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1.
用改进的种子法合成SiO2微球. 微球生长过程中连续缓慢添加正硅酸乙酯,使用动态光散射法实时监控微球粒径的增长过程,调节正硅酸乙酯的添加,实现对粒径的精确控制. 为制备禁带位置位于1000 nm 的光子晶体,合成粒径为446 nm的SiO2微球,微球粒径在4 h内从193 nm 增长到446 nm,远远快于传统种子法,微球粒径与目标粒径偏差为±5 nm. 制得的SiO2微球被组装为光子晶体,其禁带位置恰好位于1000 nm.  相似文献   

2.
 以氨水作催化剂、正硅酸乙酯为硅源、乙醇为溶剂,采用改进溶胶-凝胶法制备了系列单分散SiO2微球,研究了平均粒径为250,280,320 nm单分散SiO2微球在水、无水乙醇、丙酮等介质中的沉降与自组装过程。还对单分散体系重力沉降组装欧泊模板的形成机理进行了讨论。SEM表明,微球在无水乙醇和丙酮沉降介质中均能组装形成3维有序密堆积结构的欧泊,但在无水乙醇中要优于在丙酮中。沉降速度实验表明,相同粒径的单分散SiO2微球在水、乙醇、丙酮作为沉降介质中的沉降速度相差并不大,沉降介质对重力水平沉降组装模板的影响主要是由于其表面张力与粘度不同造成的。  相似文献   

3.
利用聚乙烯亚胺(PEI)修饰的碳酸钙仿生模板合成了具有3D花朵型形貌的SiO2微球.通过调整碳酸钙微粒表面不同浓度PEI的吸附量实现SiO2微球的形貌控制呈现花朵或刀锋的形状. 用XPS和SEM对制备的SiO2微粒进行表征. 结果表明,不用浓度的PEI修饰可以较好地控制3花朵型DSiO2微球的形貌.  相似文献   

4.
通过种子乳液聚合合成核壳结构的聚甲基丙烯酸甲酯/聚苯乙烯(PMMA/PS)复合微球,通过酸碱溶胀法进一步制备出次微米级的PS中空微球. 将此中空微球作为微反应器,使在ZnO纳米粒子前驱体溶液中溶胀, 最终ZnO纳米粒子在PS中空微球中原位生成. 实验表明, 组成ZnO纳米粒子前驱体溶液的两种组 分(CH3COO)2Zn和LiOH的滴加顺序不同对最终生成的ZnO纳米粒子的尺寸和负载效率有很大的影响,但并不改变ZnO纳米粒子的晶型. 复合物的光致发光和UV-Vis吸  相似文献   

5.
 分别以丙醇锆和正硅酸乙酯为原料,采用溶胶-凝胶工艺制备了性能稳定的ZrO2和SiO2溶胶。用旋转镀膜法在K9玻璃上分别制备了单层SiO2薄膜、单层ZrO2薄膜、ZrO2/ SiO2双层膜和SiO2/ZrO2双层膜。采用原子力显微镜观察了薄膜的表面形貌,用椭偏仪测量薄膜的厚度与折射率,用紫外-可见光分光光度计测量了薄膜的透射率。对薄膜的透射光谱和椭偏仪模拟的数据进行分析,发现SiO2/ZrO2双层膜之间的渗透十分明显,而ZrO2/SiO2双层膜之间几乎不发生渗透。利用TFCalc模系设计软件,采用三层膜模型对薄膜的透射率进行模拟,得出的透射曲线与用紫外-可见光分光光度计测量的透射曲线十分符合。  相似文献   

6.
 以正硅酸乙酯(TEOS)为硅源,采用酸碱二步催化溶胶-凝胶法,结合超临界干燥技术制备了超低密度SiO2气凝胶,最低密度为3.4 mg/cm3;进一步结合成型工艺,在解决了模具设计和脱模技术后制备了具有不同密度的柱状和微型套筒样品,密度10~50 mg/cm3。研究了水、催化剂、稀释剂对二步溶胶-凝胶过程的影响,获得了制备低密度SiO2气凝胶的最佳条件。利用扫描电镜、孔径分布及比表面积测试仪等对SiO2气凝胶微结构进行了研究。结果表明,获得的超低密度SiO2气凝胶具有较好的纳米网络,平均孔径18.9 nm,还具有高比表面积898 9 m2/g。  相似文献   

