Effect of CuO particle size on synthesis temperature and microstructure of Al_2O_(3p)-Al composites from Al-CuO system

Al2O3p-Al composites were synthesized using an in-situ reaction in the 80%Al-20%CuO （mass fraction） system. The effects of the CuO particle size on the synthesis temperature and microstructure of the composites were investigated by various methods. The results indicate that the CuO particle size has a significant effect on the temperature at which the complete reaction in the Al-CuO system occurs：the temperature is 200 ℃ lower in the Al-CuO system containing CuO particles with sizes less than 6μm than that containing CuO particles with sizes less than 100μm. The interfacial bonding between Al2O3 particles and Al is not complete when the temperature is below a critical value. The morphology of the Al2O3 particles varies from ribbon-like shape to near spherical shape when the temperature is above a critical value. These two critical temperatures are affected by the particle size of CuO, and the critical temperature of the sample containing CuO particles with sizes less than 6μm is 100 ℃ lower than that of the sample containing CuO particles with sizes less than 100μm.

Effects of synthesis temperature and raw materials composition on preparation of β-Sialon based composites from fly ash

β-Sialon based composites were successfully prepared from fly ash and carbon black under nitrogen atmosphere by carbothermal reduction-nitridation process. Effects of heating temperature and raw materials composition on synthesis process were investigated, and the formation process of the composites was also discussed. The phase composition and microstructure of the composites were characterized by X-ray diffraction and scanning electronic microscopy. The results show that increasing heating temperature or mass ratio of carbon black to fly ash can promote the formation of β-Sialon. The β-Sialon based composites can be synthesized at 1723 K for 6 h while heating the sample with mass ratio of carbon black to fly ash of 0.56. The as-received β-Sialon in the composites exists as granular with an average particle size of 2-3 μm. The preparation process of β-Sialon based composites includes the formation of O′-Sialon, X-Sialon and β-Sialon as well as the conversion processes of O′-Sialon and X-Sialon to β-Sialon.

Influence of Synthesis Temperature on Phosphate Adsorption by Zn-Al Layered Double Hydroxides in Excess Sludge Liquor

A group of Zn-Al layered double hydroxides (LDHs) were synthesized at different temperatures from 25-90 °C in order to investigate the influence of synthesis temperature on characteristics of the LDHs and their phosphate adsorption behaviour. The results reveal that an increase in the synthesis temperature generally improves the specific surface area of the sample and the phosphate adsorption capacity. The significantly enhanced crystallin- ity of the Zn-Al-30, synthesized at 30 °C, leads to a remarkable decrease in the specific surface area and consequently a poor phosphate adsorption capacity. It is suggested that the surface adsorption plays an important role in the phosphate uptake by the Zn-Al LDHs. Zn-Al-70 presents a relatively higher crystallinity and a lower specific surface area, compared with Zn-Al-60 and Zn-Al-80, but the highest phosphate adsorption capacity, indicating that surface adsorption is only one of the pathways for phosphate removal. The phosphate adsorption by the Zn-Al follows a pseudo-second-order kinetic equation. The adsorption isotherms fit Langmuir models, and the maximum a dsorption capacities of the Zn-Al-25, Zn-Al-50 and Zn-Al-70 are estimated to be 17.82, 21.01 and 27.10 mg·g-1 adsorbent, respectively.

