CN112028656A - 纤维增强石墨复合材料的制备方法 - Google Patents

纤维增强石墨复合材料的制备方法 Download PDF

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CN112028656A
CN112028656A CN202010977440.8A CN202010977440A CN112028656A CN 112028656 A CN112028656 A CN 112028656A CN 202010977440 A CN202010977440 A CN 202010977440A CN 112028656 A CN112028656 A CN 112028656A
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graphite
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刘萌戈
马小虎
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Jiangsu Senyan Fine Graphite Technology Co ltd
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Abstract

本发明涉及一种纤维增强石墨复合材料的制备方法，包括如下步骤：按重量份计，将石墨、煅后焦、改质沥青、润滑剂、耐磨剂、喷雾碳黑和短切玻璃纤维混捏、磨粉后得到粉料；将粉料与粘结剂、脱模剂添加到快速搅拌制粒机中进行造粒，得到造粒料；将造粒料在液压机上近净成型，得到石墨生坯；烧结；精加工。本发明采用石墨和煅后焦作为主要原料，采用焙烧后具有高残碳值和高强度的改质沥青作为粘结剂,具有高强度和高硬度的特性，同时具有高的耐磨性，添加喷雾碳黑和玻璃纤维作为增强成分，进一步提高材料的耐磨性；采用造粒技术提高产品的稳定性，同时采用近净成型的方式实现快速烧结。

