CN111943680A - 一种碳化硼材料的制备方法及其应用 - Google Patents

一种碳化硼材料的制备方法及其应用 Download PDF

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CN111943680A
CN111943680A CN202010822740.9A CN202010822740A CN111943680A CN 111943680 A CN111943680 A CN 111943680A CN 202010822740 A CN202010822740 A CN 202010822740A CN 111943680 A CN111943680 A CN 111943680A
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boron carbide
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CN111943680B (zh
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李春松
唐洁净
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Ningbo Plastic Metal Product Co ltd
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Abstract

碳化硼硬度高，其对于动能弹和弹药碎片的防御能力很强，而且碳化硼质量较轻，是制备防弹衣、防护装甲的理想材料。本发明首先制备多孔碳化硼材料，再通过浸渍、焙烧对部分多孔结构进行填充，得到了一种同时具有致密层和多孔层的碳化硼材料，使材料同时具有高硬度和吸波性能，提高材料应用于防弹材料时的抗冲击能力。

Description

一种碳化硼材料的制备方法及其应用
技术领域
本发明涉及一种防弹材料领域，特别是一种碳化硼材料。
背景技术
碳化硼又称黑钻石，通常为灰黑色微粉，是一种新型陶瓷材料，具有熔点高、硬度高、密度低、热稳定性好、抗化学侵蚀能力强和中子吸收能力强等特点，因而被广泛应用于能源、军事、核能以及防弹领域。碳化硼最重要的性能是其超常的硬度，是仅次于金刚石和立方氮化硼的第三硬材料，碳化硼近于恒定的高温硬度是其它材料所无法比拟的。
由于碳化硼硬度高，其对于动能弹和弹药碎片的防御能力很强，而且碳化硼质量较轻，是制备防弹衣、防护装甲的理想材料，并得到了广泛的关注。然而，现有制备工艺得到碳化硼晶粒粗大、缺陷多、致密度低，因而其强度和韧性并不理想，如何改善碳化硼的致密度以提高其硬度，并同时使材料具备足够的抗冲击性是防弹领域亟待解决的问题。
发明内容
本发明通过制备同时具有致密层和多孔层的碳化硼复合材料，使材料同时具有高硬度和吸波性能，提高材料应用于防弹材料时的抗冲击能力。
一种碳化硼材料的制备方法，包括如下步骤：
(1)制备多孔碳化硼块体
将碳化硼粉加入到含有分散剂的水溶液中，搅拌均匀，加入成孔剂，球磨3-5h，成型，真空条件下烧结，得到多孔碳化硼块体；
(2)浸渍、焙烧
将70％-85％的硼酸溶于甘油中，搅拌均匀，得到硼酸溶液；在真空条件下将多孔碳化硼块体部分浸入硼酸溶液中，浸渍20-30分钟，取出，在氩气保护下焙烧，真空下冷却到室温，得到碳化硼材料。
步骤(1)中，所述分散剂为EDTA或硬脂酸钠，用量为述B4C粉质量的0.4～0.7％。
步骤(1)中，所述成孔剂为PEG-400，用量为述B4C粉质量的5～10％。
步骤(1)中，B4C粉按固含量为30％～50％的比例加入；B4C粉的粒径为3～5μm。
步骤(1)中，所述烧结的温度为2000～2300℃，时间为3-5h。
步骤(2)中，硼酸与甘油的摩尔比为5-7∶1。
步骤(2)中，焙烧方式为通过程序升温，先以5-10℃/min的升温速度，升温至400-500℃，保温8-10h，再以10-15℃/min的升温速度，升温至1500-1600℃，保温5-6h。
步骤(2)中，将多孔碳化硼块体部分浸入硼酸溶液中时，浸入部分的高度占块体材料总高度的20-50％。
有益效果：
