氟化丙烯酸酯共聚物表面结构的形成与构建
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摘要
高分子材料表面的性能取决于其表面结构,目前对材料表面的形成过程及其对表面结构的影响研究很少。材料表面结构的设计很大程度上依赖于经验。因此,研究聚合物表面结构的形成对高分子表面形成理论模型的建立,表面结构的设计与控制以及聚合物在应用中表面与界面性能的控制都具有重要的意义。含氟聚合物材料具有极低的表面能、良好的拒水拒油和自清洁性、优异的耐热性能和化学稳定性等,在织物整理、功能涂层、航空航天、生物医用以及微电子等领域已得到广泛的应用。目前,含氟聚合物要获得优异表面性能往往需要耗费大量昂贵的含氟单体,而且含氟聚合物在使用环境中表面容易发生重构,从而丧失了优异的表面性能。因此人们希望在满足性能要求的同时,尽量减少氟单体的用量。以较少含氟量构造具有优异表面性能的稳定疏水表面一直是当今一个巨大的挑战。
本论文以甲基丙烯酸甲酯(MMA)与甲基丙烯酸-2-全氟辛基乙酯(FMA)的共聚物为研究对象,首次利用最新的、能原位测定的、具有单/准分子层灵敏度的和频振动光谱(SFG)研究共聚物表面最外层结构的形成,并结合接触角测试、X-射线光电子能谱(XPS)、原子力显微镜(AFM)、X-射线衍射(XRD)等其他手段,系统地研究了聚合物链结构、成膜方式、溶剂等因素对聚合物溶液固化时表面结构形成的影响因素,探讨了高分子表面结构形成的机理,并在此基础上以较少含氟量构造稳定的低表面能疏水表面。
成膜方式对氟化丙烯酸酯无规共聚物和二嵌段共聚物(PMMA-b-PFMA)表面结构的形成影响是截然不同的。以环已酮为溶剂时,对于无规共聚物,发现在低含氟量时(小于8 mol%),旋涂膜含氟组分的表面离析比浇铸膜容易;而较高氟含量时,结果刚好相反。两种膜的氟元素表面富集随本体中氟含量变化呈典型的“8”字形。低氟含量聚合物表面结构的形成受到构象熵主导。高氟含量时,全氟烷基在聚合物/空气界面的迁移受到焓控制。对于嵌段共聚物,浇铸膜表面的含氟组分富集量要远大于旋涂膜。氟化嵌段共聚物在溶液中聚集形成以PFMA为核、PMMA为冠的胶束。旋涂成膜时以PMMA为冠的胶束暴露在表面,疏水疏油性降低。而浇铸成时,含氟组分有足够时间从胶束聚集体中解缠,离析到表面,形成有序堆积的结构。
具有推拉结构的末端只带有少数几个FMA的聚甲基丙烯酸酯嵌段共聚物能够构建稳定的低表面能表面。末端只带3～4个FMA单元(0.38 mol%,FMA)的嵌段共聚物,其表面具备与PFMA均聚物同样良好的疏水疏油效果,且含氟组分在表面高度离析,形成排列有序紧密堆积的结构,具备良好的抗极性环境表面重构能力。含氟段的增长其表面性能下降,含氟组分反而向更深内部聚集,全氟烷基在表面的排列有序性下降,以致表面层反而出现了PMMA链段。合适的PFMA段长度是含氟嵌段聚合物优异表面性能的关键。同时还发现了非氟化段PMMA越长越有利于含氟组分的表面离析和富集。
研究发现长链的非氟化中间段PMMA(n=355)有利于三嵌段共聚物(PFMA-b-PMMA-b-PFMA)中含氟组分在表面的离析和富集,并且全氟烷基侧链能自组装形成丰富的有序结构-单层、双层和六角堆积结构,共聚物本体中形成层状聚集为主的结构,具备更好的环境稳定性。而短链PMMA(n=91)的氟化三嵌段共聚物全氟烷基却只能形成六角堆积结构,本体中自组装形成圆柱状结构。
合适的溶剂更能促进全氟烷基侧链表面离析,形成更加紧密有序堆积的自组装结构,聚合物表面具备更好的抗表面重构能力。嵌段聚合物PMMA_(857)-b-PFMA_(3.3)在三氟甲苯中以单聚体形式存在,在浇铸固化成膜后表面的环境稳定性要好于环已酮和甲苯为溶剂。而嵌段聚合物在甲苯等中以胶束聚集体形式存在,在表面形成过程中,含氟组分不能向表面充分离析甚至在近表面形成胶束状聚集体,并且全氟烷基在表面排列堆积有序性下降。此外,尽管热处理能使近表层的含氟组分离析增强,但是其表面的全氟烷基有序结构的破坏却使其表面稳定性大大降低。
本论文研究结果表明,以具有特定分子链结构的末端只带有少数几个FMA单元的氟化嵌段共聚物,经合适的溶液固化成膜后,其含氟组分向表面高度离析,且全氟烷基在表面自组装形成有序堆积结构,能够构建低表面能的稳定疏水表面。
The ultimate performance of materials in many traditional and modern applications depends not only on their bulk properties,but also relies heavily on their surface microstructure and interfacial behavior.Up to the present time,there existed few researches in the fields of formation mechanism of polymer surface structure.Progress in polymer surface and interface science and engineering will have been attributed to the ability of controlling and tailoring surface structure.Now days,fluorinated materials are widely used because of their low surface energy,chemical inertness,thermal stability,and low friction coefficient.Applications enclose low dielectric constant polymers in electronic industry,friction modifiers in lubrication oils, antifouling coating,optical fiber claddings and membranes.Since the costly fluorinated monomers were in used and the excellent surface performance of copolymer was lost when exposing in polar environment induced by surface reconstruction,it is challenging to fabricate fluorine-containing polymer surface with low-energy properties and superior long-lasting barrier properties and lower fluorine content,
