CN108191442B - 一种低磨损型陶瓷基复合刹车材料的制备方法 - Google Patents
一种低磨损型陶瓷基复合刹车材料的制备方法 Download PDFInfo
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Abstract
本发明涉及汽车制动材料制备技术领域，具体涉及一种低磨损型陶瓷基复合刹车材料的制备方法。本发明以具有丰富孔隙结构的天然有机海绵作为原料，再从毛竹中抽取毛竹纤维束，将海绵和纤维束间隔叠放，之后通过倒钩针刺穿刺处理，使得毛竹纤维束呈垂直角度分布在海绵块间，得到复合体，将复合体炭化处理后再用甲基三氯硅烷蒸气熏蒸处理，在热力作用下发生原位沉积产生碳化硅晶体，之后在用正硅酸乙酯浸泡增密，高温烧结后得到碳化硅陶瓷刹车材料，本发明制得的刹车材料抗磨损性能好，摩擦系数高，不容易在刹车过程中超过额定刹车功率，具有广阔的应用前景。
Description
技术领域
本发明涉及汽车制动材料制备技术领域，具体涉及一种低磨损型陶瓷基复合刹车材料的制备方法。
背景技术
随着科技的进步和汽车工业的发展，汽车制造开始向轻量化、高寿命的方向发展，同时对汽车制动系统以及汽车的速度提出了越来越高的要求。摩擦材料作为汽车制动器摩擦传动制动装置的关键材料，其性能的好坏直接关系到汽车的安全性、稳定性以及驾驶人员的安全、财产等重大问题。理想的摩擦材料应具有较好的稳定性、较高的摩擦系数、较小的磨损率、刹车噪音小、使用寿命长等优点。
为了衡量材料的刹车性能水平，通常采用刹车功率（单位面积承受的能载）进行定量表征。单位面积的刹车功率是指在刹车过程中，在摩擦力作用下，单位时间内单位接触面积上所产生的摩擦热随着刹车速度和刹车压力的增加，刹车功率不断提高，摩擦表面的温度也越高。对于确定的材料体系，摩擦功率具有一个额定的临界值。在刹车能量低于临界值时，材料的摩擦系数能维持在比较稳定的状态；而当能量超过临界值时，摩擦面会出现局部过热现象并产生过热点，从而导致摩擦性能衰减。提高材料体系的导热系数和比热是提高材料的摩擦功率临界值的有效途径。
而目前常见的碳/碳复合刹车材料由于摩擦系数低，容易在刹车过程中超过额定刹车功率，使得刹车性能衰减，并且碳/碳复合刹车材料存在磨损率高的缺陷，因此，提供一种摩擦系数高，磨损率低的新型陶瓷基复合刹车材料对汽车制动材料制备技术领域具有积极的意义。
发明内容
本发明主要解决的技术问题，针对目前常见的碳/碳复合刹车材料由于摩擦系数低，容易在刹车过程中超过额定刹车功率，使得刹车性能衰减，并且碳/碳复合刹车材料存在磨损率高的缺陷，提供了一种低磨损型陶瓷基复合刹车材料的制备方法。
为了解决上述技术问题，本发明所采用的技术方案是：
一种低磨损型陶瓷基复合刹车材料的制备方法，其特征在于具体制备步骤为：
（1）称取象耳海绵裁剪成海绵块，依次用无水乙醇和去离子水反复冲洗，得到洗净后的海绵块，再称取毛竹，用篾刀将毛竹劈成毛竹青篾，将其浸入氢氧化钠溶液中加热煮沸处理，自然风干，得到预处理青篾；
（2）将上述预处理青篾用石磙反复碾压，人工抽取竹纤维束，将上述洗净后的海绵块平铺，再将竹纤维束以无序状铺置在海绵块上，控制竹纤维束铺置厚度，铺置结束后继续在竹纤维束层上叠放一层相同的海绵块，按一层海绵块一层竹纤维束层的顺序循环叠加，直至总厚度达到5～6cm，得到复合体；
