[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=12.15c...[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)) .展开更多
The evolved gaseous analysis (EGA),infrared spectra,and XRD have been applied to the study of solid state reactions of KSCN with five cobalt(Ⅲ)-ammine complexes:[Co- (NH_3)_5N_3]Cl_2,[Co(NH_3)_5(NO_2)]Cl_2,[Co(NH_3)_...The evolved gaseous analysis (EGA),infrared spectra,and XRD have been applied to the study of solid state reactions of KSCN with five cobalt(Ⅲ)-ammine complexes:[Co- (NH_3)_5N_3]Cl_2,[Co(NH_3)_5(NO_2)]Cl_2,[Co(NH_3)_5(H_2O)]Cl_3,[Co(NH_3)_5Cl]Cl_2,and [Co(NH_3)_6]Cl_3 in a hydrogen atmosphere.It is found that the existence of KSCN shifts the thermal decom- position of these complexes to a lower temperature.The corresponding peak temperatures are near 140℃.The effect of KSCN is discussed and kinetic parameters of deammine reactions are calculated.展开更多
Ni/Sn couples, prepared by sequentially electroplating Ni layers and Sn layers on metallized Si wafers, were employed to study the microstructures and growth kinetics of Ni-Sn intermediate phases, when the Ni/Sn coupl...Ni/Sn couples, prepared by sequentially electroplating Ni layers and Sn layers on metallized Si wafers, were employed to study the microstructures and growth kinetics of Ni-Sn intermediate phases, when the Ni/Sn couples were aged at room temperature or armealed at temperatures from 150 to 225℃ for various times. The results show that the NiSn phase and Ni3Sn4 phase are formed, respectively, in the aged couples and annealed couples. The Ni3Sn4 layer is continuously distributed between the Ni and Sn sides in the annealed Ni/Sn couples. The Ni3Sn4 growth follows parabolic growth kinetics with an apparent activation energy of 39.0 kJ/mol.展开更多
The solid-solid state reactions of o-aminobenzoic acid with Zn(OAc)2.2H2O, Cu(OAc)2 .H2O, Ni(OAc)2.4H2O and Mn(OAc)2.4H2O result in the formation of corresponding complexes M(OAB)2 (M = Zn(Ⅱ), Cu(Ⅱ), Ni(Ⅱ), Mn(IⅡ)...The solid-solid state reactions of o-aminobenzoic acid with Zn(OAc)2.2H2O, Cu(OAc)2 .H2O, Ni(OAc)2.4H2O and Mn(OAc)2.4H2O result in the formation of corresponding complexes M(OAB)2 (M = Zn(Ⅱ), Cu(Ⅱ), Ni(Ⅱ), Mn(IⅡ)). XRD, IR and elemental analysis methods have been used to characterize the solid products. The activation energies of these reactions, which are calculated from the kinetic data obtained by means of the isothermal electrical conductivity measurement method, have been found to increase in the order: Cu(OAc)2.H2O(37.7 kJ.mol-1)~Mn(OAc)2.4H2O (39.7kJ.mol-1) < Zn(OAc)2.2H2O (56.3 kJ.mol-1) < Ni(OAc)2.4H2O (85.2 kJ.mol-1). The trend is related to their crystal structures.展开更多
olid state reactions of o-aminobenzoic acid (HOAB) with Cu (OAc)_2·H_2O,Cu(HCOO)_2 · 4H_2O, anhydrous Cu (OAc)_2 and Cu (HCOO)_2 at room or close toroom temperature have been investigated. The product Cu(OAB...olid state reactions of o-aminobenzoic acid (HOAB) with Cu (OAc)_2·H_2O,Cu(HCOO)_2 · 4H_2O, anhydrous Cu (OAc)_2 and Cu (HCOO)_2 at room or close toroom temperature have been investigated. The product Cu(OAB)_2 with a high yieldwas synthesized very conveniently compared witb the solution phase method. Thekinetic behavior was studied by means of the isothermal electrical conductivity mea-surement. The reactivity was found to decrease in the order : Cu(OAc)_2· H_2O>Cu(OAc)_2>Cu (HCOO)_2 ·4H_2O>Cu (HCOO)_2, which was attributable to the crystalstructures of the copper salts.展开更多
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 tem...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.展开更多
