纳米CeO_2制备及其对聚合物改性研究
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摘要
本文首次通过Ce(NO3)3·6H2O和三乙醇胺(TEA)反应合成Ce-TEA配合物晶体,以此配合物作为制备纳米CeO2粒子的前驱体,进一步水解制备纳米CeO2粒子。
研究表明,Ce-TEA配合物的化学式为[Ce((C2H5O)3N)(H2O)]NO3,其中Ce主要以+4价形式存在,即原料反应生成配合物期间Ce(III)被氧化成了Ce(Ⅳ)。配合物的形成使Ce(Ⅳ)离子在水溶液中的水解速率明显下降；当控制反应温度为25℃、TEA/Ce(NO3)3摩尔比为8：1、前驱体溶液浓度为0.067mol·L-1时,配合物均匀沉淀生成水合CeO2,将沉淀于室温下(25℃)在水介质中进一步老化,获得结晶度较高的纳米CeO2粒子。借助XRD, HRTEM和SAED分析表明,得到的纳米Ce02粒子具有完整的立方晶型结构,平均粒径为5-6nm,近似球形,团聚程度小,粒径分布窄,单分散性好。XPS分析表明,CeO2晶格中铈主要以Ce4+形式存在。
研究表明,水介质中室温下沉淀老化工艺可替代常规高温焙烧过程,CeO2沉淀可进一步脱水、晶化,获得高结晶度的纳米CeO2粒子。
三乙醇胺均匀沉淀法、氨水沉淀法和六次甲基四胺均匀沉淀法比较发现,三者制备的纳米CeO2粒子粒径相差不大,但三乙醇胺均匀水解法制备的纳米CeO2粒子单分散性要优于其它两种方法。研究发现,Ce(IV)-TEA配合物均匀水解法是一种制备单分散纳米Ce02晶体粒子的有效方法。
课题还进一步研究了稀土元素钇(Y)对纳米Ce02粒子改性效果及水解释放的三乙醇胺对Ce02粒子表面原位有机化改性效果。研究表明,室温下通过Ce-Y-TEA配合物的均匀沉淀,可制备Cel-xYx02-x/2(X≤0.4)纳米水分散液。增加Y元素的含量可以提高Y掺杂Ce02纳米分散液的稳定性、抗紫外光能力和可见光区的透明度；当Y元素含量达到40m01%时,可以形成稳定的溶胶,溶胶粒子为晶体粒子,其平均粒径为4-5nm,且粒度分布狭窄,Y元素已完全进入Ce02晶格；该溶胶具有优异的紫外吸收性能,在可见光区有很高的透明度,其在高分子树脂清漆、护肤化妆品和其它光学涂层等透明性要求高的工业和民用领域有潜在的应用价值。
研究进一步表明,当控制三乙醇胺含量不过量,由单-Ce(IV)-TEA配合物直接水解也能获得粒径为5～6nm的纳米Ce02粒子,并且当水解温度在50～70℃时,随着Ce02粒子的生成,前驱体中水解释放的三乙醇胺分子在Ce02粒子表面产生化学吸附,其吸附量达3.0wt%左右,使粒子的亲油性明显提高,可实现Ce02粒子的原位表面有机化改性。
为了进一步提高纳米粒子分散性,我们还在制备纳米粒子的水解液中加入甲基丙烯酸甲酯(MMA)和苯乙烯(St)两种高分子单体,前驱体水解完成后在同一反应液中引发单体聚合,制备粒子包埋于聚甲基丙烯酸甲酯(PMMA)和聚苯乙烯(PS)基质中的“纳米Ce02/PMMA"和“纳米Ce02/PS”有机-无机复合材料(粉末)
研究发现,生成的纳米CeO2晶体粒子在PMMA和PS基体中分散比较均匀,PMMA的热稳定性和玻璃化温度均得到提高,说明纳米粒子与聚合物分子间发生了相互作用。研究表明,纳米CeO2可以提高PMMA的紫外吸收性能和拉伸强度。同样,采用20mol%Y元素掺杂的纳米CeO2可以显著提高“纳米CeO2/PMMA"复合材料的可见光透过率。
本课题研究制备的“纳米CeO2/PMMA"和“纳米CeO2/PS"有机-无机复合材料在涂层材料、膜材料及其它光学材料中具有良好的潜在应用价值。
A novel cerium-triethanolamine(TEA) complex crystal was obtained through the reaction of cerium(III) nitrate and triethanolamine. It was used as the precursor to synthesize CeO2nanoparticles, i.e., it hydrolysized homogeneously to produce CeO2nanoparticles.
