CN108675793A - 一种碳化硼陶瓷的二次烧结方法 - Google Patents

一种碳化硼陶瓷的二次烧结方法 Download PDF

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CN108675793A
CN108675793A CN201810232213.5A CN201810232213A CN108675793A CN 108675793 A CN108675793 A CN 108675793A CN 201810232213 A CN201810232213 A CN 201810232213A CN 108675793 A CN108675793 A CN 108675793A
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boron carbide
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sintering
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王小华
吴方旭
崔莉
初洪超
李宗涛
王丹
马达
谢淼
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Beijing Clear Nuclear Mstar Technology Ltd
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Abstract

本发明涉及一种碳化硼陶瓷的二次烧结方法，属于陶瓷制备领域，其特征在于使用纯碳化硼进行烧结，且在传统的一次烧结基础上增加再烧结步骤。它是通过如下技术方案实现的：按质量百分比，将碳化硼80％‑94％，去离子水5％‑15％，丙三醇1％‑10％通过球磨及过筛混合均匀，冷压成型，利用真空热压烧结技术制备碳化硼陶瓷，本发明中采用二次烧结方法，在低于碳化硼熔点450℃的最高烧结温度下，得到了致密化且各项物理性能优异的碳化硼陶瓷。本发明解决了碳化硼纯粉烧结致密化困难的问题，为防弹陶瓷材料领域提供了一种致密化陶瓷制备方法。

Description

一种碳化硼陶瓷的二次烧结方法
技术领域
本发明涉及一种碳化硼陶瓷的二次烧结方法，属于陶瓷材料制备领域。
背景技术
陶瓷材料具有强度高、硬度高、耐高温、抗氧化等优异性能，已成为装甲防护领域中的主要材料之一。在装甲防护领域中，碳化硅、氧化铝及碳化硼是其中举足轻重的防弹陶瓷材料，而相比其他两种，碳化硼具有密度低、强度高、比模量高等优势，综合防弹性能更好。碳化硼是一种无机非金属材料，它的晶体结构中具有93％以上的共价键，这使得它具有优异的物理化学性能，但同时也给其制备增加了难度。
碳化硼的熔点高达2350℃，这使得其纯度越高，烧结越困难。碳化硼陶瓷可使用无压烧结及热压烧结等方法，通常会利用添加烧结助剂的方法来降低其烧结温度，从而在一定程度上降低碳化硼材料的性能。
发明内容
目前热压烧结是制备纯度较高致密碳化硼陶瓷最为有效的方法，而本专利中通过对未添加烧结助剂的纯粉采用二次烧结的方法得到致密且性能优异的碳化硼陶瓷，技术方案如下：
1.采用碳化硼纯粉，不加入烧结助剂。
2.实施步骤及工艺控制参数如下：
1)碳化硼80％-94％，去离子水5％-15％，丙三醇1％-10％，其比例为质量百分比；
2)将预选比例的碳化硼、去离子水、丙三醇置于球磨罐中，球料比为1∶3，球磨1-3h；
3)取出球磨后的混合物，将其过200目筛，以期充分混匀；
4)利用冷压机进行素坯成型，使用压力为15-30MPa；
5)将坯体置于烘箱中，70-130℃干燥12-20h，得到干燥的坯体；
6)将成型素坯与石墨模具、附件等组装，入真空热压炉进行烧结；炉内真空度保持在1-0.1Pa；
烧结温度控制机制为：室温-900℃，升温速率为15-25℃/min，保温20-30min；900-1500℃，升温速率为10-15℃/min，保温20-30min；1500℃-1900℃，升温速率为8-10℃/min，保温30min；自然降温至900℃；再次升温，900-1500℃，升温速率为10-15℃/min，保温20-30min；1500℃-1900℃，升温速率为8-10℃/min，保温30min；自然降温至安全温度后出炉。压力控制机制为：0P-30％P，30min；30P-60％P，35min；60P-85％P，45min，保压20-30min；85P-100％P，50min，保压，首次自然降温时逐渐卸载压力，再次升温时再随之升压；保温结束后逐步卸载压力至出炉。
依据本发明制得的碳化硼陶瓷与一次烧结得到的碳化硼陶瓷性能对比：
产品密度由2.35g/cm3提升至2.51g/cm3，致密度由93.25％提升至99.6％；
产品维氏硬度由2700HV提高到3100HV；
产品抗弯强度由250MPa提高到300MPa；
断裂韧性由3.0MPa·m1/2提高到3.7MPa·m1/2；
在低于碳化硼熔点450℃的最高烧结温度下，得到了性能优异的防弹陶瓷片；
具体实施方式
通过下面实例的描述，将有利于公众更清楚地理解本发明在烧结碳化硼技术上是如何解决致密化问题的，但不能将本发明的内容限制到所举实例中，它可以是本发明技术方案中的任意一个组合。
具体实施例1：本例实施原料组分碳化硼85％，去离子水8％，丙三醇7％；
1)将预选比例的碳化硼、去离子水、丙三醇置于球磨罐中，球料比为1∶3，球磨3h；
2)取出球磨后的混合物，将其过200目筛，以期充分混匀；
3)利用冷压机进行素坯成型，使用压力为25MPa；
4)将坯体置于烘箱中，70-130℃干燥12-20h，得到干燥的坯体；
5)将成型素坯与石墨模具、附件等组装，入真空热压炉进行烧结；炉内真空度保持在1-0.1Pa；
烧结温度控制机制为：室温-900℃，升温速率为15-25℃/min，保温20min；900-1500℃，升温速率为10-15℃/min，保温20min；1500℃-1900℃，升温速率为8-10℃/min，保温30min；自然降温至900℃；再次升温，900-1500℃，升温速率为10-15℃/min，保温30min；1500℃-1900℃，升温速率为8-10℃/min，保温30min；自然降温至安全温度后出炉。压力控制机制为：0P-30％P，30min；30P-60％P，35min；60P-85％P，45min，保压20-30min；85P-100％P，50min，保压，首次自然降温时逐渐卸载压力，再次升温时再随之升压；保温结束后逐步卸载压力至出炉。
具体实施例2：本例实施原料组分碳化硼80％，去离子水15％，丙三醇5％；
1)将预选比例的碳化硼、去离子水、丙三醇置于球磨罐中，球料比为1∶3，球磨3h；
2)取出球磨后的混合物，将其过200目筛，以期充分混匀；
3)利用冷压机进行素坯成型，使用压力为20MPa；
本例中素坯干燥方式与模具组装均与实施例一一致；
烧结温度控制机制为：室温-900℃，升温速率为20-25℃/min，保温20min；900-1500℃，升温速率为12-15℃/min，保温20min；1500℃-1900℃，升温速率为8-10℃/min，保温30min；自然降温至900℃；再次升温，900-1500℃，升温速率为12-15℃/min，保温30min；1500℃-1900℃，升温速率为8-10℃/min，保温30min；自然降温至安全温度后出炉。压力控制机制为：0P-30％P，30min；30P-60％P，35min；60P-85％P，45min，保压20-30min；85P-100％P，50min，保压，首次自然降温时逐渐卸载压力，再次升温时再随之升压；保温结束后逐步卸载压力至出炉。
本发明中采用的对比例为一次热压烧结方法制备得到碳化硼陶瓷，实施例与对比例物理性能对比如下表：
本发明在为添加烧结助剂的条件下利用二次热压烧结的方法制备出了致密的碳化硼陶瓷，且其各项性能优异。本发明解决了碳化硼纯粉烧结致密化困难的问题，为防弹陶瓷材料领域提供了一种致密化陶瓷制备方法。
本发明的实施例还有很多，并不限于给出的两个具体实施例，在本发明原则内做的修改或改进等均属于本发明的保护范围。

