Dry etching of TiN in N2/Cl2/Ar adaptively coupled plasma

We investigated the N₂ additive effect on the etch rates of TiN and SiO₂ and etch profile of TiN in N₂/Cl₂/Ar adaptively coupled plasma (ACP). The mixing ratio of Cl₂ and Ar was fixed at 75 and 25 sccm, respectively. The N₂ flow rate was increased from 0 to 9 sccm under the constant pressure of 10 mTorr. As N₂ flow rate was increased in N₂/Cl₂/Ar plasma, the etch rate of TiN was linearly increased, but that of SiO₂ was increased non-monotonically. The etch profile and the compositional changes of TiN was investigated with field emission-scanning electron microscope (FE-SEM), FE-Auger electron spectroscopy (FE-AES) and x-ray photoelectron spectroscopy (XPS). When 9 sccm N₂ was added into Cl₂/Ar, a steep etch profile and clean surface of TiN was obtained. In addition, the signals of TiN and Ti were disappeared in FE-AES and XPS when N₂ additive flow into Cl₂/Ar was above 6 sccm. From the experimental data, the increase in TiN etch rate was mainly caused by the increase of desorption and evacuation rate of etch by products because of the increased effective pumping speed. The etch mechanism of TiN in N₂/Cl₂/Ar ACP plasma can be concluded as the ion enhanced chemical etch.     

Pt纳米颗粒负载SrTiO3/TiO2异质结结构制备及制氢性能

本文以固定n(Sr)/n(Ti)摩尔比0.4的SrTiO_3/TiO_2(金红石相)异质结纳米颗粒,通过"光催化还原沉积方法"制备不同质量分数的纳米铂颗粒(0、1%、2%、5%),探究其催化活性的变化,采用XRD、SEM、UV-vis、XPS方法对其进行表征,并做了相关光催化分解水产氢性能测试.结果表明:负载贵金属Pt纳米颗粒量越大,对应的Pt晶粒平均尺寸为40.8 nm,1%Pt纳米颗粒SrTiO_3/TiO_2异质结构的BET比表面积在23.195 m~2/g处最高,并且介孔材料的特征是平均Barrett-Joyner-Halenda(BJH)孔径为13.60 nm,总孔体积为0.079 cm~3/g;高BET表面积和大的总孔体积强烈地支持SrTiO_3/TiO_2具有介孔结构的事实;相应的催化剂催化活性越高,其中负载5%Pt纳米颗粒的SrTiO_3/TiO_2纳米颗粒光催化8 h产氢量为3.574 mmol,平均产氢效率为0.447 mmol/(gcat·h),但从性价比的角度来考虑,其催化效率远不及负载1%Pt纳米颗粒的SrTiO_3/TiO_2纳米颗粒催化效率的5倍,因此负载5%Pt的SrTiO_3/TiO_2纳米颗粒光催化效率最高.     

Structure of double interfaces system of Si3N4/SiO2/Si irradiated by γ-rays

The interfacial structures of double interfaces system of Si₃N₄/SiO₂/Si were examined using X-ray photoelectron spectroscopy (XPS) before and after ⁶⁰Co radiation. The experimental results demonstrate that there existed two interfaces, one consisted of Si₃N₄ and SiO₂, while another was made of Si and SiO₂, the interface between SiO₂ and Si was extended towards the interface of the Si₃N₄/SiO₂ meanwhile the center of the former interface was removed in the direction of the latter interface by ⁶⁰Co. The concentration of silicon in the Si₃N₄ state (BE 101.8 eV) was decreased with the variation of radiation dosage as well as bias field within the SiO₂-Si interface, remarkably. The mechanism for the experimental results is analyzed.     

