One-pot synthesis of hollow octahedral Cu2O nanostructures at room temperature

Homogeneous hollow Cu2O octahedral nanostructures have been fabricated by a facile one-pot reduction reaction at room temperature. The microscope analysis revealed that the edges of as-prepared hollow structures were around 200 nm with a wall thickness of about 20 nm. To investigate the influence factors and formation mechanism of the hollow octahedral structure, samples subjected to different reaction conditions were studies. The results showed that the morphology and structures of Cu2O particles were greatly affected by the concentration of pH value of the reaction environment and the reaction time. Ostwald ripening process is proposed to explain the growth mechanism of the hollow octahedral nanostructures.     

Performances of lithium manganese oxide prepared by hydrothermal process

A simple hydrothermal process followed by heat treatment was applied to the preparation of spinel Li1.05Mn1.95O4. In this process, electrolytic manganese dioxide（EMD） and LiOH·H2O were used as starting materials. The physiochemical properties of the synthesized samples were investigated by thermogravimetry-differential scanning calorimetry（TG-DSC）, X-ray diffractometry（XRD）, and scanning electronic microscopy（SEM）. The results show that the hydrothermally synthesized precursor is an essential amorphous. The precursor can be easily transferred to spinel powders with a homogeneous structure and a regularly-shaped morphology by heat treatment. Li1.05Mn1.95O4 powder obtained by heat treating the precursor at 430 °C for 12 h and then calcining at 800 °C for 12 h shows an excellent cycling performance with an initial charge capacity of 118.2 mA·h·g-1 obtained at 0.5C rate and 93.8% of its original value retained after 100 cycles.     

Synthesis,characterization of monodispersed MgO microspheres and thermal decomposition kinetics of its precusor

Monodispersed MgO microspheres were successfully synthesized by a simple solvothermal method using PEG-400 as solvent. The samples were characterized by X-ray diffraction（XRD） and scanning electron microscopy（SEM）. The results reveal that the precusor was monoclinic Mg5（CO3）4（OH）2·4H2O and composed of nanosheets with the thickness of about 250 nm. By calcining the precusor at 500 °C for 5 min, cubic MgO with similar morphology was obtained. According to the SEM images, it is found that the volume ratio of PEG-400 to deionized water is considered as a crucial factor in the evolution of the morphology. Based on the SEM images obtained under different experimental conditions, a possible growth mechanism which involves self-assembly process was proposed. The thermal decomposition process of MgO precusor was studied by thermogravimetry-differential thermogravimetry（TG-DTG） at different heating rates in air. Thermal analysis kinetics results show that the most probale mechanism models of MgO precusor are An and D3, respectively. In addition, isothermal prediction was studied to quantitatively characterize the thermal decomposition process.     

Preparation of AgSnO2 composite powders by hydrothermal process

Silver-tin oxide powders were synthesized by the hydrothermal method with Ag（NH3）2^＋ solution and Na2SnO3 solution as raw materials and Na2SO3 as reductant. The precipitation conditions of Na2SnO3 solution and the reduction conditions of Ag（NH3）2^＋ were also investigated. The powders prepared were characterized by differential thermal analysis （DTA）, X-ray diffraction analysis （XRD）, scanning electron microscope （SEM） and energy spectrum analysis, The results show that pH value of the solution is a key parameter in the formation of Sn（OH）4 precipitate and the reduction reaction of Ag（NH3）2^＋ can release H^＋ ions, which results in synchronous precipitation of Sn（OH）6^2- as Sn（OH）4. The reduction of Ag（NH3）2^＋ and precipitation of Na2SnO3 occur simultaneously and the coprecipitation of silver and tin oxide is reached by the hydrothermal method. The silver-tin oxide composite powders have mainly flake shape of about 0.3 μm in thickness and there exists homogeneous distribution of tin oxide and silver in the powder synthesized.     

