CN113089327B - 一种芳纶iii纤维增强自润滑衬垫复合材料及其制备方法 - Google Patents

一种芳纶iii纤维增强自润滑衬垫复合材料及其制备方法 Download PDF

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CN113089327B
CN113089327B CN202110380861.7A CN202110380861A CN113089327B CN 113089327 B CN113089327 B CN 113089327B CN 202110380861 A CN202110380861 A CN 202110380861A CN 113089327 B CN113089327 B CN 113089327B
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杨明明
陈祖均
张招柱
李佩隆
姜葳
袁军亚
赵鑫
储凡杰
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

本发明公开了一种芳纶III纤维增强自润滑衬垫复合材料的制备方法，是采用上浆后的芳纶III纤维作为纬纱，芳纶III纤维和PTFE纤维合捻纱作为经纱，在织机上进行织造；下机后的织物经退浆处理后先浸入单宁酸‑氨丙基三乙氧基硅烷的水溶液活化，再浸入MgAl‑LDH前驱体溶液中通过水热界面反应进行增强修饰，然后浸入多巴胺‑聚乙烯亚胺的缓冲溶液增粘修饰，最后浸入aramid纳米纤维增韧修饰，得到强‑韧一体化界面修饰的芳纶III/PTFE织物坯布。本发明制备的芳纶III纤维增强自润滑衬垫将具有优异的力学性能和摩擦磨损性能，使维织物自润滑衬垫复合材料的得到大幅度提升，进而改善了织物型自润滑零部件的综合性能。

Description

一种芳纶III纤维增强自润滑衬垫复合材料及其制备方法
技术领域
本发明涉及一种纤维增强自润滑衬垫复合材料，尤其涉及一种芳纶III纤维增强自润滑衬垫复合材料及其制备方法，属于复合材料领域和润滑材料技术领域。
背景技术
自润滑衬垫在轴承中扮演着润滑剂的角色，它将轴承中两个金属面之间的摩擦转变为金属对自润滑衬垫的摩擦，其性能直接决定着自润滑轴承的服役稳定性和服役寿命。目前，自润滑衬垫中使用的增强纤维主要为芳纶纤维、玻璃纤维为主。
芳纶III纤维是对位芳纶的一种，芳纶 III是由对苯二胺、对苯二甲酰氯及含有杂环结构的二胺三种单体共聚得到的。芳纶III纤维独特的大分子结构及工艺技术赋予其低密度、超高强度、超高模量、耐高温、抗冲击、耐磨性好等优异性能。目前作为飞机、卫星等高新技术装备中的增强纤维得到了非常广泛的应用。由于芳纶III纤维优异的力学及热学性能，其作为自润滑衬垫的增强纤维可以大幅提升自润滑衬垫的力学性能和摩擦学性能。然而，芳纶III纤维虽然具有上述优异性能，但其仍然存在纤维表面活性基团含量较低，致使其与树脂基体之间的浸润性较差，纤维-树脂界面结合强度较弱。当前解决芳纶III纤维与树脂基体之间界面相互作用弱的问题，主要采用等离子体刻蚀法、辐照法、化学氧化法等方法。其中使用最多的方法是等离子体刻蚀法和表面接枝法，但是，等离子体刻蚀法处理后纤维表面活性随时间的推移会衰减，不利于长期储存，表面接枝法过程繁琐。
CN101787647B公开了一种芳纶III纤维表面处理方法，是将低分子量脂肪族二异氰酸酯或二醇类二缩水甘油醚中加入到有机溶剂中，形成质量分数为0.5~5％的均匀溶液，制得表面处理剂；再用表面处理剂浸没芳纶III丝束。通过该方法处理芳纶III纤维柔软度提升，提高了芳纶
Figure 39654DEST_PATH_IMAGE001
