CN113816756A - 一种高结合强度涂层碳/陶刹车盘的制备方法 - Google Patents
一种高结合强度涂层碳/陶刹车盘的制备方法 Download PDFInfo
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Abstract
本发明具体涉及一种高结合强度涂层碳/陶刹车盘的制备方法。包括以下步骤：步骤一，碳纤维预制体的制备；步骤二，碳/碳复合材料的制备；步骤三，涂层浆料配置；步骤四，涂层涂覆；步骤五，反应熔体浸渗处理。与传统碳陶刹车材料相比，新设计的纤维预制体规避了由于表面纤维方向性明显所造成的热膨胀系数差异，涂层与基体材料的热失配现象减弱，提高了涂层与基体材料的界面结合强度，表面涂层处理也提高了摩擦面材料的抗氧化能力，同时摩擦面物相均匀性的提高也增强了制动的平稳性和材料的抗磨损能力。
Description
技术领域
本发明涉及刹车盘的制备工艺，具体涉及一种高结合强度涂层碳/陶刹车盘的制备方法。
背景技术
碳/陶复合材料强度高、重量轻、耐磨损以及摩擦性能优异等一系列优点，目前已广泛的应用于汽车、飞机等摩擦制动领域，同时在高速列车、重型装甲和工程制动等领域也具有广泛的应用前景。
在汽车刹车应用领域，碳/陶刹车盘表面的抗磨损性能、抗氧化性能和摩擦性能的稳定性是制动过程中应关注的重点，同时对刹车盘表面的物相结构也提出了更高的要求。由于材料自身工艺特性，碳/陶刹车盘表面不均匀的分布着陶瓷区域和碳纤维聚集区域，而表面物相的均匀性将有益于提供更好的摩擦磨损性能。
通过传统的CVD SiC工艺可以在碳/陶复合材料表面制备一层非常均匀的 SiC涂层，该涂层具有与基体材料结合强度高、致密性好、抗氧化性强以及摩擦磨损性能优异等特点，但是通过CVD技术制备涂层具有制备周期长、生产成本高等缺点。
针对碳/陶刹车材料，Krenkel等研发了一种具有优异摩擦性能的SiCralee涂层，主要是通过在短切纤维结合树脂模压成型多孔碳/碳预制体的过程中，在碳/ 碳预制体表面添加过量的Si粉和C粉一体成型，随后碳化裂解并结合液相渗硅制备表面含SiC和Si涂层的刹车材料。但是该方法难以应用于CVI结合LSI方法制备的碳/陶复合材料。
国内目前直接采用浆料涂刷法结合渗硅工艺制备带Si-SiC涂层的碳/陶刹车材料的方法，存在涂层与基体材料界面结合强度不高，热失配现象严重等问题。
发明内容
为了解决现有技术的不足，本发明提出一种高结合强度涂层碳/陶刹车盘的制备方法。
本发明的一种具有高结合强度涂层碳/陶刹车盘的制备方法，主要步骤如下：
步骤一，碳纤维预制体的制备：
首先将PAN基T700(12K)碳纤维制成短纤维胎网和无纬布，其中无纬布层密度分为3种，分别是0.6g/cm3、0.4g/cm3和0.2g/cm3，将单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加铺层，在用针刺技术使无纬布和胎网成为一体。根据需要厚度，分别计算0.6g/cm3、0.4g/cm3和0.2g/cm3用量，经过反复叠层、针刺、叠层、针刺......，得到三维针刺碳纤维预制体，纤维预制体从内到外所用无纬布层密度逐渐下降，预制体最外层两面为2-5mm的胎网层。预制体密度为0.35g/cm3，碳纤维体积含量约为30％，层密度约为14层/10mm。
步骤二，碳/碳复合材料的制备：
以天然气作为先驱体，在碳纤维预制体内部沉积PyC，沉积温度为 800-1200℃，沉积时间为200-600h，得到密度为1.0-1.6g/cm3的多孔碳/碳复合材料。
步骤三，涂层浆料配置：
