XPS investigation of diffusion of two-layer ZrO2/SiO2 and SiO2/ZrO2 sol–gel films

Two-layer ZrO₂/SiO₂ and SiO₂/ZrO₂ films were deposited on K9 glass substrates by sol–gel dip coating method. X-ray photoelectron spectroscopy (XPS) technique was used to investigate the diffusion of ZrO₂/SiO₂ and SiO₂/ZrO₂ films. To explain the difference of diffusion between ZrO₂/SiO₂ and SiO₂/ZrO₂ films, porous ratio and surface morphology of monolayer SiO₂ and ZrO₂ films were analyzed by using ellipsometry and atomic force microscopy (AFM). We found that for the ZrO₂/SiO₂ films there was a diffusion layer with a certain thickness and the atomic concentrations of Si and Zr changed rapidly; for the SiO₂/ZrO₂ films, the atomic concentrations of Si and Zr changed relatively slowly, and the ZrO₂ layer had diffused through the entire SiO₂ layer. The difference of diffusion between ZrO₂/SiO₂ and SiO₂/ZrO₂ films was influenced by the microstructure of SiO₂ and ZrO₂.     

Preparation and characterization of novel Pd/SiO2 and Ca-Pd/SiO2 egg-shell catalysts with porous hollow silica

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 3d_5/2 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 mmol_CO mol⁻¹_Pd 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.     

Synthesis and characterization of core-shell structured SiO2@YVO4:Yb,Er microspheres

In this paper, the core-shell structured SiO₂@YVO₄:Yb³⁺,Er³⁺ microspheres have been successfully prepared via a facile sol-gel process followed by a heat treatment. X-ray diffraction, field emission scanning electron microscopy, energy disperse X-ray spectroscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, and photoluminescence spectra were used to characterize the samples. The results reveal that the SiO₂ spheres have been successfully coated by YVO₄:Yb³⁺,Er³⁺ phosphors to form core-shell structures and the size of obtained microspheres has a uniform distribution. Additionally, the samples exhibit bright green luminescence under the excitation of a 980 nm laser diode. The photoluminescence intensity increases with the number of coatings. These core-shell structured SiO₂@YVO₄:Yb³⁺,Er³⁺ microspheres may have great potential in the fields of infrared detection and display devices.     

Sol-gel growth of Gd2MoO6:Eu nanocrystalline layers on SiO2 spheres (SiO2@Gd2MoO6:Eu) and their luminescent properties

SiO₂@Gd₂MoO₆:Eu³⁺ core-shell phosphors were prepared by the sol-gel process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectra (EDS), transmission electron microscopy (TEM), photoluminescence (PL) spectra as well as kinetic decays were used to characterize the resulting SiO₂@Gd₂MoO₆:Eu³⁺ core-shell phosphors. The XRD results demonstrate that the Gd₂MoO₆:Eu³⁺ layers on the SiO₂ spheres begin to crystallize after annealing at 600 °C and the crystallinity increases with raising the annealing temperature. The obtained core-shell phosphors have a near perfect spherical shape with narrow size distribution (average size ca. 600 nm), are not agglomerated, and have a smooth surface. The thickness of the Gd₂MoO₆:Eu³⁺ shells on the SiO₂ cores could be easily tailored by varying the number of deposition cycles (50 nm for four deposition cycles). The Eu³⁺ shows a strong PL luminescence (dominated by ⁵D₀-⁷F₂ red emission at 613 nm) under the excitation of 307 nm UV light. The PL intensity of Eu³⁺ increases with increasing the annealing temperature and the number of coating cycles.     

Polishing behavior of PS/CeO2 hybrid microspheres with controlled shell thickness on silicon dioxide CMP

