Consecutive reaction between two solids, CuCl2.2H2O and 2,2'-bipyridyl in 1:2 molar ratio proceed in tWo steps: the salt first converts to the mediate, then the mediate turns to the final product.
[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
Oily cold rolling mill （CRM） sludge is one of the pollutants emitted by iron and steel plants. Recycling oily CRM sludge can not only reduce pollution but also bring social and environmental benefits. In this study,...Oily cold rolling mill （CRM） sludge is one of the pollutants emitted by iron and steel plants. Recycling oily CRM sludge can not only reduce pollution but also bring social and environmental benefits. In this study, using oily CRM sludge as sources of iron oxide, the strontium ferrite powders were synthesized in multiple steps including vacuum distillation, magnetic separation, oxidizing roasting, and solidstate reaction. The optimal technological conditions of vacuum distillation and oxidizing roasting were studied carefully. To consider the effects of Fe203/ SrCO3 tool ratio, calcination temperature, milling time and calcination time on magnetic properties of prepared strontium ferrite powders, the orthogonal experimental method was adopted. The maximum saturation magneti- zation （62.6 mA-m2.g-1） of the synthesized strontium ferrite powders was achieved at the Fe203/SrCO3 mol ratio of 6, 5 h milling time, 1250 ~C calcination temperature, and 1 h calcination time. Strontium ferrite powders syn- thesis method not only provides a cheap, high quality raw material for the production of strontium ferrite powders, but also effectively prevents the environmental pollution.展开更多
A precursor of BaCe0.5Zr0.4Y0. 1O3-α electrolytes was synthesized by the sol-gel method and sintered at temperature which were 150 - 250 ℃ lower than by solid state reaction. The AC impedance spectrums of electrolyt...A precursor of BaCe0.5Zr0.4Y0. 1O3-α electrolytes was synthesized by the sol-gel method and sintered at temperature which were 150 - 250 ℃ lower than by solid state reaction. The AC impedance spectrums of electrolytes were measured by AUTOLAB PGSTA30 electrochemical measuring device at different temperatures. The conductivities of the electrolytes are 1.62×10^-4 - 6.43×10^-3, 2.52×10^-5 - 3.73×10^-3S·cm^-1 in the temperature range of 350-800℃. The activity energies are 0.54 and 0.84 eV. At the same time BaCe0.9Y0.1O3-α was prepared by direct solid state reaction. The conductivity of BaCe0.9Y0.1O3-α is 1 × 10^-4- 4×10^-3 S·cm^-1 and the activation energy is 0.50 eV at the same condition. The results show that conduction of electrolyte prepared by sol-gel method is higher than the one by solid state reaction. As far as BaCe0.9Y0.1O3-α concerned, its conductivity of the Zr-substituted specimens is decreased.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
Nickel ferrite nano-powders were prepared by microwave radiating low-temperature solid-state reaction method, and then modified with Ag by dipping method. The crystal structure and morphology of the samples were chara...Nickel ferrite nano-powders were prepared by microwave radiating low-temperature solid-state reaction method, and then modified with Ag by dipping method. The crystal structure and morphology of the samples were characterized by means of X-ray diffraction（XRD）, scanning electron microscopy （SEM） and X-ray photoelectron spectroscopy （XPS）. The gas sensing properties of the samples were also investigated. The results reveal that the Ag, as amorphous structure, can efficiently prevent the reuniting and growing-up of nanosized NiFe2O4 grains, and 1.5% Ag modified NiFe2O4 sensor has a better sensitivity, up to 43, for acetone gas than 1.5%Ag mixed NiFe2O4 sensor prepared by low-temperature solid-state reaction, at an optimal working voltage of 4.5 V. The quick response time （1 s） and fast recovery time （～10 s） are the main characteristics of this sensor.展开更多
Sm2（Zr1-xCex）2O7 （x=0.1, 0.2, and 0.3） ceramics were prepared by solid reaction method at 1600°C for 10 h using Sm2O3, ZrO2, and CeO2 as starting reactants. The phase compositions, microstructures, thermal ex...Sm2（Zr1-xCex）2O7 （x=0.1, 0.2, and 0.3） ceramics were prepared by solid reaction method at 1600°C for 10 h using Sm2O3, ZrO2, and CeO2 as starting reactants. The phase compositions, microstructures, thermal expansion coefficients, and partial thermal conductivities of these materials were investigated. X-ray diffraction （XRD） results reveal that Sm2（Zr0.9Ce0.1）2O7 with pyrochlore structure and Sm2（Zr1-xCex）2O7 （x=0.2 and 0.3） with fluorite structure were synthesized, and scanning electrical microscopy （SEM） images show that the microstructures of these products are very dense. The linear thermal expansion coefficients increase with increasing temperature in the temperature range from ambient to 1200°C, and the thermal expansion coefficients increase with increasing content of doped CeO2. The thermal conductivities of Sm2（Zr0.8Ce0.2）2O7 and Sm2（Zr0.7Ce0.3）2O7 decrease gradually with an increase in temperature. These results show that the synthesized ceramic materials can be explored as novel prospective candidate materials for use in new thermal barrier coating systems in the future.展开更多