Mechanical and dielectric properties of porous Si3N4–SiO2 composite ceramics

In order to prepare a structural/functional material with not only higher mechanical properties but also lower dielectric constant and dielectric loss, a novel process combining oxidation-bonding with sol–gel infiltration-sintering was developed to fabricate a porous Si₃N₄–SiO₂ composite ceramic. By choosing 1250 °C as the oxidation-bonding temperature, the crystallization of oxidation-derived silica was prevented. Sol–gel infiltration and sintering process resulted in an increase of density and the formation of well-distributed micro-pores with both uniform pore size and smooth pore wall, which made the porous Si₃N₄–SiO₂ composite ceramic show both good mechanical and dielectric properties. The ceramic with a porosity of 23.9% attained a flexural strength of 120 MPa, a Vickers hardness of 4.1 GPa, a fracture toughness of 1.4 MPa m^1/2, and a dielectric constant of 3.80 with a dielectric loss of 3.11 × 10⁻³ at a resonant frequency of 14 GHz.     

Plasmons in double interfaces system of Si3N4/SiO2/Si irradiated by Co

The first level plasmons of Si in the pure Si state, in the SiO₂ state and in the Si₃N₄ state (corresponding to bonding energy 116.95, 122.0 and 127.0 eV) were investigated directly with X-ray photoelectron spectroscopy before and after ⁶⁰Co radiation. The experimental results demonstrate that there existed two interfaces, one consisted of plasmons of Si in the Si₃N₄ and SiO₂ states, while another was made of plasmons of Si in the pure Si state and in the SiO₂ state. When the Si₃N₄-SiO₂-Si samples were irradiated by ⁶⁰Co, the interface at Si₃N₄/SiO₂ was extended and at the same time the center of this interface moved towards the surface of Si₃N₄. The concentration of plasmon for silicon in the SiO₂ state is decreased at the SiO₂-Si interface, and the effects of radiation bias field on plasmons in the SiO₂-Si interface are observable. Finally, the mechanism of experimental results is analyzed by the quantum effect of plasmon excited by the photoelectron.     

Low-temperature synthesis of Y2SiO5:Eu powders using mesoporous silica and their luminescence properties

This paper reports the synthesis of Eu³⁺ ions-doped Y₂SiO₅ (Y₂SiO₅:Eu³⁺) powders by mesoporous template route. Using mesoporous silica SBA-15 as silica source, Y₂SiO₅:Eu³⁺ powders were prepared by solid-state reaction at a calcination temperature of 1300 °C without fluxes. The prepared Y₂SiO₅:Eu³⁺ powders were characterized by X-ray diffraction, scanning electron microscope, nitrogen adsorption-desorption isotherms, and photoluminescence spectroscopy. The results show that the crystalline Y₂SiO₅:Eu³⁺ particles are dense and have a morphology similar to SBA-15. The low calcination temperature is attributed to the high reactive activity of SBA-15 with large surface area and non-crystalline structure. The Y₂SiO₅:Eu³⁺ powders prepared at a low calcination temperature show luminescence properties similar to the reported results of Eu³⁺ doped-Y₂SiO₅ samples prepared at high temperatures.     

Low temperature biomimetic synthesis of the Li2ZrO3 nanoparticles containing Li6Zr2O7 and high temperature CO2 capture

Li₂ZrO₃ nanoparticles containing Li₆Zr₂O₇ were prepared by a biomimetic soft solution route and characterized with X-ray diffraction (XRD), transmission electron microscope (TEM) and nitrogen adsorption. The results show that the tetragonal Li₂ZrO₃ nanoparticles containing monoclinic Li₆Zr₂O₇ can be obtained using this simple method. The mean diameter of the nanoparticles is approximately 90 nm and the corresponding specific surface area is 23.7 m² g^− 1. Moreover, the Li₂ZrO₃ nanoparticles obtained were thermally analyzed under a CO₂ flux to evaluate their CO₂ capture capacity at high temperature. It was found that the as-prepared Li₂ZrO₃ nanoparticles would be an effective acceptor for high temperature CO₂ capture.     