In order to reduce the oxidation and volatilization caused by Mg element in the traditional methods for synthesizing Mg2Si compounds,Mg2Si thermoelectric materials were prepared by solid state reaction and microwave r...In order to reduce the oxidation and volatilization caused by Mg element in the traditional methods for synthesizing Mg2Si compounds,Mg2Si thermoelectric materials were prepared by solid state reaction and microwave radiation techniques.Structure and phase composition of the materials were investigated by X-ray diffraction.The electrical conductivity,Seebeck coefficient and thermal conductivity were measured as a function of temperature from 300 to 700 K.It is found that high purity Mg2Si powders can be obtained with excessive content of 8% Mg from the stoichiometric Mg2Si at 853 K and 2.5 kW for 30 min.A maximum dimensionless figure of merit,ZT,of about 0.13 was obtained for Mg2Si at 600 K.展开更多
Lithium-excess manganese layered oxides, which are commonly described in chemical formula 0.5Li2MnO3·0.5LiMn0.5Ni0.5O2, were prepared by low-heating solid state reaction. The reaction mechanisms of synthesizing p...Lithium-excess manganese layered oxides, which are commonly described in chemical formula 0.5Li2MnO3·0.5LiMn0.5Ni0.5O2, were prepared by low-heating solid state reaction. The reaction mechanisms of synthesizing precursors, the decomposition mechanism, and intermediate materials in calcination were investigated by means of Fourier transform infrared spectroscopy （FT-IR）, X-ray diffraction （XRD）, field emission scanning electron microscopy （FESEM）, thermogravimetric analysis （TGA）, and differential scanning calorimetry （DSC）. The major diffraction patterns of 0.5Li2MnO3·0.5LiMn0.5Ni0.5O2 powder calcinated at 720℃ for 15 h are indexed to the hexagonal structure with a space group of R3m, and the clear splits of doublets at （006）/（102） and （108）/（110） indicate that the sample adopts a well-layered structure. FESEM images show that the size of the agglomerated particles of the sample ranges from 100 to 300 nm.展开更多
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...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.展开更多
Wollastonite, a mineral of wide industrial applications was synthesised from rice husk ash silica and limestone. A number of raw batches consisting of these starting materials, in 1:1 molar ratio, were heat treated to...Wollastonite, a mineral of wide industrial applications was synthesised from rice husk ash silica and limestone. A number of raw batches consisting of these starting materials, in 1:1 molar ratio, were heat treated to produce it through solid state reaction from 900℃ to 1300℃. The conducted reaction was monitored by XRD step by step. Amount of Wollastonite formed at every temperature was also studied to some extent. Analyses of the obtained data indicated that the target mineral formation was quite effective and almost proportional to a rise in temperature up to 1200℃. The results from both, XRD and chemical analysis were found in fair agreement with one another展开更多
Using low-cost FePO4·2H2O as iron source,Na2FePO4F/C composite is prepared by alcohol-assisted ball milling and solid-state reaction method.The XRD pattern of Na2FePO4F/C composite demonstrates sharp peaks,indica...Using low-cost FePO4·2H2O as iron source,Na2FePO4F/C composite is prepared by alcohol-assisted ball milling and solid-state reaction method.The XRD pattern of Na2FePO4F/C composite demonstrates sharp peaks,indicating high crystalline and phase purity.The SEM and TEM images reveal that diameter of the spherical-like Na2FePO4F/C particles ranges from 50 to 300 nm,and HRTEM image shows that the surface of Na2FePO4F/C composite is uniformly coated by carbon layer with a average thickness of about 3.6 nm.The carbon coating constrains the growth of the particles and effectively reduces the agglomeration of nanoparticles.Using lithium metal as anode,the composite delivers a discharge capacities of 102.8,96.4 and 90.3 mA·h/g at rates of 0.5C,1C and 2C,respectively.After 100 cycles at 0.5C,a discharge capacity of 98.9 mA·h/g is maintained with capacity retention of 96.2%.The Li+diffusion coefficient(D)of Na2FePO4F/C composite is calculated as 1.71×10^–9 cm^2/s.This study reveals that the simple solid state reaction could be a practical and effective synthetic route for the industrial production of Na2FePO4F/C material.展开更多