Room Temperature Synthesis of Vertically Aligned Amorphous Ultrathin NiCo-LDH Nanosheets Bifunctional Flexible Supercapacitor Electrodes

Developing a simple scalable method to fabricate electrodes with high capacity and wide voltage range is desired for the real use of electrochemical supercapacitors.Herein,we synthesized amorphous NiCo-LDH nanosheets vertically aligned on activated carbon cloth substrate,which was in situ transformed from Co-metal-organic framework materials nano-columns by a simple ion exchange process at room temperature.Due to the amorphous and vertically aligned ultrathin structure of NiCo-LDH,the NiCo-LDH/activated carbon cloth composites present high areal capacities of 3770 and 1480 mF cm^(-2)as cathode and anode at 2 mA cm^(-2),and 79.5%and 80%capacity have been preserved at 50 mA cm^(-2).In the meantime,they all showed excellent cycling performance with negligible change after>10000 cycles.By fabricating them into an asymmetric supercapacitor,the device achieves high energy densities(5.61 mWh cm^(-2)and 0.352 mW cm^(-3)).This work provides an innovative strategy for simplifying the design of supercapacitors as well as providing a new understanding of improving the rate capabilities/cycling stability of NiCo-LDH materials.

Synthesis of Neodymium-Doped Yttrium Aluminum Garnet (Nd∶YAG) Nano-Sized Powders by Low Temperature Combustion

The homogeneously dispersed, less agglomerated (Nd0.01Y0.99)3Al5O12 nano-sized powders were synthesized by the low temperature combustion (LCS), using Nd2O3, Y2O3, Al(NO3)3·9H2O, ammonia water and citric acid as starting materials. This method effectively solves the problems caused by solid-state reaction at high temperature and hard agglomerates brought by the chemical precipitation method. The powders were characterized by TG-DTA, XRD, FT-IR, TEM respectively and the photoluminescence (PL) spectra of (Nd0.01Y0.99)3Al5O12 green and sintered ceramic disks were measured. The results show that the forming temperature of YAG crystal phase is 850 ℃ and YAP crystal phase appearing during the calcinations transforms to pure YAG at 1050 ℃. The particle size of the powders synthesized by the LCS is in a range of 20～50 nm depending on the thermal treatment temperatures. The effectively induced cross section (σin) with the value 4.03×10-19 cm2 of (Nd0.01Y0.99)3Al5O12 ceramics is about 44% higher than that of single crystal.

Self-propagating high temperature synthesis of MoSi_2 matrix composites

MoSi2 is presently regarded as the most important material for electrical heating and as one with huge potential for high temperature structural uses. MoSi2 and MoSi2 matrix composites were prepared by self-propagating high temperature synthesis （SHS）. Pure MoSi2 was obtained and a compound of MoSi2 and WSi2was synthesized in the form of predominant solid solution （Mo,W）Si2. By adding aluminum of 5.5 at.% to Mo-Si, the crystal structure of MoSi2 changed into a mixture of tetragonal Cllb MoSi2and hexagonal C40 Mo（Si,Al）2. The （Mo,W）Si2-Mo（Si,Al）2-W（Si,Al）2 composite materials were synthesized by adding aluminum of 5.5 at.% to Mo-W-Si. However, if the amount of the added aluminum was not larger than 2.5 at.%, it did not have any significant effect. SHS is an effective technology for synthesis of MoSi2 and MoSi2 matrix composites.

Preparation of low-oxygen Ti powder from TiO_(2) through combining self-propagating high temperature synthesis and electrodeoxidation

An effective method was reported to prepare low-oxygen Ti powder,which included two experimental steps:the fast conversion of TiO_(2) to TiO_(x<1) powder by self-propagating high-temperature synthesis(SHS)process and the generation of low-oxygen Ti powder by electrodeoxidizing TiO_(x<1) powder at the cathode in molten CaCl_(2).The key intermediate steps were analyzed by XRD,SEM and electrochemical testing techniques.The results demonstrated that TiO_(x<1) powder(TiO_(0.325) and TiO_(0.97))was generated after acid leaching MgO in SHS products with TiO_(2)/Mg molar ratio of 1:2,and the TiO_(x<1) powder with 16.3 wt.%oxygen could be transformed into pure titanium powder with 0.121 wt.%oxygen by electrodeoxidation at a constant potential of−3.3 V for 10 h.The electrodeoxidation of TiO_(x<1) powder in CaCl_(2) molten salt follows the step-by-step deoxidation mode,and the lattice of TiO_(x<1) powder after electrodeoxidation shrinks.

