Structural,optical and photocatalytic properties of (Mg,Al)-codoped ZnO powders prepared by sol–gel method

Structural and optical properties of 1 at % Al-doped Zn_1−xMg_xO (x=0–8%) powders prepared by sol–gel method were systematically investigated by means of X-ray diffraction, scanning electron microscopy, ultraviolet–visible absorbance measurement, photoluminescence and Raman scattering spectra. All the powders retained the hexagonal wurtzite structure of ZnO. The band gap and near band emission energies determined from absorbance and photoluminescence spectra increased linearly with increasing Mg content, respectively, which implied that the Mg worked effectively on ZnO band gap engineering, irrespective of Al codoping. However, according to the PL and Raman scattering studies, for the sample of x=8%, the Al doping efficiency was decreased by higher Mg codoping. On the other hand, the effect of Mg codoping on photocatalytic degradation of methylene orange was explored experimentally. The substitution of Mg ions at Zn sites shifted the conduction band toward higher energies and then enhanced the photocatalytic activity, while the incorporation of interstitial Mg ions and decreased Al doping efficiency for higher Mg doping sample (x=8%) reduced the photocatalytic activity.     

Color-Changing Sparks from Rare Earth Metal Powders

Commonly, sparks emit light according to the well-known black (gray) body radiation. Recently, we reported on color-changing sparks based on erbium powder, which switch their light emission between black body emission (surface combustion) and element-specific emission (vapor phase combustion). Herein, we investigated the spark formation from the adjacent rare-earth elements. The corresponding boiling points are significantly below (Yb, Sm, Tm) or above (Y, Lu) the boiling point of Er. While Yb and Sm evaporate too fast to form longer sparks, Y, Lu and Tm form color-changing sparks with varying length of the element-specific emission phase. The sparks were investigated by time-resolved emission spectroscopy, long-time exposures, and NIR/MIR imaging. The same basic pyrotechnic formulation containing one of these metal powders reveals a strongly differing burning behavior depending on the boiling point of the metal. The burning characteristics change from a green strobe (Yb) to intense colorful crackling (Tm) and finally a sparkling fountain with long-flying sparks (Lu, Y, Er).     

Synthesis of terbium doped calcium phosphate nanocrystalline powders by citric acid sol–gel combustion method

Terbium doped calcium phosphate (Tb-doped CaP) nanocrystalline powders were synthesized by the citric acid sol–gel combustion method. The phase composition, morphology and luminescent property of Tb-doped CaP nanocrystalline powders were characterized by powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, fluorescence spectrophotometer and fluorescence microscopy. At 700 °C, Tb-doped CaP nanocrystalline powders are composed of HAP (main phase) and β-TCP (minor phase) with Tb doping content of 0.5–4%. SEM and TEM observations show that the 4% Tb-doped CaP nanocrystalline powders are about 50–150 nm spherical particles. The 4% Tb-doped CaP nanocrystalline powders exhibit the strongest emission at 548 nm (λ_excitation = 240 nm) and show strong green fluorescence under fluorescence microscopy.     

较为宽松条件下水热合成铁酸铋粉体

Bismuth ferrite(BiFeO₃) powders were hydrothermally synthesized by using FeCl₃·6H₂O and BiCl₃ as staring materials, NaOH as a mineralizer and NH₄Cl as an additive. The results show that pure BiFeO₃ powders can be synthesized under loose hydrothermal conditions of reaction temperature ranging from 140 to 230 ℃ and NaOH concentration ranging from 2 mol·L^-1 to 5 mol·L^-1. Moreover, the morphologies of the products can be controlled by changing the hydrothermal conditions.     

XPS analysis of bio‐organic systems

A survey of the literature is made for the XPS analysis of food products (mainly spray‐dried powders, which reveal a considerable surface enrichment in lipids) and of microorganisms and related systems (extracellular polymer substances and biofilms). This survey is used as a background for discussions and recommendations regarding methodology. Sample preparation methods reviewed are freeze drying, analysis of frozen hydrated specimens and adsorption of surface‐active biocompounds on model substrates. Peak decomposition is a way to increase the wealth of information provided by the XPS spectra. It should be performed after a check that sample charge stabilization is satisfactory. Moreover, ensuring the precision needed to make comparisons within sets of samples may involve a trade‐off between imposing constraints and generating information. The examination of correlations between spectral data in the light of chemical guidelines is useful to validate or improve peak decomposition and component assignment, and may also upgrade the chemical information regarding speciation. Further upgrading may be achieved by expressing marker XPS data in terms of concentrations of compounds of interest. Different methods of computation are discussed, providing a composition in terms of ingredients, classes of biochemical compounds, or various organic and inorganic compounds. As an alternative or complement to this deterministic approach, multivariate analysis of suitable spectral windows provides spectral components, which may be used for comparing samples, and which may have a direct chemical relevance or be used to identify features of interest. Copyright © 2011 John Wiley & Sons, Ltd.     

