claims abstract description 87
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 239000000919 ceramic Substances 0.000 title claims abstract description 54
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- 238000005245 sintering Methods 0.000 claims abstract description 60
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 7
- 229910002804 graphite Inorganic materials 0.000 abstract description 7
- 239000010439 graphite Substances 0.000 abstract description 7
- 238000000280 densification Methods 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 4
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Abstract
本发明公开了一种碳化硼陶瓷的制备方法，该制备方法首先对碳化硼施加较低的恒定压力，然后在最高烧结温度时将恒定压力调整为振荡压力，最后在冷却阶段调整为较低的恒定压力得到碳化硼陶瓷。该方法将振荡压力施加在烧结中期至烧结末期，其改变了碳化硼烧结过程的致密化机理，能够在1700‑1800℃实现纯碳化硼的致密化，且烧结压力较小，此种烧结方式可引入大量晶体缺陷，实现材料性能的大幅提升，所制备得到的碳化硼陶瓷致密度高。且本发明采用的较低的烧结压力降低了对烧结设备和所用石墨模具的要求，有助于制备更大尺寸的高性能碳化硼陶瓷构件。
Description
技术领域
本发明属于碳化硼陶瓷制备技术领域，涉及一种碳化硼陶瓷的制备方法。
背景技术
碳化硼具有高硬度、高弹性模量、低密度、高熔点、优秀的化学稳定性、强的中子吸收能力、优秀的热电性质等特点，这使得碳化硼陶瓷成为轻质装甲、刀具、耐磨件和核反应堆控制棒等应用的优秀候选材料。碳化硼自身强共价键所导致的低的自扩散系数使得纯碳化硼陶瓷较难烧结，且难以达到高的烧结密度；同时现有碳化硼陶瓷还存在硬度低和强度差的问题。
纯碳化硼陶瓷的烧结方式不一，其中采用无压烧结纯碳化硼陶瓷时，即使烧结到2375℃的高温时也无法达到95％以上高的相对密度。采用压力辅助烧结纯碳化硼时，在静态压力下，随着烧结温度的降低，获得高致密度碳化硼陶瓷所需的烧结压力大幅提高。在2050-2200℃温度范围内烧结时，由于烧结温度较高，碳化硼晶粒长大严重，导致烧结得到的碳化硼陶瓷整体性能较差。降低烧结温度到1800-2000℃温度范围内烧结时，可以有效抑制碳化硼晶粒生长，减小晶粒尺寸，可获得更优异性能的碳化硼陶瓷。但是其烧结压力至少需要在80MPa 以上才可获得高致密度的碳化硼陶瓷，且随着烧结温度进一步降低，所需烧结压力大幅提高。但是所制备的高致密碳化硼陶瓷的力学性能几乎无明显改善。现有技术中有通过采用纳米粉体和超高压力烧结技术以提高碳化硼陶瓷的力学性能的方案，但纳米粉体工艺复杂，其纯度难以保证；超高压力烧结方法对烧结的设备要求高，可制备的碳化硼陶瓷尺寸小。以上可知，现阶段仍缺乏适合大批量生产高致密高性能纯碳化硼陶瓷的方法。
发明内容
为了克服现有技术的不足，本发明的目的之一在于提供一种碳化硼陶瓷的制备方法，该方法制备得到的碳化硼陶瓷具有致密度高、硬度高、抗弯强度高的特点。
本发明的目的之一采用如下技术方案实现：
一种碳化硼陶瓷的制备方法，包括以下步骤：
(1)将碳化硼粉末装填入烧结炉的模具中，对碳化硼粉末施加恒定压力，升温对碳化硼粉末进行加热；