Description

纤维增强石墨复合材料的制备方法
技术领域
本发明涉及石墨复合材料领域，具体涉及一种纤维增强石墨复合材料的制备方法。
背景技术
石墨是一种结晶形碳，六方晶系,为铁墨色至深灰色，质软,有滑腻感,可导电，化学性质不活泼,耐腐蚀,与酸、碱等不易反应。主要用作抗摩剂和润滑材料,制作坩埚、电极、干电池、铅笔芯。石墨在工业上运用极广，几乎每个行业都会用到，其中应用最多的是人造石墨，其成型的方式主要有：等静压石墨、模压石墨、挤压石墨。但是，现有的人造石墨强度、硬度和耐磨损性能物理性能不高，不能满足市场需求。
发明内容
本发明的目的在于提供一种纤维增强石墨复合材料的制备方法，用以解决现有技术中的人造石墨物理性能不能满足市场需求的问题。
本发明提供了一种纤维增强石墨复合材料的制备方法，包括如下步骤：
(1)按重量份计，将20～30份石墨、30～60份煅后焦、20～40份改质沥青、1～5份润滑剂、1～5份耐磨剂、0.1～10份的喷雾碳黑和0.1～5重量份数的短切玻璃纤维混捏、磨粉后得到粉料，所述短切玻璃纤维的长度为1-5mm；
(2)将步骤(1)所得粉料与粘结剂、脱模剂添加到快速搅拌制粒机中进行造粒，得到造粒料，所述脱模剂和粉料的重量比为1：100，所述快速搅拌制粒机的电机转速为5000～30000转/分钟，搅拌时间为0.5～2小时，搅拌温度为100～120℃；
(3)将步骤(2)所得造粒料在液压机上近净成型，得到石墨生坯，其中，近净成型的压力为100～300Mpa；
(4)烧结，其中烧成温度为800～1200℃，保温时间为1～5h；
(5)精加工。
进一步的，所述石墨为天然石墨和/或人造石墨，所述石墨的平均颗粒粒径为10～50μm。
进一步的，所述煅后焦为煅后石油焦和/或煅后沥青焦，所述煅后焦的平均颗粒粒径为10～50μm。
进一步的，所述改质沥青的软化点为105～120℃，喹啉不溶物含量为6～10％，甲苯不溶物含量为20～30％。
进一步的，所述润滑剂为二硫化钨和/或二硫化钼。
进一步的，所述耐磨剂为碳化硅、二氧化硅、氧化铝、磷酸二氢铝、硅酸镁、硅灰石中的一种或多种。
进一步的，所述粘结剂为聚丙烯酸氨、聚乙烯醇、聚氯乙烯、甘油乙醇、石蜡乙醚中的一种或多种。
进一步的，所述脱膜剂为硬脂酸、油酸、N,N'-乙撑双硬脂酰胺、石蜡、硬脂酸锌中的一种或多种。
进一步的，所述粉料的平均粒径为5～35μm。
进一步的，所述造粒料的平均粒径为30～80μm。
采用上述本发明技术方案的有益效果是：
本发明采用石墨和煅后焦作为主要原料，采用焙烧后具有高残碳值和高强度的改质沥青作为粘结剂，制备出来的碳-石墨材料，既具备碳材料高强度、高硬度的特性，又具有石墨材料的润滑特性，添加的耐磨剂和润滑剂进一步提升了材料的耐磨损性能，能够适用于运行时长期的干摩擦环境；
本发明添加喷雾碳黑和玻璃纤维作为增强成分，喷雾碳黑可以进一步的提升材料的耐磨性能，而短切玻璃纤维在提高强度的同时也能够适度的提高材料的耐磨性，这两种添加剂作为碳质原料都不会改变最终材料中碳的百分含量；
本发明通过对粉体进行造粒处理，改善了粉体的流动性，粉体能够更均匀的填充到成型模具中，压制时在模具内部也能够更好的进行流动，提高了产品的稳定性；
本发明的石墨制品采用近净成型的方式，生坯的表面积大，烧结时有利于挥发物的排放，产品不易开裂，可以实现快速烧结；同时能够极大的减少加工量，提高材料利用率，降低生产成本，易于实现大批量生产。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。
实施例1
(1)按重量份计，将25份天然石墨、37份煅后石油焦、32份改质沥青、2份二硫化钨和4份碳化硅混捏和磨粉后得到平均粒径为34.8μm为粉料，其中，天然石墨的平均颗粒粒径为35.2μm，煅后石油焦的平均颗粒粒径为18.6μm，改质沥青软化点为106℃，喹啉不溶物含量为8.5％，甲苯不溶物含量为28.3％；
(2)将100份粉料、0.5份聚丙烯酸氨添加至快速搅拌制粒机内进行造粒，得到平均粒径为65.7μm的造粒料，快速搅拌制粒机电机转速为8000转/分钟，搅拌时间为2小时，搅拌温度为105℃；
(3)将造粒料在液压机上近净成型，成型压力为200MPa，得到石墨生坯；
(4)将石墨转子生坯在1100℃下保温2h进行烧成处理；
(5)精加工。
实施例1石墨复合材料制备的石墨轴承的体积密度为1.72g/cm3，肖氏硬度为65(HSD)，电阻率为35μΩm，弹性模量为15GPa，按照GB/T8872-2002中的工作耐久性测试方法，经过6000小时石墨轴承磨损量为0.124mm。
实施例2
(1)按重量份计，将30份人造石墨、32份煅后沥青焦、24份改质沥青、1份二硫化钼和3份硅混捏和磨粉后得到平均粒径为28.5μm为粉料，人造石墨的平均颗粒粒径为28.8μm，煅后沥青焦的平均颗粒粒径为25.5μm，改质沥青软化点为112℃，喹啉不溶物含量为6.8％，甲苯不溶物含量为22.5％；
(2)将100份粉料、38份水、0.8份石蜡乙醚和0.9份硬脂酸锌添加至快速搅拌制粒机内进行造粒，得到平均粒径为55.8μm的造粒料，快速搅拌制粒机电机转速为10000转/分钟，搅拌时间为1.5小时，搅拌温度为105℃；
(3)将造粒料在液压机上近净成型，成型压力为180MPa，得到石墨转子生坯；
(4)将石墨转子生坯在1000℃下保温3.5h进行烧成处理；
(5)精加工。
该实施例2墨复合材料制备的石墨轴承的体积密度为1.75g/cm3，肖氏硬度为69(HSD)，电阻率为24μΩm，弹性模量为12GPa，按照GB/T8872-2002中的工作耐久性测试方法，经过6000小时后石墨轴承端面磨损量为0.097mm。
实施例3
(1)将15份人造石墨、10份天然石墨、58份煅后沥青焦、38份改质沥青、3份短切玻璃纤维、2份二硫化钨、2份SiO2和5份喷雾碳黑混捏和磨粉后得到平均粒径为21.2μm的粉料，人造石墨和天然石墨的混合物的平均颗粒粒径为28.2μm，煅后石油焦的平均颗粒粒径为18.9μm，改质沥青软化点为117℃，喹啉不溶物含量为8.2％，甲苯不溶物含量为35.8％；
(2)将100份粉料、85份水、0.7份石蜡乙醚和0.5份硬脂酸锌添加至快速搅拌制粒机内进行造粒，得到平均粒径为72.4μm的造粒料，快速搅拌制粒机电机转速为8000转/分钟，搅拌时间为2小时，搅拌温度为118℃；
(3)将造粒料在液压机上近净成型，成型压力为220MPa，得到石墨转子生坯；
(4)将石墨转子生坯在900℃下保温4h进行烧成处理；
(5)精加工。
该实施例3墨复合材料制备的石墨转子的体积密度为1.68g/cm3，肖氏硬度为75(HSD)，电阻率为45μΩm，弹性模量为22GPa，按照GB/T8872-2002中的工作耐久性测试方法，经过6000小时万次疲劳测试循，石墨轴承磨损量为0.063mm。
由实施例1-3实验结果可知，在原材中添加喷雾碳黑和玻璃纤维后石墨复合材料的物理性能得到明显提高，尤其表现为耐磨性显著提升。
综上，本发明采用石墨和煅后焦作为主要原料，采用焙烧后具有高残碳值和高强度的改质沥青作为粘结剂，制备出来的碳-石墨材料，既具备碳材料高强度、高硬度的特性，又具有石墨材料的润滑特性，添加的耐磨剂和润滑剂进一步提升了材料的耐磨损性能，能够适用于运行时长期的干摩擦环境；本发明添加喷雾碳黑和玻璃纤维作为增强成分，喷雾碳黑可以进一步的提升材料的耐磨性能，而短切玻璃纤维在提高强度的同时也能够适度的提高材料的耐磨性，这两种添加剂作为碳质原料都不会改变最终材料中碳的百分含量；本发明通过对粉体进行造粒处理，改善了粉体的流动性，粉体能够更均匀的填充到成型模具中，压制时在模具内部也能够更好的进行流动，提高了产品的稳定性；本发明的石墨制品采用近净成型的方式，生坯的表面积大，烧结时有利于挥发物的排放，产品不易开裂，可以实现快速烧结；同时能够极大的减少加工量，提高材料利用率，降低生产成本，易于实现大批量生产。
最后应说明的是：以上各实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述各实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分或者全部技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。