Electrolyte composition and removal mechanism of Cu electrochemical mechanical polishing

The optimization of electrolytes and the material removal mechanisms for Cu electrochemical mechanical planarization （ECMP） at different pH values including 5-methyl-1H-benzotriazole （TTA）, hydroxyethylidenediphosphoric acid （HEDP）, and tribasic ammonium citrate （TAC） were investigated by electrochemical techniques, X-ray photoelectron spectrometer （XPS） analysis, nano-scratch tests, AFM measurements, and polishing of Cu-coated blanket wafers. The experimental results show that the planarization efficiency and the surface quality after ECMP obtained in alkali-based solutions are superior to that in acidic-based solutions, especially at pH=8. The optimal electrolyte compositions （mass fraction） are 6% HEDP, 0.3% TTA and 3% TAC at pH=8. The main factor affecting the thickness of the oxide layer formed during ECMP process is the applied potential. The soft layer formation is a major mechanism for electrochemical enhanced mechanical abrasion. The surface topography evolution before and after electrochemical polishing （ECP） illustrates the mechanism of mechanical abrasion accelerating electrochemical dissolution, that is, the residual stress caused by the mechanical wear enhances the electrochemical dissolution rate. This understanding is beneficial for optimization of ECMP processes.     

Isothermal reduction of titanomagnetite concentrates containing coal

The isothermal reduction of the Panzhihua titanomagnetite concentrates （PTC） briquette containing coal under argon atmosphere was investigated by thermogravimetry in an electric resistance furnace within the temperature range of 1250-1350°C. The samples reduced in argon at 1350°C for different time were examined by X-ray diffraction （XRD） analysis. Model-fitting and model-free methods were used to evaluate the apparent activation energy of the reduction reaction. It is found that the reduction rate is very fast at the early stage, and then, at a later stage, the reduction rate becomes slow and decreases gradually to the end of the reduction. It is also observed that the reduction of PTC by coal depends greatly on the temperature. At high temperatures, the reduction degree reaches high values faster and the final value achieved is higher than at low temperatures. The final phase composition of the reduced PTC-coal briquette consists in iron and fer-rous-pseudobrookite （FeTi2O5）, while Fe2.75Ti0.25O4, Fe2.5Ti0.5O4, Fe2.25Ti0.75O4, ilmenite （FeTiO3） and wustite （FeO） are intermediate products. The reaction rate is controlled by the phase boundary reaction for reduction degree less than 0.2 with an apparent activation energy of about 68 kJ·mol-1 and by three-dimensional diffusion for reduction degree greater than 0.75 with an apparent activation energy of about 134 kJ·mol-1. For the reduction degree in the range of 0.2-0.75, the reaction rate is under mixed control, and the activation energy increases with the increase of the reduction degree.     

Facile route to prepare TaC,NbC and WC nanoparticles

By a novel solid-state reaction process using amorphous C3N4 （α-C3N4） and transition metal oxides as starting reagents, cubic TaC, NbC and hexagonal WC nanoparticles were successfully synthesized at 1150 . The products were characterized by power X-ray diffraction （XRD）, field-emission scanning electron microscope （FE-SEM）, energy-dispersive X-ray spectroscopy （EDX） transmission electron microscopy （TEM） and high-resolution TEM （HRTEM）. The experimental results show that a-C3N4 obtained by the reaction between C3N3C13 and Li3N is a highly efficient carburation reagent and the transition metal oxides are completely transformed into the corresponding metal carbide nanoparticles at 1150 ℃, respectively, which is significantly lower than that reported for the traditional preparation of carbides, typically〉 1600 ℃. The TaC, NbC and WC nanoparticles are found to have an average particle size of 10 nm, 15 nm and 8 nm by TEM observation, respectively.     

Hydrothermal synthesis and photoluminescence behavior of CeO2 nanowires with the aid of surfactant PVP

Well-crystalline CeO_2 nanowires were prepared via a surfactant-assisted hydrothermal process.Reaction temperature and reaction time were changed for the determination of optimal synthesis parameters.The as-obtained products were characterized by X-ray diffraction (XRD),high-resolution transmission electron microscopy(HRTEM),and field emission scanning electron microscopy(FESEM).The results show that single crystal CeO_2 nanowires with high yield and good uniformity can be obtained hydrothermally at 180℃...     