本发明通过部分浸渍的方法，使得硼酸和甘油浸入到碳化硼多孔材料中，在煅烧过程中，硼酸和甘油在碳化硼多孔材料的空隙中反应生成了碳化硼，填补了碳化硼多孔材料的部分空隙，使得碳化硼多孔材料的下层形成致密的结构，从而得到一种上部为多孔结构，下部为致密结构的碳化硼复合材料，其致密部分具有高硬度，从而使复合材料保持良好的硬度，其多孔部分可起到吸收剩余能量的作用，有助于材料在整体上表现出更优的硬度。由于多孔结构和致密结构为整体结构，不存在由于不同材料之间的结合而导致的能量传递效率低、结构不稳定等问题，在防弹过程中具有更好的抗热冲击性。
通过控制多孔结构的孔径、含孔率，控制在浸渍过程中的填充度，避免孔径大、通孔多造成的填充程度难以控制，以及孔径小、含孔率不足造成的致密化不足。通过控制程序升温过程避免煅烧过程中破坏上层多孔部分的结构以及在下层形成致密层。
该复合材料的洛氏硬度85-87HRA，断裂韧性为12-16MP·m1/2。
具体实施方式
采用陶瓷材料单刃缺口弯曲法测试材料的断裂韧性。
实施例1
(1)制备多孔碳化硼块体
将粒径为3μm的碳化硼粉加入到含有EDTA的水溶液中，搅拌均匀，加入PEG-400，球磨3-5h，成型，真空条件下2300℃烧结3h，得到多孔碳化硼块体；步骤(1)中，B4C粉按固含量为50％的比例加入，EDTA用量为述B4C粉质量的0.4％，PEG-400用量为B4C粉质量的10％。
(2)浸渍、焙烧
将70％-85％的硼酸溶于甘油中，硼酸与甘油的摩尔比为5∶1，搅拌均匀，得到硼酸溶液；在真空条件下将多孔碳化硼块体部分浸入硼酸溶液中，浸入部分的高度占块体材料总高度的50％，浸渍30分钟，取出，在氩气保护下，通过程序升温，先以5℃/min的升温速度，升温至500℃，保温8h，再以10℃/min的升温速度，升温至1500℃，保温5h，真空下冷却到室温，得到碳化硼材料-1。致密层、多孔层高度比大致为1∶1。该复合材料的洛氏硬度87HRA，断裂韧性为14MP·m1/2。
实施例2
(1)制备多孔碳化硼块体
将粒径为5μm的碳化硼粉加入到含有硬脂酸钠的水溶液中，搅拌均匀，加入PEG-400，球磨3-5h，成型，真空条件下2000℃烧结5h，得到多孔碳化硼块体；步骤(1)中，B4C粉按固含量为30％的比例加入，硬脂酸钠用量为述B4C粉质量的0.7％，PEG-400用量为B4C粉质量的5％。
(2)浸渍、焙烧
将70％-85％的硼酸溶于甘油中，硼酸与甘油的摩尔比为7∶1，搅拌均匀，得到硼酸溶液；在真空条件下将多孔碳化硼块体部分浸入硼酸溶液中，浸入部分的高度占块体材料总高度的20％，浸渍20分钟，取出，在氩气保护下，通过程序升温，先以10℃/min的升温速度，升温至400℃，保温10h，再以15℃/min的升温速度，升温至1600℃，保温6h，真空下冷却到室温，得到碳化硼材料-2。致密层、多孔层高度比大致为1∶4。该复合材料的洛氏硬度85HRA，断裂韧性为14MP·m1/2。
实施例3
(1)制备多孔碳化硼块体
将粒径为5μm的碳化硼粉加入到含有硬脂酸钠的水溶液中，搅拌均匀，加入PEG-400，球磨3-5h，成型，真空条件下2000℃烧结5h，得到多孔碳化硼块体；步骤(1)中，B4C粉按固含量为30％的比例加入，硬脂酸钠用量为述B4C粉质量的0.7％，PEG-400用量为B4C粉质量的5％。
(2)浸渍、焙烧
将70％-85％的硼酸溶于甘油中，硼酸与甘油的摩尔比为5∶1，搅拌均匀，得到硼酸溶液；在真空条件下将多孔碳化硼块体部分浸入硼酸溶液中，浸入部分的高度占块体材料总高度的30％，浸渍30分钟，取出，在氩气保护下，通过程序升温，先以5℃/min的升温速度，升温至500℃，保温8h，再以10℃/min的升温速度，升温至1500℃，保温5h，真空下冷却到室温，得到碳化硼材料-3。致密层、多孔层高度比大致为3∶7。该复合材料的洛氏硬度86HRA，断裂韧性为16MP·m1/2。
实施例4
(1)制备多孔碳化硼块体
将粒径为3μm的碳化硼粉加入到含有EDTA的水溶液中，搅拌均匀，加入琼脂糖，球磨3-5h，成型，真空条件下2300℃烧结3h，得到多孔碳化硼块体；步骤(1)中，B4C粉按固含量为50％的比例加入，EDTA用量为述B4C粉质量的0.4％，琼脂糖用量为B4C粉质量的10％。
(2)浸渍