The Ba2Zn1-xNixWO6 double perovskite oxides were synthesized using solid state reaction method. The effect of replacement of Zn<sup>2+</sup> with Ni<sup>2+</sup> cation on the structural proper...The Ba2Zn1-xNixWO6 double perovskite oxides were synthesized using solid state reaction method. The effect of replacement of Zn<sup>2+</sup> with Ni<sup>2+</sup> cation on the structural properties was investigated by X-ray diffraction (XRD) at room temperature. From the X-ray diffraction and by means of standard Rietiveld method, the samples showed the same cubic crystal structure with (Fm-3m) space group and the crystallite size ranging from 71.91 nm to 148.71 nm. The unit cell volume was found to decrease as a result of the replacement, while there was no significant difference in the value of tolerance factor of the samples. This is may be due to the convergence of ionic radii of Ni<sup>2+</sup> and Zn<sup>2+</sup> cations. The Fourier Transform Infrared Spectroscopy (FTIR) was performed for the samples and the resultant characteristic absorption bands confirmed the double perovskite structure.展开更多
A series of W-type ferrites with the composition ofBal-xLaxCo2Fe16O27（where, x =0.0, 0.05, 0.10, 0.15, 0.20 and 0.25） were prepared by solid-state reaction method. The structure transformations of the ferrites were ...A series of W-type ferrites with the composition ofBal-xLaxCo2Fe16O27（where, x =0.0, 0.05, 0.10, 0.15, 0.20 and 0.25） were prepared by solid-state reaction method. The structure transformations of the ferrites were examined by XRD, DTA-TG and XPS, and the microwave-absorbing properties were investigated by evaluating the permeability and permittivity of materials（μτ,ετ, ）. The results showed that the phase-transition temperature increased with the addition of La^3＋ content, and a single-phase was formed at 1250℃ at last. Microwave properties were obviously improved as a result of the substitution of La^3＋ for Ba^2＋ at the frequency range of 0.5 - 18.0 GHz.展开更多
Perovskite-type Ba0.5Sr0.5Co0.8Fe0.2O3-σ （BSCFO） powders were synthesized using two methods, solid-state reaction （SSR） method and citrate-EDTA complexing method （CC-EDTA）. Then the powders were pressed to gree...Perovskite-type Ba0.5Sr0.5Co0.8Fe0.2O3-σ （BSCFO） powders were synthesized using two methods, solid-state reaction （SSR） method and citrate-EDTA complexing method （CC-EDTA）. Then the powders were pressed to green disks of 19 nun in diameter and sintered at 1140℃ for 5 h. The shrinkage rate and relative density of the membranes prepared from the perovskite-type powders were determined and calculated, and the powders and derived membranes were characterized by X-ray diffraction （XRD） and scanning electron microscopy （SEM）. The resuits show that the shrinkage rates of the two kinds of disks are nearly the same （about 10%）. The disks prepared by the SSR method had a bigger grain size and lower relative density than those prepared by the CC-EDTA method. The conductivity of the membranes prepared by the SSR method was about 38 S/cm, higher than that of the membranes prepared by the CC-EDTA method, which was about 30 S/cm, at the same temperature of600℃.展开更多
Ag（Nb0.8Ta0.2）O3 ceramics were prepared by the traditional solid-state reaction method. The effect of CaF2 addition on the structure and dielectric properties of Ag（Nb0.8Ta0.2）O3 ceramics was investigated. The add...Ag（Nb0.8Ta0.2）O3 ceramics were prepared by the traditional solid-state reaction method. The effect of CaF2 addition on the structure and dielectric properties of Ag（Nb0.8Ta0.2）O3 ceramics was investigated. The addition of CaF2 led the ceramics to a larger grain size and distortion of lattice. With the addition of 4.5 wt.% CaF2, the permittivity of the ceramics increased from 442 to 1028, the dielectric loss decreased sharply from 6.12 × 10^-3 to 8.6 × 10^-4, and the temperature coefficient of capacitance decreased from 1834 ppm/℃ to -50 ppm/℃ （at 1 MHz）. These results indicated that the high permittivity was related with a large grain size, a low grain boundary density, and the weak Ta-O or Nb-O bond strength caused by the addition of CaF2.展开更多
文摘Consecutive reaction between two solids, CuCl2.2H2O and 2,2'-bipyridyl in 1:2 molar ratio proceed in tWo steps: the salt first converts to the mediate, then the mediate turns to the final product.