将液态酚醛树脂、呋喃树脂或糠酮树脂与粒径为1-10μm C粉进行混合，质量比为1～3:1，以TMAH作为分散剂，质量占比0.2-0.8wt％，通过滚筒球磨机混合24-48h，得到均匀分散的涂层浆料。
步骤四，涂层涂覆：
在多孔碳/碳复合材料的表面涂覆制备得到的涂层浆料，并进行烘干处理，反复进行2-4次，在碳/碳复合材料表面制得厚度为1-3mm的碳涂层。
步骤五，反应熔体浸渗处理：
将上述带涂层的碳/碳复合材料进行精加工成刹车盘，并在1300-1800℃的温度下进行反应熔体浸渗(Si、Cu-Si、Fe-Si等)处理，得到密度为1.8-2.8g/cm3的碳/陶复合材料。
与现有技术相比，本发明的有益效果为：
本发明通过对碳纤维预制体的结构进行设计，结合化学气相沉积、以及特定的浆料配置涂覆技术，最终通过反应熔体浸渗进行陶瓷化制备碳/陶刹车材料，与传统碳陶刹车材料相比，新设计的纤维预制体规避了由于表面纤维方向性明显所造成的热膨胀系数差异，涂层与基体材料的热失配现象减弱，提高了涂层与基体材料的界面结合强度，表面涂层处理也提高了摩擦面材料的抗氧化能力，同时摩擦面物相均匀性的提高也增强了制动的平稳性和材料的抗磨损能力。
具体实施方式
下面对本发明的具体实施方式作进一步说明。在此需要说明的是，对于这些实施方式的说明用于帮助理解本发明，但并不构成对本发明的限定。此外，下面所描述的本发明各个实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互组合。
实施例1
本实施例是一种高结合强度涂层碳/陶刹车盘的制备方法，具体过程是：
步骤一，碳纤维预制体的制备：
首先将PAN基T700(12K)碳纤维制成短纤维胎网和无纬布，其中无纬布层密度分为3种，分别是0.6g/cm3、0.4g/cm3和0.2g/cm3，将单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加铺层，在用针刺技术使无纬布和胎网成为一体。根据需要厚度39mm，分别计算0.6g/cm3、0.4g/cm3和0.2g/cm3用量，经过反复叠层、针刺、叠层、针刺，得到三维针刺碳纤维预制体，纤维预制体从内到外所用无纬布层密度逐渐下降，预制体最外层两面为5mm的胎网层。预制体密度为0.35g/cm3，碳纤维体积含量约为30％，层密度约为14层/10mm。将上述所制备的碳纤维预制体裁剪成尺寸为388×170×39mm的圆环。
步骤二，碳/碳复合材料的制备：
以天然气作为先驱体，在上述尺寸为388×170×39mm碳纤维预制体圆环内部沉积PyC，沉积温度为800℃，沉积时间为200h，得到密度为1.0g/cm3的多孔碳/碳复合材料。
步骤三，涂层浆料配置：
将液态酚醛树脂与粒径为1μmC粉进行混合，质量比为1:1，以TMAH作为分散剂，质量占比0.2wt％，通过滚筒球磨机混合48h，得到均匀分散的涂层浆料。
步骤四，涂层涂覆：
在沉积好的多孔碳/碳复合材料进行表面加工，通过超声波清洗机清洗后进行烘干，然后在材料表面涂覆制备得到的涂层浆料，并进行烘干处理，反复进行2次，在碳/碳复合材料表面制得厚度为1mm的碳涂层。
步骤五，反应熔体浸渗处理：
将上述带涂层的碳/碳复合材料进行精加工成刹车盘，并在1550℃的温度下进行渗硅处理，得到密度为2.2g/cm3的碳/陶刹车盘。
实施例2：
本实施例是一种高结合强度涂层碳/陶刹车盘的制备方法，具体过程是：
步骤一，碳纤维预制体的制备：
