Effect of high Pressure on the Solid-State Phase Transformation Microstructure of Cu-Zn Alloy

The solid-state phase transformation microstructure of Cu-Zn alloy under different high pressure were investigated by means of SEM and XRD. The results show that the α phase with smaller grain size, different shape and random distribution appears in the Cu-Zn alloy, when the solid-state phase transformation generation in the Cu-Zn alloy under 25～750 ℃ and 3～6 GPa high pressure, and the volume fraction of transformation phase decreases with increasing pressure, under high pressure (6 GPa), the changes of microstructure of Cu-Zn alloy is not obvious. In addition, the effect of high pressure on the solid-state phase transformation microstructure of Cu-Zn alloy was discussed.

Crystallization of amorphous (Fe_(0.99), Mo_(0.01))_(78)Si_9B_(13) alloy with solid state reaction at its surface under high pressure

Many experimental results have demonstrated that the nanocrystalline Fe-Mo-Si-B alloys prepared by crystallization of amorphous (Feo.99,Moo.o178Si9B13 （FMSB） alloy have many novel physical properties, except some brittleness. In order to solve this problem, the nanocrystalline alloy and a metal aluminum were bound together by isothermally annealing alternate layers consisting, of Al and amorphous FMSB alloy ribbons under high pressure in the present work to make an Al/Fe-Mo-Si-B alloy nanostructured composite. Different

Supercritical-hydrothermal accelerated solid state reaction route for synthesis of LiMn_2O_4 cathode material for high-power Li-ion batteries

Synthesis of the spinel structure lithium manganese oxide （LiMn2O4） by supercritical hydrothermal （SH） accelerated solid state reaction （SSR） route was studied. The impacts of the reaction pressure, reaction temperature and reaction time of SH route, and the calcination temperature of SSR route on the purity, particle morphology and electrochemical properties of the prepared LiMn2O4 materials were studied. The experimental results show that after 15 min reaction in SH route at 400 ℃ and 30 MPa, the reaction time of SSR could be significantly decreased, e.g. down to 3 h with the formation temperature of 800 ℃, compared with the conventional solid state reaction method. The prepared LiMn2O4 material exhibits good crystallinity, uniform size distribution and good electrochemical performance, and has an initial specific capacity of 120 mA.h/g at a rate of 0.1C （1C=148 mA/g） and a good rate capability at high rates, even up to 50C.

Effects of high-pressure heat treatment on the solid-state phase transformation and microstructures of Cu_(61.13)Zn_(33.94)Al_(4.93) alloys

The phase transformation activation energy of the Cu61.13Zn33.94A14.93 alloys, which were treated at 4 GPa and 700 ℃ for 15 minutes, was calculated by means of differential scanning calorimetry curves obtained at various heating and cooling rates. Then, the effects of high-pressure heat treatments on the solid-state phase transformation and the microstructures of Cu61.13Zn33.94A14.93 alloys were investigated. The results show that high-pressure heat treatments can refine the grains and can change the preferred orientation from （111） to （200） of α phase. Compared with the as-cast alloy, the sample with high-pressure heat treatment has finer grains, lower β＇→β and/β→β＇ transformation temperature and activation energy. Furthermore, we found that high cooling rate favours the formation of fine needle-like α phase in the range of 5-20℃/min.