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)) .
基金supported by the National Key Technology R&D Program (Nos. 2012BAC02B01, 2012BAC12B05, 2011BAE13B07, and 2011BAC10B02)the National High Technology Research and Development Program of China (No. 2012AA063202)+2 种基金the National Natural Science Foundation of China (Nos. 51174247 and 51004011)the Science and Technology Program of Guangdong Province, China (No. 2010A030200003)the Ph.D. Programs Foundation of the Ministry of Education of China (No. 2010000612003)
文摘Oily cold rolling mill （CRM） sludge is one of the pollutants emitted by iron and steel plants. Recycling oily CRM sludge can not only reduce pollution but also bring social and environmental benefits. In this study, using oily CRM sludge as sources of iron oxide, the strontium ferrite powders were synthesized in multiple steps including vacuum distillation, magnetic separation, oxidizing roasting, and solidstate reaction. The optimal technological conditions of vacuum distillation and oxidizing roasting were studied carefully. To consider the effects of Fe203/ SrCO3 tool ratio, calcination temperature, milling time and calcination time on magnetic properties of prepared strontium ferrite powders, the orthogonal experimental method was adopted. The maximum saturation magneti- zation （62.6 mA-m2.g-1） of the synthesized strontium ferrite powders was achieved at the Fe203/SrCO3 mol ratio of 6, 5 h milling time, 1250 ~C calcination temperature, and 1 h calcination time. Strontium ferrite powders syn- thesis method not only provides a cheap, high quality raw material for the production of strontium ferrite powders, but also effectively prevents the environmental pollution.
文摘A precursor of BaCe0.5Zr0.4Y0. 1O3-α electrolytes was synthesized by the sol-gel method and sintered at temperature which were 150 - 250 ℃ lower than by solid state reaction. The AC impedance spectrums of electrolytes were measured by AUTOLAB PGSTA30 electrochemical measuring device at different temperatures. The conductivities of the electrolytes are 1.62×10^-4 - 6.43×10^-3, 2.52×10^-5 - 3.73×10^-3S·cm^-1 in the temperature range of 350-800℃. The activity energies are 0.54 and 0.84 eV. At the same time BaCe0.9Y0.1O3-α was prepared by direct solid state reaction. The conductivity of BaCe0.9Y0.1O3-α is 1 × 10^-4- 4×10^-3 S·cm^-1 and the activation energy is 0.50 eV at the same condition. The results show that conduction of electrolyte prepared by sol-gel method is higher than the one by solid state reaction. As far as BaCe0.9Y0.1O3-α concerned, its conductivity of the Zr-substituted specimens is decreased.
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Project (2006BS04035) supported by the Youth Scientific Research Foundation of Shandong Province, China
文摘Nickel ferrite nano-powders were prepared by microwave radiating low-temperature solid-state reaction method, and then modified with Ag by dipping method. The crystal structure and morphology of the samples were characterized by means of X-ray diffraction（XRD）, scanning electron microscopy （SEM） and X-ray photoelectron spectroscopy （XPS）. The gas sensing properties of the samples were also investigated. The results reveal that the Ag, as amorphous structure, can efficiently prevent the reuniting and growing-up of nanosized NiFe2O4 grains, and 1.5% Ag modified NiFe2O4 sensor has a better sensitivity, up to 43, for acetone gas than 1.5%Ag mixed NiFe2O4 sensor prepared by low-temperature solid-state reaction, at an optimal working voltage of 4.5 V. The quick response time （1 s） and fast recovery time （～10 s） are the main characteristics of this sensor.