7.
 以正硅酸乙酯和丙醇锆为前驱体,用溶胶-凝胶法在K9基片上提拉镀制SiO2/ZrO2双层膜。采用不同实验步骤制备了2个样品,样品1镀完SiO2后直接镀ZrO2 ,样品2镀完SiO2经热处理后再镀ZrO2。采用原子力显微镜、椭偏仪、紫外-可见分光光度计对薄膜进行表征。针对SiO2/ZrO2双层膜,考虑到膜间渗透的影响,采用3层Cauchy模型进行椭偏模拟,椭偏参数的模拟值曲线与椭偏仪的测量值曲线十分吻合,进而发现热处理可以使SiO2/ZrO2双层膜之间的渗透减少近23 nm,从而提高其峰值透射率。利用输出波长1.064 mm,脉宽8.1 ns的激光束对样品进行了损伤阈值的测试,用光学显微镜观察损伤形貌,结果发现两者损伤阈值分别为13.6 J/c2和14.18 J/cm2,均为膜的本征损伤。  相似文献   

8.
 以正硅酸乙酯作为前驱体,利用碱催化方式制备了SiO2溶胶,采用提拉法在K9基片上镀制SiO2单层薄膜,分别用热处理、紫外辐射处理、氨水加六甲基二硅胺烷气氛处理和酸碱复合膜4种后处理法对膜层进行处理,采用分光光度计、红外光谱、扫描探针显微镜、静滴接触角测量仪、椭偏仪等分析了薄膜的特性,通过真空环境加速污染实验对处理前后的膜层进行抗污染能力对比,结果表明:在碱性SiO2膜层上加镀一层酸性SiO2膜的复合膜层整体透过率仍保持在99%以上,疏水角达到128°,膜层真空抗污染能力大大加强。  相似文献   

9.
改性SiO2气凝胶制备及其在ICF实验中的应用   总被引:6,自引:4,他引:2       下载免费PDF全文
 以正硅酸乙酯(TEOS)为前驱体,采用酸碱两步催化法制备了SiO2醇凝胶。醇凝胶分别经过TEOS母液、甲基三乙氧基硅烷(MTEOS)处理后,以六甲基二硅胺烷(HMDSA)为疏水改性试剂,制备了改性SiO2醇凝胶,醇凝胶经溶剂交换后以CO2作为干燥介质,采用超临界干燥法制备了密度在30~100 mg/cm3的SiO2气凝胶。用傅里叶变换红外光谱仪(FTIR)对疏水性SiO2气凝胶进行了研究。研究结果表明,经过改性的气凝胶在潮湿环境中具有极好的尺寸稳定性和疏水性。采用精密车床加工得到了满足惯性约束聚变(ICF)物理试验要求的微柱。  相似文献   

10.
采用Adler法合成了5-(4-氨基苯基)-10,15,20-三苯基卟啉铜配合物(CuAPTPP),通过甲苯二异氰酸酯(TDI)的桥联作用对TiO2微球进行表面修饰,使TDI分子中的两个活性TDI基团分别与TiO2表面的羟基和CuAPTPP的氨基反应,将CuAPTPP敏化剂分子以化学键合的方式固定在TiO2表面,形成光催化微球CuAPTPP-TDI-TiO2.通过FT-IR、XRD、SEM、EA、UV-Vis和DRS等测试手段对CuAPTPP-TDI-TiO2进行结构表征.讨论了桥联分子TDI修饰量对光催化微球性能的影响,确定了TDI与TiO2的最佳摩尔比.以亚甲基蓝(MB)为降解对象,考察了CuAPTPP-TDI-TiO2微球的可见光催化性能.结果表明,桥联分子TDI在CuAPTPP与TiO2微球表面形成了牢固的化学键,复合微球在150 W氙灯辐照下降解10 mg/LMB溶液,120 min降解率可达98.7%,其降解率过程服从一级动力学规律,测得降解速率常数为5.1×10-2 min-1,半衰期为11.3 min.催化微球在回收4次的条件下,对MB的降解率仍保持在90%以上.  相似文献   