首先将PAN基T700(12K)碳纤维制成短纤维胎网和无纬布，其中无纬布层密度分为3种，分别是0.6g/cm3、0.4g/cm3和0.2g/cm3，将单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加铺层，在用针刺技术使无纬布和胎网成为一体。根据需要厚度39mm，分别计算0.6g/cm3、0.4g/cm3和0.2g/cm3用量，经过反复叠层、针刺、叠层、针刺......，得到三维针刺碳纤维预制体，纤维预制体从内到外所用无纬布层密度逐渐下降，预制体最外层两面为5mm的胎网层。预制体密度为0.35g/cm3，碳纤维体积含量约为30％，层密度约为14层/10mm。将上述所制备的碳纤维预制体裁剪成尺寸为388×170×39mm的圆环。
步骤三，碳/碳复合材料的制备：
以天然气作为先驱体，在上述尺寸为388×170×39mm碳纤维预制体圆环内部沉积PyC，沉积温度为1000℃，沉积时间为400h，得到密度为1.2g/cm3的多孔碳/碳复合材料。
步骤三，涂层浆料配置：
将液态呋喃树脂与粒径为5μmC粉进行混合，质量比为3:1，以TMAH作为分散剂，质量占比0.5wt％，通过滚筒球磨机混合36h，得到均匀分散的涂层浆料。
步骤四，涂层涂覆：
在沉积好的多孔碳/碳复合材料进行表面加工，通过超声波清洗机清洗后进行烘干，然后在材料表面涂覆制备得到的涂层浆料，并进行烘干处理，反复进行3次，在碳/碳复合材料表面制得厚度为2mm的碳涂层。
步骤五，反应熔体浸渗处理：
将上述带涂层的碳/碳复合材料进行精加工成刹车盘，并在1600℃的温度下进行渗Fe-Si合金处理，得到密度为2.8g/cm3的碳/陶刹车盘。
实施例3：
本实施例是一种高结合强度涂层碳/陶刹车盘的制备方法，具体过程是：
步骤一，碳纤维预制体的制备：
首先将PAN基T700(12K)碳纤维制成短纤维胎网和无纬布，其中无纬布层密度分为3种，分别是0.6g/cm3、0.4g/cm3和0.2g/cm3，将单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加铺层，在用针刺技术使无纬布和胎网成为一体。根据需要厚度39mm，分别计算0.6g/cm3、0.4g/cm3和0.2g/cm3用量，经过反复叠层、针刺、叠层、针刺......，得到三维针刺碳纤维预制体，纤维预制体从内到外所用无纬布层密度逐渐下降，预制体最外层两面为5mm的胎网层。预制体密度为0.35g/cm3，碳纤维体积含量约为30％，层密度约为14层/10mm。将上述所制备的碳纤维预制体裁剪成尺寸为388×170×39mm的圆环。
步骤二，碳/碳复合材料的制备：
以天然气作为先驱体，在上述尺寸为388×170×39mm碳纤维预制体圆环内部沉积PyC，沉积温度为1200℃，沉积时间为600h，得到密度为1.6g/cm3的多孔碳/碳复合材料。
步骤三，涂层浆料配置：
将液态糠酮树脂与粒径为10μm C粉进行混合，质量比为3:1，以TMAH作为分散剂，质量占比0.8wt％，通过滚筒球磨机混合24h，得到均匀分散的涂层浆料。
步骤四，涂层涂覆：
在沉积好的多孔碳/碳复合材料进行表面加工，通过超声波清洗机清洗后进行烘干，然后在材料表面涂覆制备得到的涂层浆料，并进行烘干处理，反复进行4次，在碳/碳复合材料表面制得厚度为3mm的碳涂层。
步骤五，反应熔体浸渗处理：
将上述带涂层的碳/碳复合材料进行精加工成刹车盘，并在1800℃的温度下进行渗Si处理，得到密度为1.8g/cm3的碳/陶刹车盘。
在700℃静态空气条件下，对实施例1-3与传统碳/陶材料进行氧化试验，性能对比如表1所示：
表1表层材料700℃静态空气氧化2h性能对比
采用SAE J2522台架测试标准，对实施例1-3制得的碳陶盘和传统碳陶盘摩擦磨损性能进行对比，如表2所示：
表2摩擦磨损性能对比
