CN106478125A - 一种B4C改性C/C‑SiC刹车材料的制备方法 - Google Patents
一种B4C改性C/C‑SiC刹车材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种B4C改性C/C‑SiC刹车材料的制备方法,采用真空压力浸渍法在初始密度约为0.4~0.6g/cm3三维针刺碳毡中引入B4C粉料,并结合化学气相渗透(CVI)及反应熔体渗透(RMI)制备C/C‑SiC刹车材料的方法。采用B4C改性C/C‑SiC刹车材料,一方面B4C作为自愈合组元对碳纤维和碳基体具有保护作用,可以显著提高材料的抗氧化性;另一方面,B4C具有更高的比热容,能提高材料的整体比热,有效降低刹车温度,提高材料摩擦性能稳定性。
Description
技术领域
本发明属于C/C-SiC复合材料的制备方法,涉及一种B4C改性C/C-SiC刹车材料的制备方法,是一种采用真空压力浸渍将B4C粉料引入三维针刺碳纤维预制体,并通过化学气相沉积结合反应熔体浸渗工艺制备B4C改性C/C-SiC刹车材料的方法。
背景技术
刹车装置是飞机、高铁、汽车实现制动,保障运行安全的核心部件,主要通过摩擦表面的相对运动将动能转化为热能来实现制动的目的。在制动过程中,刹车装置在极短时间内将巨大的动能转化为热能并扩散出来。
文献Krenkel W.Cost Effective Processing of Cmc Composites by MeltInfiltration(Lsi‐Process)[M]//25th Annual Conference on Composites,AdvancedCeramics,Materials,and Structures:A:Ceramic Engineering and ScienceProceedings,Volume 22,Issue 3.John Wiley&Sons,Inc.,2008:443-454.公开了一种通过在多孔碳纤维预制体中运用液硅浸渗方法来控制成本并获得的C/SiC刹车材料,已经成功用于保时捷(Porsche9llTurbo)、宾利、布加迪、兰博基尼跑车和奥迪等高档轿车上。文献Fan S,Zhang L,Cheng L,et al.Effect of braking pressure and braking speed onthe tribological properties of C/SiC aircraft brake materials[J].CompositesScience&Technology,2010,70(6):959-965.公开了一种制备三维针刺C/SiC刹车材料的方法,这种采用化学气相渗透(CVI工艺)结合液硅浸渗(LSI工艺)制备的刹车材料,目前这种飞机刹车装置已在国内实现批量应用。
碳陶刹车材料具有摩擦系数高而且稳定,湿态条件下摩擦系数衰减小,耐磨损,强度高,使用寿命长等优异性能,是极具竞争力的新一代刹车材料。由于刹车材料是在反复热冲击的条件下工作,摩擦界面温度高,在刹车界面会形成过热点造成摩擦界面中热解碳和碳纤维氧化,导致材料磨损严重;更严重的是,由于刹车温度过高,会导致刹车盘连接处严重氧化变形,造成连接失效,发生灾难性事故。因此,在碳陶刹车材料中引入能防氧化并具有自愈合裂纹能力,而且比热容高的填料,能有效提高碳陶刹车材料碳纤维和碳基体的防氧化能力,降低刹车温度具有重要意义。
目前我国高速列车覆盖时速200公里至380公里各个速度等级,在时速380公里紧急刹车时,刹车温度已高达900-1000℃,达到粉末冶金或钢刹车材料的使用极限。而高铁想要再次提速,目前所使用的粉末冶金或钢刹车材料已不能承受紧急情况时的刹车需求。碳陶刹车材料将成为时速高于380公里时的理想刹车材料,B4C改性的碳陶刹车材料将更适用于时速高于380公里的高铁刹车。
发明内容
要解决的技术问题
为了避免现有技术的不足之处,本发明提出一种B4C改性C/C-SiC刹车材料的制备方法,针对刹车能载高的飞机用盘式刹车材料,为了克服刹车温度过高导致摩擦磨损性能不稳定,在刹车材料中引入高比热成分,提高刹车材料的比热容,降低刹车温度;针对盘/片钳式刹车***,在刹车材料中引入自愈合防氧化组元,以提高刹车材料抗氧化磨损的能力,提高刹车材料的使用寿命。
技术方案
一种B4C改性C/C-SiC刹车材料的制备方法,其特征在于步骤如下:
