CN109111231A - 一种碳化硼/碳化硅层状复合陶瓷材料的制备方法 - Google Patents

一种碳化硼/碳化硅层状复合陶瓷材料的制备方法 Download PDF

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CN109111231A
CN109111231A CN201810820198.6A CN201810820198A CN109111231A CN 109111231 A CN109111231 A CN 109111231A CN 201810820198 A CN201810820198 A CN 201810820198A CN 109111231 A CN109111231 A CN 109111231A
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silicon carbide
base layer
boron carbide
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方宁象
林文松
余建
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Zhejiang Li Tai Composite Ltd Co
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Abstract

本发明提供一种碳化硼/碳化硅层状复合陶瓷材料的制备方法及根据该方法所制备的产品，制备步骤包括：分别制备基体层和分隔层陶瓷浆料，采用凝胶注模法在模具中交替浇注基体层和分隔层陶瓷，之后进行排胶、真空热压烧结，对排胶、烧结温度及升温速度、烧结压力进行调控限定，制备得到的碳化硼/碳化硅层状陶瓷界面清晰、致密性好，材料具有高损伤容忍性和优异的抑制裂纹扩展能力；本发明制备的碳化硼/碳化硅层状复合陶瓷材料可应用于轻质防弹装甲制造领域。

Description

一种碳化硼/碳化硅层状复合陶瓷材料的制备方法
技术领域
本发明属于无机非金属材料领域，涉及碳化硼陶瓷材料的热压烧结制备工艺，尤其是一种碳化硼/碳化硅层状复合陶瓷材料的制备方法。
背景技术
碳化硼和碳化硅陶瓷材料具有超高硬度、耐高温、不易变形、质量轻等诸多优点，被用作耐高速高能冲击材料，但陶瓷的脆性，使其对缺陷的容忍性极低，在高速高能冲击过程中极易失效，难以抵抗多次冲击。
层状陶瓷材料由于具有高缺陷容忍性、高吸能的能力以及结构可设计等优点，具有满足抗高速高能冲击要求的潜力。目前公开的研究文献主要集中在具有多孔界面或者低强度的弱界面等层状陶瓷方面，通过层状材料中较弱的分隔层或较弱的层间界面，使裂纹在扩展到分隔层时发生偏转，进而引发大量的增韧机制，消耗大量的能量，最终达到提高陶瓷材料韧性的目的。这种材料虽然具有较好的静态力学性能，但由于界面强度低且界面结合强度低，在动态载荷作用下易因为界面破坏和脱粘而失效，限制了其结构完整性和能量吸收能力的提升，并不适合应用于防弹装甲领域。
发明内容
本发明的目的在于提供一种制备碳化硼/碳化硅层状陶瓷的工艺方法，以及这种层状陶瓷在装甲防护领域的应用。
本发明的技术方案是通过下述工艺步骤而得以实现的：
步骤1)将单体、交联剂和分散剂溶解于水中，制成单体溶液；单体、分散剂和交联剂的质量浓度分别为1.5％～5.0％、0.3％～1.2％、0.1％～0.3％；
步骤2)在单体溶液中分别加入基体层陶瓷粉末和分隔层陶瓷粉末，经球磨20～40小时，分别得到基体层混合浆料和分隔层混合浆料；陶瓷混合粉末的质量浓度为40％～80％；
步骤3)将步骤2)得到的两种混合浆料在真空中搅拌抽气10～30分钟后，加入引发剂并搅拌均匀，得到基体层陶瓷初始料浆和分隔层陶瓷初始料浆；引发剂的质量浓度分别为0.1％～0.3％。
步骤4)将步骤3)获得的基体层和分隔层陶瓷初始料浆在模具中交替浇注在模具中，凝固后得到层状复合陶瓷材料坯体；
步骤5)将装有坯体的模具在空气气氛下，先以<5℃/分钟的速度慢速升温至300～400℃，保温2～4小时进行排胶处理，待有机物完全排尽后，将坯体转移到石墨模具中；
步骤6)坯体在真空炉中热压烧结，升温速率为5～20℃/min，热压烧结温度为1950～2150℃，保温时间1～2小时，并在烧结过程中施加30～50MPa的压力。
优选地，步骤1)所述单体为丙烯酰胺或甲基丙烯酰胺，交联剂为亚甲基双丙烯酰胺，分散剂为聚丙烯酸铵和聚乙烯吡咯烷酮混合物，其中聚丙烯酸铵和聚丙烯酸铵的质量比为3:1；步骤(3)所述引发剂为过硫酸铵。
优选地，步骤4)所述层状复合陶瓷的层数为3层、5层或7层，其中基体层陶瓷位于复合材料的表面，分隔层陶瓷位于两个基体层陶瓷之间。
