K4Ce2Nb10O30 ultrafine powders were prepared by stearic acid method (SAM). The obtained products were analyzed by X-ray diffraction, transmission electron microscopy, energy dispersive X-ray spectrometry, scanning ele...K4Ce2Nb10O30 ultrafine powders were prepared by stearic acid method (SAM). The obtained products were analyzed by X-ray diffraction, transmission electron microscopy, energy dispersive X-ray spectrometry, scanning electron microscopy and UV-visible absorption spectra. XRD patterns revealed that K4Ce2Nb10O30 powders treated at 900 oC for 2 h presented tetragonal structure without the presence of deleterious phases. Furthermore, the K4Ce2Nb10O30 prepared by SAM had considerable activity under visible light irradiation.展开更多
The CaCu3Ti4O12 xerogels, powders and ceramics were prepared through the sol-gel method using two kinds of organic acid (decanoic acid and decanedioic acid). The xerogels, powders and ceramics were characterized by ...The CaCu3Ti4O12 xerogels, powders and ceramics were prepared through the sol-gel method using two kinds of organic acid (decanoic acid and decanedioic acid). The xerogels, powders and ceramics were characterized by the methods of TG-DTG, FT-IR, XRD, SEM and TEM. The dielectric properties of the ceramics were also measured. The results indicated that the powders calcined at 850 ℃ for 2 h are both nanometer scale particles. After sintering, the ceramics mainly consist of the CaCu3Ti4O12 phase. Compared with the powders prepared using monoacid, the particle size of the powders prepared using diacid obviously increases, and the grain size, the relative density and the whole permittivity of the ceramics increase as well. Specially, the ceramic prepared using decanedioic acid has higher relative density (97.3%), dielectric constant (316 808) and lower dielectric loss (0.242 5) at 30 ℃ (10 kIaz)展开更多
PZT nanocrystalline powder was prepared by a stearic acid gel method. Thecrystallization process from the precursor was monitored by infrared spectroscopy, differentialthermal analysis, and thermogravimetric analysis....PZT nanocrystalline powder was prepared by a stearic acid gel method. Thecrystallization process from the precursor was monitored by infrared spectroscopy, differentialthermal analysis, and thermogravimetric analysis. The nano-sized PZT powder was characterized byX-ray diffraction and transmission electron microscopy. It shows that pure single-phase PZT powdercould be obtained at 450 deg C for 1 h, and the particle size is about 20 nm. With an increase inthe calcination temperature, the PZT crystallite size increased.展开更多
In this paper, we conduct research on the high-strength coating preparation methodology based on acid catalytic and Sol-Gel method. This method has been widely used in the preparation of various functional thin film, ...In this paper, we conduct research on the high-strength coating preparation methodology based on acid catalytic and Sol-Gel method. This method has been widely used in the preparation of various functional thin film, film and protective film structure, etc. As a result of sol gel process continuously broaden the application field, this method has been more and more get the favor of people. Compared with other traditional preparation methods of inorganic material, sol-gel process has many characteristics. To adjust the solution acidity and add a small amount of acid or alkali can have the effect of" catalyst, its reaction process on sol to get and gel structure may also be affected. Our research analyze the topic theoretically and numerically which is meaningful.展开更多
The effect of different annealing temperatures on the structure, morphology,and optical properties of ZnO thin films prepared by the chelating sol-gel method was investigated.Zinc-oxide thin films were coated on quart...The effect of different annealing temperatures on the structure, morphology,and optical properties of ZnO thin films prepared by the chelating sol-gel method was investigated.Zinc-oxide thin films were coated on quartz glass substrates by dip coating. Zinc nitrate, absoluteethanol, and citric acid were used as precursor, solvent, and chelating agent, respectively. Theresults show that ZnO films derived from zinc-citrate have lower crystallization temperature (below400℃), and that the crystal structure is wurtzite. The films, treated over 500℃, consist ofnano-particles and show to be porous at 600℃. The particle size of the film increases with theincrease of the annealing temperature. The largest particle size is 60 nm at 600℃. The opticaltransmittances related to the annealing temperatures become 90% higher in the visible range. Thefilm shows a starting absorption at 380 nm, and the optical band-gap of the thin film (fired at500℃) is 3.25 eV and close to the intrinsic band-gap of ZnO (3.2 eV).展开更多