纤维表面极性。但是，该方法并不适用于芳纶III/PTFE自润滑衬垫中纤维-树脂基体界面性能改性。主要是由于芳纶III纤维织物过程中需要穿综过扣，前期修饰物在织造准备阶段和织造过程中会因摩擦而被破坏，达不到界面增强的目的。
为此，本发明中我们采用两步反应接枝法在芳纶III/PTFE自润滑衬垫中构筑强-韧一体化的界面相，实现芳纶III/PTFE长效表界面修饰，改善自润滑衬垫中纤维与树脂之间的界面相互作用，提升芳纶III/PTFE衬垫力学性能和摩擦磨损性能。
发明内容
本发明的的目的是提供一种芳纶III/PTFE自润滑衬垫复合材料的制备方法，以改善自润滑衬垫的力学性能和摩擦学性能。
一、芳纶III/PTFE自润滑衬垫复合材料的制备
本发明芳纶III/PTFE自润滑衬垫复合材料的制备方法，是采用上浆后的芳纶III纤维作为纬纱，芳纶III纤维和PTFE纤维合捻纱作为经纱，在织机上进行织造；下机后的织物经退浆处理得到芳纶III/PTFE织物坯布；将芳纶III/PTFE织物坯布浸入单宁酸-氨丙基三乙氧基硅烷的水溶液中室温活化处理5~6h，得到活化的芳纶III/PTFE织物坯布；再将活化的芳纶III/PTFE织物坯布浸入双金属氢氧化物MgAl-LDH前驱体溶液中，在60~120℃下加压反应20~24h；用去离子水洗涤、烘干后浸入多巴胺-聚乙烯亚胺的缓冲溶液中室温处理5~6h；取出用去离子水洗涤，烘干；然后浸入aramid纳米纤维的二甲亚砜溶液0.1~1h，取出后依次用二甲亚砜、去离子水冲洗，烘干，得到强-韧一体化界面修饰的芳纶III/PTFE织物坯布；最后将修饰的芳纶III/PTFE织物坯布在树脂溶液中反复浸渍，直至织物质量分数达到15~35%，最后经粘结固化，得到芳纶III/PTFE织物自润滑衬垫材料。
芳纶III纤维、PTFE纤维的规格介于50~800D之间。芳纶III和PTFE纤维合捻纱的捻度为50~800捻/米。芳纶III/PTFE织物坯布结构为平纹，斜纹，缎纹，或者上述三种三原组织结构的演变结构中的一种。
单宁酸-氨丙基三乙氧基硅烷的水溶液中，单宁酸浓度为浓度0.001mg~0.5g/ml，氨丙基三乙氧基硅烷的浓度为0.001mg~1g/ml。
层状双金属氢氧化物MgAl-LDH前驱体溶液的制备，是将Mg(NO3)2·6H2O和Al(NO3)3·9H2O以1:0.5~1:4的摩尔比分散在去离子水而得。活化的芳纶III/PTFE织物坯布浸入层状双金属氢氧化物MgAl-LDH前驱体溶液中，采用水热反应和界面反应，将MgAl-LDH修饰到芳纶III/PTFE织物坯布表面。
多巴胺-聚乙烯亚胺的缓冲水溶液中，多巴胺、聚乙烯亚胺的浓度均为0.01mg/ml~0.5g/ml。
aramid纳米纤维的二甲亚砜溶液中，aramid纳米纤维的浓度为0.01mg/ml~0.8g/ml。
所述增强树脂为酚醛树脂、聚酰亚胺树脂、环氧树脂之中的一种或者其中两者的混合物。
所述粘结固化温度介于120~200℃，固化时间为30min~3h，升温速率介于3~20℃/min。
二、芳纶III/PTFE自润滑衬垫复合材料的结构和性能
1、物理性能
本发明制备的芳纶III/PTFE织物坯布布面平整，自润滑衬垫粘接于金属基材表面的衬垫无褶皱，无气泡，平整光滑（图1）。
2、摩擦性能
在室温环境下，250MPa动载荷，摆角±25º，频率0.2Hz的低速重载摆动工况下，摆动摩擦25000次，测定自润滑衬垫的摩擦系数。图2为本发明所述芳纶III/PTFE自润滑衬垫低速重载摆动试验衬垫摩擦系数。可见，在测试25000次之后，衬垫依然完整覆盖金属基材（如图1所示），衬垫表面光滑，衬垫磨损深度≤110μm，摩擦系数在0.034左右。且摩擦系数非常稳定。可见，芳纶III/PTFE自润滑衬垫具有非常优异的承载能力和耐磨寿命。
