王平美,何玫莹,贾新利,肖沛文,罗健辉,江波.树莓形SiO2–TiO2纳米粒子的制备及其在光学涂层中的应用[J].表面技术,2022,51(6):374-381.
WANG Ping-mei,HE Mei-ying,JIA Xin-li,XIAO Pei-wen,LUO Jian-hui,JIANG Bo.Synthesis of Raspberry-like SiO2-TiO2 Nanoparticles and the Application in Optical Films[J].Surface Technology,2022,51(6):374-381
树莓形SiO2–TiO2纳米粒子的制备及其在光学涂层中的应用
Synthesis of Raspberry-like SiO2-TiO2 Nanoparticles and the Application in Optical Films
  
DOI:10.16490/j.cnki.issn.1001-3660.2022.06.036
中文关键词:  树莓形纳米粒子  Stöber法  溶胶–凝胶法  光学薄膜  自清洁性能  机械稳定性
英文关键词:raspberry-like  Stöber method  sol-gel method  optical coatings  self-cleaning  mechanical robust
基金项目:中国石油天然气股份有限公司科学研究与技术开发项目(2018A–0907,2020D–5006–82)
作者单位
王平美 中国石油勘探开发研究院,北京 100083;中国石油天然气集团有限公司 纳米化学重点实验室,北京 100083 
何玫莹 四川大学 化学学院 绿色化学与技术教育部重点实验室,成都 610064 
贾新利 四川大学 化学学院 绿色化学与技术教育部重点实验室,成都 610064 
肖沛文 中国石油勘探开发研究院,北京 100083;中国石油天然气集团有限公司 纳米化学重点实验室,北京 100083 
罗健辉 中国石油勘探开发研究院,北京 100083;中国石油天然气集团有限公司 纳米化学重点实验室,北京 100083 
江波 四川大学 化学学院 绿色化学与技术教育部重点实验室,成都 610064 
AuthorInstitution
WANG Ping-mei Research Institute of Petroleum Exploration & Development, PetroChina, Beijing 100083, China;Key Laboratory of Nano Chemistry KLNC, CNPC, Beijing 100083, China 
HE Mei-ying Key Laboratory of Green Chemistry & Technology, Ministry of Education, College of Chemistry, Sichuan University, Chengdu 610064, China 
JIA Xin-li Key Laboratory of Green Chemistry & Technology, Ministry of Education, College of Chemistry, Sichuan University, Chengdu 610064, China 
XIAO Pei-wen Research Institute of Petroleum Exploration & Development, PetroChina, Beijing 100083, China;Key Laboratory of Nano Chemistry KLNC, CNPC, Beijing 100083, China 
LUO Jian-hui Research Institute of Petroleum Exploration & Development, PetroChina, Beijing 100083, China;Key Laboratory of Nano Chemistry KLNC, CNPC, Beijing 100083, China 
JIANG Bo Key Laboratory of Green Chemistry & Technology, Ministry of Education, College of Chemistry, Sichuan University, Chengdu 610064, China 
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中文摘要:
      目的 提高TiO2纳米粒子在复合光学薄膜中的分散性及光催化自清洁效率。方法 以通过Stöber法制备的粒径为70、140 nm的SiO2粒子与酸催化法制备的粒径为5 nm的TiO2粒子为原料,分别使用硅烷偶联剂3–氨丙基三乙氧基硅烷(APTES,或KH550)与γ–缩水甘油醚氧丙基三乙氧基硅烷(GLYMO,或KH560)对2种纳米粒子进行表面改性。通过2种粒子表面的化学基团之间的化学键,将2种粒子进行偶联,形成了小粒子包覆大粒子的树莓形结构,并利用溶胶–凝胶法制备了光学涂层,通过紫外–可见分光光度计、红外光谱仪、激光粒度仪等多种表征设备对制备的复合纳米粒子及构筑的薄膜的结构、形貌和性能进行了分析。结果 粒径较小的TiO2纳米粒子通过表面基团的反应均匀地包覆在粒径较大的TiO2纳米粒子表面形成树莓形的复合结构,构筑的薄膜具有较高的透光率(>90%),较好地保留了玻璃基底的透过率,在紫外辐照条件下可在120 min内完全降解有机污染物,具有高效的光催化自清洁功能。水接触角测试表明,膜层表面具有较高的亲水性,其接触角最低可达2.68°,因此具有较好的防雾性能。此外,膜层的透过率在耐摩擦试验中表现出较高的稳定性,摩擦测试前后透过率变化在1.0%以内。结论 通过表面基团偶联的方法成功制备了树莓形复合纳米粒子,以该粒子构筑的涂层材料兼具透光性、高效光催化自清洁性以及防雾性能,并且具有良好的机械强度。
英文摘要:
      It is an novel method to synthesis SiO2-TiO2 composite nanoparticles with raspberry-like structure, which constructed multifunctional films with properties of high light transmittance, anti-fogging, photocatalytic self-cleaning, as well as mechanical robustness. Since titania is of good performance in photocatalytic self-cleaning, it is widely used in the preparation of functional surface coatings. However, dense titania has high refractive index and nano-titania is easy to agglomerate, resulting in poor optical transmission properties and photocatalytic self-cleaning effective