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） ...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.展开更多
Solid-state grinding is a simple and effective method to introduce guest species into the channels of microporous materials through filling.The structure and the surface acidity of the materials were obtained from BET...Solid-state grinding is a simple and effective method to introduce guest species into the channels of microporous materials through filling.The structure and the surface acidity of the materials were obtained from BET isotherms and NH3-TPD,respectively.XRD,UV-vis,UV diffuse-reflectance,and TEM were used to characterize the phases,and the morphology,respectively.The clustered layers of MgO-Al2O3phases were formed in the internal pore surface and were highly dispersed inside the channels of the ZSM-5 host.So the volume of MgO-Al2O3/ZSM-5 composite was larger than the ZSM-5 zeolite itself and some mesoporous channels appeared when Mg/Al species entered the channels.Meanwhile,new acid sites emerged in MgO-Al2O3/ZSM-5 composite and the acid amount of the sample changed.The improved Pt dispersion and the increased acid content would cause the increase of propane conversion and the modification of selectivity during the reaction.展开更多
An industrial mineral wollastonite (CaSiO3) was produced under solid state conditions from rice husk silica and limestone. Reaction was carried out at 900'C to 1300'C for 1 h. The product batches were subjecte...An industrial mineral wollastonite (CaSiO3) was produced under solid state conditions from rice husk silica and limestone. Reaction was carried out at 900'C to 1300'C for 1 h. The product batches were subjected to XRD and chemical analysis techniques specific for wollastonite. Mole fractions of different product batches were calculated on the basis of accumulated data to study the kinetics. Specific rate constants and reaction rate were also found out. Various probable models of mechanism for reaction were considered and testified with the laid down criterion for suggesting the suitable one. The resulting data were treated with Arrhenius equation as well and activation energy was calculated--therefrom. In addition to finding it's value from the slope of Arrhenius curve, an alternate method was also applied for this purpose. Both of the values were observed to be comparable. The activation energy required for performed reaction was found to be almost one third of that reported for synthesizing CaSiO3 by using quartz. This referred to the economical preparation of wollastonite by using rice husk as a source of silica instead of quartz.展开更多
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. ...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.展开更多
Alumina coated LiNi1/3Mn1/3Co1/3O2 particles were obtained by a simple method of solid state reaction at room temperature. The reaction mechanism of solid state reaction at room temperature was investigated. The struc...Alumina coated LiNi1/3Mn1/3Co1/3O2 particles were obtained by a simple method of solid state reaction at room temperature. The reaction mechanism of solid state reaction at room temperature was investigated. The structure and morphology of the coating materials were investigated by XRD, SEM and TEM. The electrochemical performances of uncoated and Al2O3-coated LiNi1/3Co1/3Mn1/3O2 cathode materials were studied within a voltage window of 3.00?4.35 V at current density of 30 mA/g. SEM, TEM and EDS analytical results indicate that the surface of LiNi1/3Mn1/3Co1/3O2 particles is coated with very fine Al2O3 composite, which leads to the improved cycle ability though a slight decrease in the first discharge capacity is observed. It is proposed that surface treatment by solid state reaction at room temperature is a simple and effective method to improve the cycle performance of LiNi1/3Co1/3Mn1/3O2 particles.展开更多