Magnetic properties and crystallization kinetics of Zn_(0.5) Ni_(0.5) Fe_2O_4

Precursor of nanocrystalline Zno.sNio.sFe2O4 was obtained by grinding mixture of ZnSO4.7H2O, NiSO4.6H2O, FeSO4.7H2O, and Na2CO3.10H2O under the condition of suffactant polyethylene glycol （PEG）-400 being present at room temperature, washing the mixture with water to remove soluble inorganic salts and drying it at 373 K. The spinel Zn0.5Ni0.5Fe2O4 was obtained via calcining precursor above 773 K. The precursor and its calcined products were characterized by differential scanning calorimetry （DSC）, Fourier transform infrared （FF-IR）, X-ray diffraction （XRD）, and vibrating sample magnetometer （VSM）. The result showed that Zn0.sNio.sFe204 obtained at 1073 K had a saturation magnetization of 74 A.mLkg-1. Kinetics of the crystallization process of Zn0.5Ni0.5Fe2O4 was studied using DSC technique, and kinetic parameters were determined by Kissinger equation and Moynihan et al. equation. The value of the activation energy associated with the crystallization process of Zr0.5Ni0.5Fe2O4 is 220.89 kJ-mol-1. The average value of the Avrami exponent, n, is equal to 1.59±0.13, which suggests that crystallization process of Zn0.5Ni0.5Fe2O4 is the random nucleation and growth of nuclei reaction.

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.

Solid-liquid state pressure bonding of Si_3N_4 ceramics with aluminum based alloys and its mechanism

Solid liquid state pressure bonding of Si 3N 4 ceramics with aluminum based alloys, which contain a small amount of intermetallic compounds Al 3Ti or Al 3Zr, was investigated. With this new method, the heat resistant properties of the bonding zone metal are improved, and the joints’ strengths at high temperature is increased. The joints’ shear strength at room temperature and at 600 ℃ reach 126～133 MPa and 32～34 MPa, respectively, with suitable bonding pressure. The reaction between aluminum and Si 3N 4 ceramics, which produces Al Si N O type compounds is the dominant interfacial reaction, while the reactions between the second active element Ti or Zr in the aluminum based alloys and Si 3N 4 ceramics also occur to some extend. [

STUDIES ON SOLID STATE REACTIONS OF COORDINATION COMPOUNDS(LXⅡ)Solid state synthesis and crystal structure of the complex ICu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)CIJ·0.5CS_2

[Cu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)Cl]·0.5CS_2=,Mr=895.79,monoclinic,space group P2_1/a,a=17.231(3),b=14.611(2),c=18.000(3) ,β=105.56(2)°,V=4365(1) ~3, Z=4,D_c=1.37g/cm^3.,λ(MoK_α)=0.71073 ,μ=12.15cm^(-1),F(000)=1855,R=0.052, R_W=0.045 for 3930 observed reflections with Ⅰ>1.5σ(Ⅰ).The central metal atom has a dis. torted tetrahedral geometry with bond lengths Cu-S=2.384(2) (Au-S=2.389(4)), Cu-Cl=2.481(3)(Au-Cl=2.474(1))and Cu-P=2.269(2)-2.289(2)(Au-P=2.270(4)-2.279(4)) .

THE SOLID STATE CONTROLLED PHOTOCHEMICAL REACTION OF NITROBENZALDEHYDE WITH INDOLE

The solid state photochemical reaction of nitrobenzaldehyde with indole was investigated. Seven hey products were identified by IR, MS,^(1)H HMR and elemental analysis.

Effect of high pressure on the multilayered Al/Fe-Mo-Si-B nanostructured alloy composite

Study on preparation and properties of nanocrystalline (NC) alloys prepared by an-nealing amorphous alloy ribbons (such as amorphous Ni-P, Fe-Mo-Si-B alloy) has madegreat progress. It is favorable for the application of the NC alloys to bond the NC alloyto a metal with good toughness to prepare metal/NC alloy-multilayered composite,which has both good mechanical properties and structure and properties of NC alloy.

Solid State Synthesis and Crystal Structure of 3-Methyl-1-phenyl-4-phenylbenzoylmethylene-5-pyrazolone

The solid state thermal reaction of benzil with 3-methyl-1-phenyl-5-pyrazolone gave the title compound 1 (C_24H_18N_2O_2) and its isomer 2. The crystal structure of the title compound has been determined by X-ray analysis. The crystal belongs to monoclinic system, space group P2_1/n, with cell parameters a = 7. 479 ( 1 ), b =16. 992(1), c=15. 165(1) A , β= 100. 99(1)°, V= 1891. 9 A￣3, M_r=366. 42, Z=4, D_c= 1. 286 g/cm￣3, μ= 6. 236 cm￣-1, F(000) = 768. In the molecule of 1, benzoyl group and CO group of five-member ring are in cis-positions, the interaction of oxygen atoms leads to the noncoplanarity.