基金supported by the Doctor Research Fund of Henan Institute of Engineering (No. D2007012)
文摘Sm2（Zr1-xCex）2O7 （x=0.1, 0.2, and 0.3） ceramics were prepared by solid reaction method at 1600°C for 10 h using Sm2O3, ZrO2, and CeO2 as starting reactants. The phase compositions, microstructures, thermal expansion coefficients, and partial thermal conductivities of these materials were investigated. X-ray diffraction （XRD） results reveal that Sm2（Zr0.9Ce0.1）2O7 with pyrochlore structure and Sm2（Zr1-xCex）2O7 （x=0.2 and 0.3） with fluorite structure were synthesized, and scanning electrical microscopy （SEM） images show that the microstructures of these products are very dense. The linear thermal expansion coefficients increase with increasing temperature in the temperature range from ambient to 1200°C, and the thermal expansion coefficients increase with increasing content of doped CeO2. The thermal conductivities of Sm2（Zr0.8Ce0.2）2O7 and Sm2（Zr0.7Ce0.3）2O7 decrease gradually with an increase in temperature. These results show that the synthesized ceramic materials can be explored as novel prospective candidate materials for use in new thermal barrier coating systems in the future.
文摘The Ba2Zn1-xNixWO6 double perovskite oxides were synthesized using solid state reaction method. The effect of replacement of Zn<sup>2+</sup> with Ni<sup>2+</sup> cation on the structural properties was investigated by X-ray diffraction (XRD) at room temperature. From the X-ray diffraction and by means of standard Rietiveld method, the samples showed the same cubic crystal structure with (Fm-3m) space group and the crystallite size ranging from 71.91 nm to 148.71 nm. The unit cell volume was found to decrease as a result of the replacement, while there was no significant difference in the value of tolerance factor of the samples. This is may be due to the convergence of ionic radii of Ni<sup>2+</sup> and Zn<sup>2+</sup> cations. The Fourier Transform Infrared Spectroscopy (FTIR) was performed for the samples and the resultant characteristic absorption bands confirmed the double perovskite structure.
基金Project supported by the Natural Science Foundation of Jilin Province of China (20000512-2)Institute of Applied Chemistry of Jilin Province, China (R020202k)
文摘A series of W-type ferrites with the composition ofBal-xLaxCo2Fe16O27（where, x =0.0, 0.05, 0.10, 0.15, 0.20 and 0.25） were prepared by solid-state reaction method. The structure transformations of the ferrites were examined by XRD, DTA-TG and XPS, and the microwave-absorbing properties were investigated by evaluating the permeability and permittivity of materials（μτ,ετ, ）. The results showed that the phase-transition temperature increased with the addition of La^3＋ content, and a single-phase was formed at 1250℃ at last. Microwave properties were obviously improved as a result of the substitution of La^3＋ for Ba^2＋ at the frequency range of 0.5 - 18.0 GHz.
基金supported by the National High-Tech Research and Development Program of China (No. 2006AA11A189) the National Natural Science Foundation of China (No. 50730004)
文摘Perovskite-type Ba0.5Sr0.5Co0.8Fe0.2O3-σ （BSCFO） powders were synthesized using two methods, solid-state reaction （SSR） method and citrate-EDTA complexing method （CC-EDTA）. Then the powders were pressed to green disks of 19 nun in diameter and sintered at 1140℃ for 5 h. The shrinkage rate and relative density of the membranes prepared from the perovskite-type powders were determined and calculated, and the powders and derived membranes were characterized by X-ray diffraction （XRD） and scanning electron microscopy （SEM）. The resuits show that the shrinkage rates of the two kinds of disks are nearly the same （about 10%）. The disks prepared by the SSR method had a bigger grain size and lower relative density than those prepared by the CC-EDTA method. The conductivity of the membranes prepared by the SSR method was about 38 S/cm, higher than that of the membranes prepared by the CC-EDTA method, which was about 30 S/cm, at the same temperature of600℃.
基金supported by the Program for New Century Excellent Talents in Universities (NCET)the National High-Tech Research and Development Program of China (No. 2007AA03Z423)China Postdoctoral Science Foundation
文摘Ag（Nb0.8Ta0.2）O3 ceramics were prepared by the traditional solid-state reaction method. The effect of CaF2 addition on the structure and dielectric properties of Ag（Nb0.8Ta0.2）O3 ceramics was investigated. The addition of CaF2 led the ceramics to a larger grain size and distortion of lattice. With the addition of 4.5 wt.% CaF2, the permittivity of the ceramics increased from 442 to 1028, the dielectric loss decreased sharply from 6.12 × 10^-3 to 8.6 × 10^-4, and the temperature coefficient of capacitance decreased from 1834 ppm/℃ to -50 ppm/℃ （at 1 MHz）. These results indicated that the high permittivity was related with a large grain size, a low grain boundary density, and the weak Ta-O or Nb-O bond strength caused by the addition of CaF2.