Fabrication of Titanium Diboride-Cu Composite by Self-High Temperature Synthesis plus Quick Press

Titanium diboride based composites, good candidates for contact materials, have high hardness, Young＇s modulus, high temperature stability, and excellent electrical, thermal conductivity. However a good interface of TiB2/Cu is very difficult to achieve for oxidation of TiB2. To avoid this oxidation behavior, the in situ combusting synthesis technology, SHS, was used to prepare TiB2/Cu composite. The characters of Ti-B-xCu SHS were studied in detail, such as combustion temperature, products phases and grain size. Based on the experimental results a proper technology way of self-high temperature synthesis plus quick press （SHS/QP） was determined and compact TiB2/Cu composites with relative density over than 97 pct of the theoretical were fabricated by this method. The properties and microstructures of these TiB2 based composites were also investigated.

A Self-propagating high-temperature synthesis process for the fabrication of Fe（Cr）–Al2O3 nanocomposite

Self-propagating high-temperature synthesis(SHS)was used to fabricate a Fe(Cr)–Al2O3 nanocomposite.The composite was fabricated by the reactions between the powders of Fe,Fe2O3,Cr2O3,and Al.The effect of blending ratio and mechanical activation of the initial powders and the precursor compressing pressure on the microstructure of the final product was studied by optical microscopy,scanning electron microscopy,transmission electron microscopy,and X-ray diffraction.The significance of the effect of each of the aforementioned parameters on the quality of the composite(assessed by measuring the compressive strength and wear resistance)was determined using a full-factorial design of experiments method.The results showed that the best molar powder ratio that produced the most homogeneous product through a sustainable SHS reaction was Fe:Fe2O3:Cr2O3:Al=10:1:1:4.A lower Fe content caused the Fe(Cr)phase to melt and separate from the rest of the materials.

Temperature Fluctuation Synthesis/Simultaneous Densification and Microstructure Control of Titanium Silicon Carbide (Ti_3SiC_2) Ceramics

A novel temperature fluctuation synthesis/simultaneous densification process was developed for the preparation of Ti3SiC2 bulk ceramics. In this process. Si is used as an in-situ liquid forming phase and it is favorable for both the solid-liquid synthesis and the densification of Ti3SiC2 rainies. The present work demonstrated that the temperature fluctuation synthesis/simultaneous densification process is one of the most effective and simple methods for the preparation of Ti3SiC2 bulk materials providing relatively low synthesis temperature. short reaction time; and simultaneous synthesis and densification. This work also showed the capability to control the microstructure, e.g., the preferred orientation, of the bulk Ti3SiC2 materials simply by applying the hot pressing pressure at different Stages of the temperature fluctuation process. And textured Ti3SiC2 bulk materials with {002} faces of laminated Ti3SiC2 grains normal to the hot pressing axis were prepared.

Room temperature synthesis of single-crystal Te nanorods from Na_2TeO_4

Single-crystalline tellurium nanorods were synthesized through the reduction of Na2TeO4 by hydrazine monohydrate, in the absence of surfactants, in an aqueous ammonia solution at room temperature. X-ray diffraction （XRD）, transmission electron microscopy （TEM）, and selected area electron diffraction （SAED） were used to characterize the composition and morphology of the products. The concentration of the OH ion has a significant influence on the morphology of the products and is found to be responsible for tailoring the crystal growth dynamically： the concentration of Te blocking in the solution is reduced via increasing the concentration of the OH^- ion, and subsequently the nucleation rate of Te is suppressed and Te nanorods gradually grow because of the inherently anisotropic structure of Te. New generation tellurium atoms add to the surface of the particles during the long period of reaction.