In this paper,the copolymers composed of methyl methacrylate(MMA) and 2-perfluorooctylethyl methacrylate(FMA) with various chain structures were synthesized by ATRP or free radical polymerization.The effects of chain structure,film formation methods and solvents on the polymer surface formation by solution solidness were investigated in detail using contact angle measurement,X-ray photoelectron spectroscopy(XPS),sum frequency generation spectra(SFG),atomic force microscopy(AFM) and X-ray diffraction.
The difference of film-forming techniques on surface structure and performance of fluorinated methacrylate block copolymer and random copolymer were completely different.It was found that the enrichment of fluorinated moieties at spin-coated film surface was higher than that of cast film for low fluorine content random copolymer,but there was reverse results for high fluorine content copolymer.It surprisingly exhibited the figure like "8" that the tendency of surface segregation of fluorine at cast and spin-coated films surface with increasing of fluorine content.When the fluorinated monomer content in the copolymer was low,the perfluoroalkyl group was unable to migrate to the solution/air interface and became buried in the random-coil chain conformation as a result of entropic forces dominating the interfacial structure.When the films were prepared by spin-coating,the copolymer chains in solution were likely extended due to the centrifugal force,and the entropy effect of the polymer chains was thus weakened,resulting in the segregation of the fluorinated moieties on the film surface. However,perfluoroalkyl groups could not segregate at the surface of films prepared by casting and were thus buried in the random-coil chains.For the copolymers with high FMA contents, the migration of perfluoroalkyl groups at the solution/air interface or polymer/air interface was controlled by enthalpic forces.However,the cast film surface of diblock copolymer (PMMA-b-PFMA) has more fluorinated moieties than that of spin-coated film.The micelles was exposed at the surface during spin-coated which result in the decreasing of water and oil-repellence due to fluorinated diblock copolymer forms a micelle composed of the PMMA corona and the PFMA core in cyclohexanone or toluene.With comparing,the fluorinated moieties have enough time to be disentangled from micelles and could completely segregate at the outermost surface by using solution cast.
