CN109665847A - 一种全致密碳化硼陶瓷复合材料及制备方法 - Google Patents

一种全致密碳化硼陶瓷复合材料及制备方法 Download PDF

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CN109665847A
CN109665847A CN201910167697.4A CN201910167697A CN109665847A CN 109665847 A CN109665847 A CN 109665847A CN 201910167697 A CN201910167697 A CN 201910167697A CN 109665847 A CN109665847 A CN 109665847A
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boron carbide
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邢鹏飞
王帅
闫姝
庄艳歆
都兴红
尹华意
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Abstract

本发明公开了一种全致密碳化硼陶瓷复合材料及制备方法，属于材料合成技术领域。各组分质量百分比如下：65wt％‑95wt％的碳化硼，5wt％‑35wt％的二硅化铬。所述的制备工艺如下：将碳化硼粉体和二硅化铬粉以无水乙醇为介质，球磨混合，过筛并于真空条件下烘干；将粉末装入石墨模具中真空条件下进行热压烧结得碳化硼陶瓷复合材料。本发明的碳化硼陶瓷复合材料具有几乎全致密和高力学性能的特点，同时本发明设备简单，操作便捷，方便维护和检修，可用于工业生产。

Description

一种全致密碳化硼陶瓷复合材料及制备方法
技术领域
本发明属于复合材料技术领域，具体涉及到全致密碳化硼陶瓷复合材料的制备方法。
背景技术
碳化硼陶瓷由于密度低、硬度高因而可以作为防弹装甲应用在军工领域。此外，其高中子吸收截面积使其可作为核屏蔽材料应用在核工业领域。碳化硼陶瓷还具有高熔点、耐酸碱腐蚀等优点可作为结构陶瓷应用在非氧化环境的高温领域。但是由于碳化硼共价键含量较高，烧结致密化非常困难。对于粒径小于3μm的碳化硼粉料，在2250-2350℃条件下进行无压烧结，所得碳化硼陶瓷的致密度只能到80％-93％。而对于热压烧结，即使在2000℃、40MPa条件下所得陶瓷致密度只有95％左右。致密度直接关系着碳化硼陶瓷的力学性能，如何提高碳化硼陶瓷的致密度是目前亟待解决的问题。
目前，为了提高烧结所得碳化硼陶瓷的致密度，碳化硅和二硼化铬等添加剂被添加到碳化硼中作为烧结助剂辅助提升碳化硼陶瓷的致密度和力学性能，并取得了良好的效果。二硼化铬可以与碳化硼形成共晶液相实现液相烧结，显著提升碳化硼致密度。碳化硅可以钉扎在碳化硼晶界阻碍碳化硼晶粒长大，提升碳化硼陶瓷力学性能。研究还发现，通过原未反应的方式在碳化硼中第二相粒子可以使第二相粒子分布更加均匀，更能提高碳化硼陶瓷的致密度和力学性能。
发明内容
在现有技术基础上，以二硅化铬作为烧结助剂，利用其在热压烧结碳化硼中与碳化硼反应原位生成能与碳化硼形成共晶液相的二硼化铬和碳化硅，以此提升所得碳化硼陶瓷复合材料的致密度和力学性能。
所述二硅化铬的粒径为0.1μm-10μm，二硅化铬的纯度为97wt％-99.5wt％，且相对于所述的混合物干料总质量，二硅化铬的质量百分含量可为5wt％-35wt％。
所述的碳化硼的平均粒径为0.2μm-10μm，碳化硼粉纯度为95wt％-99.8wt％，且相对于所述的混合物干料总质量，碳化硼的质量百分含量为65wt％-95wt％。
本发明的方法按以下步骤进行：
(1)按照全致密碳化硼陶瓷复合材料组成成分及其质量百分比称取，将称取好的碳化硼、二硅化铬粉放入球磨机中，以无水乙醇为介质进行湿磨，2h-24h后将浆料取出；
(2)在50℃-130℃于真空烘箱内烘干1h-20h，然后过20-120目筛；
(3)将过筛后的固体浆料装入石墨模具腔内，0.001Pa-300Pa真空条件下梯度升温至1900℃-2100℃进行烧结；
(4)达到所需温度后加压，压力为15MPa-80MPa，保温并保压0.5h-4h后随炉冷却；经切磨、抛光处理后得到全致密碳化硼陶瓷复合材料。
上述步骤(1)的湿磨过程中球料质量比为3-9，球磨转速为200r/min-700r/min.
上述步骤(3)的石墨模具内壁贴一层柔性石墨或者氮化硼。
上述步骤(3)的石墨模具腔体是单一圆柱或单一长方体，或者是圆柱和长方体并存。
上述步骤(3)的梯度升温是以10℃/min-40℃/min的升温速度自室温升至1800℃，然后以5℃/min-30℃/min升温速度自1800℃升至1900℃-2100℃。
上述步骤(4)的保温保压结束后，随炉冷却过程中保持无压或者施加无压与烧结时所加压力之间任一压力值。
本发明以二硅化铬作为烧结助剂，可在热压烧结中与碳化硼反应原位生成二硼化铬和碳化硅，并利用二硼化铬在烧结过程中与碳化硼形成共晶液相实现液相烧结，能够显著提升碳化硼基陶瓷复合材料的致密度。生成的碳化硅可以钉扎在碳化硼晶界阻碍碳化硼晶粒长大，提升碳化硼陶瓷力学性能。生成的二硼化铬由于其热扩散系数与碳化硼不匹配会导致裂纹的偏转和桥连，因而所得的碳化硼基陶瓷复合材料的力学性能显著提高。
本方法简单有效，易于实现工业化生产。
具体实施方式
为了使本发明更加清楚明白，以下结合具体实例，对本发明作进一步详细说明。应当理解，此处所描述的具体实施案例仅仅用以解释本发明，并不用于限定本发明。
本发明实例中断裂韧性的测试方法采用单边切口梁法，采用电子万能力学试验机。
本发明实例中抗弯强度的测试方法采用三点弯法，采用电子万能力学试验机。
实施例1
将平均粒径为0.7μm的碳化硼粉体40g、平均粒径为2μm二硅化铬粉体10g、250g磨球和35g无水乙醇球磨混合8h，将混合后的粉体放入100℃的烘箱内干燥5h，然后将粉料过50目筛。将过筛后的物料装入高强度、高密度石墨模具腔内，腔体为长方体，腔体四周粘贴一层柔性石墨。在20Pa真空条件下以30℃/min自室温升至1800℃，然后以25℃/min自1800℃升至2050℃。然后对物料施加20MPa压力，保温并保压1h。之后1min内卸掉全部压力，炉体空冷致室温。获得碳化硼陶瓷的致密度为99.93％，为几乎全致密。断裂韧性为5.0MPa·m1 /2，抗弯强度为490MPa，属于高力学性能。
实施例2
将平均粒径为0.6μm的碳化硼粉体35g、平均粒径为1μm二硅化铬粉体8.5g、170g磨球和36g无水乙醇球磨混合6h，将混合后的粉体放入105℃的烘箱内干燥4h，然后将粉料过40目筛。将过筛后的物料装入高强度、高密度石墨模具腔内，腔体为圆柱体，腔体四周粘贴一层柔性石墨。在0.1Pa真空条件下以35℃/min自室温升至1800℃，然后以30℃/min自1800℃升至2100℃。然后对物料施加40MPa压力，保温1h。之后炉体空冷致室温，压力保持40MPa不变。获得碳化硼陶瓷的致密度为99.99％，为几乎全致密。断裂韧性为5.6MPa·m1/2，抗弯强度为520MPa，属于高力学性能。
实施例3
将平均粒径为3μm的碳化硼粉体35g、平均粒径为3μm二硅化铬粉体10g、270g磨球和45g无水乙醇球磨混合5h，将混合后的粉体放入110℃的烘箱内干燥4h，然后将粉料过60目筛。将过筛后的物料装入高强度、高密度石墨模具腔内，腔体为圆柱体，腔体四周粘贴一层柔性氮化硼。在30Pa真空条件下以25℃/min自室温升至1800℃，然后以20℃/min自1800℃升至1900℃。然后对物料施加60MPa压力，保温3h。之后炉体空冷致室温，1min内卸压致40MPa后压力保持40MPa不变。获得碳化硼陶瓷的致密度为99.91％，为几乎全致密。断裂韧性为5.0MPa·m1/2，抗弯强度为480MPa，属于高力学性能。