To improve the cracking behavior of hydrocarbon,Ni-Mo/SiO_(2) bimetallic catalysts were synthesized by different preparation methods(sol-gel,co-impregnation and single-impregnation) and added the additives(citric acid...To improve the cracking behavior of hydrocarbon,Ni-Mo/SiO_(2) bimetallic catalysts were synthesized by different preparation methods(sol-gel,co-impregnation and single-impregnation) and added the additives(citric acid,polyethylene glycol and cetyltrimethylammonium bromide) based on the most suitable method above.The cracking reaction of methylcyclohexane under supercritical conditions was performed as the probe reaction to estimate the catalytic performance,and the properties of Ni-Mo/SiO_(2) catalyst were characterized by N_(2) absorption-desorption,XRD,XPS,H_(2)-TPR,NH_(3)-TPD,in-situ IR of NH_(3) desorption,HRTEM and STEM-mapping so as to study the structure-activity relationship.The catalyst synthesized via sol-gel method showed the best conversion and heat sink,being 81.8% and 3.81 MJ/kg,which was closely related to strong mutual effect between active components and SiO_(2) as well as strong acid sites.Besides,the introduction of additives by sol-gel method has an affirmative influence on properties of Ni-Mo/SiO_(2) catalysts,being that the acidity(more L and B acid sites) was modulated and organic groups interact with metal to suppress the aggregation of metal species(Ni and Mo),thereby enhancing the catalytic activity.At 750℃,the conversion(89.3%) as well as heat sink(3.99 MJ/kg) of MCH cracking obtained an optimum over Ni-Mo/SiO_(2) catalyst with addition of citric acid.展开更多
Li2Fe0.5Mn0.5SiO4 material was synthesized by a citric acid-assisted sol-gel method. The influence of the stoichiometric ratio value of n(citric acid) to n(Fe2+-Mn2+) on the electrochemical properties of Li2Fe0.5Mn0.5...Li2Fe0.5Mn0.5SiO4 material was synthesized by a citric acid-assisted sol-gel method. The influence of the stoichiometric ratio value of n(citric acid) to n(Fe2+-Mn2+) on the electrochemical properties of Li2Fe0.5Mn0.5SiO4 was studied. The final sample was identified as Li2Fe0.5Mn0.5SiO4 with a Pmn21 monoclinic structure by X-ray diffraction analysis. The crystal phases components and crystal phase structure of the Li2Fe0.5Mn0.4SiO4 material were improved as the increase of the stoichiometric ratio value of n(citric acid) to n(Fe2+-Mn2+). Field-emission scanning electron microscopy verified that the Li2Fe0.5Mn0.5SiO4 particles are agglomerates of Li2Fe0.5Mn0.5SiO4 primary particles with a geometric mean diameter of 220 nm. The Li2Fe0.5Mn0.5SiO4 sample was used as an electrode material for rechargeable lithium ion batteries, and the electrochemical measurements were carried out at room temperature. The Li2Fe0.5Mn0.5SiO4 electrode delivered a first discharge capacity of 230.1 mAh/g at the current density of 10 mA/g in first cycle and about 162 mAh/g after 20 cycles at the current density of 20 mA/g.展开更多
A new solid acid catalyst,SO4^2-/TiO2 modified with tin,was prepared using a sol-gel method and its physicochemical properties were revealed by nitrogen adsorption-desorption,X-ray powder diffraction,scanning electron...A new solid acid catalyst,SO4^2-/TiO2 modified with tin,was prepared using a sol-gel method and its physicochemical properties were revealed by nitrogen adsorption-desorption,X-ray powder diffraction,scanning electron microscopy,Fourier transform infrared spectroscopy,infrared spectroscopy of adsorbed pyridine,temperature-programmed desorption of ammonia and thermal gravimetric analysis.The structure,acidity and thermal stability of the SO4^2-/TiO2-SnO2 catalyst were studied.Incorporating tin enlarged the specific