The end-capped poly(methyl methacrylate) with several FMA units possessed a special push-me/pull-you architecture could be used for fabricating stable low free energy surface.The films of the end-capped PMMA with only about 3 or 4 FMA units(0.38mol%,FMA) have the same water and oil-repellence with PFMA homocopolymer,and exhibited better stability and resistance to polar environments for the perfluorinated moieties which can self-assemble to form an ordered and close-packed structure at surface.With increasing of FMA block lengths,water and oil repellency decreased,the ratio of F/C increased with increasing film depth,and the degree of ordered packing of the perfluoroalkyl side chains at the surface decreased.The PMMA segments preliminarily occupied the film surface even when FMA units were 10.It was attributed to the PFMA block length affecting molecular aggregation structure of the copolymer in the solution and the interracial structure at the air/liquid interface,which affects surface structure formation during solution solidification in turn.The results suggest that the proper PFMA block length play an important role in structure formation on the solid surface.At the same time,the longer PMMA block enhanced both the enrichment of fluorinated moieties and the order of packing orientation of the perfluoroalkyl side chains on the surface.
It seems that the longer PMMA block(n=355) in triblock fluorinated copolymer (PFMA-b-PMMA-b-PFMA) was in favor of the fluorinated moieties segregating to outer surface and the perfluoralkyl side chain self-assemble into double-layer packing,single-layer packing and hexagonal packing structure,and the bulk formed lameUar structure.Accordingly, this film exhibited better stability and resistance to polar environments.As for triblock copolymer with shorter PMMA block(n=91),the perfluoralkyl side chain only self-assemble into hexagonal packing structure and the bulk formed cylinder structure.
The proper solvent can promote the segregation of the perfluoroalykl side chain of fluorinated block copolymer at surface,forming a relatively perfect close-packed and well-ordered structure of the perfluoroalkyl side chains at the surface.The films own excellent stability and resistance to polar environments.Films of PMMA_(857)-b-PFMA_(3.3) with about four 2-perfluorooctylethyl methacrylate units casted with benzotrifluoride solution exhibited excellent resistance to polar environments compared with those cast by cyclohexanone and toluene solutions.When the film was cast with benzotrifluoride solution,in which only unimers existed.The perfluoroalkyl side chains can segregate easily on the surface and self-assemble into an ordered structure.While the perfluoroalkyl side chains could not be easily disentangled and they could not completely segregate at the outermost surface and form a well-ordered packing structure,casting with cyclohexanone and toluene solution,in which micelle existed. After annealing the extent of segregation of fluorinated moieties increased,but the ordered structure of the perfluoroalkyl side chains at the PMMA857-b-PFMA3.3 film surface was destroyed which result in the decreasing in the surface stability of the films.