综上所述，本发明将具有优异力学性能的芳纶III纤维引入到自润滑衬垫复合材料中，并采用MgAl-LDH为增强相，aramid纳米纤维（ANFs）为增韧相，聚多巴胺-聚乙烯亚胺为界面粘结层，在芳纶III/PTFE自润滑坯布表面构筑强-韧一体化的界面相，提升自润滑衬垫中纤维与树脂基体的界面相互作用，改善了芳纶III纤维和PTFE纤维与树脂基体之间的界面结合强度，抑制和减缓自润滑衬垫中微裂纹的产生和扩展，使维织物自润滑衬垫复合材料的力学性能和摩擦磨损性能得到大幅度提升，进而改善了织物型自润滑零部件的综合性能。
附图说明
图1为本发明所述芳纶III/PTFE自润滑衬垫低速重载摆动试验后衬垫照片。
图2为本发明所述芳纶III/PTFE自润滑衬垫低速重载摆动试验衬垫摩擦系数。
具体实施方式
下面通过具体实施例对本发明芳纶III纤维增强自润滑衬垫复合材料及其制备方法和性能做进一步说明。
实施例1
（1）200D的芳纶III纤维和PTFE纤维在纤维加捻设备上进行合股并加捻，得到捻度160捻/米的合捻纱；
（2）配制聚酯浆料，向其中加入抗氧化剂、抗静电剂等组分，对芳纶III纤维进行上浆处理；
（3）采用上浆芳纶III纤维为经纱，芳纶III和PTFE纤维的合捻纱为纬纱，在织机上织造，坯布为平纹组织；下机后的织物经退浆处理，得到芳纶III/PTFE织物坯布；
（4）将芳纶III/PTFE织物坯布浸入单宁酸（1mg/ml）-氨丙基三乙氧基硅烷（1mg/ml）的水溶液中，在室温反应6 h，得到表面活化的芳纶III/PTFE织物坯布；
（5）将活化的芳纶III/PTFE织物坯布浸入MgAl-LDH前驱体溶液中（0.012molMg(NO3)2·6H2O和0.004molAl(NO3)3·9H2O加入到120ml去离子水中），在120℃加压反应24h，反应结束用去离子水对织物坯布进行洗涤，80℃烘干；将烘干的芳纶III/PTFE织物坯布浸入多巴胺-聚乙烯亚胺的缓冲溶液中（1mg/ml），室温反应6h，取出用去离子水洗涤，80℃烘干后浸入ANFs的二甲亚砜溶液中（0.002g/ml），室温反应1h，取出用二甲亚砜冲洗2min，去离子水冲洗3次，80℃烘干，得到强-韧一体化界面修饰的芳纶III/PTFE织物坯布；
（6）将修饰的芳纶III/PTFE织物坯布在酚醛树脂溶液中反复浸渍，直至织物质量分数达到75%，经粘结固化（184℃，2h），得到芳纶III/PTFE织物坯布酚醛树脂自润滑衬垫；
（7）在室温环境下，250MPa动载荷，摆角±25º，频率0.2Hz的低速重载摆动工况下，摆动摩擦25000次，测定自润滑衬垫的摩擦系数。在测试25000次之后，衬垫依然完整覆盖金属基材，衬垫表面光滑，衬垫磨损深度≤110μm，摩擦系数在0.036左右。且摩擦系数非常稳定。
实施例2
（1）、（2）、（3）、（4）同实施例1；
（5）将活化的芳纶III/PTFE织物坯布浸入MgAl-LDH前驱体溶液中（0.009molMg(NO3)2·6H2O和0.003mol Al(NO3)3·9H2O加入到120ml去离子水中），在120℃加压反应24h，反应结束用去离子水对织物坯布进行洗涤，80℃烘干；将烘干的芳纶III/PTFE织物坯布浸入多巴胺-聚乙烯亚胺的缓冲溶液中（1.5mg/ml），室温反应6h，取出用去离子水洗涤，80℃烘干后浸入ANFs的二甲亚砜溶液中（0.002g/ml），室温反应1h，取出用二甲亚砜冲洗2min，去离子水冲洗3次，80℃烘干，得到强-韧一体化界面修饰的芳纶III/PTFE织物坯布；
（6）将修饰后的芳纶III/PTFE织物坯布在酚醛树脂溶液中反复浸渍，直至织物质量分数达到75%，经粘结固化（184℃，2h），得到芳纶III/PTFE织物坯布酚醛树脂自润滑衬垫；