surface area and decreased crystallite size of the SO4^2-/TiO2 catalyst.The total acid sites of the modified catalyst increased and Bronsted acid strength remarkably increased with increasing tin content.The decomposition temperature of sulfate radical in the modified catalyst was 100 ℃ greater and its mass loss was more than twice that of the SO4^2-/TiO2 catalyst.The SO4^2-/TiO2-SnO2 catalyst was designed to synthesize 1,6-hexanediol diacrylate by esterification of 1,6-hexanediol with crylic acid.The yield of 1,6-hexanediol diacrylate exceeded 87% under the optimal reaction conditions:crylic acid to 1,6-hexanediol molar ratio = 3.5,catalyst loading = 7%,reaction temperature = 130 ℃ and reaction time = 3 h.The modified catalyst exhibited excellent reusability and after 10 cycles the conversion of 1,6-hexanediol was above 81%.展开更多
LiMn<sub>2</sub>O<sub>4</sub> and LiCu<sub>x</sub>Cr<sub>y</sub>Mn<sub>2-x-y</sub>O<sub>4</sub> (x = 0.50;y = 0.05 - 0.50) powders have been synt...LiMn<sub>2</sub>O<sub>4</sub> and LiCu<sub>x</sub>Cr<sub>y</sub>Mn<sub>2-x-y</sub>O<sub>4</sub> (x = 0.50;y = 0.05 - 0.50) powders have been synthesized via sol-gel method for the first time using Myristic acid as chelating agent. The synthesized samples have been taken to physical and electrochemical characterization such as thermo gravimetric analysis (TG/DTA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and electrochemical characterization viz., electrochemical galvanostatic cycling studies, electrochemical impedance spectroscopy (EIS) and differential capacity curves (dQ/dE). XRD patterns of LiMn<sub>2</sub>O<sub>4</sub> and LiCu<sub>x</sub>Cr<sub>y</sub>Mn<sub>2-x-y</sub>O<sub>4</sub> confirm high degree of crystallinity with good phase purity. FESEM image of undoped pristine spinel lucidly depicts cauliflower morphology with good agglomerated particle size of 50 nm while 0.5-Cu doped samples depict the pebbles morphology. TEM images of the spinel LiMn<sub>2</sub>O<sub>4</sub> and LiCu<sub>0.5</sub>Cr<sub>0.05</sub>Mn<sub>1.45</sub>O<sub>4</sub> authenticate that all the synthesized particles via sol-gel method are nano-sized (100 nm) with spherical surface and cloudy particles morphology. The LiMn<sub>2</sub>O<sub>4</sub> samples calcined at 850℃ deliver the high discharge capacity of 130 mA·h/g with cathodic efficiency of 88% corresponds to 94% columbic efficiency in the first cycle. Among all four compositions studied, LiCu<sub>0.5</sub>Cr<sub>0.05</sub>Mn<sub>1.45</sub>O<sub>4</sub> delivers 124 mA·h/g during the first cycle and shows stable performance with a low capacity fade of 1.1 mA·h/g cycle over the investigated 10 cycles.展开更多
A salt-assistant stearic acid method (SAM) capable of forming ultrafine K4Ce2Nb10O30 products was described. XRD pattern re-vealed that tetragonal K4Ce2Nb10O30 products could be obtained by heat treatment at 900 ℃ ...A salt-assistant stearic acid method (SAM) capable of forming ultrafine K4Ce2Nb10O30 products was described. XRD pattern re-vealed that tetragonal K4Ce2Nb10O30 products could be obtained by heat treatment at 900 ℃ for 2 h. Transmission electron microscopy (TEM) observations indicated the introduction of KCl could lead to the formation of rod-like K4Ce2Nb10O30 products. The species of salts played a crucial role in fine tuning the shapes and sizes of K4Ce2Nb10O30 products. Furthermore, the K4Ce2Nb10O30 prepared by salt-assistant SAM had considerable activity under visible light irradiation.展开更多
A new stearic acid method(SAM) has been used to prepare ultrafine K2La2Ti3O10 nanocrystalline. Each state of synthesis process was followed by the use of FT IR analysis. The resulting materials have been characterized...A new stearic acid method(SAM) has been used to prepare ultrafine K2La2Ti3O10 nanocrystalline. Each state of synthesis process was followed by the use of FT IR analysis. The resulting materials have been characterized by means of XRD, TEM, BET surface area analysis. The acid exchanging property of the obtained product was also studied. The experimental results showed that comparing with the product of traditional solid state reaction, the particle size of the K2La2Ti3O10 synthesized by SAM is greatly reduced, BET surface area is high(more than 11.83m2· g- 1) and has different acid exchanging properties. It can be easily exfoliated in 2mol· L- 1 HNO3 solution.展开更多
