CN111285700A - 一种碳化锆膜碳纤维-陶瓷摩擦材料的制备方法 - Google Patents

一种碳化锆膜碳纤维-陶瓷摩擦材料的制备方法 Download PDF

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CN111285700A
CN111285700A CN202010014717.7A CN202010014717A CN111285700A CN 111285700 A CN111285700 A CN 111285700A CN 202010014717 A CN202010014717 A CN 202010014717A CN 111285700 A CN111285700 A CN 111285700A
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carbon fiber
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唐竹兴
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Shandong University of Technology
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Abstract

一种碳化锆膜碳纤维‑陶瓷摩擦材料的制备方法，其特征在于，将石墨化碳纤维进行渗碳处理后进行沉积碳化锆处理制成碳化锆膜碳纤维，再将其短切后与金属硅粉、陶瓷粉、碳粉和混合溶液混合制成浆料，将该浆料快速注入压滤模具中保压后加热固化，经脱模、干燥后机械加工，再进行渗硅、氮化烧制成摩擦材料毛坯，再经精加工制成碳化锆膜碳纤维‑陶瓷摩擦材料。本发明所制备的摩擦材料具有强度高、韧性高、耐磨性高、使用寿命长等特点。

Description

一种碳化锆膜碳纤维-陶瓷摩擦材料的制备方法
技术领域
本发明涉及一种碳纤维和陶瓷材料复合摩擦材料的制备方法，属于复合材料制备技术领域。
背景技术
2016年山东理工大学针对飞机刹车系统使用的摩擦材料申请了“一种氮化硅-碳化硅-碳纤维摩擦材料的制备方法，ZL201610014314.6”、“ 一种氮化硅-碳化硼-碳纤维摩擦材料的制备方法，ZL201610014313.1”等114项发明专利，它是采用石墨化的碳纤维毯或石墨化的针刺碳纤维毯或石墨化的编织碳纤维布或石墨化的三维编织碳纤维织块作为增强相，为连续碳纤维作为骨架结构增强摩擦材料，该技术在陶瓷粉体填充、渗硅等技术难度较大，成本较高。另外，目前国内外摩擦材料（特别是民用的，如，机床、轿车、大型货车、高铁等）有树脂基、金属基、陶瓷基、碳/碳复合材料等，普遍存在结构强度低、磨损率高、抵抗高温性能差、使用寿命短等问题。
发明内容
本发明的目的在于提供一种能克服上述缺陷、实现低成本制备更高强度、更高摩擦性能的摩擦材料的制备方法。其技术方案为：