（7）在室温环境下，250MPa动载荷，摆角±25º，频率0.2Hz的低速重载摆动工况下，摆动摩擦25000次，测定自润滑衬垫的摩擦系数。在测试25000次之后，衬垫依然完整覆盖金属基材，衬垫表面光滑，衬垫磨损深度≤110μm，摩擦系数在0.030左右。且摩擦系数非常稳定。
实施例3
（1）、（2）、（3）、（4）同实施例1；
（5）将活化的芳纶III/PTFE织物坯布浸入MgAl-LDH前驱体溶液中（0.006molMg(NO3)2·6H2O和0.002mol Al(NO3)3·9H2O加入到120ml去离子水中），在120℃加压反应24h，反应结束用去离子水对织物坯布进行洗涤，80℃烘干；将烘干的芳纶III/PTFE织物坯布浸入多巴胺-聚乙烯亚胺的缓冲溶液中（2mg/ml），室温反应6h，取出用去离子水洗涤，80℃烘干后浸入ANFs的二甲亚砜溶液中（0.0015g/ml），室温反应1h，取出用二甲亚砜冲洗2min，去离子水冲洗3次，80℃烘干，得到强-韧一体化界面修饰的芳纶III/PTFE织物坯布；
（6）将修饰的III/PTFE织物坯布在酚醛树脂溶液中反复浸渍，直至织物质量分数达到75%，经粘结固化（184℃，2h），得到芳纶III/PTFE织物坯布酚醛树脂自润滑衬垫；
（7）在室温环境下，250MPa动载荷，摆角±25º，频率0.2Hz的低速重载摆动工况下，摆动摩擦25000次，测定自润滑衬垫的摩擦系数。在测试25000次之后，衬垫依然完整覆盖金属基材，衬垫表面光滑，衬垫磨损深度≤110μm，摩擦系数在0.034左右。且摩擦系数非常稳定。
实施例4
（1）、（2）、（3）、（4）同实施例1；
（5）将活化的芳纶III/PTFE织物坯布浸入MgAl-LDH前驱体溶液中（0.003molMg(NO3)2·6H2O和0.001mol Al(NO3)3·9H2O加入到120ml去离子水中），在120℃加压反应24h，反应结束用去离子水对织物坯布进行洗涤，80℃烘干；将烘干的芳纶III/PTFE织物坯布浸入多巴胺-聚乙烯亚胺的缓冲溶液（1mg/ml）中，室温反应6h，取出用去离子水洗涤，80℃烘干后浸入ANFs的二甲亚砜溶液中（0.002g/ml），室温反应1h，取出用二甲亚砜冲洗2min，去离子水冲洗3次，80℃烘干，得到强-韧一体化界面修饰的芳纶III/PTFE织物坯布；
（6）将修饰的芳纶III/PTFE织物坯布在酚醛树脂溶液中反复浸渍，直至织物质量分数达到75%，经粘结固化（184℃，2h），得到芳纶III/PTFE织物坯布酚醛树脂自润滑衬垫；
（7）在室温环境下，250MPa动载荷，摆角±25º，频率0.2Hz的低速重载摆动工况下，摆动摩擦25000次，测定自润滑衬垫的摩擦系数。在测试25000次之后，衬垫依然完整覆盖金属基材，衬垫表面光滑，衬垫磨损深度≤110μm，摩擦系数在0.035左右。且摩擦系数非常稳定。

Claims (9)

1.一种芳纶
Figure DEST_PATH_IMAGE002
/PTFE织物自润滑衬垫材料的制备方法，其特征在于：是采用上浆后的芳纶
Figure 98660DEST_PATH_IMAGE002
纤维作为纬纱，芳纶
Figure 625587DEST_PATH_IMAGE002
纤维和PTFE纤维合捻纱作为经纱，在织机上进行织造；下机后的织物经退浆处理得到芳纶
Figure 828161DEST_PATH_IMAGE002
/PTFE织物坯布；将芳纶
Figure 618176DEST_PATH_IMAGE002
/PTFE织物坯布浸入单宁酸-氨丙基三乙氧基硅烷的水溶液中室温活化处理5~6h，得到活化的芳纶
