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.

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.

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.

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 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.

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.

Influence of FeO and sulfur on solid state reaction between MnO-SiO_2-FeO oxides and an Fe-Mn-Si solid alloy during heat treatment at 1473 K

To clarify the influence of Fe O and sulfur on solid state reaction between an Fe-Mn-Si alloy and Mn O-Si O2-Fe O oxides under the restricted oxygen diffusion flux, two diffusion couples with different sulfur contents in the oxides were produced and investigated after heat treatment at 1473 K. The experimental results were also compared with previous work in which the oxides contained higher Fe O. It was found that although the Fe O content in the oxides decreased from 3wt% to 1wt% which was lower than the content corresponding to the equilibrium with molten steel at 1873 K, excess oxygen still diffused from the oxides to solid steel during heat treatment at 1473 K and formed oxide particles. In addition, increasing the sulfur content in the oxides was observed to suppress the diffusion of oxygen between the alloy and the oxides.

Carbonation Reaction of Lithium Hydroxide during Low Temperature Thermal Energy Storage Process

In order to apply lithium hydroxide(LiOH)as a low temperature chemical heat storage material,the carbonation reaction of LiOH and the prevention method are focused in this research.The carbonation of raw LiOH at storage and hydration condition is experimentally investigated.The results show that the carbonation reaction of LiOH with carbon dioxide(CO_(2))is confirmed during the hydration reaction.The carbonation of LiOH can be easily carried out with CO_(2) at room temperature and humidity.LiOH can be carbonated at a humidity range of 10%to 20%,a normal humidity region that air can easily be reached.Furthermore,the carbonation reaction rate has not nearly affected by the increase of reaction temperature.An improved storage method by storing LiOH at a low humidity less than 1.0%can be effectively prevented the carbonation of LiOH.The hydration reaction ratio of LiOH at the improved storage method shows a better result compared to the ordinary storage method.Therefore,the humidity should be carefully controlled during the storage of LiOH before hydration and dehydration reaction when apply LiOH as a low heat chemical storage material.

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.

Low Temperature Heat Capacities and Thermodynamic Properties of Zinc L-Threonate Zn(C_4H_7O_5)_2(s) by Adiabatic Calorimetry

Low-temperature heat capacities of the solid compound Zn（C4H7O5）2（s） were measured in a temperature range from 78 to 374 K, with an automated adiabatic calorimeter. A solid-to-solid phase transition occurred in the temperature range of 295？322 K. The peak temperature, the enthalpy, and entropy of the phase transition were determined to be （316.269±1.039） K, （11.194±0.335） kJ？mol-1, and （35.391±0.654） J？K-1？mol-1, respectively. The experimental values of the molar heat capacities in the temperature regions of 78？295 K and 322？374 K were fitted to two polynomial equations of heat capacities（Cp,m） with reduced temperatures（X） and [X = f（T）], with the help of the least squares method, respectively. The smoothed molar heat capacities and thermodynamic functions of the compound, relative to that of the standard reference temperature 293.15 K, were calculated on the basis of the fitted polynomials and tabulated with an interval of 5 K. In addition, the possible mechanism of thermal decomposition of the compound was inferred by the result of TG-DTG analysis.

Planck’s Oscillators at Low Temperatures and Haken’s Perturbation Approach to the Quantum Oscillators Reconsidered

In the first step the extremal values of the vibrational specific heat and entropy represented by the Planck oscillators at the low temperatures could be calculated. The positions of the extrema are defined by the dimensionless ratios between the quanta of the vibrational energy and products of the actual temperature multiplied by the Boltzmann constant. It became evident that position of a local maximum obtained for the Planck’s average energy of a vibration mode and position of a local maximum of entropy are the same. In the next step the Haken’s time-dependent perturbation approach to the pair of quantum non-degenerate Schr?dinger eigenstates of energy is re-examined. An averaging process done on the time variable leads to a very simple formula for the coefficients entering the perturbation terms.

The Application of Thermomechanical Dynamics (TMD) to the Analysis of Nonequilibrium Irreversible Motion and a Low-Temperature Stirling Engine

We applied the method of Thermomechanical Dynamics (TMD) to a low-temperature Stirling engine, and the dissipative equation of motion and time-evolving physical quantities are self-consistently calculated for the first time in this field. The thermomechanical states of the heat engine are in Nonequilibrium Irreversible States (NISs), and time-dependent thermodynamic work W(t), internal energy E(t), energy dissipation or entropy Qd(t), and temperature T(t), are precisely studied and computed in TMD. We also introduced the new formalism, Q(t)-picture of thermodynamic heat-energy flows, for consistent analyses of NISs. Thermal flows in a long-time uniform heat flow and in a short-time heat flow are numerically studied as examples. In addition to the analysis of time-dependent physical quantities, the TMD analysis suggests that the concept of force and acceleration in Newtonian mechanics should be modified. The acceleration is defined as a continuously differentiable function of Class C2 in Newtonian mechanics, but the thermomechanical dynamics demands piecewise continuity for acceleration and thermal force, required from physical reasons caused by frictional variations and thermal fluctuations. The acceleration has no direct physical meaning associated with force in TMD. The physical implications are fundamental for the concept of the macroscopic phenomena in NISs composed of systems in thermal and mechanical motion.

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.