Low Temperature Direct Synthesis of Strontium Titanate Powder

Low temperature direct synthesis (LTDS) involves the preparation of a base solution of Sr^(2+),and the mixing of base solution with tetrabutyl titanate solution.LTDS is an advantageous method because it does not require the complex hydrothermal facilities and it can prevent the agglomeration in calcinations of other liquid methods.In our work,we adopted LTDS method to prepare the nano strontium titanate powders,and characterize them by XRD,FT-IR and TGA.The influences of preparation temperature and solvents on grain size and lattice parameters were investigated.The results show that preparation temperature can slightly change the lattice parameters of grain,while solvents also play important roles in the preparation.

Synthesis and Characterization of Magnesium Substituted Aluminophosphate Molecular Sieves with AEL Structure

MAPO-11 molecular sieves were synthesized by hydrothermal methods. The influence of precursor of magnesium, Mg/Al ratio, synthesis temperature, synthesis time and the type of template on the formation and properties of MAPO-11 molecular sieves was examined. The samples were characterized by the techniques of X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric/differential thermogravimetric analysis (TG-DGA), etc. The results show that the shape and size of crystal were influenced by the precursor of Mg, the Mg/Al ratio and the type of template, and the TG-DGA analysis shows that MAPO-11 molecular sieves as-synthesized have poor thermal stability.

A New Dinuclear Zinc Polymer Based on 3-Methoxy-2-hydroxybenzaldehyde:Synthesis,Structure,Spectral Characterization and Hirshfeld Surface Analysis

A highly efficient fluorescence material dinuclear zinc polymer [Zn2（mhbd）2（dca）2]n （1, Hmhbd is 3-methoxy-2-hydroxybenzaldehyde, dca is N（CN）2？） has been synthesized under room temperature and structurally characterized by elemental analysis, IR, and single-crystal X-ray diffraction. The structure belongs to the triclinic system, space group P with a = 8.475（1）, b = 9.595（1）, c = 15.001（1） A, α = 86.84（1）, β = 81.10（1）, γ = 68.78（1）°, Mr = 565.15, V = 1123.5（1） ？3, Dc = 1.671 g？cm–3, F（000） = 568, μ = 2.185 mm–1, R = 0.0451, and wR = 0.1297. 1 is a dinuclear zinc complex which further constructs a 1D chain through double μ1,5-dca bridge. Luminescent property and Hirshfeld surface analysis of 1 have been studied. The result indicates that the fluorescence intensity of complex 1 is forty-one times the fluorescence intensity of Hmhbd ligand.

A Novel Nanocrystalline TiO_2 Thin Film Electrodes Prepared at Low Temperature

Nanocrystalline TiO2 thin films were successfully prepared by a new “water-cooked” method on both conductive glass substrates and flexible substrates at low temperature. Dye-sensitized solar cells based on these films have exhibited high overall light-to-electricity conversion efficiencies of 4.67 % and 1.94 % on conductive glass substrate and flexible substrate, respectively, under the illumination at 100 mW/cm2.

Diffusion Mechanism of Energy Flow in Multi-heat-source Synthesis of SiC

Through the experiments and the numerical simulation of temperature field in multi-heatsource synthesis Si C furnace, in order to research the feature point in multi-heat-source synthesis furnace, the variation law of heat fl ux was studied and the multi-directional energy fl ow diffusion mechanism was revealed. The results show that, due to the shielding action between the heat-source and the superposition effect of thermal fields, the insulating effect is best in multi-heat-source synthesis furnace. The heat emission effect is good outside the common area between heat-sources, but the heat storage is poor. Compared with the synthesis furnace that heat source is parallelly arranged, the furnace of stereoscopic arrangement has a more obvious heat stacking effect and better heat preservation effect, but the air permeability of heat source connecting regions is worse. In the case with the same ingredients, the resistance to thermal diffusion and mass diffusion is higher in heat source connecting regions.