Solid-state Synthesis,Crystal and Band Structures,and Optical Properties of a Novel Ternary Sulfide Eu_2Ga_2S_5

One new ternary europium gallium sulfide, Eu2Ga2S5, has been synthesized by a facile solid-state route with boron as the reducing reagent. It crystallizes in the orthorhombic space group Pbca, with a = 11.976（1）, b = 11.074（1）, c = 17.446（1）A^°, V = 1650.6（3）A^°^3, and Z = 8. Its 3-D structure is built by the connection between EuS 7 monocapped trigonal prisms and GaS 4 tetrahedra, and the latter connect with each other to form layer-like slabs. Its optical energy gap is determined to be 2.17 eV, which is also verified by the electronic band structure calculation.

Highly Ordered Lattice Orientation of ZnO Nanoparticles Formed in Confined Space

Oriented aggregation of nanoparticles has been accomplished by means of solid state reac- tion. Non-crystallized and crystallized ZnO nanoparticles/clusters could be accommodated in the lamellar spacing of inorganic-organic composite, which were prepared by thermolysis of layered solid zinc-oleate complex at 260 and 300 ℃ in air, respectively. High-resolution transmission electron microscopy and selected area electron diffraction patterns indicate that aggregates are single crystals with various defects. The photoluminescence excitation spectra of both samples show two bands at 272 and 366 nm. The former may originate from electron transfer from valence band to conduction band in ZnO clusters composed of less than 200 ZnO molecules （2R〈2 nm）.

FINE STRUCTURES OF BOTH INTERFACES AND INTERFACIAL REACTION PRODUCTS

The characteristic of interface depending on the atomic structure exerts an inportant,and sometime controlling,influence on performance of the interacial materials. The present paper reviews the main studies on fine structure of both the materials inter- faces and interfacial reaction products in semiconductor uperlattice,metal multilayer ceram- ics and composite materials by mean of selected area electron doffraction patterns and high resolution electron microscopy. The following features of interfaces are reviewed:the orientation relationships;the char- acteristic of steps,facets and ronghness of interfaces;atomic bonding across the interface;the degree of coherency,the structure of misfit dislocations and elastic relaxations at the inter- faces:the presence of defects at the onterfaces:the structure of the interfacial reaction prod- ucts as well as the reaction kinetics and reaetion mechanism.

The Correlation of Miller Indices with the Conductivity Mechanism of Cu-Based High-Tc Superconductor

The high temperature superconductor of CuBa2Ca2Cu3O8+δ(Cu-1223) was synthesized experimentally by solid-state reaction. There were many pa-rameters affecting the preparation technique such as oxygen flow, sintering temperature, sintering time, and compacted pressure. The XRD-pattern exhibited a tetragonal phase for both Cu-1223, and Cu-1212. The resistivity measurement was considered the important experiment to show the predominant phase of superconductor if it was a high phase or low phase. The critical temperature (Tc) was about (128 K) for the high phase of Cu-1223, whereas the low phase of (Cu-1212) appeared at (Tc = 64 K). The correlation between the Miller indices and resistivity measurements was a good tool to predicate the expected mechanism of conductivity within the unit cell. It was clear that the arrangement of these planes was aligned in the a-c direction. That should make the motion of the charge to be simpler by a stepping plane toward c-axis.