由表1及表2可知，与传统的碳/陶材料制成的刹车盘相比，表层材料700℃静态空气氧化2h显示，本发明的实施例1-3的氧化失重率明显低于传统碳/陶，因此，本发明的实施例的抗氧化能力更强，且相对于摩擦系数，本发明的实施例1-3的摩擦系数也明显高于传统碳/陶材料制成的刹车盘，摩擦系数稳定性也高于传统碳/陶材料制成的刹车盘，而磨损率则小于传统的碳/陶材料制成的刹车盘。
综上，与传统碳陶刹车材料相比，新设计的纤维预制体规避了由于表面纤维方向性明显所造成的热膨胀系数差异，涂层与基体材料的热失配现象减弱，提高了涂层与基体材料的界面结合强度，表面涂层处理也提高了摩擦面材料的抗氧化能力，同时摩擦面物相均匀性的提高也增强了制动的平稳性和材料的抗磨损能力。
以上本发明的实施方式作了详细说明，但本发明不限于所描述的实施方式。对于本领域的技术人员而言，在不脱离本发明原理和精神的情况下，对这些实施方式进行多种变化、修改、替换和变型，仍落入本发明的保护范围内。
Claims (8)
1.一种高结合强度涂层碳/陶刹车盘的制备方法，其特征在于，包括以下步骤：
步骤一，碳纤维预制体的制备：
首先将PAN基T700碳纤维制成短纤维胎网和无纬布，将单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加铺层，再用针刺技术使无纬布和胎网成为一体；根据需要厚度，分别计算0.6g/cm3、0.4g/cm3和0.2g/cm3用量，经过反复叠层、针刺、叠层、针刺，得到三维针刺碳纤维预制体，碳纤维预制体从内到外所用无纬布层密度逐渐下降，碳纤维预制体最外层两面为2-5mm的胎网层，预制体密度为0.35g/cm3，碳纤维体积含量为30％，层密度为14层/10mm；
步骤二，碳/碳复合材料的制备：
以天然气作为先驱体，在碳纤维预制体内部沉积PyC，沉积温度为800-1200℃，沉积时间为200-600h，得到多孔碳/碳复合材料；
步骤三，涂层浆料配置：
将液态酚醛树脂、呋喃树脂或糠酮树脂与粒径为1-10μm C粉进行混合，以TMAH作为分散剂，质量占比0.2-0.8wt％，通过滚筒球磨机混合24-48h，得到均匀分散的涂层浆料；
步骤四，涂层涂覆：
在多孔碳/碳复合材料的表面涂覆制备得到的涂层浆料，并进行烘干处理，反复进行2-4次，在碳/碳复合材料表面制得碳涂层；
步骤五，反应熔体浸渗处理：
将上述带涂层的碳/碳复合材料进行精加工成刹车盘，并在1300-1800℃的温度下进行反应熔体浸渗处理，得到密度为1.8-2.8g/cm3的碳/陶复合材料。
2.根据权利要求1所述高结合强度涂层碳/陶刹车盘的制备方法，其特征在于：所述无纬布层密度分为3种，分别是0.6g/cm3、0.4g/cm3和0.2g/cm3。
3.根据权利要求1所述高结合强度涂层碳/陶刹车盘的制备方法，其特征在于：在所述步骤一种，碳纤维预制体表面设置有2-5mm纯网胎层。
4.根据权利要求1所述高结合强度涂层碳/陶刹车盘的制备方法，其特征在于：在所述步骤二中，通过化学气相沉积制备得到的多孔碳/碳复合材料的密度为1.0-1.6g/cm3。
5.根据权利要求1所述高结合强度涂层碳/陶刹车盘的制备方法，其特征在于：在所述步骤三中，液态酚醛树脂、呋喃树脂或糠酮树脂与C粉混合的质量比为1～3:1。
6.根据权利要求1所述高结合强度涂层碳/陶刹车盘的制备方法，其特征在于：在所述步骤四中，碳碳复合材料表层涂层厚度为1-3mm。
7.根据权利要求1所述高结合强度涂层碳/陶刹车盘的制备方法，其特征在于：在所述步骤五中，通过反应熔体浸渗对带涂层的碳碳复合材料进行陶瓷致密化处理。
8.根据权利要求7所述高结合强度涂层碳/陶刹车盘的制备方法，其特征在于：所述浸渗的材料为Si，或Cu-Si，或Fe-Si。
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