Preparation of nano-sized cerium and titanium pyrophosphates via solid-state reaction at room temperature

Nano-sized cerium-titanium pyrophosphates Ce1-xTixP2O7 （with x = 0, 0.2, 0.5, 0.7, 0.9, and 1.0） were obtained by grinding a mixture of Ce（SO4）2·4H2O, Ti（SO4）2, and Na4P2O7·10H2O in the presence of surfactant PEG-400 at room temperature, washing the mixture with water to remove soluble inorganic salts, and drying at 100℃. The products and their calcined samples were characterized using ultraviolet-visible spectroscopy （UV-vis）, thermogravimetry and differential thermal analyses （TG/DTA）, X-ray powder diffraction （XRD）, and transmission electron microscopy （TEM）. The results show that nano-sized Ce1-xTixP2O7 behave as an excellent UV-shielding material. Thereinto, the CeP2O7 has the most excellent UV-shielding effect, and the amorphous state of Ce0.8Ti0.2P2O7 can keep at a higher temperature than CeP2O7. Therefore, the stabilization of the amorphous state of the cerium pyrophosphates was carded out by doping titanium. This stabilization is a significant improvement, which enables to apply these amorphous pyrophosphates not only to cosmetics and paints, but also plastics and films.

Preparing Nano-ZnS by Solid State Reaction at Room Temperature

ZnS nanoparticles were prepared by using solid-state reaction method at room temperature in agate mortar for the first time. The average particle size was about 20nm. This reaction is affected by the structure of reactant, crystal water and defects.

Preparation of transparent yttrium aluminum garnet ceramics by relatively low temperature solid-state reaction

A new preparation method for a highly sinterable Y 2O 3 powder was developed, using the mixture of the powder with Al 2O 3 powder, a transparent yttrium aluminum garnet(YAG) ceramic was prepared at relatively low temperature by a solid state reaction method. Yttrium nitrate was used as a mother salt, and aqueous ammonia was used as a precipitant reagent, the fine and dendritic precursor crystalline was prepared by adding 0.5% ammonium sulfate into the precipitation reaction system. The highly pure and low agglomerated Y 2O 3 powders were obtained by calcinating the precursor at 1 100 ℃, the primary particles are spherical and 60 nm in diameter. The mixture of Y 2O 3 and Al 2O 3 powders was calcinated, and the resulting mixture compact pressed in mold could be sintered to transparency under vacuum at 1 700 ℃. The sintered transparent YAG polycrystalline exhibits a homogeneous microstructure and its transmittance reaches 45% in the visible light region and 70% in the near infrared wavelength region.

Microstructural evolution of NiFe_2O_4-10NiO powder prepared by high temperature solid state reaction

The NiFe2O4-10NiO powder for inert anode of aluminium electrolysis was prepared by high temperature solid state reaction. The microstructural evolution from the raw materials NiO and Fe2O3 to the NiFe2O4-10NiO powder was studied by SEM. The results show that the domain structure making up of the agglomerate particles of Fe2O3 remains after high temperature solid state reaction, and the diffusion of Ni2+ into Fe2O3 structure is the control step of the reaction process. A microstructure with compact structure and fine grain inside the particle results from the sintering of NiFe2O4-10NiO powder.

Synthesis of Mesoporous Chromium Aluminophosphate (CrAlPO) via Solid State Reaction at Low Temperature

Mesoporous chromium aluminophosphate （CrAIPO） was successfully synthesized via solid state reaction （SSR） route at low temperature in the presence of a cationic surfactant cetyltrimethyl ammonium bromide （CTAB） and inorganic sources such as A1C13 · 6H20, CrCI3 · 6H20 and NaH2PO4 · 2H20. Characterizations by means of powder X-ray diffraction （XRD）, N2 adsorption- desorption, high resolution transmission electron microscopy （HR-TEM）, scanning electron micrography （SEM）, energy dispersion spectroscopy （EDS）, thermo-gravimetry （TG）, Fourier transform infrared spectroscopy （FT-IR）, and ultraviolet visible light spectroscopy （UV-Vis） were carried out to understand both the pore characteristics and electron transition route of these obtained materials. The experimental results show that the meso-CrA1PO materials with various Cr/A1 molar ratios possess a mesostructure and a specific surface area of 193 to 310 m2/g corresponding to an average pore size of 5.5 to 2.2 rim, respectively. The maxium content of Cr in meso-CrA1PO materials synthesized via SSR route can achieve 16.7wt%, being significantly higher than that of the meso-CrA1PO prepared via a conventional sol-gel route. Meanwhile, the formation mechanism of the meso-CrA1PO was also proposed.

