含硅有机—无机杂化硬质薄膜的制备及其性能研究
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摘要
光学塑料表面硬度低、不耐刮划，在使用过程中表面易被擦伤起雾，导致材料的透明度下降，使其在许多方面的应用受到限制。在塑料表面涂敷硬质防护薄膜是一种简单有效的提高塑料耐划伤性能的方法。有机/无机杂化硬质透明材料能够兼具有机组分对塑料良好的粘结性及无机组分的高硬度及耐划伤性而成为塑料表面硬质薄膜的发展方向。
本文以正硅酸乙酯和有机硅氧烷为先驱物，采用溶胶-凝胶法制备了性能良好的透明SiO_2/有机硅杂化材料。在此基础上，为提高SiO_2/有机硅杂化材料的耐碱性、对聚碳酸酯(PC)基材的粘结力和材料环保友好性，通过功能化改性或分子设计，分别制备了热固化型硅/胺杂化材料、聚酯/SiO_2/有机硅杂化材料和光固化型SiO_2/超支化聚氨酯丙烯酸酯杂化材料。系统研究了含硅杂化硬质薄膜的组成、结构与性能及其内在关系，主要研究成果如下：
1、以正硅酸乙酯(TEOS)为无机相前驱体，甲基三乙氧基硅烷(MTES)、二甲基二乙氧基硅烷(DMDES)和甲基丙烯酰氧基丙基三甲氧基硅烷(MAPTMS)为有机相前驱体，采用溶胶-凝胶法合成出热固化型SiO_2/有机硅杂化材料。确定了各组分的优化配比：n_(TEOS)∶n_(MTES)∶n_(DMDES)∶n_(MAPTMS)＝5∶5∶2∶2，n_(IPA)/n_(Si-OR)=0.8，n_(H2O)/n_(Si-OR)＝1.1，n_(HAc)/n_(Si-O)＝0.008，此条件下制备的杂化涂料可稳定存放360d。由于在高度交联的SiO_2网络中引入线性的Si—O—Si链段，而且有机和无机网络通过共价键结合起来，相容性良好，使得杂化薄膜既有高硬度又有良好的粘结力。按优化配比制备的杂化薄膜的铅笔硬度为2H，附着力为1级，透光率为93.6%。研究发现随着n(R)/n(Si)值减少，杂化材料的热稳定性增强。杂化薄膜对水的接触角随n(R)/n(Si)值的增大和固化时间的延长而增大，具有一定的疏水性。PC涂覆杂化膜层后具有更低的折射率，并且涂层表面光滑致密，从而减少了PC表面的漫反射，使得薄膜对PC具有增透作用。
2、氨基树脂的种类影响SiO_2/有机硅树脂的性能。氨基树脂中醇碳链增大，硅/胺杂化树脂的相分离程度增加；醚化度增加，相分离程度降低；氨基树脂用量增加，相分离程度先降低后增加。全甲醚化氨基树脂(HMMM)比部分甲醚化氨基树脂和丁醚化氨基树脂能获得硬度与柔韧性的更良好平衡和更优越耐久性。FTIR表明氨基树脂是利用—CH_2OCH_3与SiO_2/有机硅树脂的—OH发生交联反应。SiO_2/有机硅树脂经氨基树脂改性后，具有更为致密的无机-有机网状结构，NaOH等一些小分子不易渗透进去，起到了相当好的抗碱蚀作用。当HMMM的加入量为2wt.%时，与SiO_2/有机硅树脂的相容性最好，粒子形态规则，分散均匀，杂化薄膜在碱液中浸泡24h后，表面仍然平整，失光率最小，仅为0.43%。
3、合成一种带磺酸基团的聚酯树脂用于改性SiO_2/有机硅树脂，通过共聚和共混法制备了系列聚酯/SiO_2/有机硅杂化涂料。含有磺酸基的聚酯能改善与SiO_2/有机硅树脂的混溶性，极大提高对基材的附着力。聚酯/SiO_2/有机硅杂化涂料能在不经底涂处理的PC上铺展成膜。红外表明杂化薄膜中的－OH和－SO_3H等极性基团与PC基材表面的－C=O键之间发生了化学吸引和氢键耦合作用。两种工艺法都有聚酯链段接枝在SiO_2/有机硅树脂上，杂化树脂的粘度均随聚酯含量的提高而增大，但共聚法接枝的更多，得到的杂化树脂粘度高。共聚法比共混法产生更强的有机/无机相互作用，更高的交联密度，更高的热稳定性和更好的耐磨损性。共混杂化涂层微相分离的程度和表面粗糙度更大，一般可观测到明显的团聚体，而共聚杂化涂层只在聚酯含量较高时才观察到。共聚杂化样品的热分解近似为1级反应，用Ozawa法计算其在40%分解阶段的活化能约为243kJ/mol。XRD表明共聚杂化树脂属典型的非晶相。EDS表明硅相易迁移到杂化涂层的表面，极大地降低其表面能。采用共聚法比共混法得到的杂化涂层具有更低的表面能，其表面能随着SiO_2/有机硅树脂含量的增加而降低。共聚杂化膜比共混体系表现出较好的耐水性，其吸水率随SiO_2/有机硅树脂含量随量的加而降低。
4、以TEOS和MAPTMS制备的改性硅溶胶为无机组分，以自制的超支化聚氨酯丙烯酸酯(HBPUA)为有机组分，制备了一系列可UV固化的HBPUA/(MAPTMS-SiO_2)杂化涂料。超支化HBPUA/(MAPTMS-SiO_2)杂化材料中的无机和有机组分相容性很好，硅溶胶均匀地分布于有机相中，其储存稳定性明显好于线性PUA/(MAPTMS-SiO_2)杂化涂料。HBPUA/(MAPTMS-SiO_2)杂化膜经UV固化后变得致密透亮、无裂纹和明显的微相分离，但随无机组分用量增加，观察到SiO_2团聚颗粒。HBPUA/(MAPTMS-SiO_2)杂化涂膜的热稳定性和碳碳双键最终转化率比PUA/(MAPTM-SiO_2)杂化涂膜更高，其玻璃化转变温度随着无机组分用量的增加和UV固化时间的延长相应的增大。当以n_(SiO2):n_(MAPTMS)=1:2制备的改性硅溶胶用量为30wt.%，活性单体1,6己二醇二丙烯酸酯用量为20wt.%，复合引发剂(Irgacure184+TPO)用量为3wt.%时，HBPUA/(MAPTMS-SiO_2)杂化涂料的凝胶时间高于180d，UV固化4min后，薄膜性能最优，透光率为92.8%，铅笔硬度为4H，附着力为0级，柔韧性为3mm，冲击强度为46kg·cm，磨耗量为17.5mg。