Organic-inorganic composite microspheres with PS as a core and CeO₂ nanoparticles as a shell were synthesized by in situ decomposition reaction of Ce(NO₃)₃ on the surfaces of PS microspheres prepared through soap-free emulsion polymerization. The shell thickness of the composite microspheres could be turned by varying the concentration of Ce(NO₃)₃ in the reaction solution. The whole process required neither surface treatment for PS microspheres nor additional surfactant or stabilizer. The as-synthesized PS/CeO₂ composite microsphere samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). Oxide chemical mechanical polishing (CMP) performance of the PS/CeO₂ composite abrasives with different shell thickness was characterized by atomic force microscopy (AFM). The results indicated that the as-prepared core-shell structured composite microspheres (220-260 nm in diameter) possessed thin shell (10-30 nm) composed of CeO₂ nanoparticles (particle diameter of 5-10 nm), and the final CeO₂ contents of the composite microspheres ranged from 10 to 50 wt%. A possible mechanism for the formation of PS/CeO₂ composite microspheres was discussed also. The CMP test results confirmed that the novel core-shell structured composite abrasives are useful to improve oxide CMP performance. In addition, there is an obvious effect of shell thickness of the composite abrasives on oxide CMP performance.     

Preparation of sol-gel ZrO2-SiO2 highly reflective multilayer films and laser-induced damage threshold characteristic

Sol-gel (ZrO₂/SiO₂)¹² ZrO₂ films were prepared by spin coating method. The reflectivity spectrum of the films was measured with a Lambda 900 spectrometer. In order to investigate laser-induced damage threshold (LIDT) characteristic of highly reflective films, one-layer ZrO₂ and SiO₂ films, two-layer ZrO₂/SiO₂ and SiO₂/ZrO₂ films were also prepared by spin coating method. LIDT of each film was measured. Damage morphology after laser irradiation was characterized by optical microscopy (Nikon E600K). The experimental results showed that the reflectivity of (ZrO₂/SiO₂)¹² ZrO₂ film at 1064 nm and 355 nm wavelength is 99.7%. The LIDT results decreases as the number of layer of films increases. All the films have similar damage morphology. The experimental results are explained by the different temperature profiles of the films.     

Deposition and characterization of binary Al2O3/SiO2 coating layers on the surfaces of rutile TiO2 and the pigmentary properties

Binary Al₂O₃/SiO₂-coated rutile TiO₂ composites were prepared by a liquid-phase deposition method starting from Na₂SiO₃·9H₂O and NaAlO₂. The chemical structure and morphology of binary Al₂O₃/SiO₂ coating layers were investigated by Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, TG-DSC, Zeta potential, powder X-ray diffraction, and transmission electron microscopy techniques. Binary Al₂O₃/SiO₂ coating layers both in amorphous phase were formed at TiO₂ surfaces. The silica coating layers were anchored at TiO₂ surfaces via Si-O-Ti bonds and the alumina coating layers were probably anchored at the SiO₂-coated TiO₂ surfaces via Al-O-Si bonds. The formation of continuous and dense binary Al₂O₃/SiO₂ coating layers depended on the pH value of reaction solution and the alumina loading. The binary Al₂O₃/SiO₂-coated TiO₂ composites had a high dispersibility in water. The whiteness and brightness of the binary Al₂O₃/SiO₂-coated TiO₂ composites were higher than those of the naked rutile TiO₂ and the SiO₂-coated TiO₂ samples. The relative light scattering index was found to depend on the composition of coating layers.     

Synthesis and characterization of Mn-doped Zn2SiO4/SiO2 phosphor particles in core-shell structure

Manganese-doped zinc silicate (Zn₂SiO₄:Mn) is a kind of phosphor material that has a photo-luminescent (PL) and cathode-luminescent (CL) properties with intensive green light emission at 520 nm. The particles consisting of SiO₂@Zn₂SiO₄:Mn (SiO₂ core-Zn₂SiO₄:Mn shell) were synthesized via colloidal process and forced precipitation. After drying, the Zn/Mn precipitates were coated on the surface of SiO₂ particles. The Zn/Mn precipitates reacted with SiO₂ and transformed to Zn₂SiO₄:Mn by suitable calcination. The microstructure, crystalline phase, and luminescent characteristics of the products were studied. Besides, a CL device consisting of the core-shell powder was characterized.     

A facile synthesis of monodisperse CoFe2O4/SiO2 nanoparticles

Aminated-CoFe₂O₄/SiO₂ magnetic nanoparticles (NPs) were prepared from primary silica particles using modified StÖber method. By optimizing the preparation conditions, monodisperse CoFe₂O₄/SiO₂ NPs with high amino groups’ density were obtained, which is necessary for enzyme immobilization. TEM confirm that the sample is a core/shell structure. These aminated-CoFe₂O₄/SiO₂ NPs have narrow size distributions with a mean size of about 60 nm. Moreover, the aminated-CoFe₂O₄/SiO₂ NPs can be easily dispersed in aqueous medium. The experimental results also show that the NPs have superparamagnetism, indicating that the aminated-CoFe₂O₄/SiO₂ NPs can be used as an effective carrier for the enzyme immobilization.     