Synthesis and characterization of Mo doped hierarchically porous SO4/ZrO2 solid acid catalyst

A novel hierarchically porous molybdenum-promoted SO₄²⁻/ZrO₂ solid acid with nanocrystallized framework of tetragonal phase and high surface area has been synthesized via a composite surfactant-assisted route combined with a hydrothermal treatment process. The XRD, N₂-adsorption, TEM, and FT-IR pyridine adsorption were used for the structural analysis and acidic characterization. The results show that the novel mesoporous solid acid exhibits classical tetragonal phase and excellent catalytic performance in the esterification reaction of acetic acid with n-butanol and can preserve the acid better than normal solid acids after several recycle experiments. This hierarchically zirconia solid acid has a good potential as catalysts in some chemical reactions such as esterification.     

Lightweight geopolymer made of highly porous siliceous materials with various Na2O/Al2O3 and SiO2/Al2O3 ratios

The syntheses of lightweight geopolymeric materials from highly porous siliceous materials viz. diatomaceous earth (DE) and rice husk ash (RHA) with high starting SiO₂/Al₂O₃ ratios of 13.0-33.5 and Na₂O/Al₂O₃ ratios of 0.66-3.0 were studied. The effects of fineness and calcination temperature of DE, concentrations of NaOH and KOH, DE to RHA ratio; curing temperature and time on the mechanical properties and microstructures of the geopolymer pastes were investigated. The results indicated that the optimum calcination temperature of DE was 800 °C. Increasing fineness of DE and starting Na₂O/Al₂O₃ ratio resulted in an increase in compressive strength of geopolymer paste. Geopolymer pastes activated with NaOH gave higher compressive strengths than those with KOH. The optimum curing temperature and time were 75 °C and 5 days. The lightweight geopolymer material with mean bulk density of 0.88 g/cm³ and compressive strength of 15 kg/cm² was obtained. Incorporation of 40% RHA to increase starting SiO₂/Al₂O₃ and Na₂O/Al₂O₃ ratios to 22.5 and 1.7 and enhanced the compressive strength of geopolymer paste to 24 kg/cm² with only a marginal increase of bulk density to 1.01 g/cm³. However, the geopolymer materials with high Na₂O/Al₂O₃ (>1.5) were not stable in water submersion.     

Natural and persistent superhydrophilicity of SiO2/TiO2 and TiO2/SiO2 bi-layer films

Sol-gel SiO₂/TiO₂ and TiO₂/SiO₂ bi-layer films have been deposited from a polymeric SiO₂ solution and either a polymeric TiO₂ mother solution (MS) or a derived TiO₂ crystalline suspension (CS). The chemical and structural properties of MS and CS bi-layer films heat-treated at 500 °C have been investigated by Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and transmission electron microscospy. Water contact angle measurements show that MS SiO₂/TiO₂ and CS TiO₂/SiO₂ bi-layer films exhibit a natural superhydrophilicity, but cannot maintain a zero contact angle for a long time over film aging. In contrast, CS SiO₂/TiO₂ bi-layer films exhibit a natural, persistent, and regenerable superhydrophilicity without the need of UV light. Superhydrophilic properties of bi-layer films are discussed with respect to the nature of the TiO₂ single-layer component and arrangement of the bi-layer structure, i.e. TiO₂ underlayer or overlayer.     

Large-scale synthesis and characterization of fan-shaped rutile TiO2 nanostructures

Large-scale fan-shaped rutile TiO₂ nanostructures have been synthesized by means of a simple hydrothermal method using only TiCl₄ as titanium source and chloroform/water as solvents. The physicochemical features of the fan-shaped TiO₂ nanostructures are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), nitrogen absorption-desorption, diffuse reflectance ultraviolet-visible spectroscopy (UV-vis) and Fourier transform infrared spectroscopy (FTIR). Structural characterization indicates that the fan-shaped TiO₂ nanostructures are composed of several TiO₂ nanorods with diameters of about 5 nm and lengths of 300-350 nm. The average pore size and BET surface area of the fan-shaped TiO₂ nanostructures are 6.2 nm and 59 m²/g, respectively. Optical adsorption investigation shows that the fan-shaped TiO₂ nanostructures possess optical band gap energy of 3.11 eV.     