本论文以甲基丙烯酸甲酯(MMA)与甲基丙烯酸-2-全氟辛基乙酯(FMA)的共聚物为研究对象,首次利用最新的、能原位测定的、具有单/准分子层灵敏度的和频振动光谱(SFG)研究共聚物表面最外层结构的形成,并结合接触角测试、X-射线光电子能谱(XPS)、原子力显微镜(AFM)、X-射线衍射(XRD)等其他手段,系统地研究了聚合物链结构、成膜方式、溶剂等因素对聚合物溶液固化时表面结构形成的影响因素,探讨了高分子表面结构形成的机理,并在此基础上以较少含氟量构造稳定的低表面能疏水表面。
成膜方式对氟化丙烯酸酯无规共聚物和二嵌段共聚物(PMMA-b-PFMA)表面结构的形成影响是截然不同的。以环已酮为溶剂时,对于无规共聚物,发现在低含氟量时(小于8 mol%),旋涂膜含氟组分的表面离析比浇铸膜容易;而较高氟含量时,结果刚好相反。两种膜的氟元素表面富集随本体中氟含量变化呈典型的“8”字形。低氟含量聚合物表面结构的形成受到构象熵主导。高氟含量时,全氟烷基在聚合物/空气界面的迁移受到焓控制。对于嵌段共聚物,浇铸膜表面的含氟组分富集量要远大于旋涂膜。氟化嵌段共聚物在溶液中聚集形成以PFMA为核、PMMA为冠的胶束。旋涂成膜时以PMMA为冠的胶束暴露在表面,疏水疏油性降低。而浇铸成时,含氟组分有足够时间从胶束聚集体中解缠,离析到表面,形成有序堆积的结构。
具有推拉结构的末端只带有少数几个FMA的聚甲基丙烯酸酯嵌段共聚物能够构建稳定的低表面能表面。末端只带3～4个FMA单元(0.38 mol%,FMA)的嵌段共聚物,其表面具备与PFMA均聚物同样良好的疏水疏油效果,且含氟组分在表面高度离析,形成排列有序紧密堆积的结构,具备良好的抗极性环境表面重构能力。含氟段的增长其表面性能下降,含氟组分反而向更深内部聚集,全氟烷基在表面的排列有序性下降,以致表面层反而出现了PMMA链段。合适的PFMA段长度是含氟嵌段聚合物优异表面性能的关键。同时还发现了非氟化段PMMA越长越有利于含氟组分的表面离析和富集。
研究发现长链的非氟化中间段PMMA(n=355)有利于三嵌段共聚物(PFMA-b-PMMA-b-PFMA)中含氟组分在表面的离析和富集,并且全氟烷基侧链能自组装形成丰富的有序结构-单层、双层和六角堆积结构,共聚物本体中形成层状聚集为主的结构,具备更好的环境稳定性。而短链PMMA(n=91)的氟化三嵌段共聚物全氟烷基却只能形成六角堆积结构,本体中自组装形成圆柱状结构。
合适的溶剂更能促进全氟烷基侧链表面离析,形成更加紧密有序堆积的自组装结构,聚合物表面具备更好的抗表面重构能力。嵌段聚合物PMMA_(857)-b-PFMA_(3.3)在三氟甲苯中以单聚体形式存在,在浇铸固化成膜后表面的环境稳定性要好于环已酮和甲苯为溶剂。而嵌段聚合物在甲苯等中以胶束聚集体形式存在,在表面形成过程中,含氟组分不能向表面充分离析甚至在近表面形成胶束状聚集体,并且全氟烷基在表面排列堆积有序性下降。此外,尽管热处理能使近表层的含氟组分离析增强,但是其表面的全氟烷基有序结构的破坏却使其表面稳定性大大降低。
本论文研究结果表明,以具有特定分子链结构的末端只带有少数几个FMA单元的氟化嵌段共聚物,经合适的溶液固化成膜后,其含氟组分向表面高度离析,且全氟烷基在表面自组装形成有序堆积结构,能够构建低表面能的稳定疏水表面。
The ultimate performance of materials in many traditional and modern applications depends not only on their bulk properties,but also relies heavily on their surface microstructure and interfacial behavior.Up to the present time,there existed few researches in the fields of formation mechanism of polymer surface structure.Progress in polymer surface and interface science and engineering will have been attributed to the ability of controlling and tailoring surface structure.Now days,fluorinated materials are widely used because of their low surface energy,chemical inertness,thermal stability,and low friction coefficient.Applications enclose low dielectric constant polymers in electronic industry,friction modifiers in lubrication oils, antifouling coating,optical fiber claddings and membranes.Since the costly fluorinated monomers were in used and the excellent surface performance of copolymer was lost when exposing in polar environment induced by surface reconstruction,it is challenging to fabricate fluorine-containing polymer surface with low-energy properties and superior long-lasting barrier properties and lower fluorine content,
In this paper,the copolymers composed of methyl methacrylate(MMA) and 2-perfluorooctylethyl methacrylate(FMA) with various chain structures were synthesized by ATRP or free radical polymerization.The effects of chain structure,film formation methods and solvents on the polymer surface formation by solution solidness were investigated in detail using contact angle measurement,X-ray photoelectron spectroscopy(XPS),sum frequency generation spectra(SFG),atomic force microscopy(AFM) and X-ray diffraction.