Solid state reactions between β diketones (HPMBP, HDBM) and LnAc 3· x H 2O(La,Nd: x =3/2;Tb: x =4) have been investigated at low heating temperature. Pure compounds of Ln(PMBP) 3 and Ln(DBM) 3 are obt...Solid state reactions between β diketones (HPMBP, HDBM) and LnAc 3· x H 2O(La,Nd: x =3/2;Tb: x =4) have been investigated at low heating temperature. Pure compounds of Ln(PMBP) 3 and Ln(DBM) 3 are obtained by solid state reaction, and characterized by elemental analysis, infrared radiation (IR),X ray diffraction (XRD) and photoacoustic spectra. The solid state reaction properties of β diketones and their influences on the structures of products are discussed.展开更多
The aldol condensation reactions of acetylferrocene with several aromatic aldehydes have been studied in the solid state.The results showed that they revealed different reactivities in the solid slate from that in sol...The aldol condensation reactions of acetylferrocene with several aromatic aldehydes have been studied in the solid state.The results showed that they revealed different reactivities in the solid slate from that in solution and eight compounds have been prepared. Their structures have been characterized by UV,IR,1~HNMR,HS and elemental analysis.展开更多
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 parti...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.展开更多
Nanometer cerium-zirconium oxide solution Ce1-x ZrxO2 was synthesized by mechanically activated solid state re- action at middle-low temperatures, with Ce2（CO3）3, ZrOCl2-SH2O and H2C2O4·2H2O as raw materials. T...Nanometer cerium-zirconium oxide solution Ce1-x ZrxO2 was synthesized by mechanically activated solid state re- action at middle-low temperatures, with Ce2（CO3）3, ZrOCl2-SH2O and H2C2O4·2H2O as raw materials. The crystal structure and microstructure of the nanometer Ce1-x Zrx O2 were studied with X-ray diffractometry （XRD） and transmission electron microscope （TEM）. The results show that the product is single-cubic-phase solid solution with an average crystal size 19.64 nm. In this article, the influence of surface active agent is also evaluated. Mechanically activated solid state reaction for the preparation of Ce1-xZrxO2 is a new technique of green chemistry without solvent and waste.展开更多
基金Project supported by the National Natural Science Foundation of China
文摘[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)) .
文摘The evolved gaseous analysis (EGA),infrared spectra,and XRD have been applied to the study of solid state reactions of KSCN with five cobalt(Ⅲ)-ammine complexes:[Co- (NH_3)_5N_3]Cl_2,[Co(NH_3)_5(NO_2)]Cl_2,[Co(NH_3)_5(H_2O)]Cl_3,[Co(NH_3)_5Cl]Cl_2,and [Co(NH_3)_6]Cl_3 in a hydrogen atmosphere.It is found that the existence of KSCN shifts the thermal decom- position of these complexes to a lower temperature.The corresponding peak temperatures are near 140℃.The effect of KSCN is discussed and kinetic parameters of deammine reactions are calculated.
基金the Natural Sciences and Engineering Research Council(NSERC) of Canada and Micralyne Inc.for providing the research fund and Si substrates for electroplating(Micralyne)
文摘Ni/Sn couples, prepared by sequentially electroplating Ni layers and Sn layers on metallized Si wafers, were employed to study the microstructures and growth kinetics of Ni-Sn intermediate phases, when the Ni/Sn couples were aged at room temperature or armealed at temperatures from 150 to 225℃ for various times. The results show that the NiSn phase and Ni3Sn4 phase are formed, respectively, in the aged couples and annealed couples. The Ni3Sn4 layer is continuously distributed between the Ni and Sn sides in the annealed Ni/Sn couples. The Ni3Sn4 growth follows parabolic growth kinetics with an apparent activation energy of 39.0 kJ/mol.
基金Project supported by the National Natural Science Foundation of China and the Center of Analysis of Nanjing University.
