耐磨耐高温聚苯硫醚复合涂层的研究
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摘要
本论文以聚苯硫醚（PPS）为基本成膜物质，其中的填料分为两个体系：（1）原位反应生成氧化铜；（2）添加有机改性纳米碳酸钙。通过对配方、工艺的调整以及涂层性能的检测，优选出能满足耐高温、耐磨损的聚苯硫醚涂层；分别考察了不同金属表面处理法方法、TiO_2含量、固化时间、固化温度对底层涂层粘结强度的影响；用XRD分析了涂层中填料的成分及涂层的结晶度；用FTIR分析了PPS氧化交联前后分子基团的变化，分析了涂层固化时的交联机理；用DTA分析了涂层的热稳定性及热分解温度；测试了涂层在干摩擦和水润滑条件下的摩擦磨损性能，并通过SEM对涂层磨损机理进行分析。得到的主要结论如下：
（1）在底层涂料中添加15%的TiO_2，对金属基材表面进行酸洗和硅烷处理，采用330℃、30min的固化工艺后，涂层与基材结合紧密，结合强度达到42MPa。
（2）XRD分析表明，涂层经交联、固化、淬火后，涂层的衍射峰强度明显降低，表明PPS树脂由结晶聚合物向非晶转变；减小结晶度有利于PPS涂层韧性的提高。
（3）涂层的红外光谱分析结果表明，固化前后PPS树脂分子链的主体结构未发生改变。但涂层中的硫原子在涂料熔融固化过程中发生氧化反应，硫醚（—S—）被氧化成亚砜（—SO—）或砜（—SO_2—）；涂层的交联主要发生在苯环上，苯环上的氢原子被氧化，形成芳醚。
（4）面层涂料中，通过CuSO_4与NaOH原位反应生成Cu(OH)_2，加热脱水后生成CuO，这与XRD结果分析一致；原位反应实现了无机粒子在乳液中的均匀分散。
（5）CuO/PPS/PTFE复合涂层的摩擦学性能明显优于PPS涂层，涂层的摩擦系数随CuO含量的增加而减小，磨损量呈先减后增的趋势，含CuO1.5%的涂层，其磨损量减少为原涂层的1/3。SEM分析表明，随CuO含量的增加，涂层的磨损机制由粘附磨损向磨粒磨损和疲劳磨损转变。
（6）PPS/纳米CaCO_3复合涂层在水润滑条件下的摩擦学性能明显优于干摩擦，摩擦系数和磨损量都只有干摩擦条件下的1/3左右；添加3%纳米CaCO_3，涂层干摩擦系数降低了25%，相应的磨损率降低了32%。
In this paper, the polyphenylene sulfide was the basical film foemation,in whichthe two kinds of addition systems were the copper oxide produced by in-situ reactionand the nano-CaCO_3modified by organic. The polyphenylene sulfide coating withhigh temperature resistant and wear-resisting was optimized by the different formula,coating technics and performance testing. The effects of different metal surfacetreatment methods, TiO_2contents, curing time and curing temperature on the bondingstrength of the bottom layer were investigated. The addition’s composition in thecoating and crystallinity of the coating were analyzed by XRD. The variation ofmolecular groups after PPS been cross-linkinged were analyzed by FIR and thecross-linking mechanism was analyzed when the coating was solidified. Thethermostability and heat decomposed temperature of the coating was analyzed byDTA. The tribological property of the coating was tested under dry friction conditionand water lubrication condition. The friction and wear mechanism was analyzed bySEM. The main conclusions are as follows:
(1) Coating and substrate were combined strongly when the subbing was filledwith15wt.%TiO_2and metal substrate surface was acid-washed and silane treated.Theadhesive strength is42MPa.
(2) XRD analysis showed that diffraction maximum of the coating wassignificant lower after the coating had been cross-linked, solidified and quenched andPPS was transformed into non-crystallizable polymer. The crystallinity decreasementof PPS coating is advantages for the enhancement of its toughness.
(3) FIR analysis showed that the major structure of molecular chain in the curingPPS was not changed. The sulfur atom was oxidized, including that—S—wasoxidized into—SO—or—SO_2—. The cross linkage between the coating wasmainly in the benzene ring, of which hydrogen atom was oxidized into aryloxide.
(4) The in-situ reaction is run between CuSO_4and NaOH, whose product isCu(OH)_2in the investment precoat. Cu(OH)_2is then dehydrated to produce CuO,which realized the homodisperse of inorganic particles in the emulsion. XRD atlasshowed the in-situ reaction product is CuO.
(5) The tribological performance of CuO/PPS/PTFE composite coating wasapparently better than pure PPS coating. The friction coefficient was decreased withthe increase of CuO content. The abrasion loss was firstly increased and then decreased, the abrasion loss of PPS coating was decreased to1/3when the CuOcontent was1.5%.