将石墨化碳纤维进行渗碳处理后进行沉积碳化锆处理制成碳化锆膜碳纤维，再将碳化锆膜碳纤维短切制成碳化锆膜碳纤维粉，将碳化锆膜碳纤维粉、金属硅粉、陶瓷粉、碳粉均匀混合制成混合粉体，将混合粉体与混合溶液均匀混合制成浆料，将浆料充分搅拌后快速注入压滤模具、快速压滤保压并加热固化，经脱模、干燥后机械加工，再进行渗硅、氮化烧制成摩擦材料毛坯，再经精加工制成碳化锆膜碳纤维-陶瓷摩擦材料，其中，陶瓷粉为碳化硅粉，碳化硼粉，碳化钛粉，碳化锆粉，碳化钒粉，碳化镧粉，硼化锆粉，硼化铪粉，硼化钛粉，氮化硅粉，氮化硼粉，氮化铝粉，或上述两种或两种以上粉体的混合物，混合溶液为酚醛树脂-乙醇溶液，合脂-乙醇溶液，酚醛树脂-水溶液，具体步骤如下：
（1）将石墨化碳纤维在900~1100℃温度下通入天然气和氮气的混合气体，天然气:氮气的摩尔比为1:8~16，流量控制在100~1200 ml/min，渗碳处理1~10小时获得碳膜碳纤维；
（2）将上述碳膜碳纤维在900~1100℃温度下通入四氯化锆、甲烷、氢气和氩气的混合气体，四氯化锆:甲烷:氢气:氩气的摩尔比为1:1~2:3~6:4~6，流量控制在100~1200ml/min，沉积碳化硅处理1~10小时获得沉积碳化锆膜碳纤维；
（3）将碳化锆膜碳纤维短切制成长度为20μm-3mm的碳化锆膜碳纤维粉；
（4）将碳化锆膜碳纤维粉:粒度为0.5-100μm的金属硅粉:粒度为0.5-100μm的陶瓷粉:粒度为0.5-100μm的碳粉以重量百分比为10-70:10-5:20-10:60-15的比例均匀混合制成混合粉体；
（5）将混合粉体:含混合物浓度为5-50%的混合溶液以重量百分比为50:30-100的比例均匀混合制成浆料；
（6）将浆料充分搅拌后快速注入压滤模具、快速压滤、保压并在80-120℃的温度下加热固化，经脱模、干燥后机械加工制成尺寸精确的摩擦材料坯体；
（7）将摩擦材料坯体埋入渗硅料里，在真空气氛下1500~1800℃的温度下渗硅3~5小时制得摩擦材料毛坯，其中，渗硅料为粒度为2-5mm的单晶硅颗粒；
（8）将摩擦材料毛坯在1350~1700℃的温度下氮化处理4~10小时并冷加工制得碳化锆膜碳纤维-陶瓷摩擦材料。
本发明与现有技术相比，其优点为：
1、本发明是采用碳膜和碳化锆膜保护的短石墨化碳纤维作为增强相，所制备的摩擦材料的强度和耐磨性能是普通的摩擦材料的3-5倍；
2、由于本发明在摩擦材料坯料内预先加入了金属硅和碳粉，在高温渗硅过程中金属硅和碳粉反应生成碳化硅把碳纤维和加入的陶瓷颗粒结合起来，提高材料的结合强度，同时金属硅和碳粉反应生成碳化硅的过程又能更好地引导渗硅过程中熔融硅的渗入，使摩擦材料的致密度得到进一步提高；
3、通过浆料的不同搅拌方式、快速注入压滤模具、快速压滤保压并加热固化能够使浆料中的碳化锆膜碳纤维更均匀地分散在摩擦材料坯体中，使得碳化锆膜碳纤维-陶瓷摩擦材料的显微结构更加均匀；
4、本发明通过氮化反应使摩擦材料坯体中的金属硅部分或全部形成氮化硅，另外配方中添加了六方相片状的氮化硼，由于氮化硅、氮化硼具有一定的自润滑作用，可以使摩擦材料在更大范围内调整其摩擦系数。
具体实施方式
实施例1
（1）将石墨化碳纤维在900℃温度下通入天然气和氮气的混合气体，天然气:氮气的摩尔比为1:8，流量控制在100 ml/min，渗碳处理1小时获得碳膜碳纤维；
（2）将上述碳膜碳纤维在900℃温度下通入四氯化锆、甲烷、氢气和氩气的混合气体，四氯化锆:甲烷:氢气:氩气的摩尔比为1:1:3:4，流量控制在100ml/min，沉积碳化硅处理1小时获得沉积碳化锆膜碳纤维；
（3）将碳化锆膜碳纤维短切制成长度为20μm的碳化锆膜碳纤维粉；