Claims (10)

1.一种纤维增强石墨复合材料的制备方法，其特征在于，包括如下步骤：
(1)按重量份计，将20～30份石墨、30～60份煅后焦、20～40份改质沥青、1～5份润滑剂、1～5份耐磨剂、0.1～10份的喷雾碳黑和0.1～5重量份数的短切玻璃纤维混捏、磨粉后得到粉料，所述短切玻璃纤维的长度为1-5mm；
(2)将步骤(1)所得粉料与粘结剂、脱模剂添加到快速搅拌制粒机中进行造粒，得到造粒料，所述脱模剂和粉料的重量比为1：100，所述快速搅拌制粒机的电机转速为5000～30000转/分钟，搅拌时间为0.5～2小时，搅拌温度为100～120℃；
(3)将步骤(2)所得造粒料在液压机上近净成型，得到石墨生坯，其中，近净成型的压力为100～300Mpa；
(4)烧结，其中烧成温度为800～1200℃，保温时间为1～5h；
(5)精加工。
2.根据权利要求1所述的纤维增强石墨复合材料的制备方法，其特征在于，所述石墨为天然石墨和/或人造石墨，所述石墨的平均颗粒粒径为10～50μm。
3.根据权利要求1所述的纤维增强石墨复合材料的制备方法，其特征在于，所述煅后焦为煅后石油焦和/或煅后沥青焦，所述煅后焦的平均颗粒粒径为10～50μm。
4.根据权利要求1所述的纤维增强石墨复合材料的制备方法，其特征在于，所述改质沥青的软化点为105～120℃，喹啉不溶物含量为6～10％，甲苯不溶物含量为20～30％。
5.根据权利要求1所述的纤维增强石墨复合材料的制备方法，其特征在于，所述润滑剂为二硫化钨和/或二硫化钼。
6.根据权利要求1所述的纤维增强石墨复合材料的制备方法，其特征在于，所述耐磨剂为碳化硅、二氧化硅、氧化铝、磷酸二氢铝、硅酸镁、硅灰石中的一种或多种。
7.根据权利要求1所述的纤维增强石墨复合材料的制备方法，其特征在于，所述粘结剂为聚丙烯酸氨、聚乙烯醇、聚氯乙烯、甘油乙醇、石蜡乙醚中的一种或多种。
8.根据权利要求1所述的纤维增强石墨复合材料的制备方法，其特征在于，所述脱膜剂为硬脂酸、油酸、N,N'-乙撑双硬脂酰胺、石蜡、硬脂酸锌中的一种或多种。
9.根据权利要求1所述的纤维增强石墨复合材料的制备方法，其特征在于，所述粉料的平均粒径为5～35μm。
10.根据权利要求1所述的纤维增强石墨复合材料的制备方法，其特征在于，所述造粒料的平均粒径为30～80μm。
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