Salt-assisted Low Temperature Solid State Synthesis of High Surface Area CoFe_2O_4 Nanoparticles

A novel salt-assisted low temperature solid state method using CoCl2.6H2O, FeCl3.6H2O and NaOH as precursor and using NaCI as a dispersant to synthesize high surface area CoFe2O4 nanoparticles, has been investigated. The effects of the molar ratio of added salt and calcination temperature on the characteristics of the products were investigated by X-ray diffraction （XRD）, transmission electron microscopy （TEM）, vibrating sample magnetometer （VSM） and Brunauer, Emmett and Teller （BET） surface area analysis. Results showed that the introduction of leachable inert inorganic salt as a hard agglomeration inhibitor in the mixture precursor led to the formation of high dispersive CoFe2O4 nanoparticles; and the increase in specific surface area from 28.28 to 73.97 m^2/g, and the saturation magnetization is 84.6 emu/g.

Room-temperature strong coupling between dipolar plasmon resonance in single gold nanorod and two-dimensional excitons in monolayer WSe_2

All-solid-state strong coupling systems with large vacuum Rabi splitting energy have great potential applications in future quantum information technologies, such as quantum manipulations, quantum information storage and processing,and ultrafast optical switches. Monolayer transition metal dichalcogenides（TMDs） have recently been explored as excellent candidates for the observation of solid-state strong coupling phenomena. In this work, from both experimental and theoretical aspects, we explored the strong coupling effect by integrating an individual plasmonic gold nanorod into the monolayer tungsten diselenide（WSe2）. Evident anti-crossing behavior was observed from the coupled energy diagram at room temperature; a Rabi splitting energy of 98 meV was extracted.

Solid-state synthesis of Sr-and Co-doped LaMnO_3 perovskites

The synthesis process for La 1- x Sr x Mn 1- y Co y O 3- δ ( x = 0.2, 0.3; y = 0.2, 0.8, designated as LSMC below) perovskite oxides prepared by solid state reaction was investigated using DSC/TG, XRD, EPMA and particle size analysis methods. It was found that LSMCs were all of single phase and the synthesis process might be divided into three stages: the decomposition of reactants, the formation of LaMn(Co)O 3 based oxides, and the formation of LSMC solid solution. Typical average and the peak value of particle size, and the specific surface area are 14.65?μm, 16.4?μm and 1.38?m 2/mL, respectively, for mixed reactants and are 23.81?μm, 32.11?μm and 0.5?m 2/mL, respectively, for powder synthesized at 1?200?℃ for 8?h in air.

Modeling of Solid-state Polycondensation of Poly (ethylene terephthalate)

A mathematical model has been developed to handle the reactions in Poly(ethylene terephthalate) (PET) undergoing polycondensation reactions in the solid state. The effect of temperature on chain mobility was considered to estimate the rate constants of chemical reactions. The polymer crystalline fraction is modeled as containing only repeat units, thus concentrating end groups and conden-sates in the amorphous fraction. This model is compared with PET reaction data with good results.

Cr^(3+)掺杂F^(-)修饰BaScO_(2)F钙钛矿结构宽带近红外荧光粉

Cr^(3+)掺杂的近红外荧光材料,因具有高量子效率、可调的宽带发射及在蓝色光谱范围内的强吸收特性而备受关注。通过晶体场工程,可以调节Cr^(3+)掺杂的近红外荧光材料的发射范围,但常规的阳离子取代对发射范围的调节通常限制在近红外Ⅰ区(波长<1000 nm)。在生物医学成像领域,由于生物组织的吸收、散射和自发荧光较低,在近红外Ⅱ区,能够实现更高的穿透深度及无创或微创的深部组织成像。采用高温固相法,以Ba_(2)Sc_(2)O_(5)类钙钛矿型氧化物为基体,合成了一系列基于F^(-)修饰的近红外荧光粉BaSc_(1-x)O_(2)F:xCr^(3+)(x=0.001—0.01)。通过XRD图谱和容差因子计算,证明了合成的样品具有立方钙钛矿结构。另外,通过漫反射光谱(DRS)和X射线光电子能谱(XPS)等表征手段,确认了Cr离子的价态为Cr^(3+)。利用电子顺磁共振(EPR)对Cr^(3+)周围的晶体环境进行检测分析发现,样品在波长700—1400 nm范围内表现出近红外宽带发射,发射中心约在1040 nm处,半峰宽(FWHM)高达250 nm。表明,Cr^(3+)的发射有效覆盖了近红外Ⅱ区。同时,也证明了通过阴离子掺杂调节晶体场强度是可行的。由于PLE光谱和PL光谱在波长700—850 nm范围内存在重叠,随着Cr^(3+)掺杂浓度的增加,发射部分被重吸收,导致发射中心出现明显的红移现象。由于BaSc_(1-x)O_(2)F:xCr^(3+)近红外荧光粉的吸收峰与蓝光LED芯片能够匹配,表明其具有商业化潜力。本研究为生物医学成像领域的近红外Ⅱ区荧光粉转换LED器件提供了优异的宽带近红外光源材料。