11.
Fluorinated TiO2 hollow microspheres with three-dimensional hierarchical architecture were prepared by solvothermally treatment using solid microspheres as precursor. The obtained solid and hollow TiO2 microspheres were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET), X-ray photoelectron spectroscopy (XPS), UV-Vis diffuse reflectance spectrum (DRS) and photoluminescence (PL) spectra. The photocatalytic activity of as-prepared solid and hollow TiO2 microspheres was determined by degradation of methyl orange (MO) under visible light irradiation. The results showed that the surface fluorination, the existence of accessible mesopores channels, and the increased light harvesting abilities could remarkably improve the photocatalytic activity of TiO2 hollow microspheres.  相似文献   

12.
This work reported basically aims at understanding the extent of SiO2-coated carbon nanofibers using two different sol-gel precursors for the silicate glass. The silicate precursors employed were tetraethoxysilane (TEOS) and pre-hydrolysed ethyl silicate. The first route consisted in an acid hydrolysis and polycondensation of the TEOS and the second one in a polycondensation of the pre-hydrolysed ethyl silicate. The techniques of Fourier Infra Red spectroscopy, thermogravimetric analysis, scanning electron microscopy and X-ray diffraction were used to characterize the materials obtained. Both kinds of SiO2 precursor can coat the CNF effectively. However, the use of pre-hydrolysed ethyl silicate (faster gelation times and higher surface areas) can be considered a low-cost and facile alternative with respect to the use of TEOS, to obtain industrially silica-coated carbon nanofibers.  相似文献   

13.
We present a strategy to synthesize porous BaSnO3 hollow architectures with that were 150-300 nm in diameter and 1.5-5 μm in length using precursor of BaCO3@SnO2 nanorods prepared by hydrothermal treatment. BaCO3@SnO2 nanorods, consisting of a BaCO3 core and a SnO2 shell, could be used effectively for the solid-state synthesis of polycrystalline BaSnO3 powder at 800 °C (lower than convention for BaCO3 and SnO2 mixtures). The core/shell structure of the precursor could play a role as a structural directing template for preparing BaSnO3 hollow architectures during the calcination process. The X-ray diffractometer (XRD), scanning electron microscope (SEM), and transmission electron microscope (TEM) are employed to characterize the structures and morphologies. When applied to DSSC, the porous BaSnO3 hollow architectures exhibit distinct photovoltaic effect.  相似文献   

14.
Novel egg-shell structured monometallic Pd/SiO2 and bimetallic Ca-Pd/SiO2 catalysts were prepared by an impregnation method using porous hollow silica (PHS) as the support and PdCl2 and Ca(NO3)2·4H2O as the precursors. It was found from transmission electron microscope (TEM), scanning electron microscope (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) that Pd was loaded on PHS with a particle size of 5-12 nm in Pd/SiO2 samples and the Pd particle size in Ca-Pd/SiO2 was smaller than that in Pd/SiO2 since Ca could prevent Pd particles from aggregating. X-ray photoelectron spectroscopy (XPS) analyses exhibited that Pd 3d5/2 binding energies of Pd/SiO2 and Ca-Pd/SiO2 were 0.2 and 0.9 eV lower than that of bulk Pd, respectively, as a result of the shift of the electron cloud from Pd to oxygen in Pd/SiO2 and to both oxygen and Ca in Ca-Pd/SiO2. The activity of Ca-Pd/SiO2 egg-shell catalyst for CO hydrogenation and the selectivity to methanol, with a value of 36.50 mmolCO mol−1Pd s−1 and 100%, respectively, were much higher than those of the catalysts prepared with traditional silica gel as the support, owing to the porous core-shell structure of the PHS support.  相似文献   