步骤1:将B4C粉加入到质量分数为0.5%~1.5%的羧甲基纤维束钠CMC水溶液中,球墨24~48小时以上制备得到B4C浆料;
步骤2:在真空条件下,将密度为0.4~0.6g/cm3三维针刺碳纤维毡浸入B4C浆料中,然后通入惰性气体加压到0.5~3MPa,保压30~60min,然后取出干燥,得到含有B4C粉料的三维针刺碳纤维预制体;
步骤3:将三维针刺碳纤维预制体通过化学气相渗透CVI沉积热解碳或通过含碳聚合物浸渍裂解法PIP得到C/C复合材料;再进行真空高温热处理;
步骤4:将C/C复合材料在高温真空炉中进行渗硅处理,反应熔体为含Si合金,炉内气压低于50Pa,反应温度为1300~1900℃,保温时间为0.5~4h,随后自然冷却至室温,获得B4C改性C/C-SiC刹车材料。
所述步骤1中加入质量比为5∶1~2(H2O:B4C)的B4C粉料。
所述步骤3制备的含有B4C粉料的C/C复合材料的密度为1.3~1.7g/cm3,工艺参数为:丙烯作为先驱体,在三维针刺C纤维预制体内沉积PyC,沉积温度为930℃,沉积时间为300h。
所述步骤3的真空高温热处理的处理温度为2500℃,保温时间为lh。
所述B4C粉的粒径小于5um。
有益效果
本发明提出的一种B4C改性C/C-SiC刹车材料的制备方法,B4C作为陶瓷相与SiC硬度相当,都是耐高温、耐磨陶瓷,可以改善材料的摩擦磨损性能。摩擦界面的B4C氧化成B2O3可以愈合摩擦界面的缺陷,阻止热解碳和碳纤维的氧化磨损,保护了碳纤维的增韧作用,降低了摩擦界面的脆性剥落。B4C具有更高的比热,加入一定量的B4C,可以有效提高材料的比热容,降低刹车温度,改善摩擦磨损性能。
所以在碳陶刹车材料中引入高比热改性填料B4C,可有效增加刹车材料的比热,从而降低刹车温度,并且B4C能在氧化过程中对碳纤维和碳基体起到保护作用,降低材料氧化磨损,提高刹车材料摩擦磨损性能的稳定性,同时提高碳陶刹车材料服役的可靠性。因此,B4C改性C/C-SiC刹车材料将成为新一代碳陶刹车材料。
本发明采用真空压力浸渍法在初始密度约为0.4~0.6g/cm3三维针刺碳毡中引入B4C粉料,并结合化学气相渗透(CVI)及反应熔体渗透(RMI)制备C/C-SiC刹车材料的方法。采用B4C改性C/C-SiC刹车材料,一方面B4C作为自愈合组元对碳纤维和碳基体具有保护作用,可以显著提高材料的抗氧化性;另一方面,B4C具有更高的比热容,能提高材料的整体比热,有效降低刹车温度,提高材料摩擦性能稳定性。
附图说明
图1是B4C改性C/C-SiC刹车材料的制备工艺流程图
图2是本发明实施例1中C/C-B4C-SiC刹车材料XRD图谱
图3是本发明实施例1中C/C-B4C-SiC刹车材料表面SEM照片
具体实施方式
现结合实施例、附图对本发明作进一步描述:
实施例1:
步骤1,C纤维预制体的制备:
首先将PAN基T-300(6~50K)碳纤维制成短纤维胎网和无纬布,然后将单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加铺层,再利用针刺技术使无纬布和胎网成为一体。根据需要的厚度经过反复叠层、针刺、叠层、针刺……,得到三维针刺碳纤维预制体。预制体密度约为0.55g/cm3,胎网层密度约为0.2g/cm3,无纬布层密度约为0.6g/cm3,碳纤维的体积含量约为40%,层密度约为14层/10mm。
步骤2,B4C浆料的制备:
在蒸馏水中加入0.5wt%的CMC(羧甲基纤维素钠),混合均匀并以氨水和盐酸调节PH值至11~12,然后加入质量比为5:1(H2O:B4C)的B4C粉料,经球磨24h得到混合均匀的B4C浆料。
步骤3,真空压力浆料浸渍:
将步骤1所得到的三维针刺碳纤维预制体放入浸渍罐中,抽真空30min后,注入B4C浆料,通过惰性气体加压至0.9MPa,浸渍约30min后取出,在150℃条件下干燥4h得到含有B4C粉料的三维针刺碳纤维预制体。
步骤4,含有B4C的C/C复合材料的制备:
以丙烯作为先驱体,在三维针刺C纤维预制体内沉积PyC,沉积温度为930℃,沉积时间为300h,制备出密度为1.5g/cm3含有B4C粉料的C/C复合材料。将沉积得到含有B4C的C/C复合材料进行真空高温热处理,处理温度为2500℃,保温时间为lh。
步骤5,反应熔体浸渗:
将步骤4所得的含B4C粉料的C/C复合材料在真空条件下,通过反应熔体浸渗工艺制备B4C改性C/C-SiC刹车材料。反应熔体为Si,炉内气压低于50Pa,反应温度为1580℃,保温时间为1h。