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。

Towards High Molecular Weight Poly(bisphenol A carbonate) with Excellent Thermal Stability and Mechanical Properties by Solid-State Polymerization

Poly（bisphenol A carbonate） （BPA-PC） was post-polymerized by solid-state polymerization （SSP） after supercritical CO2-induced crystallization in low molecular weight particles prepolymerized via melt transesterification reaction. The effects of the crystallization conditions on melting behavior and SSP of BPA-PC were investigated with differential scanning calorimetry （DSC）, Ubbelohde viscosity method and gel permeation chromatography （GPC）. The reaction kinetics of the SSP of crystallized prepolymers was studied as a function of reaction temperatures for various reaction periods. As a result, the viscosity average molecular weight of BPA-PC particles （2 mm） increased from 1.9 × 10^4 g/mol to 2.8 × 10^4 g/mol after SSP. More importantly, the significantly enhanced thermal stability and mechanical properties of solid-state polymerized BPA-PC, compared with those of melt transesterification polymerized BPA-PC with the same molecular weight, can be ascribed to the substantial avoidance of undergoing high temperature during polymerization. Our work provides a useful method to obtain practical product of BPA-PC with high quality and high molecular weight.

合成工艺对固相法制备高四方性纯钛酸钡粉体的影响

钛酸钡是一种重要的功能陶瓷材料,因具有优异的电学性能而被广泛应用于多层陶瓷电容器(MLCC)等电子元器件。本研究以碳酸钡和二氧化钛为原料,采用固相法制备形貌均匀且四方性高的BaTiO_(3)粉体,系统研究了合成工艺(合成温度、升温速率和保温时间)对BaTiO_(3)粉体的影响。通过TG/DTA、XRD和SEM等测试手段对BaTiO_(3)粉体进行表征,结果表明:合成温度主要影响BaTiO_(3)粉体的四方性,保温时间和升温速率主要影响BaTiO_(3)粉体的粒径和粒度分布;原材料经过90 r/min球磨24 h后,在合成温度1050℃、升温速率5℃/min和保温时间3 h的条件下,制备了平均粒径为400 nm、四方性(c/a)为1.0091的形貌均匀的BaTiO_(3)粉体。本工作为固相法制备高可靠性MLCC用纯BaTiO_(3)粉体提供了良好的研究思路。

高熵过渡金属二硼化物的高温高压合成

高熵过渡金属二硼化物因其优异的力学性能及热物理性能受到了人们的广泛关注。然而,过去通过高温固相反应合成的效率较低。为此,通过高温高压固相反应,在5.5 GPa、2300℃的温压条件下合成了以VB_(2)、NbB_(2)、TaB_(2)为基底的6类高熵过渡金属二硼化物。高压提高了高温下的固相反应效率,促进了高熵过渡金属二硼化物的合成。通过X射线衍射和能量色散X射线光谱仪表征并确认了6类高熵过渡金属二硼化物均由纯相组成,不存在氧化物杂质或第二相,且元素分布均匀,不存在元素偏析,证明了高温高压合成高熵过渡金属二硼化物的有效性和普适性。

纳米SiO_(2)包覆Na_(2)Ca_(2.93)Si_(6)O_(16):7% Eu^(3+)荧光粉的制备及性能研究

采用传统高温固相法在1050℃烧结下制备了Na_(2)Ca_(3-x)Si_(6)O_(16)∶xEu^(3+)红色荧光粉,其中Na_(2)Ca_(2.93)Si_(6)O_(16)∶7%Eu^(3+)荧光粉的发光性能最好。采用溶胶-凝胶法制备出纳米SiO_(2)并包覆在Na_(2)Ca_(2.93)Si_(6)O_(16)∶7%Eu^(3+)荧光粉表面,包覆量为2%~10%(wt,质量分数,下同)。通过X射线衍射仪、激发-发射光谱分别对荧光粉物相结构和发光性能进行表征,采用CIE色度坐标分析软件对样品的色度图进行绘制。结果表明纳米SiO_(2)包覆量不同的荧光粉其基质结构未发生改变,纳米SiO_(2)包覆膜是无定型的,样品的发射峰位置没有变化,但发射强度不同;当纳米SiO_(2)包覆量为8%时,荧光粉发射强度最高,比Na_(2)Ca_(2.93)Si_(6)O_(16)∶7%Eu^(3+)荧光粉的发光强度明显提高,且此时色纯度更高,更接近正红色,CIE色度坐标为(0.5282,0.3210)。