Influence of SiO2 interlayer on the hydrophilicity of TiO2/SiO2/glass produced by RF-magnetron sputtering

The effect of silicon dioxide (SiO₂) on the hydrophilicity of the TiO₂ thin film is investigated. SiO₂ and TiO₂ films were deposited on the glass by RF-magnetron sputtering. Heat-treatment for 15 h at 573 K on TiO₂/glass and TiO₂/SiO₂/glass is carried out to make Na⁺-ion diffused from the glass to the TiO₂ thin film, which results in no band-gap change but instead the enhanced crystallinity of the anatase phase-TiO₂. This in turn leads to the improvement in hydrophilicity. Irrespective of the SiO₂ interlayer, the anatase phase-TiO₂ thin film with enhanced crystallinity shows outstanding super-hydrophilicity. Consequently, under the heat-treatment condition, the SiO₂ interlayer played an important role in improving the crystallinity of the anatase phase-TiO₂ rather than preventing Na⁺-ion diffusion.     

Luminescence and energy transfer of Mn co-doped SrSi2O2N2:Eu green-emitting phosphors

Eu²⁺ and Mn²⁺ co-doped SrSi₂O₂N₂ green-phosphors, with promising luminescent properties (examined by their powder diffuse reflection, photoluminescence excitation and emission spectra) suitable for UV converted white LEDs, were produced by high temperature solid-state reaction method. The produced materials exhibited intense broad absorption bands at 220–500 nm and a broad emission band centered at ca. 530 nm, attributed to 4f–5d transitions of Eu²⁺. The emission intensity of Eu²⁺ ions was greatly enhanced by introducing Mn²⁺ ions into SrSi₂O₂N₂:Eu²⁺ due to the energy transfer from Mn²⁺ to Eu²⁺. The energy transfer probability from Mn²⁺ to Eu²⁺ depends strongly on the Mn²⁺ concentration, which is maximized at a Mn²⁺ concentration of 3 mol%. It drastically decreases for higher concentrations. The results indicated that SrSi₂O₂N₂:Eu²⁺, Mn²⁺ is a promising green-emitting phosphor for white-light emitting diodes with near-UV LED chips.     

SiO2/TiO2 multilayer films grown on cotton fibers surface at low temperature by a novel two-step process

A novel two-step process was developed to synthesize and deposit SiO₂/TiO₂ multilayer films onto the cotton fibers. In the first step, SiO₂ particles on cotton fiber surface were synthesized via tetraethoxysilane hydrolysis in the presence of cotton fibers, in order to protect the fibers against photo-catalytic decomposition by TiO₂ nanoparticles. In the second step, the growth of TiO₂ nanoparticles into the modified cotton fiber surface was carried out via a sol-gel method at the temperature as low as 100 °C. The as-obtained SiO₂/TiO₂ multilayer films coated on cotton fibers were characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, atomic force microscopy and X-ray diffraction, respectively.     

Surfactant/co-polymer template hydrothermal synthesis of thermally stable, mesoporous TiO2 from TiOSO4

Industrial TiOSO₄ solution was used as inorganic precursor to prepare mesoporous titania via composite template route, using cetyl-trimethylammonium bromide (CTAB) and tri-block copolymer EO₂₀PO₇₀EO₂₀ (P-123) as structure-directing agents (SDA) under high acidic conditions. Mesoporous TiO₂ with high thermal stability was obtained via controlling the hydrolysis and condensation rate of industrial TiOSO₄ solution by adjusting the pH value and post hydrothermal treating. The as-prepared materials were characterized by XRD, nitrogen adsorption-desorption, SEM and HRTEM. The powder calcined at 723 K for 2 h showed higher thermal stability, with BET specific surface area of 218.7 m²/g and an average pore diameter of 3.63 nm.     

Solvothermal preparation and characterization of sheet-like CuInSe2 with hierarchically mesoporous structures

By using a solvothermal reaction in mixed solvent of ethylenediamine and ethylene glycol, nanoparticle-assembled sheet-like CuInSe₂ with hierarchically mesoporous structures were successfully fabricated with the absence of any template or structure-directing agent. The as-synthesized products were characterized by XRD, EDX, FESEM, TEM, HRTEM, BET nitrogen adsorption and NIR absorption spectrum. The possible formation mechanism was simply discussed. The size of mesopores is hierarchically distributed in the range of 2-30 nm and the specific surface area was estimated to be 10.15 m²/g. The value of band gap (E_g) was calculated to be 1.00 eV based on its NIR absorption spectrum.     