ZrO2／SiO2多层膜中膜厚组合周期数及基底材料对残余应力的影响

ZrO₂／SiO₂多层膜由相同沉积条件下的电子束蒸发方法制备而成， 通过改变多层膜中高(ZrO₂)、低(SiO₂)折射率材料膜厚组合周期数的方法，研究了沉积 在熔石英和BK7玻璃 基底上多层膜中残余应力的变化. 用ZYGO光学干涉仪测量了基底镀膜前后曲率半径的变化， 并确定了薄膜中的残余应力. 结果发现，该多层膜中的残余应力为压应力，随着薄膜中膜厚 组合周期数的增加，压应力值逐渐减小. 而且在相同条件下，石英基底上所沉积多层膜中的 压应力值要小于BK7玻璃基底上所沉积多层膜中的压应力值. 用x射线衍射技术测量分析了膜 厚组合周期数不同的ZrO₂／SiO₂多层膜微结构，发现随着周期数增 加，多层膜的结晶程 度增强. 同时多层膜的微结构应变表现出了与所测应力不一致的变化趋势，这主要是由多层 膜中，膜层界面之间复杂的相互作用引起的. 关键词： 2／SiO₂多层膜')" href="#">ZrO₂／SiO₂多层膜 残余应力 膜厚组合周期数     

Characterization of ZrO2-promoted Cu/ZnO/nano-Al2O3 methanol steam reforming catalysts

Three Cu/ZnO/ZrO₂/Al₂O₃ methanol reforming catalysts were investigated using X-ray photoelectron spectroscopy (XPS). The catalysts which contained ZrO₂ from a monoclinic nanoparticle ZrO₂ precursor exhibit both a higher activity toward the methanol steam reforming reaction and a lower CO production rate compared to catalysts composed of an XRD-amorphous ZrO₂ produced by impregnation using a Zr(NO₃)₂ precursor. The presence of a monoclinic phase appears to result in an increased charge transfer between the Zr and Cu species, as evidenced by a relatively electron-rich ZrO₂ phase and a partially oxidized Cu species on reduced catalysts. This electron deficient Cu species is more reactive toward the methanol reforming reaction and partially suppresses CO formation through the reverse water gas shift or methanol decomposition reactions.     

980 nm激发下Er3+/Yb3+共掺杂ZrO2-Al2O3粉末的上转换发光特性

通过固相反应法制备了Er³⁺/Yb³⁺共掺杂ZrO₂-Al₂O₃粉末的样品，并对样品在980nm激光激发下的上转换发光特性进行了研究.从发射光谱可以发现，在可见光范围内有3个强的发光带，一个位于654nm附近的红光带和两个分别位于545nm、525nm附近的绿光带，分别对应于Er³⁺离子的以下辐射跃迁：⁴F_9/2→⁴I_15/2、⁴S_3/2→⁴I_15/2、 ²H_11/2→⁴I_15/2.其中又以Er³⁺离子的⁴F_9/2→⁴I_15/2跃迁产生的红色荧光辐射最强.对其上转换发光机制进行了分析，发现这三个发光过程都是双光子过程.对样品粉末进行了XRD检测，发现ZrO₂主要以立方相为主，并且计算得到了这种立方结构的晶格常数.Al₂O₃固溶于ZrO₂中，Al³⁺嵌入ZrO₂后产生氧空位，导致ZrO₂晶体的对称性降低，这种结构变化更有利于提高上转换效率，即上转换发光强度增强. 关键词： 3+/Yb³⁺')" href="#">Er³⁺/Yb³⁺ 上转换 2-Al₂O₃')" href="#">ZrO₂-Al₂O₃ 荧光 稀土     

Synthesis and characterization of TiO2/Fe2O3 core-shell nanocomposition film and their photoelectrochemical property