The difference of film-forming techniques on surface structure and performance of fluorinated methacrylate block copolymer and random copolymer were completely different.It was found that the enrichment of fluorinated moieties at spin-coated film surface was higher than that of cast film for low fluorine content random copolymer,but there was reverse results for high fluorine content copolymer.It surprisingly exhibited the figure like "8" that the tendency of surface segregation of fluorine at cast and spin-coated films surface with increasing of fluorine content.When the fluorinated monomer content in the copolymer was low,the perfluoroalkyl group was unable to migrate to the solution/air interface and became buried in the random-coil chain conformation as a result of entropic forces dominating the interfacial structure.When the films were prepared by spin-coating,the copolymer chains in solution were likely extended due to the centrifugal force,and the entropy effect of the polymer chains was thus weakened,resulting in the segregation of the fluorinated moieties on the film surface. However,perfluoroalkyl groups could not segregate at the surface of films prepared by casting and were thus buried in the random-coil chains.For the copolymers with high FMA contents, the migration of perfluoroalkyl groups at the solution/air interface or polymer/air interface was controlled by enthalpic forces.However,the cast film surface of diblock copolymer (PMMA-b-PFMA) has more fluorinated moieties than that of spin-coated film.The micelles was exposed at the surface during spin-coated which result in the decreasing of water and oil-repellence due to fluorinated diblock copolymer forms a micelle composed of the PMMA corona and the PFMA core in cyclohexanone or toluene.With comparing,the fluorinated moieties have enough time to be disentangled from micelles and could completely segregate at the outermost surface by using solution cast.
The end-capped poly(methyl methacrylate) with several FMA units possessed a special push-me/pull-you architecture could be used for fabricating stable low free energy surface.The films of the end-capped PMMA with only about 3 or 4 FMA units(0.38mol%,FMA) have the same water and oil-repellence with PFMA homocopolymer,and exhibited better stability and resistance to polar environments for the perfluorinated moieties which can self-assemble to form an ordered and close-packed structure at surface.With increasing of FMA block lengths,water and oil repellency decreased,the ratio of F/C increased with increasing film depth,and the degree of ordered packing of the perfluoroalkyl side chains at the surface decreased.The PMMA segments preliminarily occupied the film surface even when FMA units were 10.It was attributed to the PFMA block length affecting molecular aggregation structure of the copolymer in the solution and the interracial structure at the air/liquid interface,which affects surface structure formation during solution solidification in turn.The results suggest that the proper PFMA block length play an important role in structure formation on the solid surface.At the same time,the longer PMMA block enhanced both the enrichment of fluorinated moieties and the order of packing orientation of the perfluoroalkyl side chains on the surface.
It seems that the longer PMMA block(n=355) in triblock fluorinated copolymer (PFMA-b-PMMA-b-PFMA) was in favor of the fluorinated moieties segregating to outer surface and the perfluoralkyl side chain self-assemble into double-layer packing,single-layer packing and hexagonal packing structure,and the bulk formed lameUar structure.Accordingly, this film exhibited better stability and resistance to polar environments.As for triblock copolymer with shorter PMMA block(n=91),the perfluoralkyl side chain only self-assemble into hexagonal packing structure and the bulk formed cylinder structure.
The proper solvent can promote the segregation of the perfluoroalykl side chain of fluorinated block copolymer at surface,forming a relatively perfect close-packed and well-ordered structure of the perfluoroalkyl side chains at the surface.The films own excellent stability and resistance to polar environments.Films of PMMA_(857)-b-PFMA_(3.3) with about four 2-perfluorooctylethyl methacrylate units casted with benzotrifluoride solution exhibited excellent resistance to polar environments compared with those cast by cyclohexanone and toluene solutions.When the film was cast with benzotrifluoride solution,in which only unimers existed.The perfluoroalkyl side chains can segregate easily on the surface and self-assemble into an ordered structure.While the perfluoroalkyl side chains could not be easily disentangled and they could not completely segregate at the outermost surface and form a well-ordered packing structure,casting with cyclohexanone and toluene solution,in which micelle existed. After annealing the extent of segregation of fluorinated moieties increased,but the ordered structure of the perfluoroalkyl side chains at the PMMA857-b-PFMA3.3 film surface was destroyed which result in the decreasing in the surface stability of the films.
引文
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