Figure 42335DEST_PATH_IMAGE002
/PTFE织物坯布；再将活化的芳纶
Figure 740164DEST_PATH_IMAGE002
/PTFE织物坯布浸入双金属氢氧化物MgAl-LDH前驱体溶液中，在120℃下加压反应24h；用去离子水洗涤、烘干后浸入多巴胺-聚乙烯亚胺的缓冲溶液中室温处理5~6h；取出用去离子水洗涤，烘干；然后浸入aramid纳米纤维的二甲亚砜溶液0.1~1h，取出后依次用二甲亚砜、去离子水冲洗，烘干，得到强-韧一体化界面修饰的芳纶
Figure 413722DEST_PATH_IMAGE002
/PTFE织物坯布；最后将修饰的芳纶
Figure 19146DEST_PATH_IMAGE002
/PTFE织物坯布在树脂溶液中反复浸渍，直至织物质量分数达到50~80%，最后经粘结固化，得到芳纶
Figure 110861DEST_PATH_IMAGE002
/PTFE织物自润滑衬垫材料；层状双金属氢氧化物MgAl-LDH前驱体溶液的制备，是将Mg(NO3)2·6H2O和Al(NO3)3·9H2O以1:0.5~1:3的摩尔比分散在去离子水而得。
2.如权利要求1所述一种芳纶
Figure 510750DEST_PATH_IMAGE002
/PTFE织物自润滑衬垫材料的制备方法，其特征在于：芳纶
Figure 671604DEST_PATH_IMAGE002
纤维、PTFE纤维的规格介于50~800D之间。
3.如权利要求1所述一种芳纶
Figure 815140DEST_PATH_IMAGE002
/PTFE织物自润滑衬垫材料的制备方法，其特征在于：芳纶
Figure 495783DEST_PATH_IMAGE002
和PTFE纤维合捻纱的捻度为50~800捻/米。
4.如权利要求1所述一种芳纶
Figure 535414DEST_PATH_IMAGE002
/PTFE织物自润滑衬垫材料的制备方法，其特征在于：芳纶
Figure 980302DEST_PATH_IMAGE002
/PTFE织物坯布结构为平纹，斜纹，缎纹，或者上述三种三原组织结构的演变结构中的一种。
5.如权利要求1所述一种芳纶
Figure 661950DEST_PATH_IMAGE002
/PTFE织物自润滑衬垫材料的制备方法，其特征在于：所述单宁酸-氨丙基三乙氧基硅烷的水溶液中，单宁酸浓度为浓度0.001mg~0.5g/ml，氨丙基三乙氧基硅烷的浓度为0.001mg~1g/ml。
6.如权利要求1所述一种芳纶
Figure 474397DEST_PATH_IMAGE002
/PTFE织物自润滑衬垫材料的制备方法，其特征在于：多巴胺-聚乙烯亚胺的缓冲水溶液中，多巴胺、聚乙烯亚胺的浓度均为0.01mg/ml~0.5g/ml。
7.如权利要求1所述一种芳纶
Figure 419350DEST_PATH_IMAGE002
/PTFE织物自润滑衬垫材料的制备方法，其特征在于：aramid纳米纤维的二甲亚砜溶液中，aramid纳米纤维的浓度为0.01mg/ml~0.8g/ml。
8.如权利要求1所述一种芳纶
Figure 820376DEST_PATH_IMAGE002
/PTFE织物自润滑衬垫材料的制备方法，其特征在于：所述树脂为酚醛树脂、聚酰亚胺树脂、环氧树脂之中的一种或者其中两者的混合物。
9.如权利要求1所述一种芳纶
Figure 305715DEST_PATH_IMAGE002
/PTFE织物自润滑衬垫材料的制备方法，其特征在于：所述固化处理温度介于120~200℃，固化时间为30min~3h，升温速率介于3~20℃/min。
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