[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
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
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
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 X...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
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
The photochemical reaction of nilrobenzaldehyde with indole and antipyrine was investigated in solid state.The structures of the new products were identified by means of IR,MS,'H NMR and elemental analysis,and the...The photochemical reaction of nilrobenzaldehyde with indole and antipyrine was investigated in solid state.The structures of the new products were identified by means of IR,MS,'H NMR and elemental analysis,and the crystal structure of audition product 2c was determined by X-ray diffraction analysis.The mechanism of this reaction was also proposed.展开更多
Precursors were prepared by solid state chemical reaction between LaCl_3 and C_2H_2O_4·2H_2O or NH_4HCO_3 at ambient temperature. Differential temperature analysis (DTA) and thermogravimetric analysis (TGA) were ...Precursors were prepared by solid state chemical reaction between LaCl_3 and C_2H_2O_4·2H_2O or NH_4HCO_3 at ambient temperature. Differential temperature analysis (DTA) and thermogravimetric analysis (TGA) were used to determine the decomposing temperature. Oxide (La_2O_3) was obtained by decomposing the precursor for about 2.5 h. X-ray diffraction (XRD), scanning electronic microscope (SEM) and ZETA potentiometer were respectively used to analyze the composition, morphology and size distribution of the products. The results show that La_2O_3 prepared by LaCl_3 and C_2H_2O_4·2H_2O is of ball-like shape and the diameter of particles (95%) is below 50 nm, while La_2O_3 prepared by LaCl_3 and NH_4HCO_3 is net-like.展开更多
Doped with Sb and Te, Mg2Si based compounds were prepared respectively by solid state reaction at 823 K for 8 h. Effects of dopants of Sb and Te on the structure and thermoelectric properties of the compounds were inv...Doped with Sb and Te, Mg2Si based compounds were prepared respectively by solid state reaction at 823 K for 8 h. Effects of dopants of Sb and Te on the structure and thermoelectric properties of the compounds were investigated. By calculating the values of the electrical conductivity for Sb-doped sample, the mechanism of electric conduction at 625 K is different. The figure of merit for sample doped with 0.4 wt% Te at500K is 2.4 × 10-3W/mK2,and it reaches 3. 3 ×10-3 W/mK2 at 650K for the sample doped with 0. 5wt% Sb. The values are more than 1.4 times and 2.3 times of the pure Mg2 Si sample.展开更多
Ag3PO4 microcrystals with highly enhanced visible light photocatalytic activity are prepared by a facile and simple solid state reaction at room temperature. The composition, morphology and optical properties of the a...Ag3PO4 microcrystals with highly enhanced visible light photocatalytic activity are prepared by a facile and simple solid state reaction at room temperature. The composition, morphology and optical properties of the asprepared Ag3PO4 microcrystMs are characterized by x-ray diffraction, scanning electron microscopy and UV-vis diffuse reflectance spectra. The photocatalytie properties of Ag3PO4 are investigated by the degradation of both methylene blue and methyl orange dyes under visible light irradiation. The as-prepared Ag3PO4 microcrystals possess high photocatalytic oxygen production with the rate of 673μmolh-1g-1. Moreover, the as-prepared Ag3PO4 microcrystals show an enhanced photoelectrochemistry performance under irradiation of visible light.展开更多
The crystal structure of a solid electrolyte, beta-A12O3, was investigated by XRD analysis and demonstrated by Diamond software. Its chemical formula was verified by the Ag ion molten salt exchange method and X-ray fl...The crystal structure of a solid electrolyte, beta-A12O3, was investigated by XRD analysis and demonstrated by Diamond software. Its chemical formula was verified by the Ag ion molten salt exchange method and X-ray fluorescence analysis (XRF). The chemical formula of β- A12O3 is Na2O·8.52A12O3, and its crystal is of hexagonal, space group P63/mmc, with a = 5.5941 A and c = 22.5300 A. The chemical formula of β-Al20 is Na2O·6.03A12O3, and its crystal is of trigonal, space group R3m, with a = 5.6017 A and c = 33.6219 A. The maximum span in the sodion migration of β-phase (2.4283 A) is only about a third of that for the β-phase (6.9037 A), so the β-phase has higher ionic conductivity than the r-phase.展开更多
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 anal...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.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.