本发明提出的制备方法能方便地调制陶瓷基体层和界面层的厚度比，避免较高强度的冲击应力波在界面内发生叠加，通过限定制备工艺，制备得到的层状陶瓷界面清晰、致密性好，材料具有高强度、高损伤容忍性和优异的抑制裂纹扩展能力。
本发明的另一个目的在于提供一种所述方法得到的碳化硼/碳化硅层状陶瓷，其中，所述基体层陶瓷粉末由B4C和碳黑两种粉末组成，其质量配比为：B4C:C＝(95～98):(5～2)；所述分隔层的陶瓷粉末由B4C和SiC两种粉末组成，其质量配比为：B4C:SiC＝(60～80):(40～20)。
优选地，所述碳化硼的平均颗粒尺寸为3～8μm，碳化硅粉末的平均颗粒尺寸为0.5～2μm。
优选地，步骤(4)所述层状复合陶瓷的基体层与分隔层的层厚比为2:1～5:1。
本发明的再一个目的在于提供上述所述的碳化硼/碳化硅层状陶瓷可应用于轻质防弹装甲制造领域。
相对于现有技术，本发明提供的制备工艺能显著提高碳化硼陶瓷的缺陷容忍度和力学性能；制备得到的碳化硼/碳化硅层状陶瓷界面清晰、致密性好，材料具有高损伤容忍性和优异的抑制裂纹扩展能力。本发明制备的碳化硼/碳化硅层状复合陶瓷材料可应用于轻质防弹装甲制造领域；特别适用于特种车辆的防护领域；本发明提供的碳化硼/碳化硅层状复合陶瓷可抵抗多发子弹侵彻，
具体实施方式
以下结合两个具体实施例，示例性说明及帮助进一步理解本发明。但实施例具体细节仅是为了说明本发明，并不代表本发明构思下的全部技术方案，因此不应理解为对本发明的技术方案的限定。一些不偏离本发明构思的非实质性改动，例如以具有相同或相似技术效果的技术特征简单改变或替换，均属本发明权利保护范围。
实施例1
一种碳化硼/碳化硅层状陶瓷的工艺方法，制备工艺包括以下步骤：
步骤1)，将丙烯酰胺3.5份(质量份数，下同)、亚甲基双丙烯酰胺0.5份、聚丙烯酸铵0.15份和聚乙烯吡咯烷酮0.05份溶解于100份水中，制成单体溶液。
步骤2)，在步骤1)制得的单体溶液中加入平均颗粒尺寸为3～8μm的碳化硼粉末48份和2份的碳黑粉末，球磨30小时后得到基体层陶瓷粉末混合料；将所得粉末混合料在真空中搅拌抽气20分钟后，加入过硫酸铵0.2份，再搅拌10分钟后，得到均匀的基体层陶瓷初始料浆。
步骤3)，在步骤1)制得的另一份单体溶液中加入平均颗粒尺寸为3～8μm的碳化硼粉末30份，平均颗粒尺寸为0.5～2μm的碳化硅粉末20份，球磨30小时后得到分隔层陶瓷粉末混合料；将所得粉末混合料在真空中搅拌抽气20分钟后，加入过硫酸铵0.2份，再搅拌10分钟后，得到均匀的分隔层陶瓷初始料浆。
步骤4)，在模具中交替浇注步骤2)得到的基体层陶瓷初始料浆和步骤3)得到的分隔层陶瓷初始料浆，得到两层的基体层陶瓷初始料浆和一层的分隔层陶瓷初始料浆，凝固后得到层状复合陶瓷材料坯体；操作过程中，控制基体层初始料浆和分隔层陶瓷初始料浆的厚度比约为2.5:1。
步骤5)，将坯体及装有坯体的模具以<5℃/分钟的速度慢速升温至400℃，在大气环境下保温2小时进行排胶处理，待有机物完全排尽后，将坯体转移到石墨模具中。
步骤6)，坯体在真空炉中热压烧结，升温速率为10℃/min，热压烧结温度为2050℃，保温时间1小时，并在烧结过程中施加30MPa的压力。随炉冷却后，得到碳化硼/碳化硅层状陶瓷。
实施例2
步骤1)，将丙烯酰胺2.0份(质量份数，下同)、亚甲基双丙烯酰胺1.0份、聚丙烯酸铵0.18份和聚乙烯吡咯烷酮0.06份溶解于100份水中，制成单体溶液。
步骤2)，在步骤1)制得的单体溶液中加入平均颗粒尺寸为3～8μm的碳化硼粉末49份和1份的碳黑粉末，球磨25小时后得到基体层陶瓷粉末混合料；将所得粉末混合料在真空中搅拌抽气30分钟后，加入过硫酸铵0.3份，再搅拌10分钟后，得到均匀的基体层陶瓷初始料浆。
步骤3)，在步骤一制得的另一份单体溶液中加入平均颗粒尺寸为3～8μm的碳化硼粉末40份，平均颗粒尺寸为0.5～2μm的碳化硅粉末10份，球磨30小时后得到分隔层陶瓷粉末混合料；将所得粉末混合料在真空中搅拌抽气30分钟后，加入过硫酸铵0.3份，再搅拌10分钟后，得到均匀的分隔层陶瓷初始料浆。
步骤4)，在模具中交替浇注步骤2)得到的基体层陶瓷初始料浆和步骤3)得到的分隔层陶瓷初始料浆，得到三层的基体层陶瓷初始料浆和两层的分隔层陶瓷初始料浆，凝固后得到层状复合陶瓷材料坯体。操作过程中，控制基体层初始料浆和分隔层陶瓷初始料浆的厚度比约为3.5:1。
步骤5)，将坯体及装有坯体的模具以<5℃/分钟的速度慢速升温至350℃，在大气环境下保温2小时进行排胶处理，待有机物完全排尽后，将坯体转移到石墨模具中。
步骤6)，坯体在真空炉中热压烧结，升温速率为10℃/min，热压烧结温度为2150℃，保温时间1小时，并在烧结过程中施加30MPa的压力。随炉冷却后，得到碳化硼/碳化硅层状陶瓷。

