CN110041076B - 一种大厚度轻质叠层装甲陶瓷及其制备方法 - Google Patents

一种大厚度轻质叠层装甲陶瓷及其制备方法 Download PDF

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CN110041076B
CN110041076B CN201910451479.3A CN201910451479A CN110041076B CN 110041076 B CN110041076 B CN 110041076B CN 201910451479 A CN201910451479 A CN 201910451479A CN 110041076 B CN110041076 B CN 110041076B
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孙海滨
郭学
李蛟
张振昊
张玉军
吴童
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Shandong University of Technology
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Abstract

本发明涉及一种大厚度轻质叠层装甲陶瓷材料及制备方法。该轻质装甲陶瓷材料由B4C/SiC硬质层和B4C/SiC/BN软质层复合而成。其制备方法包括凝胶注模、浆料喷涂、压制成型、排胶、二次层压、热压烧结等工艺步骤。本发明的装甲陶瓷质量轻、厚度大、密度均匀、硬度高、断裂韧性高，在抗弹领域具有广阔的应用前景。该工艺能够制备出大厚度抗弹陶瓷，且生产效率高。

Description

一种大厚度轻质叠层装甲陶瓷及其制备方法
技术领域
本发明属于抗弹陶瓷技术领域，具体涉及一种大厚度轻质叠层装甲陶瓷及其制备方法。
背景技术
随着反装甲武器技术的高速发展，武器装备的战场生存能力对装甲防护材料的性能提出了非常高的要求。装甲防护材料正朝着强韧化、轻量化和高效化的方向发展。
碳化硼(B4C)陶瓷具有低密度、高硬度、高弹性模量等优异性能，是一种理想的轻质装甲材料。但其脆性大，断裂韧性低(2.2～3.0MPa·m1/2)，易崩裂，无法满足高端工程需求，因此亟待开发高强、高韧B4C陶瓷。传统的增韧方式主要有相变增韧、微裂纹增韧、纤维及晶须增韧、颗粒弥散增韧等。这些增韧方式的作用区域仅局限于几十微米的范围，对B4C陶瓷的韧性提高非常有限。尽管增大陶瓷的厚度可以在一定程度上提高抗弹性能，但是大厚度抗弹陶瓷受制备工艺的限制，其表层和中心的密度差异较大，导致抗弹性能不理想。
发明内容
针对现有技术的不足，为了在保证在B4C陶瓷硬度不降低的前提下提高其断裂韧性，本发明采用凝胶注模、浆料喷涂、压制成型、排胶、二次层压、热压烧结工艺制备一种大厚度的B4C/SiC基轻质叠层装甲陶瓷。所制备的装甲陶瓷具有断裂韧性高、硬度高、抗弹性能好等优点。
本发明的B4C/SiC基叠层装甲陶瓷材料，由B4C/SiC硬质层和B4C/SiC/BN软质层复合而成。B4C/SiC硬质层和B4C/SiC/BN软质层的厚度比为(30～10)：1。B4C/SiC硬质层原料的质量百分比为70-85％B4C粉、15-25％SiC粉、2-4％烧结助剂、1-3％炭黑。B4C/SiC/BN软质层原料的质量百分比为20-35％B4C粉、4-8％SiC粉、2-4％烧结助剂、1～3％炭黑、55-70％BN粉。烧结助剂指的是Al2O3-MgO-Y2O3复合粉体，其中Al2O3：MgO：Y2O3的质量比为33:37:30。
所述B4C粉平均粒径为0.5微米，纯度≥96％；所述SiC粉平均粒径为0.5微米，纯度≥98％；所述BN粉为六方氮化硼，平均粒径为3微米，纯度≥98％；Al2O3、MgO和Y2O3的纯度≥98.5％。