Claims (4)

1.一种碳化硼陶瓷的二次烧结方法，其特征在于使用纯碳化硼进行烧结，且在传统的一次烧结基础上增加再烧结步骤。
2.根据权利要求1所述碳化硼在素坯制备过程中，按质量百分比，碳化硼80％-94％，去离子水5％-15％，丙三醇1％-10％进行混合。
3.根据权利要求1所述碳化硼在素坯在成型之后，水分去除，烧结过程中丙三醇也会全部挥发，因此，烧结有效成分为纯碳化硼。
4.一种碳化硼陶瓷的二次烧结方法，它的实施步骤以及工艺控制参数特征在于：
S1、碳化硼80％-94％，去离子水5％-15％，丙三醇1％-10％，其比例为质量百分比；
S2、将预选比例的碳化硼、去离子水、丙三醇置于球磨罐中，球料比为1∶3，球磨1-3h；
S3、取出球磨后的混合物，将其过200目筛，以期充分混匀；
S4、利用冷压机进行素坯成型，使用压力为15-30MPa；
S5、将坯体置于烘箱中，70-130℃干燥12-20h，得到干燥的坯体；
S6、将成型素坯与石墨模具、附件等组装，入真空热压炉进行烧结；炉内真空度保持在1-0.1Pa；
烧结温度控制机制为：室温-900℃，升温速率为15-25℃/min，保温20-30min；900-1500℃，升温速率为10-15℃/min，保温20-30min；1500℃-1900℃，升温速率为8-10℃/min，保温30min；自然降温至900℃；再次升温，900-1500℃，升温速率为10-15℃/min，保温20-30min；1500℃-1900℃，升温速率为8-10℃/min，保温30min；自然降温至安全温度后出炉；压力控制机制为：0P-30％P，30min；30P-60％P，35min；60P-85％P，45min，保压20-30min；85P-100％P，50min，保压，首次自然降温时逐渐卸载压力，再次升温时再随之升压；保温结束后逐步卸载压力至出炉。
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Cited By (2)

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CN111606712A (zh) * 2020-06-12 2020-09-01 中南大学 一种低温脉冲加压制备碳化硼陶瓷的方法
CN113943159A (zh) * 2021-12-20 2022-01-18 山东金鸿新材料股份有限公司 一种碳化硼复合陶瓷的制备方法

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