Due to the low surface hardness, transparent plastic is easy to be scratched in use, whichmakes the loss of operation life and limits extended application. The surface scratch behaviorcan be reduced effectively through coating a hard protective film on it. The organic/inorganichard film can integrate good adhesion to substrate of organic film with excellent hardness ofinorganic film, which has become the hot study spot of hard film on plastic.
The transparent and hard SiO_2/organosilicone hybrid coatings were prepared onpolycarbonate(PC) with tetraethoxysilane and organosiloxane as the main raw materials bysol-gel method. In order to improve anti-alkali corrosion properties, adhesion andenvironmentally friendly of the SiO_2/organosilicone hybrid materials, heat-curablesilicone/amine hybrid materials, polyester/SiO_2/organosilicone hybrid materials and UVcurable SiO_2/hyperbranched polyurethane acrylate hybrid materials were preparedrespectively. The relationship of composition, structure and properties of hybrid hard filmswith silicon was studied systemically. The detailed research contents and results weredescribed as follows:
1. With tetraethoxysilane(TEOS) as inorganic precursor, methyltriethoxysilane(MTES),dimethyldiethoxysilane(DMDES) and3-(methacryloxypropyl)trimethoxysilane(MAPTMS)as organic precursor, the heat-curable SiO_2/organosilicone hybrid coatings was synthesized bysol-gel method. When the molar ratio of SiO_2/organosilicone hybrid coating was n_(TEOS):n_(MTES):n_(DMDES):n_(MAPTMS)=5:5:2:2, n_(IPA)/n_(Si-OR)=0.8, n_(H2O)/n_(Si-OR)=1.1, n_(HAc)/nSi-O=0.008, the gelation timeexceeded360days. The hybrid film had high hardness and good adhesion because linearSi-O-Si segmers were introduced into high-density crosslinked SiO_2network. The hybridfilms prepared in accordance with the optimized ratio had optimal properties withtransmittance of93.6%, pencil hardness of2H, adhesion of0degree. It was found that thehybrid coating had excellent thermal stability, which increases gradually with the decrease ofn(R)/n(Si) value. The contact angle of the hybrid coating to the water increased with theincrease of n(R)/n(Si) value and curing time. Higher light transmittance of hybrid coatingswas probably due to lower refractive index of hybrid coatings than that of the PC sheet. It wasalso considered that the hybrid coating reduces light reflection on the surface of the substrate.
