CN116655383A - 用于中子屏蔽材料的多孔碳化硼陶瓷材料及其制备方法 - Google Patents

用于中子屏蔽材料的多孔碳化硼陶瓷材料及其制备方法 Download PDF

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CN116655383A
CN116655383A CN202310639390.6A CN202310639390A CN116655383A CN 116655383 A CN116655383 A CN 116655383A CN 202310639390 A CN202310639390 A CN 202310639390A CN 116655383 A CN116655383 A CN 116655383A
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boron carbide
sintering
ceramic material
neutron shielding
carbide ceramic
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郭学
张振昊
孙海滨
冯玉润
许伟
高鹏
吕源涛
张玉军
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Shandong Yasai Ceramic Technology Co ltd
Shandong University of Technology
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Shandong Yasai Ceramic Technology Co ltd
Shandong University of Technology
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Abstract

本发明公开了一种用于中子屏蔽材料的多孔碳化硼陶瓷材料及其制备方法，包括如下步骤：将碳化硼粉体与烧结助剂按比例混合球磨，制备浆料，浆料经过喷雾干燥制备成混合物粉体；所述碳化硼粉体的D50小于2μm，烧结助剂选自酚醛树脂、氧化铝或稀土氧化物中的一种或其组合；将混合物粉体与造孔剂按比例混合均匀，等静压压制成坯体，坯体在真空或惰性气氛中排胶和无压烧结，得到多孔碳化硼陶瓷材料。