The molecular formula of the cerium-TEA complex was deduced to be [Ce((C2H5O)3N)(H2O)]NO3, wherein tetravalent cerium was predominante, i.e., spontaneous oxidation of cerium(III) to cerium(IV) by oxygen took place in the synthesis process of the complex. Hydrolysis of cerium(IV) cation was slown down substantially by the coordination, which facilitated the generation of a hydrated CeO2precipitate under such optimizated condition as hydrolysis temperature of25℃, concentration of0.067mol-L-1for the precursor solution and TEA/Ce(NO3)3molar ratio of8. The hydrated CeO2precipitate can be transformed finally to CeO2nanoparticles with higher crystallinity via being aged further in water at room temperature. The obtained particles showed uniform size distribution with an mean particle size of5-6nm, which was observed by transmission electron microscopy (TEM). X-ray diffraction (XRD) as well as high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) gave evidence that all of the as-synthesized nanoparticles were well crystalline in the cubic fluorite structure. X-ray photoelectron spectroscopy(XPS) demonstrated that cerium in CeO2was tetravalent.
According to the results, the age process in aqueous media can substitute for the calcination at high temperature for the further dehydration and crystallization of the hydrated CeO2precipitate.
CeO2nanoparticle prepared in this study showed near identical size with those prepared by the precipitation method using hexamethylenetetramine and ammonia, but its monodispersion was more excellent. The results indicated that the homogeneous precipitation method using Ce-TEA complex is an effective method to prepare monodispersed CeO2nanoparticles.
In this study, property-modification effect of CeO2nanoparticles by the element yttrium(Y) and organic modification effect of the particles by the TEA realeased from the hydrolysis were also investigated.
The results indicated that the homogeneous precipitation method using Ce-Y-TEA complex is effective to prepare Ce1-xYxO2-x/2(x≤0.4) nanoparticle aqueous dispersion. The as-synthesized nanoparticles were well crystalline. Yttrium was dopped into CeO2lattice and the dispersion stability, UV shielding ability and high transparency in visible light region were improved with the increase of yttrium content. When x=0.4, a sol was achieved and it showed an mean particle size of4-5nm and possessed excellent UV shielding ability and high transparency in visible light region. The obtained sol had potential applications in industrial or civil fields with high transparency being required such as acrylic varnishes, personal care products and other optical coatings.
The results further indicated that under no excess TEA, the Ce-TEA complex can also hydrolysis directly to generate CeO2with particle size of5-6nm. Moreover, along with the hydrolysis at50～70℃, chemical adsorption onto the nanoparticles for the TEA released from the precursor would occurr, and the adsorption capacity was about3.0wt%, which improved greatly the lipophilicity of CeO2nanoparticles and can fulfill in situ organic surface-modification of the nanoparticles.
In order to further enhance the dispersion stability and inhibit the aggregate, the monomer such as methylmethacrylate(MMA) and styrene(St) were introduced into the feed aqueous solution for hydrolysis respectively. The polymerization of the monomer was initiated after the hydrolysis in one pot, and a nano-CeO2/PMMA as well as nano-CeO2/PS organic-inorganic composite were achieved respectively.
The results showed that CeO2nanoparticles were embedded into the polymethylmethacrylate (PMMA) and polystyrene(PS) matrix of the composite and dispersed homogeneously. For the obtained composite, The thermal stability and the glass transition temperature of PMMA were enhanced, which indicated the formation of the bond between the nanoparticles and the polymer chains. Moreover, under some range of the weight content, CeO2nanoparticles can improve the UV absorption ability and tensile strengh of the PMMA. Meantime, the dopping of20mol%yttrium can improve greatly the transparency in visible light region of the CeO2/PMMA composite.