Claims (7)

1.一种碳化硼/碳化硅层状复合陶瓷材料，其特征在于：该复合材料由基体层和分隔层组成，所述基体层陶瓷粉末由B4C和碳黑两种粉末组成，其质量配比为：B4C:C＝95～98:5～2；所述分隔层的陶瓷粉末由B4C和SiC两种粉末组成，其质量配比为：B4C:SiC＝60～80:40～20。
2.根据权利要求1所述的碳化硼/碳化硅层状复合陶瓷材料，所述碳化硼的平均颗粒尺寸为3～8μm，碳化硅粉末的平均颗粒尺寸为0.5～2μm。
3.根据权利要求1所述的碳化硼/碳化硅层状复合陶瓷材料的制备方法，其特征在于：该方法包括如下步骤：
步骤1)将单体、交联剂和分散剂溶解于水中，制成单体溶液；单体、分散剂和交联剂的质量浓度分别为1.5％～5.0％、0.3％～1.2％、0.1％～0.3％。
步骤2)在单体溶液中分别加入基体层陶瓷粉末和分隔层陶瓷粉末，经高能球磨20～40小时，分别得到基体层混合浆料和分隔层混合浆料；陶瓷粉末的质量浓度为40％～80％。
步骤3)将步骤2)得到的两种混合浆料在真空中搅拌抽气10～30分钟后，加入引发剂并搅拌均匀，得到基体层陶瓷初始料浆和分隔层陶瓷初始料浆；引发剂的质量浓度分别为0.1％～0.3％。
步骤4)将步骤(3)获得的基体层和分隔层陶瓷初始料浆在模具中交替浇注在模具中，凝固后得到层状复合陶瓷材料坯体；
步骤5)将装有坯体的模具在空气气氛下，先以<5℃/分钟的速度慢速升温至300～400℃，保温2～4小时进行排胶处理，待有机物完全排尽后，将坯体转移到石墨模具中；
步骤6)坯体在真空炉中热压烧结，升温速率为5～20℃/min，热压烧结温度为1950～2150℃，保温时间1～2小时，并在烧结过程中施加30～50MPa的压力。
4.根据权利要求2所述的碳化硼/碳化硅层状复合陶瓷材料的制备方法，其特征在于：步骤1)中所述单体为丙烯酰胺或甲基丙烯酰胺，交联剂为亚甲基双丙烯酰胺，分散剂为聚丙烯酸铵和聚乙烯吡咯烷酮混合物，聚丙烯酸铵和聚乙烯吡咯烷酮质量比为3:1；步骤3)中所述引发剂为过硫酸铵。
5.根据权利要求2所述的碳化硼/碳化硅层状复合陶瓷材料的制备方法，其特征在于：步骤4)中所述层状复合陶瓷的层数为3层、5层或7层，其中基体层陶瓷位于复合材料的表面，分隔层陶瓷位于两个基体层陶瓷之间。
6.根据权利要求2所述的碳化硼/碳化硅层状复合陶瓷材料的制备方法，基体层与分隔层的层厚比为2:1～5:1。
7.根据权利1所述的碳化硼/碳化硅层状复合陶瓷材料在轻质防弹装甲中的应用。
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