Description

用于中子屏蔽材料的多孔碳化硼陶瓷材料及其制备方法
技术领域
本发明属于中子屏蔽材料技术领域，具体涉及一种用于中子屏蔽材料的多孔碳化硼陶瓷材料及其制备方法。
背景技术
这里的陈述仅提供与本发明相关的背景技术，而不必然地构成现有技术。
碳化硼具有较高的中子吸收截面，且不产生放射性同位素，二次射线能量低，耐腐蚀，热稳定性好的高效清洁特性，使其广泛应用于核反应堆中。
碳化硼应用于核反应堆中主要有如下形式：碳化硼粉体经过高温烧结，制备成堆芯控制鼓和控制棒；与石墨混合熔炼制作成硼碳砖，防止放射性物质外泄；与高密度聚乙烯复合形成含硼聚乙烯板；与涂料基体混合形成碳化硼中子屏蔽涂料；碳化硼与铝复合制成铝基复合材料，可用于压水堆核电厂乏燃料贮存和转运过程中的中子屏蔽等，但是目前的碳化硼的中子屏蔽性能较差。
发明内容
最近的研究发现，高强度、高气孔率、高通孔率、气孔尺寸小而且分布均匀的多孔碳化硼也是一种优异的中子屏蔽材料。
针对现有技术存在的不足，本发明的目的是提供一种用于中子屏蔽材料的多孔碳化硼陶瓷材料及其制备方法，制备得到的多孔碳化硼陶瓷具有气孔尺寸小、气孔分布均匀、通孔率高、气孔直径小以及强度高等优势。研究发现，高强度、高气孔率、高通孔率、气孔尺寸小而且分布均匀的多孔碳化硼是一种优异的中子屏蔽材料。
为了实现上述目的，本发明是通过如下的技术方案来实现：
第一方面，本发明首先提供一种烧结致密的碳化硼基体，通过添加粒度分布范围较窄的造孔剂，在较高压力下等静压成型坯体，并在真空炉中缓慢升温排出造孔剂，在2100-2200℃下烧成，得到用于中子屏蔽材料的多孔碳化硼陶瓷材料。
其制备方法包括如下步骤：
将碳化硼粉体与烧结助剂按比例混合球磨，制备浆料，浆料经过喷雾干燥制备成混合物粉体；所述氮化硼粉体的D50小于2μm，烧结助剂选自酚醛树脂、氧化铝或稀土氧化物中的一种或其组合；
将混合物粉体与造孔剂按比例混合均匀，等静压压制成坯体，坯体在真空或惰性气氛中排胶和烧结，得到多孔碳化硼陶瓷材料；
造孔剂的粒径为20-60μm；
碳化硼粉体与烧结助剂的质量比为90-98:1-12；
造孔剂与碳化硼的体积比为20-50:50-70；
烧结过程中，烧结温度低于700℃时，升温速度为0.5-2℃/min(造孔剂是有机物，如果升温过快就会造成开裂，控制升温速度的目的是缓慢排出造孔剂，防止产品开裂)；
烧结温度为700-1200℃时，升温速度为2-4℃/min(升温速度太慢，烧成时间太长，过快就会造成没有排出完的造孔剂挥发造成产品开裂)；
烧结温度大于1200℃时，升温速度3-8℃/min；
最高烧结温度为2180-2230℃，在最高烧结温度保温时间为2-6h。
在一些实施例中，所述氮化硼粉体的D50为0.5-1.8μm。
优选的，所述氮化硼粉体的D50为0.5-0.8μm。
造孔剂粒度分布范围窄，有利于形成均匀空隙的通道。
在一些实施例中，所述稀土氧化物为氧化钇、氧化镝、氧化钐、氧化铕或氧化镱。
在一些实施例中，所述烧结助剂为酚醛树脂，或为酚醛树脂与氧化铝和/或稀土氧化物的组合。
优选的，当烧结助剂为酚醛树脂、氧化铝和稀土氧化物的混合物时，酚醛树脂、氧化铝和稀土氧化物的质量比为5-10:1-2:2-3。
优选的，所述烧结助剂为酚醛树脂与钇铝石榴石的混合物，酚醛树脂与钇铝石榴石的质量比为6-10:4。两种烧结助剂都能提高烧结致密度，如果组合效果更好。
在一些实施例中，所述造孔剂选自糊精、碳酰二胺、淀粉、石墨粉、聚乙烯醇中的一种或多种。
优选的，所述造孔剂为糊精或淀粉。
在一些实施例中，烧结过程中，烧结温度低于700℃时，升温速度为0.5-1.5℃/min；
烧结温度为700-1200℃时，升温速度为2.5-3.5℃/min；
烧结温度大于1200℃时，升温速度5-7℃/min；
最高烧结温度为2180-2210℃，在最高烧结温度保温时间为2-4h。
优选的，烧结过程中，烧结温度低于700℃时，升温速度为1℃/min；
烧结温度为700-1200℃时，升温速度为3℃/min；
烧结温度大于1200℃时，升温速度6℃/min；
最高烧结温度为2200℃，在最高烧结温度保温时间为3h。
第二方面，本发明提供一种用于中子屏蔽材料的多孔碳化硼陶瓷材料，由所述制备方法制备而成。
上述本发明的一种或多种实施例取得的有益效果如下：
本发明制备的多孔碳化硼的密度为1.5～2.2g/cm3；孔隙率12％～40％；通孔率≥75％；抗压强度≥120MPa。
附图说明
构成本发明的一部分的说明书附图用来提供对本发明的进一步理解，本发明的示意性实施例及其说明用于解释本发明，并不构成对本发明的不当限定。
图1是实施例1制备的多孔碳化硼中子屏蔽材料试样的SEM像。
具体实施方式
应该指出，以下详细说明都是例示性的，旨在对本发明提供进一步的说明。除非另有指明，本发明使用的所有技术和科学术语具有与本发明所属技术领域的普通技术人员通常理解的相同含义。
下面结合实施例对本发明作进一步说明。
实施例1
将100重量份D50为0.5μm的碳化硼粉体与8份酚醛树脂和5份氧化铝与氧化钇(氧化铝与氧化钇的摩尔比5:3)的混合物放入球磨机中，按照固体粉体重量的50％加入去离子水，球磨混合8小时，得到碳化硼浆料；浆料经过喷雾干燥塔按照通用的工艺制备成喷雾造粒粉体。
喷雾造粒粉体与淀粉(20-60μm)按10:4的体积比混合，然后放入等静压模具，100MPa压力下压制成块体；再经过通用机械设备修整后，放入烧结炉烧结，按照1℃/min升温至700℃保温1小时，随后以3℃/min的升温速度升温到1200℃，保温1小时；继续以6℃/min的速度升温到2200℃，保温3h，随炉冷却。得到多孔碳化硼中子屏蔽材料。
多孔碳化硼中子屏蔽材料的密度为2.2g/cm3；孔隙率为36％；通孔率为80％；抗压强度为140MPa；平均气孔直径约为10微米。
多孔碳化硼中子屏蔽材料的扫描电子显微镜照片如图1所示。
实施例2
与实施例1的不同点在于：1)氧化钇换成氧化镝，比例不变；2)最高烧结温度为2180℃。
制备的多孔碳化硼中子屏蔽材料的密度为1.8g/cm3；孔隙率为35％；通孔率为80％；抗压强度为120MPa。
实施例3
与实施例1的不同点在于：1)碳化硼粉体的D50为1.5μm；2)烧结助剂只含有酚醛树脂，而且碳化硼粉体的重量份为100份，酚醛树脂的重量份为12份；3)最高烧结温度为2200℃。
制备的中子屏蔽材料的密度为1.9g/cm3；孔隙率为34％；通孔率为80％；抗压强度为130MPa。
实施例4
与实施例1的不同点在于：1)造孔剂为聚乙烯醇；2)喷雾造粒粉体与聚乙烯醇的体积比为10:0.36。
制备的中子屏蔽材料的密度为2.0g/cm3；孔隙率为28％；通孔率为75％；抗压强度为140MPa。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (10)