Fabrication and characterization of SmO_(0.7)F_(0.2)FeAs bulk with a transition temperature of 56.5 K

The superconductivity of iron-based superconductor SmO 0.7 F 0.2 FeAs was investigated. The SmO 0.7 F 0.2 FeAs sample was prepared by the two-step solid-state reaction method. The onset resistivity transition temperature is as high as 56.5 K. X-ray diffraction （XRD） results show that the lattice parameters a and c are 0.39261 and 0.84751 nm, respectively. Furthermore, the global J c was more than 2.3 × 10 5 A/cm 2 at T = 10 K and H = 9 T, which was calculated by the formula of J c = 20ΔM/[a（1-a/（3b））]. The upper critical fields, H c2 ≈ 256 T （T = 0 K）, was determined according to the Werthamer-Helfand-Hohenberg formula, indicating that the SmO 0.7 F 0.2 FeAs was a superconductor with a very promising application.

面向超声压电换能器的MnO_(2)掺杂Pb(Sc,Nb)O_(3)-Pb(Hf,Ti)O_(3)陶瓷研究

该文采用固相反应法成功合成了高性能MnO_(2)掺杂的0.07Pb(Sc_(1/2)Nb_(1/2))O_(3)-0.93Pb(Hf_(0.47)Ti_(0.53))O_(3)(PSN-PHT)陶瓷,并从微观形貌、相结构和电学性能等方面综合分析了PSN-PHT陶瓷性能提高的原因。实验结果表明,MnO_(2)的引入改变了PSN-PHT陶瓷的相结构,使其铁电四方相含量降低,并导致准同型相界(MPB)的出现,同时增大了晶粒尺寸并使晶粒均匀化。当MnO_(2)掺杂量(摩尔分数)为0.8%时,样品达到最佳性能,其d_(33)、k_(p)、T_(C)、Q_(m)和tanδ分别为450 pC/N、0.65、348℃、1200和0.0032。该组分样品的温度稳定性远高于商用PZT-5和PZT-8陶瓷,故其在压电陶瓷换能器领域有着巨大的应用前景。

W^(6+)掺杂Pb(Sc,Nb)O_(3)-Pb(Hf,Ti)O_(3)陶瓷的制备和性能研究

该文采用传统固相反应法制备了W^(6+)掺杂的0.07Pb(Sc_(0.5)Nb_(0.5))O_(3)-0.93Pb(Hf_(0.47)Ti__(0.53))O_(3)(PSN-PHT)陶瓷,详细分析了样品的晶体结构、压电和介电性能。实验结果表明,W^(6+)掺杂可以提高钙钛矿结构中三方相的含量,有效增加晶粒尺寸,提高压电系数。当W^(6+)掺杂量(摩尔分数)为1.0%时,样品具有最佳的压电和介电性能,即d_(33)=585 pC/N,TC=323℃,ε_(r)=2088。同时,样品的d_(33)在200℃去极化温度下仍保持570 pC/N的高值,且经过1080 min保温后,压电常数略微降低,此时d_(33)仍可达到537 pC/N,变化仅为5.7%。上述结果表明,W^(6+)掺杂不仅可以提高压电系数,同时也可增强陶瓷的温度稳定性,使该陶瓷体系能在更宽的温度范围内使用。