Tribological Properties of MoSi2 Against AISI10045 Steel Under Sliding Friction

MoSi2 samples were prepared by a self-propagating high-temperature synthesis （SHS） and a hot-press technique. The sliding friction and wear properties of intermetallic MoSi2 against AISI10045 steel under dry friction and oil lubrication conditions were investigated with a MRH-5A type ring-on-block friction and wear tester. The elemental composition, microstructure and worn surface morphology of the MoSi2 material were observed and analyzed by means of scanning electron microscopy （SEM） and X-ray diffraction （XRD）. The synthetic parameter pv value reflecting friction work, was used to discuss the tribological properties of MoSi2 material. The results show that 1） oil lubrication can obviously improve the tribological properties of MoSi2, 2） the bigger the pv value, the greater the antifriction and the abrasive resistance of MoSi2 under oil lubrication, 3） with an increase in the pv value, the wear mechanism of MoSi2 material under dry sliding friction is the fatigue fracture and adhesive wear and 4） under oil lubrication the wear mechanism is mainly fatigue pitting.     

Synthesis of spin-ladder Sr<Subscript>14</Subscript>Cu<Subscript>24</Subscript>O<Subscript>41</Subscript> material by citrates sol-gel method

A new process to synthesize polycrystalline samples of Sr14Cu24O41 was presented. Firstly, dry gel powder of Sr14Cu24O41 was synthesized by the citrates sol-gel method, using Sr（NO3）2, Cu（NO3）2, ethylene glycol and citrate acid as raw materials. Then, polycrystalline samples of Sr14Cu24O41 were prepared by solid-state reaction. Thermal Gravimetric and Differential Thermal Analysis（TG-DTA） showed that the temperature for solid-state reaction is at 942 ℃. The samples are identified to be single phase by X-ray Diffraction（XRD） and Scanning Electron Microscopy（SEM）. The SEM pictures showed that the first-step particles were at even size of about 100 nm by this technique. The electronic transport measurements showed that the doping compound were semiconductor with a crossover temperature T in the Arrhenius plot of the resistivity versus temprature.     

Microwave Synthesis of CdTe/TGA Quantum Dots and Their Thermodynamic Interaction with Bovine Serum Albumin

The thioglycollic acid(TGA) as a capping agent, CdTe/TGA quantum dots(QDs) with excellent properties were synthesized under microwave irradiation. The TGA/Cd/Te molar ratios, reaction time, temperature and p H are the crucial factors for properties of QDs. The QDs were characterized by UVvis absorption and fluorescence spectra, transmission electron microscopy and Fourier transform infrared spectroscopy. The experimental results show that when the p H value is 11.5 and molar ratio of TGA:Cd:Te is 1.2:1:0.4 at 100 ℃ heating for 15 min, the resulted QDs exhibit a high fluorescence quantum yield of 78%. The fluorescence full width at half maximum(FHMW) of QDs is around 23 nm. The products are spherical with average size of 3-5 nm. There is a strong coordination effect between TGA and Cd2+. Moreover, the results of interaction between as-made QDs and bovine serum albumin(BSA) suggest that the QDs-BSA binding reaction is a static quenching. The negative values of free energy(△G0) suggest that the binding process is spontaneous, △H0 and △S0 show that hydrogen bonds and van der Waals interactions play a major role in the binding reaction between QDs and BSA.     

Mechanism and Microstructure of Electroless Ni-Fe-P Plating on CNTs

Electroless Ni-Fe-P alloy plating on the surface of CNTs was carded out with a bath using citrate salt and lactic acid as complex agents. We proposed a chemical reaction mechanism. The morphology, structure and chemical composition of the Ni-Fe-P/CNTs were studied with the aid of a scanning electronic microscope （SEM）, X-ray diffraction （XRD） and an energy-dispersive X-ray spectral analysis （EDS）. The results show that through a correct pre-treatment and electroless plating, Ni-Fe-P/CNTs composite particles can be obtained. The optimum electroless plating parameters of 35-42℃ and pH of 8.5-9.7 were achieved. The as-plated Ni-Fe-P alloy is amorphous. After a heat treatment at 500℃ for 90 min in H2, the coating is transformed into crystalloid Ni3E Fe2NiP and （Fe,Ni）3R The Ni-Fe-P alloy coating on the surface of CNTs is smooth and unique. The amount of Ni on the surface （mass fraction） of the Ni-Fe-P/CNTs composite particles is 29.13%, that of Fe 3.19% and that of P 2.28%.     