基金Project supported by the National Natural Science Foundation of China (20872051) "Zijin Star" of NJUST
文摘K4Ce2Nb10O30 ultrafine powders were prepared by stearic acid method (SAM). The obtained products were analyzed by X-ray diffraction, transmission electron microscopy, energy dispersive X-ray spectrometry, scanning electron microscopy and UV-visible absorption spectra. XRD patterns revealed that K4Ce2Nb10O30 powders treated at 900 oC for 2 h presented tetragonal structure without the presence of deleterious phases. Furthermore, the K4Ce2Nb10O30 prepared by SAM had considerable activity under visible light irradiation.
基金Projects(CC20120031,CC20110048)supported by Changzhou Science and Technology Innovation Project,China
文摘The CaCu3Ti4O12 xerogels, powders and ceramics were prepared through the sol-gel method using two kinds of organic acid (decanoic acid and decanedioic acid). The xerogels, powders and ceramics were characterized by the methods of TG-DTG, FT-IR, XRD, SEM and TEM. The dielectric properties of the ceramics were also measured. The results indicated that the powders calcined at 850 ℃ for 2 h are both nanometer scale particles. After sintering, the ceramics mainly consist of the CaCu3Ti4O12 phase. Compared with the powders prepared using monoacid, the particle size of the powders prepared using diacid obviously increases, and the grain size, the relative density and the whole permittivity of the ceramics increase as well. Specially, the ceramic prepared using decanedioic acid has higher relative density (97.3%), dielectric constant (316 808) and lower dielectric loss (0.242 5) at 30 ℃ (10 kIaz)
基金This work was financially supported by the Ministry of Science and Technology of China through 973-project (No. 2002CB613301).
文摘PZT nanocrystalline powder was prepared by a stearic acid gel method. Thecrystallization process from the precursor was monitored by infrared spectroscopy, differentialthermal analysis, and thermogravimetric analysis. The nano-sized PZT powder was characterized byX-ray diffraction and transmission electron microscopy. It shows that pure single-phase PZT powdercould be obtained at 450 deg C for 1 h, and the particle size is about 20 nm. With an increase inthe calcination temperature, the PZT crystallite size increased.
文摘In this paper, we conduct research on the high-strength coating preparation methodology based on acid catalytic and Sol-Gel method. This method has been widely used in the preparation of various functional thin film, film and protective film structure, etc. As a result of sol gel process continuously broaden the application field, this method has been more and more get the favor of people. Compared with other traditional preparation methods of inorganic material, sol-gel process has many characteristics. To adjust the solution acidity and add a small amount of acid or alkali can have the effect of" catalyst, its reaction process on sol to get and gel structure may also be affected. Our research analyze the topic theoretically and numerically which is meaningful.
基金This work was financially supported by the Natural Science Foundation of Tianjin (No. 33802311)
文摘The effect of different annealing temperatures on the structure, morphology,and optical properties of ZnO thin films prepared by the chelating sol-gel method was investigated.Zinc-oxide thin films were coated on quartz glass substrates by dip coating. Zinc nitrate, absoluteethanol, and citric acid were used as precursor, solvent, and chelating agent, respectively. Theresults show that ZnO films derived from zinc-citrate have lower crystallization temperature (below400℃), and that the crystal structure is wurtzite. The films, treated over 500℃, consist ofnano-particles and show to be porous at 600℃. The particle size of the film increases with theincrease of the annealing temperature. The largest particle size is 60 nm at 600℃. The opticaltransmittances related to the annealing temperatures become 90% higher in the visible range. Thefilm shows a starting absorption at 380 nm, and the optical band-gap of the thin film (fired at500℃) is 3.25 eV and close to the intrinsic band-gap of ZnO (3.2 eV).