文摘The solid-solid state reactions of o-aminobenzoic acid with Zn(OAc)2.2H2O, Cu(OAc)2 .H2O, Ni(OAc)2.4H2O and Mn(OAc)2.4H2O result in the formation of corresponding complexes M(OAB)2 (M = Zn(Ⅱ), Cu(Ⅱ), Ni(Ⅱ), Mn(IⅡ)). XRD, IR and elemental analysis methods have been used to characterize the solid products. The activation energies of these reactions, which are calculated from the kinetic data obtained by means of the isothermal electrical conductivity measurement method, have been found to increase in the order: Cu(OAc)2.H2O(37.7 kJ.mol-1)~Mn(OAc)2.4H2O (39.7kJ.mol-1) < Zn(OAc)2.2H2O (56.3 kJ.mol-1) < Ni(OAc)2.4H2O (85.2 kJ.mol-1). The trend is related to their crystal structures.
文摘olid state reactions of o-aminobenzoic acid (HOAB) with Cu (OAc)_2·H_2O,Cu(HCOO)_2 · 4H_2O, anhydrous Cu (OAc)_2 and Cu (HCOO)_2 at room or close toroom temperature have been investigated. The product Cu(OAB)_2 with a high yieldwas synthesized very conveniently compared witb the solution phase method. Thekinetic behavior was studied by means of the isothermal electrical conductivity mea-surement. The reactivity was found to decrease in the order : Cu(OAc)_2· H_2O>Cu(OAc)_2>Cu (HCOO)_2 ·4H_2O>Cu (HCOO)_2, which was attributable to the crystalstructures of the copper salts.
基金Project supported by the Research Funds of the Key Laboratory of Fuel Cell Technology of Guangdong Province,ChinaProject(7411793079907)supported by the Guangzhou Special Foundation for Applied Basic Research+1 种基金Project(2013A15GX048)supported by the Dalian Science and Technology Project Foundation,ChinaProject(21376035)supported by the National Natural Science Foundation of China
文摘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.
基金Project (2009BB4228) supported by the Natural Science Foundation Project of Chongqing Science and Technology Commission,ChinaProject (CK2010Z09) supported by the Research Foundation of Chongqing University of Science and Technology,China
文摘In order to reduce the oxidation and volatilization caused by Mg element in the traditional methods for synthesizing Mg2Si compounds,Mg2Si thermoelectric materials were prepared by solid state reaction and microwave radiation techniques.Structure and phase composition of the materials were investigated by X-ray diffraction.The electrical conductivity,Seebeck coefficient and thermal conductivity were measured as a function of temperature from 300 to 700 K.It is found that high purity Mg2Si powders can be obtained with excessive content of 8% Mg from the stoichiometric Mg2Si at 853 K and 2.5 kW for 30 min.A maximum dimensionless figure of merit,ZT,of about 0.13 was obtained for Mg2Si at 600 K.
基金supported by the National High-Tech Research and Development Program of China (No.2009AA03Z226)the National Natural Science Foundation of China (No.50702007)+1 种基金the Fundamental Research Funds for the Central Universities (No.FRF-MP-12-005B)the Special Funds for Excellent Doctoral Dissertation of Beijing (No.YB20081000801)
文摘Lithium-excess manganese layered oxides, which are commonly described in chemical formula 0.5Li2MnO3·0.5LiMn0.5Ni0.5O2, were prepared by low-heating solid state reaction. The reaction mechanisms of synthesizing precursors, the decomposition mechanism, and intermediate materials in calcination were investigated by means of Fourier transform infrared spectroscopy （FT-IR）, X-ray diffraction （XRD）, field emission scanning electron microscopy （FESEM）, thermogravimetric analysis （TGA）, and differential scanning calorimetry （DSC）. The major diffraction patterns of 0.5Li2MnO3·0.5LiMn0.5Ni0.5O2 powder calcinated at 720℃ for 15 h are indexed to the hexagonal structure with a space group of R3m, and the clear splits of doublets at （006）/（102） and （108）/（110） indicate that the sample adopts a well-layered structure. FESEM images show that the size of the agglomerated particles of the sample ranges from 100 to 300 nm.