本发明技术方案如下：
1、凝胶注模
按质量百分比称取70-85％B4C粉、15-25％SiC粉、2-4％烧结助剂、1-3％炭黑，混合均匀，得到粉料A。向粉料A添加质量百分比的0.8-1.2％四甲基氢氧化铵、25-30％丙烯酸胺单体、1.5-2.5％N’N-亚甲基双丙烯酰胺、0.3-0.6％磷酸三丁酯、35-45％去离子水。球磨1-2小时，向浆料中添加3-5％过硫酸铵。真空搅拌5-8分钟，充分去除气泡。
将上述浆料倒入平行固定放置的平板玻璃模具中，玻璃平板间隙在50-80微米范围内可控。在室温条件下，浆料静置固化12-20小时。脱模，得到薄层坯体。在温度为50-65℃、湿度为70-85％的条件下烘干，得到B4C/SiC生坯层。经裁剪，得到所需尺寸和形状。
2、浆料喷涂
按质量百分比称20-35％B4C粉、4-8％SiC粉、2-4％烧结助剂、1～3％炭黑、55-70％BN粉，混合均匀，得到粉料B。将粉料B加入无水乙醇溶剂中，搅拌均匀得到浆料，其固含量为15-35％。将浆料均匀喷涂在步骤1制备的B4C/SiC生坯层的表面，B4C/SiC硬质层和B4C/SiC/BN软质层的厚度比为(30～10)：1，自然晾干。
3、压制成型
将5-10层步骤2制备的坯体层叠，在30-50MPa压制成型，得到平整的预制坯体。
4、排胶
将步骤3制备的预制坯体放置在气氛炉中，在氮气气氛下，以2-5℃/min的速率升温至500℃，保温1-3小时，充分排胶。
5、二次层压
取20-30层步骤4制备的预制坯体层叠，在30-50MPa压制成型，得到密度均匀的厚度为5-24mm的坯体。
6、热压烧结
取8-15层步骤5制备的坯体层叠在热压烧结炉的石墨模具中，抽真空至5-15Pa，以3-6℃/min的速率升温至1450℃，保温30-50min，然后，继续升温至1800-1900℃，压力保持在25-35MPa，保温30-60min。自然降温，得到密度均匀的厚度为40-360mm的B4C/SiC基轻质叠层装甲陶瓷。
根据本发明优选的，步骤1的球磨介质为碳化硅球。
根据本发明优选的，步骤1粉料A的质量百分比为75-80％B4C粉、15-20％SiC粉、3％烧结助剂、2％炭黑。
根据本发明优选的，步骤1的固化时间为16-18小时。
根据本发明优选的，步骤1坯体的烘干温度为55-60℃，湿度为75-80％。
根据本发明优选的，步骤2粉料B的质量百分比为25-30％B4C粉、5-7％SiC粉、3％烧结助剂、1％炭黑、60-66％BN粉。
根据本发明优选的，步骤2中浆料固含量为25-30％。
根据本发明优选的，步骤2中B4C/SiC硬质层和B4C/SiC/BN软质层的厚度比为(25～18):1。
根据本发明优选的，步骤3的成型压力为40-45MPa。
根据本发明优选的，步骤4的升温速率为3-4℃/min。
根据本发明优选的，步骤5的成型压力为43-48MPa。
根据本发明优选的，步骤6的热压烧结工艺为：抽真空至5-8Pa，以3-5℃/min的速率升温至1450℃，保温40-45min，然后，继续升温至1850-1880℃，压力保持在28-30MPa，保温45-50min。
根据本发明优选的，步骤6制备的轻质叠层装甲陶瓷的密度小于2.8g/cm3。
有益效果
1、本发明的叠层装甲陶瓷由B4C/SiC硬质层和B4C/SiC/BN软质层复合而成。添加SiC颗粒能够提高B4C/SiC层内断裂韧性，层间断裂方式为贝壳仿生裂纹偏转机制。该叠层装甲陶瓷的断裂韧性是纯B4C陶瓷的2倍以上。
2、本发明采用二次层压和热压烧结相结合的工艺，能够制备出厚度大于10cm的大厚度抗弹陶瓷，而且，陶瓷上下表面和中心的密度一致，可有效解决传统粉料热压烧结制备大厚度抗弹陶瓷所存在的因密度不均匀而导致抗弹性能下降的问题。