(6) The tribological performance of PPS/Nano-CaCO_3composite coating underwater lubrication condition was much better than dry friction. Both the frictioncoefficient and abrasion loss were decreased to1/3of that tested under waterlubrication with compared todry friction. The friction coefficient was decreased by25%and wear rate by32%under dry friction condition with the addion of3%Nano-CaCO_3.
（1）在底层涂料中添加15%的TiO_2，对金属基材表面进行酸洗和硅烷处理，采用330℃、30min的固化工艺后，涂层与基材结合紧密，结合强度达到42MPa。
（2）XRD分析表明，涂层经交联、固化、淬火后，涂层的衍射峰强度明显降低，表明PPS树脂由结晶聚合物向非晶转变；减小结晶度有利于PPS涂层韧性的提高。
（3）涂层的红外光谱分析结果表明，固化前后PPS树脂分子链的主体结构未发生改变。但涂层中的硫原子在涂料熔融固化过程中发生氧化反应，硫醚（—S—）被氧化成亚砜（—SO—）或砜（—SO_2—）；涂层的交联主要发生在苯环上，苯环上的氢原子被氧化，形成芳醚。
（4）面层涂料中，通过CuSO_4与NaOH原位反应生成Cu(OH)_2，加热脱水后生成CuO，这与XRD结果分析一致；原位反应实现了无机粒子在乳液中的均匀分散。
（5）CuO/PPS/PTFE复合涂层的摩擦学性能明显优于PPS涂层，涂层的摩擦系数随CuO含量的增加而减小，磨损量呈先减后增的趋势，含CuO1.5%的涂层，其磨损量减少为原涂层的1/3。SEM分析表明，随CuO含量的增加，涂层的磨损机制由粘附磨损向磨粒磨损和疲劳磨损转变。
（6）PPS/纳米CaCO_3复合涂层在水润滑条件下的摩擦学性能明显优于干摩擦，摩擦系数和磨损量都只有干摩擦条件下的1/3左右；添加3%纳米CaCO_3，涂层干摩擦系数降低了25%，相应的磨损率降低了32%。
In this paper, the polyphenylene sulfide was the basical film foemation,in whichthe two kinds of addition systems were the copper oxide produced by in-situ reactionand the nano-CaCO_3modified by organic. The polyphenylene sulfide coating withhigh temperature resistant and wear-resisting was optimized by the different formula,coating technics and performance testing. The effects of different metal surfacetreatment methods, TiO_2contents, curing time and curing temperature on the bondingstrength of the bottom layer were investigated. The addition’s composition in thecoating and crystallinity of the coating were analyzed by XRD. The variation ofmolecular groups after PPS been cross-linkinged were analyzed by FIR and thecross-linking mechanism was analyzed when the coating was solidified. Thethermostability and heat decomposed temperature of the coating was analyzed byDTA. The tribological property of the coating was tested under dry friction conditionand water lubrication condition. The friction and wear mechanism was analyzed bySEM. The main conclusions are as follows:
(1) Coating and substrate were combined strongly when the subbing was filledwith15wt.%TiO_2and metal substrate surface was acid-washed and silane treated.Theadhesive strength is42MPa.
(2) XRD analysis showed that diffraction maximum of the coating wassignificant lower after the coating had been cross-linked, solidified and quenched andPPS was transformed into non-crystallizable polymer. The crystallinity decreasementof PPS coating is advantages for the enhancement of its toughness.
(3) FIR analysis showed that the major structure of molecular chain in the curingPPS was not changed. The sulfur atom was oxidized, including that—S—wasoxidized into—SO—or—SO_2—. The cross linkage between the coating wasmainly in the benzene ring, of which hydrogen atom was oxidized into aryloxide.
(4) The in-situ reaction is run between CuSO_4and NaOH, whose product isCu(OH)_2in the investment precoat. Cu(OH)_2is then dehydrated to produce CuO,which realized the homodisperse of inorganic particles in the emulsion. XRD atlasshowed the in-situ reaction product is CuO.
(5) The tribological performance of CuO/PPS/PTFE composite coating wasapparently better than pure PPS coating. The friction coefficient was decreased withthe increase of CuO content. The abrasion loss was firstly increased and then decreased, the abrasion loss of PPS coating was decreased to1/3when the CuOcontent was1.5%.
(6) The tribological performance of PPS/Nano-CaCO_3composite coating underwater lubrication condition was much better than dry friction. Both the frictioncoefficient and abrasion loss were decreased to1/3of that tested under waterlubrication with compared todry friction. The friction coefficient was decreased by25%and wear rate by32%under dry friction condition with the addion of3%Nano-CaCO_3.
引文
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