（3）用倒钩刺针与复合体海绵块层呈直角方向刺穿复合体，并回拉倒钩刺针使得复合体中的无序竹纤维束垂直刺入相邻的海绵块层中，进行针刺处理，针刺处理结束后得到刹车材料预制体；
（4）将上述刹车材料预制体放入炭化炉中，在氮气保护状态下加热升温，保温炭化，得到炭化刹车材料预制体，将炭化刹车材料预制体放入反应器中，将甲基三氯硅烷加热升温直至沸腾，产生甲基三氯硅烷蒸气，以氢气作为载气将甲基三氯硅烷蒸气通入反应器中，对炭化刹车材料预制体熏蒸处理；
（5）待上述熏蒸处理结束后，取出熏蒸后的炭化刹车材料预制体放入电阻炉中，在氩气氛围下加热升温，保温处理，保温处理结束后，得到刹车材料粗品；
（6）将石墨粉和正硅酸乙酯混合后得到浸渍液，将刹车材料粗品浸入浸渍液中，摇床振荡浸渍处理，再将浸渍后的刹车材料粗品放入马弗炉中，煅烧后出料，即得低磨损型陶瓷基复合刹车材料。
步骤（1）中所述的海绵块的尺寸为20cm×10cm，毛竹青篾的长度为20～30cm，加热煮沸处理的时间为1～3h。
步骤（2）中所述的竹纤维束铺置厚度为4～5mm。
步骤（3）中所述的针刺处理的针刺密度为100～150针/cm2。
步骤（4）中所述的加热升温的温度为600～700℃，保温炭化的时间为3～5h，将甲基三氯硅烷加热升温的温度为75～85℃，载气氢气的流速为10～15mL/min，熏蒸处理时间为5～7h。
步骤（5）中所述的加热升温的温度为600～700℃，保温处理的时间为1～2h。
步骤（6）中所述的石墨粉和正硅酸乙酯的质量比为1:10，摇床振荡浸渍处理时间为10～12h，煅烧的温度为1000～1100℃，煅烧的时间为20～24h。
本发明的有益效果是：
（1）本发明以具有丰富孔隙结构的天然有机海绵作为原料，再从毛竹中抽取毛竹纤维束，将海绵和纤维束间隔叠放，之后通过倒钩针刺穿刺处理，使得毛竹纤维束呈垂直角度分布在海绵块间，得到复合体，将复合体炭化处理后再用甲基三氯硅烷蒸气熏蒸处理，在热力作用下发生原位沉积产生碳化硅晶体，之后在用正硅酸乙酯浸泡增密，高温烧结后得到碳化硅陶瓷刹车材料，本发明制得的刹车材料中由海绵块层制成的碳化硅陶瓷结构层面和刹车材料的摩擦面方向平行，有利于提高材料的抗磨损性能，刺入到海绵块之间的竹纤维束制成的碳化硅陶瓷结构不仅能够提高刹车材料层间的剪切强度，而且能够提高垂直于刹车材料摩擦面层方向的导热系数，避免在刹车过程中超过额定刹车功率，使得刹车性能衰减，从而提高刹车材料的摩擦性能，使得刹车材料的摩擦系数稳定性提高，摩擦系数也得以提高；
（2）本发明由天然有机材料制成的刹车材料中含有热解炭，而热解炭的硬度低，当其参与刹车过程后，主要通过与空气中的水分形成摩擦膜，以起到很好的润滑作用，从而能减小或完全消除粘结和卡滞，促使刹车过程平稳，并且本发明制得的刹车材料中还存在少量残留硅，其硬度仅次于刹车材料本身的碳化硅，硅不但能提高摩擦系数，同时在高速高能载刹车过程中易氧化生成二氧化硅，以摩擦膜的形式存在于摩擦表面，提高摩擦稳定性，减少刹车材料的磨损量，具有广阔的应用前景。
具体实施方式