Synthesis and characterization of nanocrystalline manganese pyrophosphate Mn2P2O7

Mn₂P₂O₇ polyhedral particles were synthesized by simple and cost-effective method using manganese nitrate hydrate and phosphoric acid in the presence of nitric acid with further calcinations at the temperature of 800 °C. The crystallite size obtained from X-ray line broadening is 31 ± 13 nm for the Mn₂P₂O₇. The X-ray diffraction and SEM results indicated that the synthesized nanoparticles have only the structure without the presence of any other phase impurities. The FT-IR and FT-Raman spectra show characteristic bands of the P₂O₇⁴⁻ anion. The UV–Vis–NIR spectrum confirms the octahedral coordination of Mn²⁺ ion.     

Gravitational waves detector mirrors: Spectroscopic ellipsometry study of Ta2O5 films on SiO2 substrates

A stack of Ta₂O₅/SiO₂ layers is presently used as coating layer of mirrors in interferometric detectors for gravitational waves. The sensitivity of these detectors is limited in the 50-300 Hz frequency range by the mirror thermal noise, and it was suggested that mechanical losses in the Ta₂O₅ are the dominant source of noise. We focus here on Spectroscopic Ellipsometry (SE) results (in the 0.75 ÷ 5 eV spectral range) obtained on high quality Ta₂O₅ films deposited on SiO₂ substrates by Double Ion Beam Sputtering at the Laboratoire des Matériaux Avancés (Lyon, France). The films are extremely flat as indicated by the 0.2 nm RMS roughness determined by Atomic Force Microscopy (AFM) on (20 × 20) μm² areas. The comparison of the optical properties determined by SE with literature data, corroborated by X-ray Photoelectron Spectroscopy (XPS) data, suggests that the films present a non-ideal bulk stoichiometry and/or some degree of nanoporosity. The possible influence of an interface layer is also discussed.     

Mesoporous TiO2 thin films embedded with Au nanoparticles for the enhancement of the photocatalytic properties

Mesoporous TiO₂ thin films were prepared by hydrothermal-oxidation of titanium metal thin films, which were obtained by DC magnetron sputtering technique. Gold nanoparticles, which were prepared by reduction of HAuCl₄, were embedded into the holes of the mesoporous TiO₂ films by capillary method followed by annealing in air up to 400 °C. The size of pore of TiO₂ films is about 100 nm and that of Au nanoparticles is about 10 nm in average. The morphology of the films was analyzed by field emission scanning electron microscope (FE-SEM) and scanning probe microscopes (SPMs). Subsequently, the photocatalytic performances of the obtained nanosystems in the decomposition of methylene blue solution are discussed. The obtained results show that the dispersion of Au nanoparticles on the mesoporous TiO2 matrix will help enhancing the photocatalytic activity with respect to pure TiO₂ under visible light irradiation.     

Near UV-based LED fabricated with Ba5SiO4(F,Cl)6:Eu as blue- and green-emitting phosphor

A series of halosilicate phosphor, Ba₅SiO₄(F,Cl)₆:Eu²⁺, were synthesized by a solid state reaction. Excited by 370-nm light, Ba₅SiO₄Cl₆:Eu²⁺ exhibits a broad emission band peaking at 440 nm. Partial substitution of Cl⁻ with F⁻ in the host lattice leads to red-shift in the emission band with centering wavelength from 440 nm to 503 nm. The possible mechanism for the luminescence change was discussed based on the XRD patterns. Blue and green LEDs were fabricated by combination of a 370 nm-emitting near UV chip and the optimal Ba₅SiO₄Cl₆:Eu²⁺ and Ba₅SiO₄(F₃Cl₃):Eu²⁺, respectively. This series of phosphors is considered as a promising blue and green component used in fabrication of near UV-based white LEDs.