基金the National Natural Science Foundation of China (Nos. 51374021 and 51304016)the Fundamental Research Funds for the Central Universities of China (No. FRF-TP-14-114A2)Research Funds of State Key Laboratory of Advanced Metallurgy (No. 41603014)
文摘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.
文摘Wollastonite, a mineral of wide industrial applications was synthesised from rice husk ash silica and limestone. A number of raw batches consisting of these starting materials, in 1:1 molar ratio, were heat treated to produce it through solid state reaction from 900℃ to 1300℃. The conducted reaction was monitored by XRD step by step. Amount of Wollastonite formed at every temperature was also studied to some extent. Analyses of the obtained data indicated that the target mineral formation was quite effective and almost proportional to a rise in temperature up to 1200℃. The results from both, XRD and chemical analysis were found in fair agreement with one another
基金Projects(51472211,51502256)supported by the National Natural Science Foundation of ChinaProjects(2016GK4005,2016GK4030)supported by the Strategic New Industry of Hunan Province,ChinaProject(13C925)supported by the Research Foundation of Education Bureau of Hunan Province,China
文摘Using low-cost FePO4·2H2O as iron source,Na2FePO4F/C composite is prepared by alcohol-assisted ball milling and solid-state reaction method.The XRD pattern of Na2FePO4F/C composite demonstrates sharp peaks,indicating high crystalline and phase purity.The SEM and TEM images reveal that diameter of the spherical-like Na2FePO4F/C particles ranges from 50 to 300 nm,and HRTEM image shows that the surface of Na2FePO4F/C composite is uniformly coated by carbon layer with a average thickness of about 3.6 nm.The carbon coating constrains the growth of the particles and effectively reduces the agglomeration of nanoparticles.Using lithium metal as anode,the composite delivers a discharge capacities of 102.8,96.4 and 90.3 mA·h/g at rates of 0.5C,1C and 2C,respectively.After 100 cycles at 0.5C,a discharge capacity of 98.9 mA·h/g is maintained with capacity retention of 96.2%.The Li+diffusion coefficient(D)of Na2FePO4F/C composite is calculated as 1.71×10^–9 cm^2/s.This study reveals that the simple solid state reaction could be a practical and effective synthetic route for the industrial production of Na2FePO4F/C material.
基金Funded by the Program for New Century Excellent Talents in Universitythe Ministry of Education of China+3 种基金the National Natural Science Foundation of China (No.21061006)the Research of Natural Science and Technology Foundation of Guizhou Province ([2010]2006),Chinathe Natural Science Research Foundation of Education Bureau of Guizhou Province (No.2007083)the China Guizhou Province Characteristic Leading Academic Discipline Project in Material Physics and Chemistry (No.[2011]208)
文摘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.
基金the financial supports of the National Natural Science Foundation of China(Grant No.21376051,21106017,21306023 and 51077013)the Natural Science Foundation of Jiangsu(Grant No.BK20131288)+3 种基金the Fund Project for Transformation of Scientific and Technological Achievements of Jiangsu Province of China(Grant No.BA2011086)the Specialized Research Fund for the Doctoral Program of Higher Education of China(Grant No.20100092120047)the Key Program for the Scientific Research Guiding Fund of Basic Scientific Research Operation Expenditure of Southeast University(Grant No.3207043101)Instrumental Analysis Fund of Southeast University
文摘Solid-state grinding is a simple and effective method to introduce guest species into the channels of microporous materials through filling.The structure and the surface acidity of the materials were obtained from BET isotherms and NH3-TPD,respectively.XRD,UV-vis,UV diffuse-reflectance,and TEM were used to characterize the phases,and the morphology,respectively.The clustered layers of MgO-Al2O3phases were formed in the internal pore surface and were highly dispersed inside the channels of the ZSM-5 host.So the volume of MgO-Al2O3/ZSM-5 composite was larger than the ZSM-5 zeolite itself and some mesoporous channels appeared when Mg/Al species entered the channels.Meanwhile,new acid sites emerged in MgO-Al2O3/ZSM-5 composite and the acid amount of the sample changed.The improved Pt dispersion and the increased acid content would cause the increase of propane conversion and the modification of selectivity during the reaction.