（4）将碳化锆膜碳纤维粉:粒度为0.5μm的金属硅粉:粒度为0.5μm的陶瓷粉:粒度为0.5μm的碳粉以重量百分比为10:10:20:60的比例均匀混合制成混合粉体，其中陶瓷粉为碳化硅粉；
（5）将混合粉体:含混合物浓度为5%的酚醛树脂-乙醇混合溶液以重量百分比为50:30的比例均匀混合制成浆料；
（6）将浆料充分搅拌后快速注入压滤模具、快速压滤、保压并在80℃的温度下加热固化，经脱模、干燥后机械加工制成尺寸精确的摩擦材料坯体；
（7）将摩擦材料坯体埋入渗硅料里，在真空气氛下1500℃的温度下渗硅3小时制得摩擦材料毛坯，其中，渗硅料为粒度为2mm的单晶硅颗粒；
（8）将摩擦材料毛坯在1350℃的温度下氮化处理4小时并冷加工制得碳化锆膜碳纤维-陶瓷摩擦材料。
实施例2
（1）将石墨化碳纤维在1000℃温度下通入天然气和氮气的混合气体，天然气:氮气的摩尔比为1:12，流量控制在700 ml/min，渗碳处理5小时获得碳膜碳纤维；
（2）将上述碳膜碳纤维在1000℃温度下通入四氯化锆、甲烷、氢气和氩气的混合气体，四氯化锆:甲烷:氢气:氩气的摩尔比为1:1.5:4.5:5，流量控制在700ml/min，沉积碳化硅处理5小时获得沉积碳化锆膜碳纤维；
（3）将碳化锆膜碳纤维短切制成长度为0.5mm的碳化锆膜碳纤维粉；
（4）将碳化锆膜碳纤维粉:粒度为50μm的金属硅粉:粒度为50μm的陶瓷粉:粒度为50μm的碳粉以重量百分比为4:8:15:35的比例均匀混合制成混合粉体，其中陶瓷粉为碳化硅粉；
（5）将混合粉体:含混合物浓度为30%的酚醛树脂-乙醇混合溶液以重量百分比为50:65的比例均匀混合制成浆料；
（6）将浆料充分搅拌后快速注入压滤模具、快速压滤、保压并在100℃的温度下加热固化，经脱模、干燥后机械加工制成尺寸精确的摩擦材料坯体；
（7）将摩擦材料坯体埋入渗硅料里，在真空气氛下1650℃的温度下渗硅4小时制得摩擦材料毛坯，其中，渗硅料为粒度为3.5mm的单晶硅颗粒；
（8）将摩擦材料毛坯在1500℃的温度下氮化处理7小时并冷加工制得碳化锆膜碳纤维-陶瓷摩擦材料。
实施例3
（1）将石墨化碳纤维在1100℃温度下通入天然气和氮气的混合气体，天然气:氮气的摩尔比为1: 16，流量控制在1200 ml/min，渗碳处理10小时获得碳膜碳纤维；
（2）将上述碳膜碳纤维在1100℃温度下通入四氯化锆、甲烷、氢气和氩气的混合气体，四氯化锆:甲烷:氢气:氩气的摩尔比为1: 2: 6: 6，流量控制在1200ml/min，沉积碳化硅处理10小时获得沉积碳化锆膜碳纤维；
（3）将碳化锆膜碳纤维短切制成长度为1mm的碳化锆膜碳纤维粉；
（4）将碳化锆膜碳纤维粉:粒度为100μm的金属硅粉:粒度为100μm的陶瓷粉:粒度为100μm的碳粉以重量百分比为70: 5: 10: 15的比例均匀混合制成混合粉体，其中陶瓷粉为碳化硅粉；
（5）将混合粉体:含混合物浓度为50%的酚醛树脂-乙醇混合溶液以重量百分比为50:100的比例均匀混合制成浆料；
（6）将浆料充分搅拌后快速注入压滤模具、快速压滤、保压并在120℃的温度下加热固化，经脱模、干燥后机械加工制成尺寸精确的摩擦材料坯体；
（7）将摩擦材料坯体埋入渗硅料里，在真空气氛下1800℃的温度下渗硅5小时制得摩擦材料毛坯，其中，渗硅料为粒度为5mm的单晶硅颗粒；