Preparation of superabsorbent by graft copolymerization of acrylic acid onto corn starch using K_2S_2O_8 and rare earths as initiators

K2 S2 O8 and rare earths （RE） were used as initiators to prepare superabsorbents by graft copolymerization of acrylic acid （ AA ） onto corn starch. The effects of monomer concentration, initiator K2 S2 O8 concentration, cross-linker concentration, reaction temperature and the concentration ratio of RE and K2 S2O8 on the graft copolymerization were studied in terms of the water absorption capacity of superabsorbents. Results indicate that the optimum conditions obtained for the grafting of AA onto 5g starch are as follows： AA of 75. 773 g/L, K2S20s of 0. 437 g/L, RE of 0. 874 g/L, cross-linker of 0. 381 g/L and temperature of 70 ℃. The maximum water absorption capacity obtained is 740 g/g. The new method of graft polymerization is easily proceeded and controlled. The graft copolymers were characterized by infra-red spectroscopy, scanning electron microscopy and TG. Results characterized by IR and SEM give strong evidence for grafting of AA onto corn starch, and those characterized by TG reveal that the grafting of AA improves the theimostability of corn starch.     

Preparation of the supported heteropolyacids catalyst by ultrasound-plasma treatment

Novel catalysts of phosphotungstic heteropolyacids （PW12） supported on neutral alumina were prepared by assistance of ultrasound and plasma treatment. The prepared catalysts were characterized by FT-IR pyridine adsorption （Py-IR）, temperature programmed desorption of Pyridine （Py-TPD）, BET and X-ray diffraction （XRD）, and their catalytic performances were evaluated by the cationic polymerization of tetrahydrofuran. The results indicate that plasma treatment remarkably increases the surface acidity of the prepared catalyst while ultrasonic treatment induces PW12 to uniformly disperse on the support surface and expose more active sites for the acid catalytic reaction. A higher catalytic activity （69.7%） is obtained on the novel catalyst, which significantly outstripped that on the conventional sample （57.5%）.     

Preparation of p-menthane hydroperoxide from p-menthane in presence of metalloporphyrins

The aerobic oxidation of p-menthane to p-menthane hydroperoxide (PMHP) in the presence of metalloporphyrins was investigated in an intermittent mode under an atmospheric pressure of air. Several important reaction parameters, such as the structure of metalloporphyrin, the air flow rate, and the temperature, were studied. The preliminary mechanism of the aerobic oxidation of p-menthane catalyzed by metalloporphyrins was also discussed. The results show that the reaction is greatly accelerated by the addition of metalloporphyrins at very low concentration, in terms of both the yield and formation rate of PMHP, and the high selectivity of PMHP is maintained during the reaction. Temperature of 120 ℃ and reaction time of around 5 h are the optimal conditions for the best result in the presence of 0.06 mmol/L monomanganeseporphyrins ((p-Cl)TPPMnCl). Furthermore, the yield of PMHP is increased remarkably when the reaction is carried out under programmed temperature compared with the constant temperature. When the reaction is catalyzed by 0.06 mmol/L((p-Cl)TPPMnCl) at the air flow rate of 600 mL/min and 120 ℃ for 4 h, and then the temperature is reduced to 110 ℃, for another 4 h, the yield of PMHP reaches 24.3%, which is higher than that of the reaction at a constant temperature of 120 ℃ or 110 ℃ for 8 h.     

Synthesis of brookite-typed titania from titanium chloride solution

The brookite-phase TiO_2 was prepared by a hydrothermal synthesis of titanium chloride solution. The thermolysis time and the pH value of the solution were controlled during the synthesis. X-ray diffraction experiments showed that TiO_2 powders partially containing the brookite-phase were successfully obtained. A great amount of OH-in the reaction solution was found to be important to obtain the brookite phase because the intermediate complex leading to the brookite phase consumes more OH- than other phases like the rutile.     