(2)当步骤(1)烧结炉内达到设定温度后进入保温状态，同时升压至振荡压力谷值，随后对碳化硼粉末施加振荡压力；
(3)保温结束后停止加热，降温的同时将振荡压力改为恒定压力直至降温结束，即得碳化硼陶瓷。
进一步地，所述步骤(2)升压速率为5-10kN/min，所述振荡压力的振荡波形为正弦波，压力中值为40-80MPa，振幅为5-15MPa，振荡频率为1-10Hz。
进一步地，所述步骤(2)设定温度为1700-1800℃，保温时间为0.5-2h。
进一步地，所述步骤(1)的升温过程为8℃/min升温加热200分钟至1600℃，再以5℃ /min升温加热20-40分钟至1700-1800℃。
进一步地，所述步骤(1)、(3)的恒定压力为5-10MPa。
进一步地，所述步骤(1)至(3)的烧结过程均在真空条件下进行。
相比现有技术，本发明的有益效果在于：
本发明提供了一种碳化硼陶瓷的制备方法，该方法将振荡压力施加在烧结中期至烧结末期，改变了碳化硼烧结过程的致密化机理，能够在1600-1800℃实现纯碳化硼的致密化，且烧结压力较小。此种烧结方式可引入大量晶体缺陷，实现材料性能的大幅提升，所制备得到的碳化硼陶瓷致密度高，相对密度达99.1％-99.7％，维氏硬度达38-39.5GPa，抗弯强度达 590-710MPa。本发明采用的较低的烧结压力降低了对烧结设备和所用石墨模具的要求，有助于制备更大尺寸的高性能碳化硼陶瓷构件。
附图说明
图1为本发明实施例1所用振荡压力示意图；
图2为本发明实施例1烧结工艺图；
图3为本发明实施例1制备得到的碳化硼陶瓷的微观断面形貌图。
具体实施方式
下面，结合附图以及具体实施方式，对本发明做进一步描述，需要说明的是，在不相冲突的前提下，以下描述的各实施例之间或各技术特征之间可以任意组合形成新的实施例。
实施例1
一种碳化硼陶瓷的制备方法：
(1)将碳化硼粉末装填入烧结炉的石墨模具中，在真空条件下进行烧结，首先对碳化硼粉末施加5MPa恒定压力，然后升温对碳化硼粉末进行加热，升温制式为首先以8℃/min升温加热200分钟至1600℃，再以5℃/min升温加热40分钟至1800℃；
(2)当步骤(1)烧结炉内达到设定温度1800℃后进入保温状态，保温时间0.5h，同时以5kN/min升压至振荡压力谷值30MPa，随后对碳化硼粉末施加振荡压力，振荡压力的振荡波形为正弦波，振荡压力中值为40MPa，振幅10MPa，振动频率5Hz；
(3)保温结束后停止加热，随炉降温，降温的同时将振荡压力改为5MPa恒定压力直至降温结束，即得碳化硼陶瓷。
实施例2
一种碳化硼陶瓷的制备方法：
(1)将碳化硼粉末装填入烧结炉的石墨模具中，在真空条件下进行烧结，首先对碳化硼粉末施加5MPa恒定压力，然后升温对碳化硼粉末进行加热，升温制式为首先以8℃/min升温加热200分钟至1600℃，再以5℃/min升温加热30分钟至1750℃；
(2)当步骤(1)烧结炉内达到设定温度1750℃后进入保温状态，保温时间0.5h，同时以5kN/min升压至振荡压力谷值55MPa，随后对碳化硼粉末施加振荡压力，振荡压力的振荡波形为正弦波，振荡压力中值为60MPa，振幅5MPa，振动频率1Hz；
(3)保温结束后停止加热，随炉降温，降温的同时将振荡压力改为5MPa恒定压力直至降温结束，即得碳化硼陶瓷。
实施例3
一种碳化硼陶瓷的制备方法：
(1)将碳化硼粉末装填入烧结炉的石墨模具中，在真空条件下进行烧结，首先对碳化硼粉末施加10MPa恒定压力，然后升温对碳化硼粉末进行加热，升温制式为首先以8℃/min 升温加热200分钟至1600℃，再以5℃/min升温加热20分钟至1700℃；
(2)当步骤(1)烧结炉内达到设定温度1700℃后进入保温状态，保温时间2h，同时以10kN/min升压至振荡压力谷值65MPa，随后对碳化硼粉末施加振荡压力，振荡压力的振荡波形为正弦波，振荡压力中值为80MPa，振幅15MPa，振动频率10Hz；
(3)保温结束后停止加热，随炉降温，降温的同时将振荡压力改为10MPa恒定压力直至降温结束，即得碳化硼陶瓷。
对比例1