（8）将摩擦材料毛坯在1700℃的温度下氮化处理10小时并冷加工制得碳化锆膜碳纤维-陶瓷摩擦材料。
实施例4
（1）将石墨化碳纤维在1000℃温度下通入天然气和氮气的混合气体，天然气:氮气的摩尔比为1:10，流量控制在300 ml/min，渗碳处理2小时获得碳膜碳纤维；
（2）将上述碳膜碳纤维在900℃温度下通入四氯化锆、甲烷、氢气和氩气的混合气体，四氯化锆:甲烷:氢气:氩气的摩尔比为1: 2:3:5，流量控制在100ml/min，沉积碳化硅处理1小时获得沉积碳化锆膜碳纤维；
（3）将碳化锆膜碳纤维短切制成长度为1.5mm的碳化锆膜碳纤维粉；
（4）将碳化锆膜碳纤维粉:粒度为0.5μm的金属硅粉:粒度为0.5μm的陶瓷粉:粒度为0.5μm的碳粉以重量百分比为10:10:20:60的比例均匀混合制成混合粉体，其中陶瓷粉为碳化锆粉:硼化铪粉:氮化硼粉以重量比1:1:1的混合物；
（5）将混合粉体:含混合物浓度为5%的酚醛树脂-水混合溶液以重量百分比为50:30的比例均匀混合制成浆料；
（6）将浆料充分搅拌后快速注入压滤模具、快速压滤、保压并在80℃的温度下加热固化，经脱模、干燥后机械加工制成尺寸精确的摩擦材料坯体；
（7）将摩擦材料坯体埋入渗硅料里，在真空气氛下1700℃的温度下渗硅3小时制得摩擦材料毛坯，其中，渗硅料为粒度为2mm的单晶硅颗粒；
（8）将摩擦材料毛坯在1350℃的温度下氮化处理4小时并冷加工制得碳化锆膜碳纤维-陶瓷摩擦材料。
实施例5
（1）将石墨化碳纤维在900℃温度下通入天然气和氮气的混合气体，天然气:氮气的摩尔比为1:13，流量控制在700 ml/min，渗碳处理5小时获得碳膜碳纤维；
（2）将上述碳膜碳纤维在1000℃温度下通入四氯化锆、甲烷、氢气和氩气的混合气体，四氯化锆:甲烷:氢气:氩气的摩尔比为1:1:5:4，流量控制在700ml/min，沉积碳化硅处理5小时获得沉积碳化锆膜碳纤维；
（3）将碳化锆膜碳纤维短切制成长度为2mm的碳化锆膜碳纤维粉；
（4）将碳化锆膜碳纤维粉:粒度为50μm的金属硅粉:粒度为50μm的陶瓷粉:粒度为50μm的碳粉以重量百分比为4:8:15:35的比例均匀混合制成混合粉体，其中陶瓷粉为碳化锆粉:硼化铪粉:氮化硼粉: 碳化硅粉以重量比1:1:1:1的混合物；
（5）将混合粉体:含混合物浓度为30%的合脂-乙醇混合溶液以重量百分比为50:65的比例均匀混合制成浆料；
（6）将浆料充分搅拌后快速注入压滤模具、快速压滤、保压并在100℃的温度下加热固化，经脱模、干燥后机械加工制成尺寸精确的摩擦材料坯体；
（7）将摩擦材料坯体埋入渗硅料里，在真空气氛下1650℃的温度下渗硅4小时制得摩擦材料毛坯，其中，渗硅料为粒度为3.5mm的单晶硅颗粒；
（8）将摩擦材料毛坯在1500℃的温度下氮化处理7小时并冷加工制得碳化锆膜碳纤维-陶瓷摩擦材料。
实施例6
（1）将石墨化碳纤维在1000℃温度下通入天然气和氮气的混合气体，天然气:氮气的摩尔比为1: 14，流量控制在1200 ml/min，渗碳处理10小时获得碳膜碳纤维；
（2）将上述碳膜碳纤维在1100℃温度下通入四氯化锆、甲烷、氢气和氩气的混合气体，四氯化锆:甲烷:氢气:氩气的摩尔比为1:1.5:4:4，流量控制在1200ml/min，沉积碳化硅处理10小时获得沉积碳化锆膜碳纤维；