Synthesis gas production on glass cloth catalysts modified by Ni and Co oxides

The catalytic activity of nanostructured low percent (1%) Co-Ni catalysts on the basis of glass fiber (GF) prepared by a"solution combustion" (SC) method was studied.The catalytic activity of the prepared samples was studied in the reaction of dry reforming of methane (DRM) with CO2.The obtained samples were characterized by a number of physico-chemical methods,including XRD,SEM,TEM,TGA and AFM.The active component was shown to be dispersed in the near-surface layer of the support as nanoparticles of 10—20 nm in size.The active component showed a Co3O4 or(Co,Ni)Co2O4 spinel structure,depending on the catalyst composition.The spinel structure of the active component interacted strongly with the carrier,providing resistance to carbonization,high catalytic activity toward DRM,and high activity and stability in oxidation reactions.

Room-temperature synthesis of layered open framework cathode for sodium-ion batteries

The synthesis of active electrode materials at room temperature is one of the effective strategies to reduce the fabrication cost of sodium ion batteries(SIBs).Herein,a layered material(Na_(2)[(VO)_(2)(HPO_(4))_(2)C_(2)O_(4)]·2H_(2)O,abbreviated as NVPC followingly)with open-framework structures has been successfully prepared at room temperature under ambient conditions and is evaluated as a cathode for SIBs.It is revealed that NVPC cathode can deliver a maximum reversible capacity of ca.70 mAh/g at 10 mA/g,and exhibit superior rate capability and cycling performance:at 50 mA/g,maximum reversible capacity ca.50 m Ah/g with capacity retention of 88.4%over 250 cycles corresponds to only 0.046%capacity decay per cycle;at 100 mA/g,a maximum reversible capacity of 35 mAh/g with capacity retention of60.9%over 500 cycles.This study demonstrates a practical example of a low-cost synthesis of the cathode materials for SIBs.At the same time,the systematic electrochemical research results also show promising prospects for long lifespan low-cost SIBs.

A New Route for the Rapid Synthesis of Metal–Organic Frameworks at Room Temperature

Rapid synthesis of metal–organic frameworks(MOFs),especially high-valence MOFs at roomtemperature without external energy,is a challenging topic.In this work,a stable radical solution has been discovered.Various MOFs with versatile metal nodes and ligands were rapidly synthesized at room temperature in the absence of external energy.Especially,MOFs with conjugated ligands achieved instantaneous architecture(in less than 1 s)and quantitative yield.Radicals in the solution play a crucial role in the accelerated kinetics,and the new radical route paves a cyclic pathway for the MOF synthesis.The mechanism has been thoroughly investigated by electron paramagnetic resonance,in situ proton nuclear magnetic resonance,X-ray absorption spectra,in situ small-angle X-ray scattering-wide-angle X-ray scattering,and density functional theory calculations.

The relationship between the microstructures and catalytic behaviors of iron–oxygen precursors during direct coal liquefaction

A series of both unsupported and coal‐supported iron–oxygen compounds with gradual changes in microstructure were synthesized by a precipitation‐oxidation process at 20 to 70°C.The relationship between the microstructures and catalytic activities of these precursors during direct coal liquefaction was studied.The results show that the microstructure could be controlled through adjusting the synthesis temperature during the precipitation‐oxidation procedure,and that compounds synthesized at lower temperatures exhibit higher catalytic activity.As a result of their higher proportions ofγ‐FeOOH orα‐FeOOH crystalline phases,the unsupported iron–oxygen compounds synthesized at 20–30°C,which also had high specific surface areas and moisture levels,generate oil yields 4.5%–4.6%higher than those obtained with precursors synthesized at 70°C.It was also determined that higher oil yields were obtained when the catalytically‐active phase formed by the precursors during liquefaction(pyrrhotite,Fe1-xS)had smaller crystallites.Feed coal added as a carrier was found to efficiently disperse the active precursors,which in turn significantly improved the catalytic activity during coal liquefaction.