3、本发明通过添加适量的Al2O3-MgO-Y2O3复合烧结助剂，可显著提高抗弹陶瓷的烧结性能，有助于提高致密度，进而提高抗弹性能。
具体实施方式
下面结合实施例对本发明的技术方案做进一步说明，但本发明所保护范围不限于此。
实施例1：
按质量百分比称取80％B4C粉、15％SiC粉、3％烧结助剂、2％炭黑，混合均匀，得到粉料A。向粉料A添加质量百分比的0.8％四甲基氢氧化铵、26％丙烯酸胺单体、2％N’N-亚甲基双丙烯酰胺、0.5％磷酸三丁酯、40％去离子水。球磨1小时，向浆料中添加4％过硫酸铵。真空搅拌5分钟，充分去除气泡。将上述浆料倒入平行固定放置的平板玻璃模具中，玻璃平板间隙为50微米。在室温条件下，浆料静置固化16小时。脱模，得到薄层坯体。在温度为60℃、湿度为75％的条件下烘干，得到B4C/SiC生坯层。经裁剪，得到所需尺寸和形状。
按质量百分比称25％B4C粉、5％SiC粉、3％烧结助剂2％炭黑、65％BN粉，混合均匀，得到粉料B。将粉料B加入无水乙醇溶剂中，搅拌均匀，其固含量为30％。将溶液均匀喷涂在B4C/SiC生坯层的表面，B4C/SiC硬质层和B4C/SiC/BN软质层的厚度比为20:1，自然晾干。取8层上述坯体，层叠，在40MPa压制成型，得到平整的预制坯体。将平整的预制坯体放置在气氛炉中，在氮气气氛下，以3℃/min的速率升温至500℃，保温2小时，充分排胶。取10层上述预制坯体层叠，在45MPa压制成型，得到密度均匀的厚度约为4mm的坯体。
取15层厚度为4mm的坯体层叠在热压烧结炉的石墨模具中，抽真空至8Pa，以5℃/min的速率升温至1450℃，保温40min，然后，继续升温至1850℃，压力保持在28MPa，保温45min。自然降温，得到密度均匀的厚度大于40mm的轻质叠层装甲陶瓷。
该抗弹陶瓷的密度约为2.61g/cm3，维氏硬度为30GPa，断裂韧性为7.1MPa·m1/2。
实施例2：
按质量百分比称取75％B4C粉、20％SiC粉、3％烧结助剂、2％炭黑，混合均匀，得到粉料A。向粉料A添加质量百分比的1％四甲基氢氧化铵、27％丙烯酸胺单体、1.5％N’N-亚甲基双丙烯酰胺、0.4％磷酸三丁酯、36％去离子水。球磨1.5小时，向浆料中添加3.5％过硫酸铵。真空搅拌7分钟，充分去除气泡。将上述浆料倒入平行固定放置的平板玻璃模具中，玻璃平板间隙为80微米。在室温条件下，浆料静置固化18小时。脱模，得到薄层坯体。在温度为65℃、湿度为80％的条件下烘干，得到B4C/SiC生坯层。经裁剪，得到所需尺寸和形状。
按质量百分比称28％B4C粉、7％SiC粉、3％烧结助剂2％炭黑、60％BN粉，混合均匀，得到粉料B。将粉料B加入无水乙醇溶剂中，搅拌均匀，其固含量为28％。将溶液均匀喷涂在B4C/SiC生坯层的表面，B4C/SiC硬质层和B4C/SiC/BN软质层的厚度比为24:1，自然晾干。取6层上述坯体，层叠，在45MPa压制成型，得到平整的预制坯体。将平整的预制坯体放置在气氛炉中，在氮气气氛下，以4℃/min的速率升温至500℃，保温2小时，充分排胶。取20层上述预制坯体层叠，在45MPa压制成型，得到密度均匀的厚度约为9.6mm的坯体。
取13层厚度为9.6mm的坯体层叠在热压烧结炉的石墨模具中，抽真空至5Pa，以5℃/min的速率升温至1450℃，保温40min，然后，继续升温至1880℃，压力保持在30MPa，保温50min。自然降温，得到密度均匀的厚度大于100mm的轻质叠层装甲陶瓷。
该抗弹陶瓷的密度约为2.66g/cm3，硬度为28GPa，断裂韧性为7.4MPa·m1/2。
需要说明的是，以上列举的仅是本发明的若干个具体实施例，显然本发明不仅仅限于以上实施例，还可以有其他变形。本领域的技术人员从本发明公开内容直接导出或间接引申的所有变形，均应认为是本发明的保护范围。