1.一种用于中子屏蔽材料的多孔碳化硼陶瓷材料的制备方法，其特征在于：包括如下步骤：
将碳化硼粉体与烧结助剂按比例混合球磨，制备浆料，浆料经过喷雾干燥制备成混合物粉体；所述氮化硼粉体的D50小于2μm，烧结助剂选自酚醛树脂、氧化铝或稀土氧化物中的一种或其组合；
将混合物粉体与造孔剂按比例混合均匀，等静压压制成坯体，坯体在真空或惰性气氛中排胶和烧结，得到多孔碳化硼陶瓷材料；
造孔剂的粒径为20-60μm；
碳化硼粉体与烧结助剂的质量比为90-98:1-12；
造孔剂与碳化硼的体积比为20-50:50-70；
烧结过程中，烧结温度低于700℃时，升温速度为0.5-2℃/min；
烧结温度为700-1200℃时，升温速度为2-4℃/min；
烧结温度大于1200℃时，升温速度3-8℃/min；
最高烧结温度为2180-2230℃，在最高烧结温度保温时间为2-6h。
2.根据权利要求1所述的用于中子屏蔽材料的多孔碳化硼陶瓷材料的制备方法，其特征在于：所述氮化硼粉体的D50为0.5-1.8μm。
3.根据权利要求2所述的用于中子屏蔽材料的多孔碳化硼陶瓷材料的制备方法，其特征在于：所述氮化硼粉体的D50为0.5-0.8μm。
4.根据权利要求1所述的用于中子屏蔽材料的多孔碳化硼陶瓷材料的制备方法，其特征在于：所述稀土氧化物为氧化钇、氧化镝、氧化钐、氧化铕或氧化镱；
优选的，所述烧结助剂为酚醛树脂，或为酚醛树脂与氧化铝和/或稀土氧化物的组合；
优选的，当烧结助剂为酚醛树脂、氧化铝和稀土氧化物的混合物时，酚醛树脂、氧化铝和稀土氧化物的质量比为5-10:1-2:2-3。
5.根据权利要求4所述的用于中子屏蔽材料的多孔碳化硼陶瓷材料的制备方法，其特征在于：所述烧结助剂为酚醛树脂与钇铝石榴石的混合物。
6.根据权利要求5所述的用于中子屏蔽材料的多孔碳化硼陶瓷材料的制备方法，其特征在于：酚醛树脂与钇铝石榴石的质量比为6-10:4。
7.根据权利要求1所述的用于中子屏蔽材料的多孔碳化硼陶瓷材料的制备方法，其特征在于：所述造孔剂选自糊精、碳酰二胺、淀粉、石墨粉、聚乙烯醇中的一种或多种；
优选的，所述造孔剂为糊精或淀粉。
8.根据权利要求1所述的用于中子屏蔽材料的多孔碳化硼陶瓷材料的制备方法，其特征在于：烧结过程中，烧结温度低于700℃时，升温速度为0.5-1.5℃/min；
烧结温度为700-1200℃时，升温速度为2.5-3.5℃/min；
烧结温度大于1200℃时，升温速度5-7℃/min；
最高烧结温度为2180-2210℃，在最高烧结温度保温时间为2-4h。
9.根据权利要求8所述的用于中子屏蔽材料的多孔碳化硼陶瓷材料的制备方法，其特征在于：烧结过程中，烧结温度低于700℃时，升温速度为1℃/min；
烧结温度为700-1200℃时，升温速度为3℃/min；
烧结温度大于1200℃时，升温速度6℃/min；
最高烧结温度为2200℃，在最高烧结温度保温时间为3h。
10.一种用于中子屏蔽材料的多孔碳化硼陶瓷材料，其特征在于：由权利要求1-9任一所述制备方法制备而成。
CN202310639390.6A 2023-05-30 2023-05-30 用于中子屏蔽材料的多孔碳化硼陶瓷材料及其制备方法 Pending CN116655383A (zh)

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