2. The type of amine resin significantly affected the alkali resistance of the SiO_2/organo-silicone film. In comparison with part methoxymethyl and butoxymethyl melamine resin,Hexamethoxymethyl melamine resin(HMMM) had better durability and balance betweenhardness and flexibility for hybrid coatings. FTIR showed that the co-condensation betweenthe methoxymethyl groups in HMMM and the hydroxyl groups in SiO_2/organosilicone resin.The SiO_2/organosilicone resin formed more dense inorganic-organic network after HMMMmodified, resulted in NaOH and other small molecules not easy to penetrate into hybrid films.When the content of HMMM was2wt.%, SiO_2/organosilicone resin had best compatibilitywith HMMM and hybrid particles had regular morphology. The hybrid film was still smoothand had minimum transmittance loss of0.43%after immersion in NaOH solution for24h.
3. A series of polyester/SiO_2/organosilicone hybrid coatings were synthesized throughcopolymerization and blending method between SiO_2/organosilicone resin and sulfonicgroup-containing polyester made from carefully selected proper monomers in my ownlaboratory. The polyester containing strong polarity of the sulfonic group, which not only toimprove the compatibility with SiO_2/organosilicone resin, but also improve the adhesion toPC, resulted in polyester/SiO_2/organosilicone coatings could be spread on PC without primer.The grafting rate of co-polymerizable resin is greater than that of the blends. The viscosity ofco-polymerizable and blending hybrid resin increased with polyester content increasing. Incomparison with blending method, co-polymerizable method had much stronger interactionsbetween organic phases and inorganic phases, resulting in higher crosslinking density, higherthermal stability and wear resistance for hybrid coatings. The extent of microphase separationand the surface roughness of the blending coatings became bigger. Obvious agglomerateswere observed for the blending coatings while those agglomerates were only observed for theco-polymerizable coatings at relatively high polyester content. The thermal decompositionprocess of the co-polymerizable sample followed one-order kinetics with the higher activationenergy of243kJ/mol. XRD studies showed that the co-polymerizable materials wasamorphous. EDS analysis showed that the silica particles could move towards the surface ofco-polymerizable coatings to lower free energies. The co-polymerizable coating had a lowersurface energy and better water resistance than the blends, and its surface free energy andwater absorption decreased with increasing of SiO_2/organosilicone content.
4. The modified silicone sol from TEOS and MAPTMS were used as inorganiccomponents and hyperbranched polyurethane acrylate(HBPUA) were used as organiccomponents for preparing a series of UV-curable HBPUA/(MAPTMS-SiO_2) hybrid coatings.The results showed that HBPUA/(MAPTMS-SiO_2) hybrid films hand good interfacialcompatibility and SiO_2were well distributed in organic matrix. The stability ofHBPUA/(MAPTMS-SiO_2) hybrid coatings were higher than that of PUA/(MAPTMS-SiO_2)hybrid coatings. The HBPUA/(MAPTMS-SiO_2) hybrid film became transparent, dense, nocracks and microphase separation after UV curing. However, the gel particles of hybridcoatings increased with the content of inorganic component increasing. The terminalconversion degree of C=C bonds of HBPUA/(MAPTMS-SiO_2) hybrid coatings were higherand thermal stable was better than those of PUA/(MAPTMS-SiO_2) hybrid coatings. The TgofHBPUA/(MAPTMS-SiO_2) hybrid coatings increased with the content of inorganic componentand UV curing time increasing. When the content of modified silicone sol (nTEOS: nMAPTMS=1:2) was30wt.%,1,6-hexanediol diacrylate was20wt.%, composite initiators (Irgacure184+TPO) was3wt.%, the gel time of HBPUA/(MAPTMS-SiO_2) hybrid coatings exceed180days.After UV curing for4min, hybrid coatings had optimal properties with transmittance of92.8%, pencil hardness of4H, adhesion of0degree, flexibility of3mm, impact strength of46kg·cm and abrasion resistance of only17.5mg.