基金supported by National Natural Science Foundation of China [grant number 91841301]Fundamental Research Funds for the Central Universities [grant number YJ201791]。
文摘To improve the cracking behavior of hydrocarbon,Ni-Mo/SiO_(2) bimetallic catalysts were synthesized by different preparation methods(sol-gel,co-impregnation and single-impregnation) and added the additives(citric acid,polyethylene glycol and cetyltrimethylammonium bromide) based on the most suitable method above.The cracking reaction of methylcyclohexane under supercritical conditions was performed as the probe reaction to estimate the catalytic performance,and the properties of Ni-Mo/SiO_(2) catalyst were characterized by N_(2) absorption-desorption,XRD,XPS,H_(2)-TPR,NH_(3)-TPD,in-situ IR of NH_(3) desorption,HRTEM and STEM-mapping so as to study the structure-activity relationship.The catalyst synthesized via sol-gel method showed the best conversion and heat sink,being 81.8% and 3.81 MJ/kg,which was closely related to strong mutual effect between active components and SiO_(2) as well as strong acid sites.Besides,the introduction of additives by sol-gel method has an affirmative influence on properties of Ni-Mo/SiO_(2) catalysts,being that the acidity(more L and B acid sites) was modulated and organic groups interact with metal to suppress the aggregation of metal species(Ni and Mo),thereby enhancing the catalytic activity.At 750℃,the conversion(89.3%) as well as heat sink(3.99 MJ/kg) of MCH cracking obtained an optimum over Ni-Mo/SiO_(2) catalyst with addition of citric acid.
基金Projects(13A047,10B054)supported by the Scientific Research Fund of Hunan Provincial Education Department,ChinaProjects(2011GK2002,2011FJ3160)supported by the Planned Science and Technology Project of Hunan Province,China
文摘Li2Fe0.5Mn0.5SiO4 material was synthesized by a citric acid-assisted sol-gel method. The influence of the stoichiometric ratio value of n(citric acid) to n(Fe2+-Mn2+) on the electrochemical properties of Li2Fe0.5Mn0.5SiO4 was studied. The final sample was identified as Li2Fe0.5Mn0.5SiO4 with a Pmn21 monoclinic structure by X-ray diffraction analysis. The crystal phases components and crystal phase structure of the Li2Fe0.5Mn0.4SiO4 material were improved as the increase of the stoichiometric ratio value of n(citric acid) to n(Fe2+-Mn2+). Field-emission scanning electron microscopy verified that the Li2Fe0.5Mn0.5SiO4 particles are agglomerates of Li2Fe0.5Mn0.5SiO4 primary particles with a geometric mean diameter of 220 nm. The Li2Fe0.5Mn0.5SiO4 sample was used as an electrode material for rechargeable lithium ion batteries, and the electrochemical measurements were carried out at room temperature. The Li2Fe0.5Mn0.5SiO4 electrode delivered a first discharge capacity of 230.1 mAh/g at the current density of 10 mA/g in first cycle and about 162 mAh/g after 20 cycles at the current density of 20 mA/g.
文摘A new solid acid catalyst,SO4^2-/TiO2 modified with tin,was prepared using a sol-gel method and its physicochemical properties were revealed by nitrogen adsorption-desorption,X-ray powder diffraction,scanning electron microscopy,Fourier transform infrared spectroscopy,infrared spectroscopy of adsorbed pyridine,temperature-programmed desorption of ammonia and thermal gravimetric analysis.The structure,acidity and thermal stability of the SO4^2-/TiO2-SnO2 catalyst were studied.Incorporating tin enlarged the specific surface area and decreased crystallite size of the SO4^2-/TiO2 catalyst.The total acid sites of the modified catalyst increased and Bronsted acid strength remarkably increased with increasing tin content.The decomposition temperature of sulfate radical in the modified catalyst was 100 ℃ greater and its mass loss was more than twice that of the SO4^2-/TiO2 catalyst.The SO4^2-/TiO2-SnO2 catalyst was designed to synthesize 1,6-hexanediol diacrylate by esterification of 1,6-hexanediol with crylic acid.The yield of 1,6-hexanediol diacrylate exceeded 87% under the optimal reaction conditions:crylic acid to 1,6-hexanediol molar ratio = 3.5,catalyst loading = 7%,reaction temperature = 130 ℃ and reaction time = 3 h.The modified catalyst exhibited excellent reusability and after 10 cycles the conversion of 1,6-hexanediol was above 81%.