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.
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Supported by National Laboratory of Applied Organic ChemistryLanzhou University
文摘The photochemical reaction of nilrobenzaldehyde with indole and antipyrine was investigated in solid state.The structures of the new products were identified by means of IR,MS,'H NMR and elemental analysis,and the crystal structure of audition product 2c was determined by X-ray diffraction analysis.The mechanism of this reaction was also proposed.
文摘Precursors were prepared by solid state chemical reaction between LaCl_3 and C_2H_2O_4·2H_2O or NH_4HCO_3 at ambient temperature. Differential temperature analysis (DTA) and thermogravimetric analysis (TGA) were used to determine the decomposing temperature. Oxide (La_2O_3) was obtained by decomposing the precursor for about 2.5 h. X-ray diffraction (XRD), scanning electronic microscope (SEM) and ZETA potentiometer were respectively used to analyze the composition, morphology and size distribution of the products. The results show that La_2O_3 prepared by LaCl_3 and C_2H_2O_4·2H_2O is of ball-like shape and the diameter of particles (95%) is below 50 nm, while La_2O_3 prepared by LaCl_3 and NH_4HCO_3 is net-like.
文摘Doped with Sb and Te, Mg2Si based compounds were prepared respectively by solid state reaction at 823 K for 8 h. Effects of dopants of Sb and Te on the structure and thermoelectric properties of the compounds were investigated. By calculating the values of the electrical conductivity for Sb-doped sample, the mechanism of electric conduction at 625 K is different. The figure of merit for sample doped with 0.4 wt% Te at500K is 2.4 × 10-3W/mK2,and it reaches 3. 3 ×10-3 W/mK2 at 650K for the sample doped with 0. 5wt% Sb. The values are more than 1.4 times and 2.3 times of the pure Mg2 Si sample.
基金Supported by the Beijing Higher Education Young Elite Teacher Project under Grant No YETP1297the Fundamental Research Funds for the Central Universities under Grant No 2014MDLXYZY05+1 种基金the Undergraduate Innovative Test Program of China under Grant Nos GCCX2015110009 and BEIJ2015110024the National Natural Science Foundation of China under Grant Nos11074312 and 11374377
文摘Ag3PO4 microcrystals with highly enhanced visible light photocatalytic activity are prepared by a facile and simple solid state reaction at room temperature. The composition, morphology and optical properties of the asprepared Ag3PO4 microcrystMs are characterized by x-ray diffraction, scanning electron microscopy and UV-vis diffuse reflectance spectra. The photocatalytie properties of Ag3PO4 are investigated by the degradation of both methylene blue and methyl orange dyes under visible light irradiation. The as-prepared Ag3PO4 microcrystals possess high photocatalytic oxygen production with the rate of 673μmolh-1g-1. Moreover, the as-prepared Ag3PO4 microcrystals show an enhanced photoelectrochemistry performance under irradiation of visible light.
基金supported by NSFC projects(21203095)China Postdoctoral Science Foundation Projects(2012M511261)Jiangsu Colleges and Universities Advantage Discipline Construction projects
文摘The crystal structure of a solid electrolyte, beta-A12O3, was investigated by XRD analysis and demonstrated by Diamond software. Its chemical formula was verified by the Ag ion molten salt exchange method and X-ray fluorescence analysis (XRF). The chemical formula of β- A12O3 is Na2O·8.52A12O3, and its crystal is of hexagonal, space group P63/mmc, with a = 5.5941 A and c = 22.5300 A. The chemical formula of β-Al20 is Na2O·6.03A12O3, and its crystal is of trigonal, space group R3m, with a = 5.6017 A and c = 33.6219 A. The maximum span in the sodion migration of β-phase (2.4283 A) is only about a third of that for the β-phase (6.9037 A), so the β-phase has higher ionic conductivity than the r-phase.
文摘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.