本文以正硅酸乙酯和有机硅氧烷为先驱物，采用溶胶-凝胶法制备了性能良好的透明SiO_2/有机硅杂化材料。在此基础上，为提高SiO_2/有机硅杂化材料的耐碱性、对聚碳酸酯(PC)基材的粘结力和材料环保友好性，通过功能化改性或分子设计，分别制备了热固化型硅/胺杂化材料、聚酯/SiO_2/有机硅杂化材料和光固化型SiO_2/超支化聚氨酯丙烯酸酯杂化材料。系统研究了含硅杂化硬质薄膜的组成、结构与性能及其内在关系，主要研究成果如下：
1、以正硅酸乙酯(TEOS)为无机相前驱体，甲基三乙氧基硅烷(MTES)、二甲基二乙氧基硅烷(DMDES)和甲基丙烯酰氧基丙基三甲氧基硅烷(MAPTMS)为有机相前驱体，采用溶胶-凝胶法合成出热固化型SiO_2/有机硅杂化材料。确定了各组分的优化配比：n_(TEOS)∶n_(MTES)∶n_(DMDES)∶n_(MAPTMS)＝5∶5∶2∶2，n_(IPA)/n_(Si-OR)=0.8，n_(H2O)/n_(Si-OR)＝1.1，n_(HAc)/n_(Si-O)＝0.008，此条件下制备的杂化涂料可稳定存放360d。由于在高度交联的SiO_2网络中引入线性的Si—O—Si链段，而且有机和无机网络通过共价键结合起来，相容性良好，使得杂化薄膜既有高硬度又有良好的粘结力。按优化配比制备的杂化薄膜的铅笔硬度为2H，附着力为1级，透光率为93.6%。研究发现随着n(R)/n(Si)值减少，杂化材料的热稳定性增强。杂化薄膜对水的接触角随n(R)/n(Si)值的增大和固化时间的延长而增大，具有一定的疏水性。PC涂覆杂化膜层后具有更低的折射率，并且涂层表面光滑致密，从而减少了PC表面的漫反射，使得薄膜对PC具有增透作用。
2、氨基树脂的种类影响SiO_2/有机硅树脂的性能。氨基树脂中醇碳链增大，硅/胺杂化树脂的相分离程度增加；醚化度增加，相分离程度降低；氨基树脂用量增加，相分离程度先降低后增加。全甲醚化氨基树脂(HMMM)比部分甲醚化氨基树脂和丁醚化氨基树脂能获得硬度与柔韧性的更良好平衡和更优越耐久性。FTIR表明氨基树脂是利用—CH_2OCH_3与SiO_2/有机硅树脂的—OH发生交联反应。SiO_2/有机硅树脂经氨基树脂改性后，具有更为致密的无机-有机网状结构，NaOH等一些小分子不易渗透进去，起到了相当好的抗碱蚀作用。当HMMM的加入量为2wt.%时，与SiO_2/有机硅树脂的相容性最好，粒子形态规则，分散均匀，杂化薄膜在碱液中浸泡24h后，表面仍然平整，失光率最小，仅为0.43%。
3、合成一种带磺酸基团的聚酯树脂用于改性SiO_2/有机硅树脂，通过共聚和共混法制备了系列聚酯/SiO_2/有机硅杂化涂料。含有磺酸基的聚酯能改善与SiO_2/有机硅树脂的混溶性，极大提高对基材的附着力。聚酯/SiO_2/有机硅杂化涂料能在不经底涂处理的PC上铺展成膜。红外表明杂化薄膜中的－OH和－SO_3H等极性基团与PC基材表面的－C=O键之间发生了化学吸引和氢键耦合作用。两种工艺法都有聚酯链段接枝在SiO_2/有机硅树脂上，杂化树脂的粘度均随聚酯含量的提高而增大，但共聚法接枝的更多，得到的杂化树脂粘度高。共聚法比共混法产生更强的有机/无机相互作用，更高的交联密度，更高的热稳定性和更好的耐磨损性。共混杂化涂层微相分离的程度和表面粗糙度更大，一般可观测到明显的团聚体，而共聚杂化涂层只在聚酯含量较高时才观察到。共聚杂化样品的热分解近似为1级反应，用Ozawa法计算其在40%分解阶段的活化能约为243kJ/mol。XRD表明共聚杂化树脂属典型的非晶相。EDS表明硅相易迁移到杂化涂层的表面，极大地降低其表面能。采用共聚法比共混法得到的杂化涂层具有更低的表面能，其表面能随着SiO_2/有机硅树脂含量的增加而降低。共聚杂化膜比共混体系表现出较好的耐水性，其吸水率随SiO_2/有机硅树脂含量随量的加而降低。
4、以TEOS和MAPTMS制备的改性硅溶胶为无机组分，以自制的超支化聚氨酯丙烯酸酯(HBPUA)为有机组分，制备了一系列可UV固化的HBPUA/(MAPTMS-SiO_2)杂化涂料。超支化HBPUA/(MAPTMS-SiO_2)杂化材料中的无机和有机组分相容性很好，硅溶胶均匀地分布于有机相中，其储存稳定性明显好于线性PUA/(MAPTMS-SiO_2)杂化涂料。HBPUA/(MAPTMS-SiO_2)杂化膜经UV固化后变得致密透亮、无裂纹和明显的微相分离，但随无机组分用量增加，观察到SiO_2团聚颗粒。HBPUA/(MAPTMS-SiO_2)杂化涂膜的热稳定性和碳碳双键最终转化率比PUA/(MAPTM-SiO_2)杂化涂膜更高，其玻璃化转变温度随着无机组分用量的增加和UV固化时间的延长相应的增大。当以n_(SiO2):n_(MAPTMS)=1:2制备的改性硅溶胶用量为30wt.%，活性单体1,6己二醇二丙烯酸酯用量为20wt.%，复合引发剂(Irgacure184+TPO)用量为3wt.%时，HBPUA/(MAPTMS-SiO_2)杂化涂料的凝胶时间高于180d，UV固化4min后，薄膜性能最优，透光率为92.8%，铅笔硬度为4H，附着力为0级，柔韧性为3mm，冲击强度为46kg·cm，磨耗量为17.5mg。