TiO₂/Fe₂O₃ core-shell nanocomposition film has been fabricated via two-step method. TiO₂ nanorod arrays are synthesized by a facile hydrothermal method, and followed by Fe₂O₃ nanoparticles deposited on TiO₂ nanorod arrays through an ordinary chemical bath deposition. The phase structures, morphologies, particle size, chemical compositions of the composites have been characterized by X-ray diffraction (XRD), field emission scanning electron microscope (FESEM) and ultraviolet-visible (UV-vis) spectrophotometer. The results confirm that Fe₂O₃ nanoparticles of mean size ca. 10 nm coated on the surface of TiO2 NRs. After depositing Fe₂O₃, UV-vis absorption property is induces the shift to the visible-light range, the annealing temperature of 600 °C is the best condition for UV-vis absorption property of TiO₂/Fe₂O₃ nanocomposite film, and increasing Fe content, optical activity are enhanced one by one. The photoelectrochemical (PEC) performances of the as-prepared composite nanorods are determined by measuring the photo-generated currents under illumination of UV-vis light. The TiO₂ NRs modified by Fe₂O₃ show the photocurrent value of 1.36 mA/cm² at 0 V vs Ag/AgCl, which is higher than those of unmodified TiO₂ NRs.     

Al2O3-Y2O3-ZrO2三相复合陶瓷的介电谱研究

采用传统的固相反应法,在1400–1500 ℃下烧结,制备得到Al₂O₃-Y₂O₃-ZrO₂三相复合陶瓷.样品的结构、形貌和电性能分别用X射线衍射(XRD)、扫描电子显微镜(SEM)及介电谱表征.XRD表明此三相复合体系无其他杂相,加入Y₂O₃及ZrO₂后使得Al₂O₃成瓷温度降低;SEM表明此体系晶粒直径为200–500 nm,并且样品随烧结温度的升高而变得更加致密,晶界更加清晰;介电损耗谱中出现峰值弛豫现象,根据Cole-Cole复阻抗谱得出其为非德拜弛豫. 关键词： 2O₃-Y₂O₃-ZrO₂三相陶瓷')" href="#">Al₂O₃-Y₂O₃-ZrO₂三相陶瓷 介电弛豫 阻抗谱 热导率     

Preparation and characterization of amine-functionalized SiO2/TiO2 films for formaldehyde degradation

This paper investigated the gaseous formaldehyde degradation by the amine-functionalized SiO₂/TiO₂ photocatalytic films for improving indoor air quality. The films were synthesized via the co-condensation reaction of methyltrimethoxysilane (MTMOS) and 3-aminopropyltrimethoxysilane (APTMS). The physicochemical properties of prepared photocatalysts were characterized with N₂ adsorption/desorption isotherms measurement, X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FT/IR). The effect of amine-functional groups and the ratio of MTMOS/APTMS precursors on the formaldehyde adsorption and photocatalytic degradation were investigated. The results showed that the formaldehyde adsorption and photocatalytic degradation of the APTMS-functionalized SiO₂/TiO₂ film was higher than that of SiO₂/TiO₂ film due to the surface adsorption on amine sites and the relatively high of the specific surface area of the APTMS-functionalized SiO₂/TiO₂ film (15 times higher than SiO₂/TiO₂). The enhancement of the formaldehyde degradation of the film can be attributed to the synergetic effect of adsorption and subsequent photocatalytic decomposition. The repeatability of photocatalytic film was also tested and the degradation efficiency was 91.0% of initial efficiency after seven cycles.     

ZnSe/SiO2复合薄膜光学常数与荧光光谱的研究

采用溶胶-凝胶工艺与原位生长技术，制备了ZnSe/SiO₂复合薄膜.X射线衍射分 析表明薄膜中ZnSe晶体呈立方闪锌矿结构.X射线荧光分析结果显示薄膜中Zn与Se摩尔比为1 ∶1.01—1∶1.19.利用场发射扫描电子显微镜观察了复合薄膜的表面形貌，结果表明复合薄 膜表面既存在尺寸约为400nm的ZnSe晶粒，也存在尺寸小于100nm的ZnSe晶粒.利用椭偏仪测 量了薄膜椭偏角Ψ，Δ与波长λ的关系，采用Maxwell-Garnett有效介质理论对薄膜的光学 常数、厚度、气孔率、ZnS 关键词： 2复合薄膜')" href="#">ZnSe/SiO₂复合薄膜 光学性质 椭偏光度法 荧光光谱     