称取象耳海绵裁剪成尺寸为20cm×10cm的海绵块，依次用无水乙醇和去离子水反复冲洗3～5遍，得到洗净后的海绵块，再称取毛竹，用篾刀将毛竹劈成长度为20～30cm的毛竹青篾，将其浸入浓度为1mol/L的氢氧化钠溶液中加热煮沸处理1～3h后，自然风干，得到预处理青篾；将预处理青篾用石磙反复碾压20～30min，人工抽取竹纤维束，将上述洗净后的海绵块平铺，再将竹纤维束以无序状铺置在海绵块上，控制竹纤维束铺置厚度为4～5mm，铺置结束后继续在竹纤维束层上叠放一层相同的海绵块，按一层海绵块一层竹纤维束层的顺序循环叠加，直至总厚度达到5～6cm，得到复合体；用倒钩刺针与复合体海绵块层呈直角方向刺穿复合体，并回拉倒钩刺针使得复合体中的无序竹纤维束垂直刺入相邻的海绵块层中，按100～150针/cm2的针刺密度进行针刺处理，针刺处理结束后得到刹车材料预制体；将刹车材料预制体放入炭化炉中，在氮气保护状态下加热升温至600～700℃，保温炭化3～5h，得到炭化刹车材料预制体，将炭化刹车材料预制体放入反应器中，将甲基三氯硅烷加热升温到75～85℃直至沸腾，产生甲基三氯硅烷蒸气，以流速为10～15mL/min的氢气作为载气将甲基三氯硅烷蒸气通入反应器中，对炭化刹车材料预制体熏蒸处理5～7h；待熏蒸处理结束后，取出熏蒸后的炭化刹车材料预制体放入电阻炉中，在氩气氛围下加热升温至600～700℃，保温处理1～2h，保温处理结束后，得到刹车材料粗品；将石墨粉和正硅酸乙酯按质量比为1:10混合后得到浸渍液，将刹车材料粗品浸入浸渍液中，摇床振荡浸渍处理10～12h，再将浸渍后的刹车材料粗品放入马弗炉中，在1000～1100℃下煅烧20～24h后出料，即得低磨损型陶瓷基复合刹车材料。
实例1
称取象耳海绵裁剪成尺寸为20cm×10cm的海绵块，依次用无水乙醇和去离子水反复冲洗3遍，得到洗净后的海绵块，再称取毛竹，用篾刀将毛竹劈成长度为20cm的毛竹青篾，将其浸入浓度为1mol/L的氢氧化钠溶液中加热煮沸处理1h后，自然风干，得到预处理青篾；将预处理青篾用石磙反复碾压20min，人工抽取竹纤维束，将上述洗净后的海绵块平铺，再将竹纤维束以无序状铺置在海绵块上，控制竹纤维束铺置厚度为4mm，铺置结束后继续在竹纤维束层上叠放一层相同的海绵块，按一层海绵块一层竹纤维束层的顺序循环叠加，直至总厚度达到5cm，得到复合体；用倒钩刺针与复合体海绵块层呈直角方向刺穿复合体，并回拉倒钩刺针使得复合体中的无序竹纤维束垂直刺入相邻的海绵块层中，按100针/cm2的针刺密度进行针刺处理，针刺处理结束后得到刹车材料预制体；将刹车材料预制体放入炭化炉中，在氮气保护状态下加热升温至600℃，保温炭化3h，得到炭化刹车材料预制体，将炭化刹车材料预制体放入反应器中，将甲基三氯硅烷加热升温到75℃直至沸腾，产生甲基三氯硅烷蒸气，以流速为10mL/min的氢气作为载气将甲基三氯硅烷蒸气通入反应器中，对炭化刹车材料预制体熏蒸处理5h；待熏蒸处理结束后，取出熏蒸后的炭化刹车材料预制体放入电阻炉中，在氩气氛围下加热升温至600℃，保温处理1h，保温处理结束后，得到刹车材料粗品；将石墨粉和正硅酸乙酯按质量比为1:10混合后得到浸渍液，将刹车材料粗品浸入浸渍液中，摇床振荡浸渍处理10h，再将浸渍后的刹车材料粗品放入马弗炉中，在1000℃下煅烧20h后出料，即得低磨损型陶瓷基复合刹车材料。