Claims (9)

1.一种全致密碳化硼陶瓷复合材料，其特征在于，该复合材料的组分包含两种物质，各组分的质量百分比为：65wt％-95wt％的碳化硼，5wt％-35wt％的二硅化铬。
2.根据权利要求1所述的全致密碳化硼陶瓷复合材料，其特征在于，所述的碳化硼粉纯度为95wt％-99.8wt％，平均粒径为0.2μm-10μm。
3.根据权利要求1所述的全致密碳化硼陶瓷复合材料，其特征在于，所述的二硅化铬的纯度为97wt％-99.5wt％，平均粒径为0.1μm-10μm。
4.权利要求1-3任一全致密碳化硼陶瓷复合材料的制备方法，其特征在于，包括如下步骤：
(1)按照全致密碳化硼陶瓷复合材料组成成分及其质量百分比称取，将称取好的碳化硼、二硅化铬粉放入球磨机中，以无水乙醇为介质进行湿磨，2h-24h后将浆料取出；
(2)在50℃-130℃于真空烘箱内烘干1h-20h，然后过20-120目筛；
(3)将过筛后的固体浆料装入石墨模具腔内，0.001Pa-300Pa真空条件下梯度升温至1900℃-2100℃进行烧结；
(4)达到所需温度后加压，压力为15MPa-80MPa，保温并保压0.5h-4h后随炉冷却；经切磨、抛光处理后得到全致密碳化硼陶瓷复合材料。
5.根据权利要求4所述全致密碳化硼陶瓷复合材料的制备方法，其特征在于，步骤(1)中所述湿磨过程球料质量比为3-9，球磨转速为200r/min-700r/min。
6.根据权利要求4所述全致密碳化硼陶瓷复合材料的制备方法，其特征在于，步骤(3)中石墨模具内壁贴一层柔性石墨或者氮化硼。
7.根据权利要求4所述全致密碳化硼陶瓷复合材料的制备方法，其特征在于，步骤(3)中石墨模具腔体是单一圆柱或单一长方体，或者是圆柱和长方体并存。
8.根据权利要求4所述全致密碳化硼陶瓷复合材料的制备方法，其特征在于，步骤(3)中所述梯度升温是以10℃/min-40℃/min的升温速度自室温升至1800℃，然后以5℃/min-30℃/min升温速度自1800℃升至1900℃-2100℃。
9.根据权利要求4所述全致密碳化硼陶瓷复合材料的制备方法，其特征在于，步骤(4)中所述保温保压结束后，随炉冷却过程中保持无压或者施加无压与烧结时所加压力之间任一压力值。
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