of surface coatings prepared with titania. To solve this problem, a composite nanostructure was created to improve the dispersing stability and photocatalytic effective of small titania nanospheres in optical films. In this paper, SiO2 nanospheres with sizes of 70 nm and 140 nm were synthesized through Stöber method, and 5 nm TiO2 nanospheres were prepared under acid catalysis. SiO2 nanospheres were modified by hexamethyldisilane (HMDS) and then decorated by (3-aminopropyl) triethoxysilane (APTES, or KH550) to graft amino groups on surfaces. TiO2 nanospheres were modified by γ-glycidoxy-propyltrimethoxysilane (GLYMO, or KH560) to graft epoxy groups on surfaces. followed by silica-titania composite nanoparticles with raspberry-like morphology were fabricated via the assembly of silica nanospheres and hydrophilic titania nanoparticles through chemical interactions between amino groups and epoxy groups. Then, optical films were prepared through dip-coating met hod by using raspberry-like SiO2-TiO2 nanoparticles as building blocks. By wrapping around SiO2 nanospheres, small TiO2 spheres can be uniformly distributed in the film without agglomeration, thus more chemical activity can be retained. Characterization instruments such as DLS, TEM, EDX, XRD, UV-vis spectrophotometer, Infrared spectrometer were involved to analyze the structure, morphology, properties and performances of raspberry-like particles and optical films they built. As the results, raspberry-like morphology was successfully prepared since SiO2 nanospheres with larger size were covered evenly by smaller TiO2 nanospheres. The optical films built by SiO2-TiO2 nanoparticles have a high transmittance, which is more than 90%, thus the light transmission of substrates was largely reserved. Organic contaminants on the films can be totally degraded within 120 min under UV illumination. The water contact angles of films were as low as 2.68°, which means the films were superhydrophilic, water drops can spread rapidly on the surface, thus they have a good performance in anti-fogging. Furthermore, films exhibited a strong adhesion to the substrates and a good friction resistance, transmittance of films showed a high stability after abrasion-resistant testing, only 1.0% decrease on average. Briefly, raspberry-like SiO2-TiO2 nanoparticles were synthesized successfully through surface-connection between SiO2 and TiO2 nanospheres and as building blocks to form optical films which can provide a high light transmittance, photocatalytic self-cleaning property for the substrates, and also have a good performance in mechanical robustness, therefore, these films can perform well in outdoor application with harsh conditions. Also, in this work, an advanced preparation method of SiO2-TiO2 hybrid films was created, the whole preparation process was carried out under mild conditions, which avoids the influences of high temperature calcination for template removal and chemical corrosion on the performance of optical substrates, as well as high energy consumption and environmental pollution, which is in line with the concept of environmentally friendly and sustainable development.
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