实例2
称取象耳海绵裁剪成尺寸为20cm×10cm的海绵块，依次用无水乙醇和去离子水反复冲洗4遍，得到洗净后的海绵块，再称取毛竹，用篾刀将毛竹劈成长度为25cm的毛竹青篾，将其浸入浓度为1mol/L的氢氧化钠溶液中加热煮沸处理2h后，自然风干，得到预处理青篾；将预处理青篾用石磙反复碾压25min，人工抽取竹纤维束，将上述洗净后的海绵块平铺，再将竹纤维束以无序状铺置在海绵块上，控制竹纤维束铺置厚度为4mm，铺置结束后继续在竹纤维束层上叠放一层相同的海绵块，按一层海绵块一层竹纤维束层的顺序循环叠加，直至总厚度达到6cm，得到复合体；用倒钩刺针与复合体海绵块层呈直角方向刺穿复合体，并回拉倒钩刺针使得复合体中的无序竹纤维束垂直刺入相邻的海绵块层中，按130针/cm2的针刺密度进行针刺处理，针刺处理结束后得到刹车材料预制体；将刹车材料预制体放入炭化炉中，在氮气保护状态下加热升温至650℃，保温炭化4h，得到炭化刹车材料预制体，将炭化刹车材料预制体放入反应器中，将甲基三氯硅烷加热升温到80℃直至沸腾，产生甲基三氯硅烷蒸气，以流速为13mL/min的氢气作为载气将甲基三氯硅烷蒸气通入反应器中，对炭化刹车材料预制体熏蒸处理6h；待熏蒸处理结束后，取出熏蒸后的炭化刹车材料预制体放入电阻炉中，在氩气氛围下加热升温至650℃，保温处理1h，保温处理结束后，得到刹车材料粗品；将石墨粉和正硅酸乙酯按质量比为1:10混合后得到浸渍液，将刹车材料粗品浸入浸渍液中，摇床振荡浸渍处理11h，再将浸渍后的刹车材料粗品放入马弗炉中，在1050℃下煅烧22h后出料，即得低磨损型陶瓷基复合刹车材料。
实例3
称取象耳海绵裁剪成尺寸为20cm×10cm的海绵块，依次用无水乙醇和去离子水反复冲洗5遍，得到洗净后的海绵块，再称取毛竹，用篾刀将毛竹劈成长度为30cm的毛竹青篾，将其浸入浓度为1mol/L的氢氧化钠溶液中加热煮沸处理3h后，自然风干，得到预处理青篾；将预处理青篾用石磙反复碾压30min，人工抽取竹纤维束，将上述洗净后的海绵块平铺，再将竹纤维束以无序状铺置在海绵块上，控制竹纤维束铺置厚度为5mm，铺置结束后继续在竹纤维束层上叠放一层相同的海绵块，按一层海绵块一层竹纤维束层的顺序循环叠加，直至总厚度达到6cm，得到复合体；用倒钩刺针与复合体海绵块层呈直角方向刺穿复合体，并回拉倒钩刺针使得复合体中的无序竹纤维束垂直刺入相邻的海绵块层中，按150针/cm2的针刺密度进行针刺处理，针刺处理结束后得到刹车材料预制体；将刹车材料预制体放入炭化炉中，在氮气保护状态下加热升温至700℃，保温炭化5h，得到炭化刹车材料预制体，将炭化刹车材料预制体放入反应器中，将甲基三氯硅烷加热升温到85℃直至沸腾，产生甲基三氯硅烷蒸气，以流速为15mL/min的氢气作为载气将甲基三氯硅烷蒸气通入反应器中，对炭化刹车材料预制体熏蒸处理7h；待熏蒸处理结束后，取出熏蒸后的炭化刹车材料预制体放入电阻炉中，在氩气氛围下加热升温至700℃，保温处理2h，保温处理结束后，得到刹车材料粗品；将石墨粉和正硅酸乙酯按质量比为1:10混合后得到浸渍液，将刹车材料粗品浸入浸渍液中，摇床振荡浸渍处理12h，再将浸渍后的刹车材料粗品放入马弗炉中，在1100℃下煅烧24h后出料，即得低磨损型陶瓷基复合刹车材料。