Curing mechanism of TDE-85/MeTHPA epoxy resin modified by polyurethane

Diglycidyl 4,5-epoxy tetrahydro phthalate/methyl tetrahydrophthalic anhydride （TDE-85/MeTHPA） epoxy resin modified by polyurethane （PU） was prepared with 1,4-butanediol （1,4-BDO）, trimethylol propane （TMP） and polyurethane prepolymer synthesized by polypropylene glycol and toluene diisocynate. Chemical reaction and curing mechanism of this system were discussed by incorporating the results of infra spectrum analysis. The results indicate that the epoxy polymeric network I is obtained by the curing reaction between TDE-85 and MeTHPA, while the PU polymeric network II is obtained by the chain-extended and crosslinking reaction between 1,4-BDO, TMP and polyurethane prepolymer（PUP）. The graft chemical bonds are formed between polymer networks I and II that therefore increase the degree of blend and compatibility between epoxy polymer and PU.     

Surface resistivity of carbonaceous fiber/PTFE antistatic coatings

Abstract： PAN （Polyacrylonitrile）-based carbonaceous fibers were prepared at the heat treatment temperature （HTT） range of 650 to 900 ℃. The relationships among HTT, carbon content and volume resistivity of the carbonaceous fibers were investigated. The carbonaceous fibers/PTFE （Polytetrafluoroethylene） antistatic coatings were prepared by the spraying technology and the effects of carbonaceous fibers and pigments on surface resistivity of the coatings were systematically discussed. Micrographs provide insight into the antistatic mechanism of the coating. The results show that carbon content of the carbonaceous fibers increases from 68.8% to 74.8% （mass fraction） and the volume resistivity decreases drastically from 1.94× 10^-3 to 8.27× 10 ^-2.cm. The surface resistivity of the antistatic coating is adjustable between 10^5 and 10^8Ω2 to fit the different antistatic materials. Static is dissipated by a conductive network of short fibers and the tunneling effect between the neighboring fibers and conductive pigments. Conductive pigments make the conductive network more perfect and improve the antistatic ability, but insulating pigments acting as barriers for the formation of conductive channel increases the surface resistivity of the coatings. The influence of pigments on the surface resistivity drops gradually with the decrease of the carbonaceous fibers volume resistivity.     

Co-precipitation/hydrothermal synthesis of BiFeO<Subscript>3</Subscript> powder

A coprecipitation/hydrothermal route was utilized to fabricate pure phase BiFeO3 powders using FeCl3·6H2O and Bi（NO3）3·5H2O as starting materials, ammonia as precipitant and NaOH as mineralizer. The synthesized powders were characterized by XRD, SEM and DSC-TG analysis. In the process, single-phase BiFeO3 powders could be obtained at a hydrothermal reaction temperature of 180 ℃, with NaOH of 0.15 mol/L, in contrast to 200 ℃ and 4 mol/L for conventional hydrothermal route. Meanwhile, the micro-morphology of synthesized BiFeO3 powders changed with different reaction temperatures and concentrations of NaOH. The N6el temperature, Curie temperature and decomposition temperature of the synthesized BiFeO3 powders were detected to be 301 ℃, 828 ℃ and 964 ℃, respectively. The hydrothermal reactions mechanism to fabricate BiFeO3 powders were discussed based on the in-situ transformation process.     

Interfacial reaction between solid nickel and liquid zinc

Interfacial reactions between solid nickel and liquid zinc at 450-650 ℃ for 30-600 s were studied. The morphology and growth behavior of intermetallic compound layers at the interface between solid nickel and liquid zinc were observed and analyzed by SEM and EDS. The results show that γ and 8 phases are formed at 450 ℃ at the Ni/Zn interface, and at 550 ℃ and 650 ℃ only ）,phase is formed at the interthce and some δ phase particles will be participated during solidification on the surface of γphase layer. The β1 phase is absent under experimental conditions. Many cracks occur in the layers due to the difference in thermal expansion coefficients of these phases. It is found that the kinetics of the intermetallic compounds growth follows a parabolic law of time, as controlled by the diffusion mechanism. The apparent activation energies are 113.9 kJ/mol for the growth of γphase and 125.87 kJ/mol for γ1 phase, respectively.