Due to the low surface hardness, transparent plastic is easy to be scratched in use, whichmakes the loss of operation life and limits extended application. The surface scratch behaviorcan be reduced effectively through coating a hard protective film on it. The organic/inorganichard film can integrate good adhesion to substrate of organic film with excellent hardness ofinorganic film, which has become the hot study spot of hard film on plastic.
The transparent and hard SiO_2/organosilicone hybrid coatings were prepared onpolycarbonate(PC) with tetraethoxysilane and organosiloxane as the main raw materials bysol-gel method. In order to improve anti-alkali corrosion properties, adhesion andenvironmentally friendly of the SiO_2/organosilicone hybrid materials, heat-curablesilicone/amine hybrid materials, polyester/SiO_2/organosilicone hybrid materials and UVcurable SiO_2/hyperbranched polyurethane acrylate hybrid materials were preparedrespectively. The relationship of composition, structure and properties of hybrid hard filmswith silicon was studied systemically. The detailed research contents and results weredescribed as follows:
1. With tetraethoxysilane(TEOS) as inorganic precursor, methyltriethoxysilane(MTES),dimethyldiethoxysilane(DMDES) and3-(methacryloxypropyl)trimethoxysilane(MAPTMS)as organic precursor, the heat-curable SiO_2/organosilicone hybrid coatings was synthesized bysol-gel method. When the molar ratio of SiO_2/organosilicone hybrid coating was n_(TEOS):n_(MTES):n_(DMDES):n_(MAPTMS)=5:5:2:2, n_(IPA)/n_(Si-OR)=0.8, n_(H2O)/n_(Si-OR)=1.1, n_(HAc)/nSi-O=0.008, the gelation timeexceeded360days. The hybrid film had high hardness and good adhesion because linearSi-O-Si segmers were introduced into high-density crosslinked SiO_2network. The hybridfilms prepared in accordance with the optimized ratio had optimal properties withtransmittance of93.6%, pencil hardness of2H, adhesion of0degree. It was found that thehybrid coating had excellent thermal stability, which increases gradually with the decrease ofn(R)/n(Si) value. The contact angle of the hybrid coating to the water increased with theincrease of n(R)/n(Si) value and curing time. Higher light transmittance of hybrid coatingswas probably due to lower refractive index of hybrid coatings than that of the PC sheet. It wasalso considered that the hybrid coating reduces light reflection on the surface of the substrate.