文摘An industrial mineral wollastonite (CaSiO3) was produced under solid state conditions from rice husk silica and limestone. Reaction was carried out at 900'C to 1300'C for 1 h. The product batches were subjected to XRD and chemical analysis techniques specific for wollastonite. Mole fractions of different product batches were calculated on the basis of accumulated data to study the kinetics. Specific rate constants and reaction rate were also found out. Various probable models of mechanism for reaction were considered and testified with the laid down criterion for suggesting the suitable one. The resulting data were treated with Arrhenius equation as well and activation energy was calculated--therefrom. In addition to finding it's value from the slope of Arrhenius curve, an alternate method was also applied for this purpose. Both of the values were observed to be comparable. The activation energy required for performed reaction was found to be almost one third of that reported for synthesizing CaSiO3 by using quartz. This referred to the economical preparation of wollastonite by using rice husk as a source of silica instead of quartz.
基金supported by the National Natural Sci-ence Foundation of China under grant No. 50602024the Youth Foundation of North University of China
文摘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.
基金Project(50604018) supported by the National Natural Science Foundation of China
文摘Alumina coated LiNi1/3Mn1/3Co1/3O2 particles were obtained by a simple method of solid state reaction at room temperature. The reaction mechanism of solid state reaction at room temperature was investigated. The structure and morphology of the coating materials were investigated by XRD, SEM and TEM. The electrochemical performances of uncoated and Al2O3-coated LiNi1/3Co1/3Mn1/3O2 cathode materials were studied within a voltage window of 3.00?4.35 V at current density of 30 mA/g. SEM, TEM and EDS analytical results indicate that the surface of LiNi1/3Mn1/3Co1/3O2 particles is coated with very fine Al2O3 composite, which leads to the improved cycle ability though a slight decrease in the first discharge capacity is observed. It is proposed that surface treatment by solid state reaction at room temperature is a simple and effective method to improve the cycle performance of LiNi1/3Co1/3Mn1/3O2 particles.
文摘Solid state reactions between β diketones (HPMBP, HDBM) and LnAc 3· x H 2O(La,Nd: x =3/2;Tb: x =4) have been investigated at low heating temperature. Pure compounds of Ln(PMBP) 3 and Ln(DBM) 3 are obtained by solid state reaction, and characterized by elemental analysis, infrared radiation (IR),X ray diffraction (XRD) and photoacoustic spectra. The solid state reaction properties of β diketones and their influences on the structures of products are discussed.
文摘The aldol condensation reactions of acetylferrocene with several aromatic aldehydes have been studied in the solid state.The results showed that they revealed different reactivities in the solid slate from that in solution and eight compounds have been prepared. Their structures have been characterized by UV,IR,1~HNMR,HS and elemental analysis.
文摘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.
基金Project supported by the Key Project for Industry of Guangdong Province (Grant No,2004A10701005)the Natural Science Foundation of Guangdong Province (Grant No.04205301)
文摘Nanometer cerium-zirconium oxide solution Ce1-x ZrxO2 was synthesized by mechanically activated solid state re- action at middle-low temperatures, with Ce2（CO3）3, ZrOCl2-SH2O and H2C2O4·2H2O as raw materials. The crystal structure and microstructure of the nanometer Ce1-x Zrx O2 were studied with X-ray diffractometry （XRD） and transmission electron microscope （TEM）. The results show that the product is single-cubic-phase solid solution with an average crystal size 19.64 nm. In this article, the influence of surface active agent is also evaluated. Mechanically activated solid state reaction for the preparation of Ce1-xZrxO2 is a new technique of green chemistry without solvent and waste.