现有技术Xiaorong Zhang等Effects of pressure on densificationbehaviour,microstructures and mechanical properties of boron carbide ceramicsfabricated by hot pressing，Ceramics International，2017,43(8):6345-6352。
对比例2
采用真空热压烧结法，起始烧结温度为420℃，温度升至1500℃保温4min，接着升温到1600℃保温4min，继续升温到1700℃保温5min，继而升温到1800℃保温6min，接着升温到1900℃，保温5min，最后温度达到2000℃，保温4min，升温速率皆为80℃/min。然后以200℃/min速率降温得到样品，整个过程压力保持35MPa。
实验例1
将实施例1至3、对比例1至3制备得到的碳化硼陶瓷进行相对密度、维氏硬度、抗弯强度测试，测试结果如表1所示。
表1
由表1可知，本发明实施例1至3烧结温度较低，烧结压力为振荡压力，所得到的碳化硼陶瓷相对密度达99.1％-99.7％，维氏硬度达38-39.5GPa，抗弯强度达590-710MPa，表现出致密度高、维氏硬度高、抗弯强度高的特点。
对比例 1与实施例1的区别在于，实施例1在最高温度保温阶段向碳化硼粉体施加的振荡压力及降温阶段施加的恒定压力，而对比例 1烧结最高温度为1900℃，全程施加恒定压力100MPa。虽然对比例 1得到的碳化硼陶瓷致密度与实施例1相近，但是其烧结最高温度比实施例1的高100℃，烧结过程的压力比实施例1高50-60MPa。本发明实施例1 的方法采用的较低烧结温度和烧结压力降低了对设备和所用石墨磨具的要求。
对比例 2与实施例1的区别在于：对比例 2采用多阶段升温的方式对碳化硼粉末进行真空热压烧结，但是该方法得到的碳化硼陶瓷相对密度仅仅达到96.03％，维氏硬度仅仅达 34GPa，与实施例1相比性能较差。
本发明实施例1得到的碳化硼陶瓷的微观断面形貌图(SEM)如图3所示，由图中可以看出制备得到的碳化硼陶瓷组织均匀。
综上，本发明提供了一种碳化硼陶瓷的制备方法，该方法将振荡压力施加在烧结中期至烧结末期，其改变了碳化硼烧结过程的致密化机理，能够在1700-1800℃实现纯碳化硼的致密化，且烧结压力较小，此种烧结方式可引入大量晶体缺陷，实现材料性能的大幅提升，所制备得到的碳化硼陶瓷致密度高，相对密度达99.1％-99.7％，维氏硬度达38-39.5GPa，抗弯强度达590-710MPa。且本发明采用的较低的烧结压力降低了对烧结设备和所用石墨模具的要求，有助于制备更大尺寸的高性能碳化硼陶瓷构件。
上述实施方式仅为本发明的优选实施方式，不能以此来限定本发明保护的范围，本领域的技术人员在本发明的基础上所做的任何非实质性的变化及替换均属于本发明所要求保护的范围。
Claims (2)
1.一种碳化硼陶瓷的制备方法，其特征在于，包括以下步骤：
(1)将碳化硼粉末装填入烧结炉的模具中，对碳化硼粉末施加恒定压力，升温对碳化硼粉末进行加热；
(2)当步骤(1)烧结炉内达到设定温度后进入保温状态，同时升压至振荡压力谷值，随后对碳化硼粉末施加振荡压力；
(3)保温结束后停止加热，降温的同时将振荡压力改为恒定压力直至降温结束，即得碳化硼陶瓷；
其中，所述步骤(1)的升温过程为8℃/min升温加热200分钟至1600℃，再以5℃/min升温加热20-40分钟至1700-1800℃；
所述步骤(2)升压速率为5-10kN/min，所述振荡压力的振荡波形为正弦波，压力中值为40-80MPa，振幅为5-15MPa，振荡频率为1-10Hz；
所述步骤(2)设定温度为1700-1800℃，保温时间为0.5-2h；
所述步骤(1)、(3)的恒定压力为5-10MPa。
2.如权利要求1所述的碳化硼陶瓷的制备方法，其特征在于，所述步骤(1)至(3)的烧结过程均在真空条件下进行。
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