2. The type of amine resin significantly affected the alkali resistance of the SiO_2/organo-silicone film. In comparison with part methoxymethyl and butoxymethyl melamine resin,Hexamethoxymethyl melamine resin(HMMM) had better durability and balance betweenhardness and flexibility for hybrid coatings. FTIR showed that the co-condensation betweenthe methoxymethyl groups in HMMM and the hydroxyl groups in SiO_2/organosilicone resin.The SiO_2/organosilicone resin formed more dense inorganic-organic network after HMMMmodified, resulted in NaOH and other small molecules not easy to penetrate into hybrid films.When the content of HMMM was2wt.%, SiO_2/organosilicone resin had best compatibilitywith HMMM and hybrid particles had regular morphology. The hybrid film was still smoothand had minimum transmittance loss of0.43%after immersion in NaOH solution for24h.
3. A series of polyester/SiO_2/organosilicone hybrid coatings were synthesized throughcopolymerization and blending method between SiO_2/organosilicone resin and sulfonicgroup-containing polyester made from carefully selected proper monomers in my ownlaboratory. The polyester containing strong polarity of the sulfonic group, which not only toimprove the compatibility with SiO_2/organosilicone resin, but also improve the adhesion toPC, resulted in polyester/SiO_2/organosilicone coatings could be spread on PC without primer.The grafting rate of co-polymerizable resin is greater than that of the blends. The viscosity ofco-polymerizable and blending hybrid resin increased with polyester content increasing. Incomparison with blending method, co-polymerizable method had much stronger interactionsbetween organic phases and inorganic phases, resulting in higher crosslinking density, higherthermal stability and wear resistance for hybrid coatings. The extent of microphase separationand the surface roughness of the blending coatings became bigger. Obvious agglomerateswere observed for the blending coatings while those agglomerates were only observed for theco-polymerizable coatings at relatively high polyester content. The thermal decompositionprocess of the co-polymerizable sample followed one-order kinetics with the higher activationenergy of243kJ/mol. XRD studies showed that the co-polymerizable materials wasamorphous. EDS analysis showed that the silica particles could move towards the surface ofco-polymerizable coatings to lower free energies. The co-polymerizable coating had a lowersurface energy and better water resistance than the blends, and its surface free energy andwater absorption decreased with increasing of SiO_2/organosilicone content.
4. The modified silicone sol from TEOS and MAPTMS were used as inorganiccomponents and hyperbranched polyurethane acrylate(HBPUA) were used as organiccomponents for preparing a series of UV-curable HBPUA/(MAPTMS-SiO_2) hybrid coatings.The results showed that HBPUA/(MAPTMS-SiO_2) hybrid films hand good interfacialcompatibility and SiO_2were well distributed in organic matrix. The stability ofHBPUA/(MAPTMS-SiO_2) hybrid coatings were higher than that of PUA/(MAPTMS-SiO_2)hybrid coatings. The HBPUA/(MAPTMS-SiO_2) hybrid film became transparent, dense, nocracks and microphase separation after UV curing. However, the gel particles of hybridcoatings increased with the content of inorganic component increasing. The terminalconversion degree of C=C bonds of HBPUA/(MAPTMS-SiO_2) hybrid coatings were higherand thermal stable was better than those of PUA/(MAPTMS-SiO_2) hybrid coatings. The TgofHBPUA/(MAPTMS-SiO_2) hybrid coatings increased with the content of inorganic componentand UV curing time increasing. When the content of modified silicone sol (nTEOS: nMAPTMS=1:2) was30wt.%,1,6-hexanediol diacrylate was20wt.%, composite initiators (Irgacure184+TPO) was3wt.%, the gel time of HBPUA/(MAPTMS-SiO_2) hybrid coatings exceed180days.After UV curing for4min, hybrid coatings had optimal properties with transmittance of92.8%, pencil hardness of4H, adhesion of0degree, flexibility of3mm, impact strength of46kg·cm and abrasion resistance of only17.5mg.
引文
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