文摘LiMn<sub>2</sub>O<sub>4</sub> and LiCu<sub>x</sub>Cr<sub>y</sub>Mn<sub>2-x-y</sub>O<sub>4</sub> (x = 0.50;y = 0.05 - 0.50) powders have been synthesized via sol-gel method for the first time using Myristic acid as chelating agent. The synthesized samples have been taken to physical and electrochemical characterization such as thermo gravimetric analysis (TG/DTA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and electrochemical characterization viz., electrochemical galvanostatic cycling studies, electrochemical impedance spectroscopy (EIS) and differential capacity curves (dQ/dE). XRD patterns of LiMn<sub>2</sub>O<sub>4</sub> and LiCu<sub>x</sub>Cr<sub>y</sub>Mn<sub>2-x-y</sub>O<sub>4</sub> confirm high degree of crystallinity with good phase purity. FESEM image of undoped pristine spinel lucidly depicts cauliflower morphology with good agglomerated particle size of 50 nm while 0.5-Cu doped samples depict the pebbles morphology. TEM images of the spinel LiMn<sub>2</sub>O<sub>4</sub> and LiCu<sub>0.5</sub>Cr<sub>0.05</sub>Mn<sub>1.45</sub>O<sub>4</sub> authenticate that all the synthesized particles via sol-gel method are nano-sized (100 nm) with spherical surface and cloudy particles morphology. The LiMn<sub>2</sub>O<sub>4</sub> samples calcined at 850℃ deliver the high discharge capacity of 130 mA·h/g with cathodic efficiency of 88% corresponds to 94% columbic efficiency in the first cycle. Among all four compositions studied, LiCu<sub>0.5</sub>Cr<sub>0.05</sub>Mn<sub>1.45</sub>O<sub>4</sub> delivers 124 mA·h/g during the first cycle and shows stable performance with a low capacity fade of 1.1 mA·h/g cycle over the investigated 10 cycles.
基金supported by the National Natural Science Foundation of China (50902070)the Natural Science Foundation of Jiangsu province (BK2009391)+1 种基金the Research Fund for the Doctoral Program of Higher Education of China (20093219120011)NUST Research Funding (ZDJH07)
文摘A salt-assistant stearic acid method (SAM) capable of forming ultrafine K4Ce2Nb10O30 products was described. XRD pattern re-vealed that tetragonal K4Ce2Nb10O30 products could be obtained by heat treatment at 900 ℃ for 2 h. Transmission electron microscopy (TEM) observations indicated the introduction of KCl could lead to the formation of rod-like K4Ce2Nb10O30 products. The species of salts played a crucial role in fine tuning the shapes and sizes of K4Ce2Nb10O30 products. Furthermore, the K4Ce2Nb10O30 prepared by salt-assistant SAM had considerable activity under visible light irradiation.
文摘A new stearic acid method(SAM) has been used to prepare ultrafine K2La2Ti3O10 nanocrystalline. Each state of synthesis process was followed by the use of FT IR analysis. The resulting materials have been characterized by means of XRD, TEM, BET surface area analysis. The acid exchanging property of the obtained product was also studied. The experimental results showed that comparing with the product of traditional solid state reaction, the particle size of the K2La2Ti3O10 synthesized by SAM is greatly reduced, BET surface area is high(more than 11.83m2· g- 1) and has different acid exchanging properties. It can be easily exfoliated in 2mol· L- 1 HNO3 solution.