Structural, photochemical and photocatalytic properties of zirconium oxide doped TiO2 nanocrystallites

Composite photocatalysts composed of TiO₂ and ZrO₂ have been prepared via the sol-gel method. The as-prepared nanocomposites are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), UV-vis spectrometry and fluorescence emission spectra. The results shows that TiO₂/ZrO₂ nanocomposites are composed of mainly anatase titania and tetragonal ZrO₂. Incorporating TiO₂ particles with ZrO₂ plays an important role in promoting the formation of nanoparticles with an anatase structure and leads to decreased fluorescence emission intensity. Most of the TiO₂/ZrO₂ nanocomposites exhibited comparable photocatalytic activity compared with commercial TiO₂ for the degradation aqueous methyl orange (MO) under ultraviolet irradiation, while the composite with Zr/Ti mass ratio of 15.2% shows the highest photocatalytic performances. Furthermore, the as-prepared nanocomposites can be reused with little photocatalytic activity loss. Without any further treatment besides rinsing, the photocatalytic activity of TiO₂/ZrO₂ (15.2%) composites is still higher than after five-cycle utilization.     

Electron beam-physical vapor deposition of SiC/SiO2 high emissivity thin film

When heated by high-energy electron beam (EB), SiC can decompose into C and Si vapor. Subsequently, Si vapor reacts with metal oxide thin film on substrate surface and formats dense SiO₂ thin film at high substrate temperature. By means of the two reactions, SiC/SiO₂ composite thin film was prepared on the pre-oxidized 316 stainless steel (SS) substrate by electron beam-physical vapor deposition (EB-PVD) only using β-SiC target at 1000 °C. The thin film was examined by energy dispersive spectroscopy (EDS), grazing incidence X-ray asymmetry diffraction (GIAXD), scanning electron microscopy (SEM), atomic force microscopy (AFM), backscattered electron image (BSE), electron probe microanalysis (EPMA), X-ray photoelectron spectroscopy (XPS) and Fourier transformed infra-red (FT-IR) spectroscopy. The analysis results show that the thin film is mainly composed of imperfect nano-crystalline phases of 3C-SiC and SiO₂, especially, SiO₂ phase is nearly amorphous. Moreover, the smooth and dense thin film surface consists of nano-sized particles, and the interface between SiC/SiO₂ composite thin film and SS substrate is perfect. At last, the emissivity of SS substrate is improved by the SiC/SiO₂ composite thin film.     

Synthesis and CO2 capture property of high aspect-ratio Li2ZrO3 nanotubes arrays

High aspect-ratio Li₂ZrO₃ nanotubes were prepared by hydrothermal method using ZrO₂ nanotubes layers as templates. Characterizations of SEM, XRD, TEM and CO₂ adsorption were performed. The results showed that tetragonal Li₂ZrO₃ nanotubes arrays containing a little monoclinic ZrO₂ can be obtained using this simple method. The mean diameter of the nanotubes is approximately 150 nm and the corresponding specific surface area is 57.9 m² g⁻¹. Moreover, the obtained Li₂ZrO₃ nanotubes were thermally analyzed under a CO₂ flow to evaluate their CO₂ capture property. It was found that the as-prepared Li₂ZrO₃ nanotubes arrays would be an effective acceptor for CO₂ at high temperature.     

Synthesis of Y2Si2O7:Eu nanocrystal and its optical properties

Nanocrystalline Y₂Si₂O₇:Eu phosphor with an average size about 60 nm is easily prepared using silica aerogel as raw material under ultrasonic irradiation and annealing temperature at 300-600 °C and this nanocrystalline decomposes into Y₂O₃:Eu and silica by heat treatment at 700-900 °C. The excitation broad band centered at 283 and 254 nm results from Eu³⁺ substituting for Y³⁺ in Y₂Si₂O₇ and Y₂O₃/SiO₂, respectively. Compared with Y₂O₃:Eu/SiO₂ crystalline, the PL excitation and emission peaks of Y₂Si₂O₇:Eu nanocrystalline red-shift and lead to the enhance of its luminescence intensity due to the different chemical surroundings of Eu³⁺ in above nanocrystallines. The decrease of PL intensity may be ascribed to quenching effect resulting from more defects in Y₂O₃:Eu/SiO₂ crystalline.