B4C改性C/C-SiC刹车材料XRD结果如图2所示,表明材料由C、SiC、B4C和Si四种物相组成。材料SEM照片如图3所示,表明B4C主要存在于胎网层内部的大孔隙中。改性后C/C-SiC材料与未改性材料700℃氧化10h质量损失对比如表1所示:
表1
表1材料700℃氧化10h后质量损失率
由表可知,B4C粉料引入对C/C-SiC材料自身抗氧化性具有极大提升,对材料起到有效的保护作用。
改性后C/C-SiC材料与未改性材料质量热容J/(g·K)变化如表2所示:
表2
表2材料的质量热容
由表可知,B4C粉料的引入可有效提高材料比热,有利于降低刹车温度。
实施例2:
步骤1,C纤维预制体的制备:
首先将PAN基T-300(6~50K)碳纤维制成短纤维胎网和无纬布,然后将单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加铺层,再利用针刺技术使无纬布和胎网成为一体。根据需要的厚度经过反复叠层、针刺、叠层、针刺……,得到三维针刺碳纤维预制体。预制体密度约为0.55g/cm3,胎网层密度约为0.2g/cm3,无纬布层密度约为0.6g/cm3,碳纤维的体积含量约为40%,层密度约为14层/10mm。
步骤2,B4C浆料的制备:
在蒸馏水中加入1.0wt%的CMC(羧甲基纤维素钠),混合均匀并以氨水和盐酸调节PH值至11~12,然后加入质量比为5∶2(H2O:B4C)的B4C粉料,经球磨48h得到混合均匀的B4C浆料。
步骤3,真空压力浆料浸渍:
将步骤1所得到的三维针刺碳纤维预制体放入浸渍罐中,抽真空30min后,注入B4C浆料,通过惰性气体加压至1.5MPa,浸渍约60min后取出,在150℃条件下干燥4h得到含有B4C粉料的三维针刺碳纤维预制体。
步骤4,含有B4C的C/C复合材料的制备:
以丙烯作为先驱体,在三维针刺C纤维预制体内沉积PyC,沉积温度为930℃,
沉积时间为300h,制备出密度为1.6g/cm3含有B4C粉料的C/C复合材料。将沉积得到含有B4C的C/C复合材料进行真空高温热处理,处理温度为2500℃,保温时间为lh。
步骤5,反应熔体浸渗:
将步骤4所得的含B4C粉料的C/C复合材料在真空条件下,通过反应熔体浸渗工艺制备B4C改性C/C-SiC刹车材料。反应熔体为Fe-Si合金,炉内气压低于50Pa,反应温度为1500℃,保温时间为2h。
Claims (5)
1.一种B4C改性C/C-SiC刹车材料的制备方法,其特征在于步骤如下:
步骤1:将B4C粉加入到质量分数为0.5%~1.5%的羧甲基纤维束钠CMC水溶液中,球墨24~48小时以上制备得到B4C浆料;
步骤2:在真空条件下,将密度为0.4~0.6g/cm3三维针刺碳纤维毡浸入B4C浆料中,然后通入惰性气体加压到0.5~3MPa,保压30~60min,然后取出干燥,得到含有B4C粉料的三维针刺碳纤维预制体;
步骤3:将三维针刺碳纤维预制体通过化学气相渗透CVI沉积热解碳或通过含碳聚合物浸渍裂解法PIP得到C/C复合材料;再进行真空高温热处理;
步骤4:将C/C复合材料在高温真空炉中进行渗硅处理,反应熔体为含Si合金,炉内气压低于50Pa,反应温度为1300~1900℃,保温时间为0.5~4h,随后自然冷却至室温,获得B4C改性C/C-SiC刹车材料。
2.根据权利要求1所述B4C改性C/C-SiC刹车材料的制备方法,其特征在于:所述步骤1中加入质量比为5∶1~2(H2O:B4C)的B4C粉料。
所述含Si合金为Si或Si-Zr合金、Fe-Si合金、Si-Al合金。
3.根据权利要求1或2所述B4C改性C/C-SiC刹车材料的制备方法,其特征在于:所述步骤3制备的含有B4C粉料的C/C复合材料的密度为1.3~1.7g/cm3,工艺参数为:丙烯作为先驱体,在三维针刺C纤维预制体内沉积PyC,沉积温度为930℃,沉积时间为300h。
4.根据权利要求1或2所述B4C改性C/C-SiC刹车材料的制备方法,其特征在于:所述步骤3的真空高温热处理的处理温度为2500℃,保温时间为lh。
5.根据权利要求1或2所述B4C改性C/C-SiC刹车材料的制备方法,其特征在于:所述B4C粉的粒径小于5um。
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