The prepared nano-CeO2/PMMA and nano-CeO2/PS organic-inorganic composite powders in this study had potential applications in film, coating materials and other optical materials.
研究表明,Ce-TEA配合物的化学式为[Ce((C2H5O)3N)(H2O)]NO3,其中Ce主要以+4价形式存在,即原料反应生成配合物期间Ce(III)被氧化成了Ce(Ⅳ)。配合物的形成使Ce(Ⅳ)离子在水溶液中的水解速率明显下降；当控制反应温度为25℃、TEA/Ce(NO3)3摩尔比为8：1、前驱体溶液浓度为0.067mol·L-1时,配合物均匀沉淀生成水合CeO2,将沉淀于室温下(25℃)在水介质中进一步老化,获得结晶度较高的纳米CeO2粒子。借助XRD, HRTEM和SAED分析表明,得到的纳米Ce02粒子具有完整的立方晶型结构,平均粒径为5-6nm,近似球形,团聚程度小,粒径分布窄,单分散性好。XPS分析表明,CeO2晶格中铈主要以Ce4+形式存在。
研究表明,水介质中室温下沉淀老化工艺可替代常规高温焙烧过程,CeO2沉淀可进一步脱水、晶化,获得高结晶度的纳米CeO2粒子。
三乙醇胺均匀沉淀法、氨水沉淀法和六次甲基四胺均匀沉淀法比较发现,三者制备的纳米CeO2粒子粒径相差不大,但三乙醇胺均匀水解法制备的纳米CeO2粒子单分散性要优于其它两种方法。研究发现,Ce(IV)-TEA配合物均匀水解法是一种制备单分散纳米Ce02晶体粒子的有效方法。
课题还进一步研究了稀土元素钇(Y)对纳米Ce02粒子改性效果及水解释放的三乙醇胺对Ce02粒子表面原位有机化改性效果。研究表明,室温下通过Ce-Y-TEA配合物的均匀沉淀,可制备Cel-xYx02-x/2(X≤0.4)纳米水分散液。增加Y元素的含量可以提高Y掺杂Ce02纳米分散液的稳定性、抗紫外光能力和可见光区的透明度；当Y元素含量达到40m01%时,可以形成稳定的溶胶,溶胶粒子为晶体粒子,其平均粒径为4-5nm,且粒度分布狭窄,Y元素已完全进入Ce02晶格；该溶胶具有优异的紫外吸收性能,在可见光区有很高的透明度,其在高分子树脂清漆、护肤化妆品和其它光学涂层等透明性要求高的工业和民用领域有潜在的应用价值。
研究进一步表明,当控制三乙醇胺含量不过量,由单-Ce(IV)-TEA配合物直接水解也能获得粒径为5～6nm的纳米Ce02粒子,并且当水解温度在50～70℃时,随着Ce02粒子的生成,前驱体中水解释放的三乙醇胺分子在Ce02粒子表面产生化学吸附,其吸附量达3.0wt%左右,使粒子的亲油性明显提高,可实现Ce02粒子的原位表面有机化改性。
为了进一步提高纳米粒子分散性,我们还在制备纳米粒子的水解液中加入甲基丙烯酸甲酯(MMA)和苯乙烯(St)两种高分子单体,前驱体水解完成后在同一反应液中引发单体聚合,制备粒子包埋于聚甲基丙烯酸甲酯(PMMA)和聚苯乙烯(PS)基质中的“纳米Ce02/PMMA"和“纳米Ce02/PS”有机-无机复合材料(粉末)
研究发现,生成的纳米CeO2晶体粒子在PMMA和PS基体中分散比较均匀,PMMA的热稳定性和玻璃化温度均得到提高,说明纳米粒子与聚合物分子间发生了相互作用。研究表明,纳米CeO2可以提高PMMA的紫外吸收性能和拉伸强度。同样,采用20mol%Y元素掺杂的纳米CeO2可以显著提高“纳米CeO2/PMMA"复合材料的可见光透过率。
本课题研究制备的“纳米CeO2/PMMA"和“纳米CeO2/PS"有机-无机复合材料在涂层材料、膜材料及其它光学材料中具有良好的潜在应用价值。
A novel cerium-triethanolamine(TEA) complex crystal was obtained through the reaction of cerium(III) nitrate and triethanolamine. It was used as the precursor to synthesize CeO2nanoparticles, i.e., it hydrolysized homogeneously to produce CeO2nanoparticles.