15.
A new type of multicoated silica/zirconia/silver (SiO2/ZrO2/Ag) core-shell composite microspheres is synthesized in this paper. In the process, ZrO2-decorated silica (SiO2/ZrO2) core-shell composites were firstly fabricated by the modification of zirconia on silica microspheres through the hydrolysis of zirconium precursor. Subsequently, on SiO2/ZrO2 composite cores, silver nanoparticles were introduced via ultrasonic irradiation and acted as “Ag seeds” for the formation of integrate silver shell by further reduction of silver ions using formaldehyde as reducer. The resulting samples were characterized by transmission electron microscopy, X-ray diffraction, Fourier-transform infrared, energy-dispersive X-ray, and UV-vis spectroscopy, indicating that zirconia and silver layers were successfully coated on the surfaces of silica microspheres.  相似文献   

16.
Mn2+-doped Zn2SiO4 phosphors had been prepared by hydrothermal method in stainless-steel autoclaves. Effects of synthesized methods, reaction temperature, ambience of heat treatment on the structure and the luminescence properties of this silicate were studied with X-ray diffraction apparatus (XRD), transmission electron microscope (TEM), scanning electron microscope (SEM) and fluorescence spectrum. Results show that Zn2SiO4 nanocrystalline can be obtained by hydrothermal method at relatively low temperatures. The absorption pattern shows an absorption edge at about 380 nm originated from ZnO crystals and two absorption bands at about 215 and 260 nm. Mn2+-doped Zn2SiO4 has a luminescence band with the wavelength at about 522 nm under 255 nm excitation, and the luminescent intensity increases after being heat treated.  相似文献   

17.
朱永政  尹计秋  邱明辉 《物理学报》2008,57(12):7725-7728
利用胶体自组装、高温烧结和HF酸刻蚀技术,制备了SiO2微球非密堆积面心立方(FCC)结构的胶体晶体,并以此为模板,利用溶胶凝胶方法和NaOH湿法刻蚀技术制备了TiO2空心微球非密堆积FCC结构光子晶体.利用电子显微镜分析了晶体的结构,用平面波展开法对该结构进行了能带计算与分析.计算结果表明,制备的TiO2空心微球非密堆积FCC结构光子晶体在低能区的第二、第三能带之间除布里渊区的W点仍保持简并外,其余各点简并都已经消除. 关键词: 空心微球 非密堆积 光子晶体 光子带隙  相似文献   

18.
将玻璃基底依次在低成本的SiO2溶胶和TiO2溶胶中浸渍后,在500 oC下煅烧制备了同时具备减反射与自清洁性能的SiO2/TiO2双层膜.该膜的光学性能与结构特征分别通过紫外-可见分光光度计和场发射扫描电镜进行了表征.同时,源于超亲水性和光催化作用的自清洁性能也凸显出来.实验结果表明制备SiO2/TiO2双层膜对光的透射率最高可达到95%,同时具备自清洁性能.  相似文献   

19.
Thin SiO2 shell consisting of nano-SiO2 particles can be deposited on to LiMn2O4 through the facile hydrolysis of tetraethoxysilane (TEOS) as a solution in either methanol or ethanol. The structure and surface morphologies of the modified and pristine materials were characterized by means of X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The choice of solvent (methanol vs. ethanol) for TEOS hydrolysis has a profound effect on the physical and electrochemical properties of the resultant SiO2-coated LiMn2O4. Coated LiMn2O4 demonstrated an improved cycling ability compared to the uncoated counterpart. Moreover, samples coated using a TEOS–methanol solution showed better cycling ability in extended potential windows and at an elevated temperature than that coated using ethanol.  相似文献   

20.
A SiO2 protective coating was deposited on an IN738LC alloy using CCVD. The physical properties of a SiO2 protective layer are influenced by the amount of tetraethyl orthosilicate (TEOS, C8H20O4Si). Therefore, the SiO2 protective coating was deposited using different TEOS concentrations and deposition times to optimize the conditions. The deposited coating layer was confirmed to be a SiO2 layer by SEM, EDX, and ESCA analyses. The oxidation resistance of the alloy was evaluated by thermo gravimetric analysis. The oxidation resistance of the SiO2 protective coating was highest when the coating was processed at a TEOS concentration of 0.05 mol/l, which is the highest concentration of source material used. The surface roughness of the SiO2 protective layer also increased with increasing TEOS concentration. The surface roughness of the coating had little effect on the oxidation resistance for a film thickness of approximately 1 μm.  相似文献   

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