（3）将碳化锆膜碳纤维短切制成长度为3mm的碳化锆膜碳纤维粉；
（4）将碳化锆膜碳纤维粉:粒度为100μm的金属硅粉:粒度为100μm的陶瓷粉:粒度为100μm的碳粉以重量百分比为70: 5: 10: 15的比例均匀混合制成混合粉体，其中陶瓷粉为硼化钛粉:氮化硅粉:碳化硅粉:碳化钒粉:氮化铝粉以重量比1:1:1:1:1的混合物；
（5）将混合粉体:含混合物浓度为50%的酚醛树脂-乙醇混合溶液以重量百分比为50:100的比例均匀混合制成浆料；
（6）将浆料充分搅拌后快速注入压滤模具、快速压滤、保压并在120℃的温度下加热固化，经脱模、干燥后机械加工制成尺寸精确的摩擦材料坯体；
（7）将摩擦材料坯体埋入渗硅料里，在真空气氛下1800℃的温度下渗硅5小时制得摩擦材料毛坯，其中，渗硅料为粒度为5mm的单晶硅颗粒；
（8）将摩擦材料毛坯在1700℃的温度下氮化处理10小时并冷加工制得碳化锆膜碳纤维-陶瓷摩擦材料。

Claims (1)

1.一种碳化锆膜碳纤维-陶瓷摩擦材料的制备方法，其特征在于，将石墨化碳纤维进行渗碳处理后进行沉积碳化锆处理制成碳化锆膜碳纤维，再将碳化锆膜碳纤维短切制成碳化锆膜碳纤维粉，将碳化锆膜碳纤维粉、金属硅粉、陶瓷粉、碳粉均匀混合制成混合粉体，将混合粉体与混合溶液均匀混合制成浆料，将浆料充分搅拌后快速注入压滤模具、快速压滤保压并加热固化，经脱模、干燥后机械加工，再进行渗硅、氮化烧制成摩擦材料毛坯，再经精加工制成碳化锆膜碳纤维-陶瓷摩擦材料，其中，陶瓷粉为碳化硅粉，碳化硼粉，碳化钛粉，碳化锆粉，碳化钒粉，碳化镧粉，硼化锆粉，硼化铪粉，硼化钛粉，氮化硅粉，氮化硼粉，氮化铝粉，或上述两种或两种以上粉体的混合物，混合溶液为酚醛树脂-乙醇溶液，合脂-乙醇溶液，酚醛树脂-水溶液，具体步骤如下：
（1）将石墨化碳纤维在900~1100℃温度下通入天然气和氮气的混合气体，天然气:氮气的摩尔比为1:8~16，流量控制在100~1200 ml/min，渗碳处理1~10小时获得碳膜碳纤维；
（2）将上述碳膜碳纤维在900~1100℃温度下通入四氯化锆、甲烷、氢气和氩气的混合气体，四氯化锆:甲烷:氢气:氩气的摩尔比为1:1~2:3~6:4~6，流量控制在100~1200ml/min，沉积碳化硅处理1~10小时获得沉积碳化锆膜碳纤维；
（3）将碳化锆膜碳纤维短切制成长度为20μm-3mm的碳化锆膜碳纤维粉；
（4）将碳化锆膜碳纤维粉:粒度为0.5-100μm的金属硅粉:粒度为0.5-100μm的陶瓷粉:粒度为0.5-100μm的碳粉以重量百分比为10-70:10-5:20-10:60-15的比例均匀混合制成混合粉体；
（5）将混合粉体:含混合物浓度为5-50%的混合溶液以重量百分比为50:30-100的比例均匀混合制成浆料；
（6）将浆料充分搅拌后快速注入压滤模具、快速压滤、保压并在80-120℃的温度下加热固化，经脱模、干燥后机械加工制成尺寸精确的摩擦材料坯体；
（7）将摩擦材料坯体埋入渗硅料里，在真空气氛下1500~1800℃的温度下渗硅3~5小时制得摩擦材料毛坯，其中，渗硅料为粒度为2-5mm的单晶硅颗粒；
（8）将摩擦材料毛坯在1350~1700℃的温度下氮化处理4~10小时并冷加工制得碳化锆膜碳纤维-陶瓷摩擦材料。
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