将70％-85％的硼酸溶于甘油中，硼酸与甘油的摩尔比为5∶1，搅拌均匀，得到硼酸溶液；在真空条件下将多孔碳化硼块体部分浸入硼酸溶液中，浸入部分的高度占块体材料总高度的30％，浸渍30分钟，取出，在氩气保护下，通过程序升温，先以5℃/min的升温速度，升温至500℃，保温8h，再以10℃/min的升温速度，升温至1500℃，保温5h，真空下冷却到室温，得到碳化硼复合材料-4。该多孔材料孔径大，孔隙率高，在浸渍过程中难以控制浸渍程度，导致碳化硼复合材料-4中致密层厚度难以控制，且在块体材料中部较大高度范围内既有致密层又有多孔层，同一横截面上材料结构不一致，无法得到具有一定致密层、多孔层高度比的材料。该复合材料的洛氏硬度75HRA，断裂韧性为6MP·m1/2。
实施例5
(1)制备多孔碳化硼块体
将粒径为3μm的碳化硼粉加入到含有EDTA的水溶液中，搅拌均匀，加入PEG-400，球磨3-5h，成型，真空条件下2300℃烧结3h，得到多孔碳化硼块体；步骤(1)中，B4C粉按固含量为50％的比例加入，EDTA用量为述B4C粉质量的0.4％，PEG-400用量为B4C粉质量的10％。
(2)浸渍
将70％-85％的硼酸溶于甘油中，硼酸与甘油的摩尔比为5∶1，搅拌均匀，得到硼酸溶液；在真空条件下将多孔碳化硼块体部分浸入硼酸溶液中，浸入部分的高度占块体材料总高度的60％，浸渍30分钟，取出，在氩气保护下，通过程序升温，先以5℃/min的升温速度，升温至500℃，保温8h，再以10℃/min的升温速度，升温至1500℃，保温5h，真空下冷却到室温，得到碳化硼复合材料-5。致密层、多孔层高度比大致为6∶4。碳化硼复合材料-5中多孔层比例小，吸能效果显著下降。该复合材料的洛氏硬度75HRA，断裂韧性为7MP·m1/2。
实施例6
(1)制备多孔碳化硼块体
将粒径为3μm的碳化硼粉加入到含有EDTA的水溶液中，搅拌均匀，加入PEG-400，球磨3-5h，成型，真空条件下2300℃烧结3h，得到多孔碳化硼块体；步骤(1)中，B4C粉按固含量为50％的比例加入，EDTA用量为述B4C粉质量的0.4％，PEG-400用量为B4C粉质量的10％。
(2)浸渍
将70％-85％的硼酸溶于甘油中，硼酸与甘油的摩尔比为5∶1，搅拌均匀，得到硼酸溶液；在真空条件下将多孔碳化硼块体部分浸入硼酸溶液中，浸入部分的高度占块体材料总高度的10％，浸渍30分钟，取出，在氩气保护下，通过程序升温，先以5℃/min的升温速度，升温至500℃，保温8h，再以10℃/min的升温速度，升温至1500℃，保温5h，真空下冷却到室温，得到碳化硼复合材料-6。致密层、多孔层高度比大致为1∶9。碳化硼复合材料-6中致密层比例小，硬度显著下降。该复合材料的洛氏硬度63HRA，断裂韧性为8MP·m1/2。
实施例7
(1)制备多孔碳化硼块体
将粒径为3μm的碳化硼粉加入到含有EDTA的水溶液中，搅拌均匀，加入PEG-400，球磨3-5h，成型，真空条件下2300℃烧结3h，得到多孔碳化硼块体；步骤(1)中，B4C粉按固含量为50％的比例加入，EDTA用量为述B4C粉质量的0.4％，PEG-400用量为B4C粉质量的10％。
(2)浸渍
将70％-85％的硼酸溶于甘油中，硼酸与甘油的摩尔比为5∶1，搅拌均匀，得到硼酸溶液；在真空条件下将多孔碳化硼块体部分浸入硼酸溶液中，浸入部分的高度占块体材料总高度的100％，浸渍30分钟，取出，在氩气保护下，通过程序升温，先以5℃/min的升温速度，升温至500℃，保温8h，再以10℃/min的升温速度，升温至1500℃，保温5h，真空下冷却到室温，得到致密结构碳化硼复合材料。
(3)黏结泡沫铝
利用环氧树脂黏结所得致密结构碳化硼复合材料和泡沫铝，制备出碳化硼与泡沫铝双层复合材料。该复合材料的洛氏硬度79HRA，断裂韧性为6MP·m1/2。
实施例8
(1)制备多孔碳化硼块体
将粒径为5μm的碳化硼粉加入到含有硬脂酸钠的水溶液中，搅拌均匀，加入PEG-400，球磨3-5h，成型，真空条件下2000℃烧结5h，得到多孔碳化硼块体；步骤(1)中，B4C粉按固含量为30％的比例加入，硬脂酸钠用量为述B4C粉质量的0.7％，PEG-400用量为B4C粉质量的5％。
(2)浸渍、焙烧
将70％-85％的硼酸溶于甘油中，硼酸与甘油的摩尔比为5∶1，搅拌均匀，得到硼酸溶液；在真空条件下将多孔碳化硼块体部分浸入硼酸溶液中，浸入部分的高度占块体材料总高度的30％，浸渍30分钟，取出，在氩气保护下，通过程序升温，先以15℃/min的升温速度，升温至700℃，保温8h，再以20℃/min的升温速度，升温至1700℃，保温5h，真空下冷却到室温，得到碳化硼材料-8。升温速度过快或煅烧温度高均会破坏多孔结构。该复合材料的洛氏硬度80HRA，断裂韧性为6MP·m1/2。