NaYSiO_(4)∶Ce^(3+)蓝色荧光粉的发光性质及其在白光发光二极管上的应用

采用高温固相法合成了NaYSiO_(4)∶xCe^(3+)(0.01≤x≤0.05)系列蓝色荧光粉。NaYSiO_(4)∶xCe^(3+)荧光粉在250~360 nm之间的宽带吸收能与紫外LED芯片很好地匹配。NaYSiO_(4)∶xCe^(3+)荧光粉中存在多个Ce^(3+)离子荧光中心,且在紫外光激发下表现出峰值波长位于414 nm附近的宽带蓝光发射。NaYSiO_(4)∶0.02Ce^(3+)荧光粉在300~350 nm紫外光激发下量子效率在25%以上。NaYSiO_(4)∶0.02Ce^(3+)荧光粉表现出优良的化学稳定性,在水中浸泡14 d后荧光强度和量子效率几乎不变。将NaYSiO_(4)∶0.02Ce^(3+)蓝色荧光粉、商用(Sr,Ba)_2SiO_(4)∶Eu^(2+)绿色荧光粉和商用(Ca,Sr)AlSiN_(3)∶Eu^(2+)红色荧光粉涂覆于310 nm紫外LED芯片上制备得到了显色指数高达95的LED器件。当驱动电流从50 mA逐渐增大到300 mA时,制备的LED器件表现出稳定的暖白光发射,其色坐标几乎不变。上述结果说明,本研究报道的NaYSiO_(4)∶0.02Ce^(3+)蓝色荧光粉在紫外LED芯片驱动的白光发光二极管照明上有着潜在应用价值。

Synthesis of trans-bis(glycin- ato) copper(II) complex nanorods by room tempera- ture solid-state reaction

Trans-[Cu(glyo)2(H2O)] nanoparticles with average diameters about 20—30 nm were prepared by one- step room temperature solid-state reaction. Trans-[Cu(glyo)2] nanorods with diameters ranging from 100 to 150 nm and lengths up to several ìm were also prepared by one-step room temperature solid-state reaction in the presence of a suitable nonionic surfactant PEG400. The chemical composi- tion and structural features of the products were investigated by elemental analyses, XRD, TG, SEM and TEM, respec- tively. The mechanisms of formation were also discussed.

室温固相反应一步合成N-亚水杨基-4-氨基安替比林

4 氨基安替比林与水杨醛通过室温固相反应合成N 亚水杨基 4 氨基安替比林 ,反应无溶剂 ,15min即可完成 ,产率达 95 % ,用元素分析 ,IR ,1HNMR ,X射线粉末衍射和X射线单晶衍射对产物进行了表征 .

室温固相结合水热处理制备纳米Mg-Al层状双金属氢氧化物

采用室温固相反应结合水热处理制备了纳米层状双金属氢氧化物(LDHs)。利用X射线粉末衍射(XRD)、傅里叶变换红外光谱(FT-IR)、扫描电镜(SEM)、热重(TG-DTA)等分析方法对样品的物相、形貌、粒径、热稳定性进行了表征。研究结果表明经水热处理后,产品颗粒由不规则的团聚体转化为规则的六方形片状结构,改善了晶体结晶性能,生成了分散性良好的层状双金属氢氧化物。

CuO-CeO_2的固相反应法制备及其催化CO低温氧化性能

采用固相化学反应法制备了一系列CuO-CeO_2催化剂,并用X-射线衍射(XRD)、程序升温还原(H_2-TPR)和氮吸附等技术对样品进行了表征,利用微反-色谱装置考察了其催化CO低温氧化反应的活性,研究了CuO含量和催化剂焙烧温度对CuO-CeO_2催化活性的影响。结果表明,随着CuO含量的增加,CuO-CeO_2的催化活性提高,至不小于15%时达到稳定;随焙烧温度的升高,CuO-CeO_2的催化活性先提高,至650℃时达到最大,之后又降低。CuO-CeO_2的催化活性与其CuO的还原性之间有较好的对应关系。

室温固相法合成纳米Mg-Al-CO_3层状双金属氢氧化物

首次报道了室温固相法合成纳米层状双金属氢氧化物(LDH)。采用XRD、FTIR、TEM分别对样品的物相、形貌、粒径等进行了表征。结果表明,产物呈针状,长约80nm,宽约10nm。室温固相法合成纳米LDH操作简单、转化率高、污染少,产物粒径小,粒度分布均匀,无团聚现象。

室温固态反应制备纳米Ba_(1-x)Sr_xTiO_3固溶体及其结构与介电性能研究

采用室温固态反应合成了一系列Ba1-xSrxTiO3固溶体纳米粉末(0≤x≤1.0).经XRD物相分析和d-间距-组成图证明,产品为立方晶系的完全互溶取代固溶体.TEM形貌观察,粒子基本为球形,平均粒径40nm.该方法具有产率高,无需溶剂,对环境无污染等优点.通过制陶实验,分别测定了该系列固溶体的室温介电常数、介电损失以及介电常数随温度的变化.结果发现,采用室温固态反应在BaTiO3中掺入适量锶,由于掺杂离子均匀进入母体晶格,引起居里点降低,室温介电常数达11000以上,介电损耗由BaTiO3纯相的0.03(3%)降为0.008(0.8%).纳米粉体的烧结温度为1180℃,比传统微米级粉体的烧结温度降低100～150℃.