Low-heating solid state synthetic reactions of cyclopeantadienyl organolanthanide complexes

A novel and simple one-step, solid state reaction of multicomponent systems has been developed to synthesize cyclopentadienyl-containing organolanthanide complexes, in which the effects of the coordinated solvent molecules and the nature of the reactants were also studied. We also studied the solid state decomposition reaction of Cp2YbPz(HPz), and the formation of [CpYb(Pz)2]2 may indicate that the constrained environment in solid state can lead to a novel chemical transformation, with product selectivity possibly different from that in the liquid phase.

液相Y、Nb共掺杂BaTiO_3基PTC陶瓷的制备与性能

本文以Ba(OH)2.8H2O、Sr(OH)2.8H2O、TiCl4、NbCl5、YCl3和Mn(Ac)2为原料,采用室温研磨、低温固态反应合成了一系列的纳米钛酸钡基PTCR陶瓷粉,首先实现了Y和Nb双施主以离子的形式共掺杂。采用XRD,TEM对样品进行了表征。研究表明,产品为立方晶系的完全互溶取代固溶体。粒子基本成球形,分布均匀,粒径大约60 nm。通过优化Y和Nb的掺杂量,使材料的室温电阻得到了进一步降低,并提高了材料的升阻比。当Y、Nb和Mn的用量分别为0.2 mol%、0.18 mol%和0.04 mol%时,加入定量的AST烧结助剂,控制最高烧结温度为1310℃,制备出了室温电阻17.6Ω,正温度系数为18.6%/℃,升阻比为6.5×104的性能优异的PTCR电阻材料。另外还就烧结条件对材料PTC性能的影响进行了讨论。

Low temperature solid-state synthesis and characterization of uniform YF_3 submicroparticles

In this paper, submicro-scaled YF3 particles with uniform rice-like morphologies were facilely synthesized by reacting yttrium nitrate with tetrabutylammonium fluoride via a solid-state reaction process at 50 °C for 12 h.The phase confirmation and morphology of the as-prepared YF3 particles were investigated by X-ray powder diffraction（XRD） and scanning electron microscopy（SEM）.SEM results reveal that the YF3 submicroparticles are about 700 nm in length and 260 nm in width. Eu^3＋ and Tb^3＋ doped YF3 submicroparticles were also prepared with similar process and their photoluminescence properties were studied. Results demonstrate that the doping of Eu^3＋ and Tb^3＋ has slight effect on the morphologies of the product. Owing to the small average crystallite size or the low crystallinity of the product, the photoluminescence intensity of the Eu^3＋ and Tb^3＋ doped YF3 submicroparticles is very weak. Some characteristic peaks even cannot be observed in the emission spectrum.

Bi掺杂BaTiO_3基PTC陶瓷的制备、微结构和电性能

采用液相掺杂及低温固相反应法制备了Bi掺杂BaTiO3纳米晶体,然后经烧结制得了Bi掺杂BaTiO3基PTC陶瓷。分析了所制Bi掺杂BaTiO3晶体的物相、晶粒大小及微结构,研究了烧结条件对所制PTC陶瓷电性能的影响。结果表明:Bi掺杂BaTiO3晶体在常温下为立方晶系,颗粒基本呈球形且大小均匀,粒径约为60 nm;在烧结温度为1 330℃、保温时间为20 min条件下所制PTC陶瓷性能最佳:室温电阻为26.29,升阻比为3.585×104。

Preparation and gas sensing properties for acetone of amorphous Ag modified NiFe_2O_4 sensor

Nickel ferrite nano-powders were prepared by microwave radiating low-temperature solid-state reaction method, and then modified with Ag by dipping method. The crystal structure and morphology of the samples were characterized by means of X-ray diffraction（XRD）, scanning electron microscopy （SEM） and X-ray photoelectron spectroscopy （XPS）. The gas sensing properties of the samples were also investigated. The results reveal that the Ag, as amorphous structure, can efficiently prevent the reuniting and growing-up of nanosized NiFe2O4 grains, and 1.5% Ag modified NiFe2O4 sensor has a better sensitivity, up to 43, for acetone gas than 1.5%Ag mixed NiFe2O4 sensor prepared by low-temperature solid-state reaction, at an optimal working voltage of 4.5 V. The quick response time （1 s） and fast recovery time （～10 s） are the main characteristics of this sensor.

无铅高居里点BaTiO_3-Bi_(0.5)K_(0.5)TiO_3陶瓷的制备及其PTC性能的研究

采用固相反应法制备了(1-x)BaTiO3-xBi0.5K0.5TiO3(BT-BKT,x=0,0.1和0.2),对陶瓷样品进行X射线衍射、扫描电镜、介电常数-温度及电阻率-温度测试分析,研究了掺杂BKT对该系统陶瓷相组成、显微结构和电性能的影响。结果表明:BaTiO3陶瓷的晶格参数c轴值随着BKT含量的增加基本不变,而a轴值有所减小。BT-BKT陶瓷的居里温度(Tc)随着BKT的加入向高温移动,当x=0.1和0.2时,Tc分别提高至170℃和185℃左右;但室温电阻率随着BKT含量的增加明显增大。

基于LTCC技术的BaTiO_3-NiCuZn复合材料的研制

采用高纯度原材料,严格控制主配方和生产工艺,由固相反应法制备出高性能的低温烧结NiCuZn铁氧体材料,然后再与高介电钙钛矿(BaTiO3)混合低温烧结制得一类新型介电-铁磁复合材料。固定助溶剂Bi2O3比例2%,研究了铁电-铁磁含量对复合材料的电容、电感双性的影响,并将材料在生产线进行流延测试,表明流延效果良好。这种材料解决了介电与铁磁材料层低温共烧兼容的问题。