Claims (2)

1.一种大厚度轻质叠层装甲陶瓷材料，其特征在于，由B4C/SiC硬质层和B 4C/SiC/BN软质层复合而成；B4C/SiC硬质层和B4C/SiC/BN软质层的厚度比为(30～10):1，所述B4C/SiC硬质层的成分为质量百分比70-85％B4C粉、15-25％SiC粉、2-4％烧结助剂、1-3％炭黑,所述B4C/SiC硬质层中各组分质量百分比之和为100％，所述B4C/SiC/BN软质层的成分为质量百分比20-35％B4C粉、4-8％SiC粉、2-4％烧结助剂、1～3％炭黑、55-70％BN粉，所述大厚度轻质叠层装甲陶瓷材料按以下步骤制备而成：
(1)凝胶注模
按质量百分比称取70-85％B4C粉、15-25％SiC粉、2-4％烧结助剂、1-3％炭黑，混合均匀，得到粉料A；向粉料A添加质量百分比的0.8-1.2％四甲基氢氧化铵、25-30％丙烯酸胺单体、1.5-2.5％N’N-亚甲基双丙烯酰胺、0.3-0.6％磷酸三丁酯、35-45％去离子水；球磨1-2小时，向浆料中添加3-5％过硫酸铵；真空搅拌5-8分钟，充分去除气泡；将浆料倒入平行固定放置的平板玻璃模具中，玻璃平板间隙在50-80微米范围内可控；在室温条件下，浆料静置固化12-20小时；脱模，得到薄层坯体；在温度为50-65℃、湿度为70-85％的条件下烘干，得到B4C/SiC生坯层；经裁剪，得到所需尺寸和形状；
(2)浆料喷涂
按质量百分比称20-35％B4C粉、4-8％SiC粉、2-4％烧结助剂、1～3％炭黑、55-70％BN粉，混合均匀，得到粉料B；将粉料B加入无水乙醇溶剂中，搅拌均匀，其固含量为15-35％；将浆料均匀喷涂在步骤(1)制备的B4C/SiC生坯层的表面，B4C/SiC硬质层和B4C/SiC/BN软质层的厚度比为(30～10):1，自然晾干；
(3)压制成型
将5-10层步骤(2)制备的坯体层叠，在30-50MPa压制成型，得到平整的预制坯体；
(4)排胶
将步骤(3)制备的预制坯体放置在气氛炉中，在氮气气氛下，以2-5℃/min的速率升温至500℃，保温1-3小时，充分排胶；
(5)二次层压
取20-30层步骤(4)制备的预制坯体层叠，在30-50MPa压制成型，得到密度均匀的厚度为5-24mm的坯体；
(6)热压烧结
取8-15层步骤(5)制备的坯体层叠在热压烧结炉的石墨模具中，抽真空至5-15Pa，以3-6℃/min的速率升温至1450℃，保温30-50min，然后，继续升温至1800-1900℃，压力保持在25-35MPa，保温30-60min；自然降温，得到密度均匀的厚度为40-360mm的轻质叠层装甲陶瓷。
2.如权利要求1所述大厚度轻质叠层装甲陶瓷材料，其特征在于，所述烧结助剂是Al2O3-MgO-Y2O3复合粉体，Al2O3:MgO: Y2O3的质量比为33:37:30。
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