对照例
以西安市某公司生产的C/C复合刹车材料作为对照例；
对本发明制得的刹车材料和对照例中的刹车材料进行性能检测，测试结果如表1所示；
表1
由上表中检测数据可以看出，本发明制得的低磨损型陶瓷基复合刹车材料摩擦系数高，磨损率低，刹车性能稳定，具有广阔的应用前景。
Claims (6)
1.一种低磨损型陶瓷基复合刹车材料的制备方法，其特征在于具体制备步骤为：
（1）称取象耳海绵裁剪成海绵块，依次用无水乙醇和去离子水反复冲洗，得到洗净后的海绵块，再称取毛竹，用篾刀将毛竹劈成毛竹青篾，将其浸入氢氧化钠溶液中加热煮沸处理，自然风干，得到预处理青篾；
（2）将上述预处理青篾用石磙反复碾压，人工抽取竹纤维束，将上述洗净后的海绵块平铺，再将竹纤维束以无序状铺置在海绵块上，控制竹纤维束铺置厚度，铺置结束后继续在竹纤维束层上叠放一层相同的海绵块，按一层海绵块一层竹纤维束层的顺序循环叠加，直至总厚度达到5～6cm，得到复合体；
（3）用倒钩刺针与复合体海绵块层呈直角方向刺穿复合体，并回拉倒钩刺针使得复合体中的无序竹纤维束垂直刺入相邻的海绵块层中，进行针刺处理，针刺处理结束后得到刹车材料预制体；
（4）将上述刹车材料预制体放入炭化炉中，在氮气保护状态下加热升温，保温炭化，得到炭化刹车材料预制体，将炭化刹车材料预制体放入反应器中，将甲基三氯硅烷加热升温到75～85℃直至沸腾，产生甲基三氯硅烷蒸气，以流速为10～15mL/min的氢气作为载气将甲基三氯硅烷蒸气通入反应器中，对炭化刹车材料预制体熏蒸处理5～7h；
（5）待上述熏蒸处理结束后，取出熏蒸后的炭化刹车材料预制体放入电阻炉中，在氩气氛围下加热升温，保温处理，保温处理结束后，得到刹车材料粗品；
（6）将石墨粉和正硅酸乙酯按质量比为1:10混合后得到浸渍液，将刹车材料粗品浸入浸渍液中，摇床振荡浸渍处理，再将浸渍后的刹车材料粗品放入马弗炉中，煅烧后出料，即得低磨损型陶瓷基复合刹车材料。
2.根据权利要求1所述的一种低磨损型陶瓷基复合刹车材料的制备方法，其特征在于：步骤（1）中所述的海绵块的尺寸为20cm×10cm，毛竹青篾的长度为20～30cm，加热煮沸处理的时间为1～3h。
3.根据权利要求1所述的一种低磨损型陶瓷基复合刹车材料的制备方法，其特征在于：步骤（2）中所述的竹纤维束铺置厚度为4～5mm。
4.根据权利要求1所述的一种低磨损型陶瓷基复合刹车材料的制备方法，其特征在于：步骤（3）中所述的针刺处理的针刺密度为100～150针/cm2。
5.根据权利要求1所述的一种低磨损型陶瓷基复合刹车材料的制备方法，其特征在于：步骤（5）中所述的加热升温的温度为600～700℃，保温处理的时间为1～2h。
6.根据权利要求1所述的一种低磨损型陶瓷基复合刹车材料的制备方法，其特征在于：步骤（6）中所述的摇床振荡浸渍处理时间为10～12h，煅烧的温度为1000～1100℃，煅烧的时间为20～24h。
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