Claims (10)

1.一种碳化硼材料的制备方法，其特征在于：包括如下步骤：
(1)制备多孔碳化硼块体
将碳化硼粉加入到含有分散剂的水溶液中，搅拌均匀，加入成孔剂，球磨3-5h，成型，真空条件下烧结，得到多孔碳化硼块体；
(2)浸渍、焙烧
将70％-85％的硼酸溶于甘油中，搅拌均匀，得到硼酸溶液；在真空条件下将多孔碳化硼块体部分浸入硼酸溶液中，浸渍20-30分钟，取出，在氩气保护下焙烧，真空下冷却到室温，得到碳化硼材料。
2.根据权利要求1所述的制备方法，其特征在于：步骤(1)中，所述分散剂为EDTA或硬脂酸钠，用量为述B4C粉质量的0.4～0.7％。
3.根据权利要求1所述的制备方法，其特征在于：步骤(1)中，所述成孔剂为PEG-400，用量为述B4C粉质量的5～10％。
4.根据权利要求1所述的制备方法，其特征在于：步骤(1)中，B4C粉按固含量为30％～50％的比例加入；B4C粉的粒径为3～5μm。
5.根据权利要求1所述的制备方法，其特征在于：步骤(1)中，所述烧结的温度为2000～2300℃，时间为3-5h。
6.根据权利要求1所述的制备方法，其特征在于：步骤(2)中，硼酸与甘油的摩尔比为5-7∶1。
7.根据权利要求1所述的制备方法，其特征在于：步骤(2)中，焙烧方式为通过程序升温，先以5-10℃/min的升温速度，升温至400-500℃，保温8-10h，再以10-15℃/min的升温速度，升温至1500-1600℃，保温5-6h。
8.根据权利要求1所述的制备方法，其特征在于：步骤(2)中，将多孔碳化硼块体部分浸入硼酸溶液中时，浸入部分的高度占块体材料总高度的20-50％。
9.根据权利要求1-8所述的制备方法制备得到的碳化硼材料。
10.根据权利要求1-8所述的制备方法制备得到的碳化硼材料用于防弹衣材料的用途。
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