The molecular formula of the cerium-TEA complex was deduced to be [Ce((C2H5O)3N)(H2O)]NO3, wherein tetravalent cerium was predominante, i.e., spontaneous oxidation of cerium(III) to cerium(IV) by oxygen took place in the synthesis process of the complex. Hydrolysis of cerium(IV) cation was slown down substantially by the coordination, which facilitated the generation of a hydrated CeO2precipitate under such optimizated condition as hydrolysis temperature of25℃, concentration of0.067mol-L-1for the precursor solution and TEA/Ce(NO3)3molar ratio of8. The hydrated CeO2precipitate can be transformed finally to CeO2nanoparticles with higher crystallinity via being aged further in water at room temperature. The obtained particles showed uniform size distribution with an mean particle size of5-6nm, which was observed by transmission electron microscopy (TEM). X-ray diffraction (XRD) as well as high resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED) gave evidence that all of the as-synthesized nanoparticles were well crystalline in the cubic fluorite structure. X-ray photoelectron spectroscopy(XPS) demonstrated that cerium in CeO2was tetravalent.
According to the results, the age process in aqueous media can substitute for the calcination at high temperature for the further dehydration and crystallization of the hydrated CeO2precipitate.
CeO2nanoparticle prepared in this study showed near identical size with those prepared by the precipitation method using hexamethylenetetramine and ammonia, but its monodispersion was more excellent. The results indicated that the homogeneous precipitation method using Ce-TEA complex is an effective method to prepare monodispersed CeO2nanoparticles.
In this study, property-modification effect of CeO2nanoparticles by the element yttrium(Y) and organic modification effect of the particles by the TEA realeased from the hydrolysis were also investigated.
The results indicated that the homogeneous precipitation method using Ce-Y-TEA complex is effective to prepare Ce1-xYxO2-x/2(x≤0.4) nanoparticle aqueous dispersion. The as-synthesized nanoparticles were well crystalline. Yttrium was dopped into CeO2lattice and the dispersion stability, UV shielding ability and high transparency in visible light region were improved with the increase of yttrium content. When x=0.4, a sol was achieved and it showed an mean particle size of4-5nm and possessed excellent UV shielding ability and high transparency in visible light region. The obtained sol had potential applications in industrial or civil fields with high transparency being required such as acrylic varnishes, personal care products and other optical coatings.
The results further indicated that under no excess TEA, the Ce-TEA complex can also hydrolysis directly to generate CeO2with particle size of5-6nm. Moreover, along with the hydrolysis at50～70℃, chemical adsorption onto the nanoparticles for the TEA released from the precursor would occurr, and the adsorption capacity was about3.0wt%, which improved greatly the lipophilicity of CeO2nanoparticles and can fulfill in situ organic surface-modification of the nanoparticles.
In order to further enhance the dispersion stability and inhibit the aggregate, the monomer such as methylmethacrylate(MMA) and styrene(St) were introduced into the feed aqueous solution for hydrolysis respectively. The polymerization of the monomer was initiated after the hydrolysis in one pot, and a nano-CeO2/PMMA as well as nano-CeO2/PS organic-inorganic composite were achieved respectively.
The results showed that CeO2nanoparticles were embedded into the polymethylmethacrylate (PMMA) and polystyrene(PS) matrix of the composite and dispersed homogeneously. For the obtained composite, The thermal stability and the glass transition temperature of PMMA were enhanced, which indicated the formation of the bond between the nanoparticles and the polymer chains. Moreover, under some range of the weight content, CeO2nanoparticles can improve the UV absorption ability and tensile strengh of the PMMA. Meantime, the dopping of20mol%yttrium can improve greatly the transparency in visible light region of the CeO2/PMMA composite.
The prepared nano-CeO2/PMMA and nano-CeO2/PS organic-inorganic composite powders in this study had potential applications in film, coating materials and other optical materials.
引文
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