催化反应制备碳化硅纳米粉体的密度泛函理论计算及实验研究

以Si_(55),Si_(43)M_(12)和Si_(37)M_(18)(M=Fe,Co或Ni)团簇为模型,采用密度泛函理论(DFT)研究了Fe,Co及Ni纳米团簇催化硅粉转化为SiC的机理.计算结果表明,Fe,Co及Ni纳米催化剂先与Si形成合金,拉长并弱化Si—Si键的强度,起到活化Si粉的作用;合金的形成有利于C原子的吸附及Si原子和C原子间的反应;Fe的催化能力强于Co和Ni.在此基础上,以Si粉和酚醛树脂为原料,以Fe,Co及Ni硝酸盐为催化剂前驱体,通过微波加热反应制备了3C-SiC纳米粉体.研究了催化剂种类、反应温度、催化剂用量和反应时间等对制备3C-SiC纳米粉体的影响.结果表明,催化剂Fe,Co和Ni的加入均可显著降低3C-SiC的合成温度.当以2.0%(质量分数)的Fe为催化剂时,Si粉在1100℃下反应30 min后即可全部转化为3C-SiC纳米粉体;而在相同条件下,无催化剂时Si粉的完全转化温度为1250℃;Fe的催化效果优于Co和Ni,与DFT计算结果吻合.     

Bi-2223喷雾热分解粉末热处理工艺优化

Bi-2223 带材目前在电流引线、 超导电机、 超导电缆、 超导限流器等领域实现了许多示范性应用, 载流性能是表征其性能的重要指标, 而高质量的前驱体粉末是最终带材性能的关键保障. 本文选用具有工艺简单、 粉末效率高、 批次稳定性好等优点的喷雾热分解法制备的Bi-2223 前驱体粉末, 利用 TG-DSC、XRD、SEM 等测试手段对低氧条件下不同保温时间烧结的粉末进行分析, 并结合最终带材的载流性能测试结果, 获得了最优粉末烧结参数, 为后续喷雾热分解粉末的进一步生成 Bi-2223 相以及高性能粉末的制备提供了依据.     

煅烧制度对Lu2Ti2O7粉体生长形貌的影响

采用熔盐法制备Lu2Ti2O7粉体,研究了不同煅烧工艺对粉体形貌的影响,确定了适用于Lu2Ti2O7粉体合成的工艺条件,并在利用XRD、SEM等方法分析表征样品的基础上,提出了初步的粉体形貌生长转变机制。实验结果表明:形核速率和生长速率对粉体的颗粒尺寸和形状影响很大,过快的形核速率和生长速率有利于多面棱柱状晶粒的生长,反之则有利于八面体形状的晶粒生长。     

Characterization of Pd Blacks by Temperature Programmed Oxidation

Using different reduction conditions Pd powders have been prepared and characterized by chemisorption and TPO (Temperature Programmed Oxidation) measurements. The amount of carbon deposits introduced during preparation seems to be peculiar to the preparation procedure. The O₂ consumption curves attributed to PdO formation have shown two peak minima suggesting strong differences in the accessibility of Pd particles.     

纳米SiC蓝光发射的研究

在４．６８ｅＶ的激光激发下，室温ＣＶＤ合成的纳米ＳｉＣ粉体，可发射４７５ｎｍ的蓝光，经６００～１１００℃在Ｎ２气氛下进行快速退火（ＲＴＡ）处理，其荧光强度随退火温度升高而增强，当Ｔ≥９００℃时，荧光强度下降，但发光峰位与退火温度无关．通过ＸＲＤ、ＩＲ、ＴＥＭ、ＸＰＳ等研究，认为纳米ＳｉＣ中与氧有关的缺陷可能是引起４７５ｎｍ蓝光发射的主要原因