The thermal decomposition process of （NH4）3AlF6 was studied by DTA-TGA method and the related thermodynamic data were obtained. The results show that AlF3 is obtained after three-step decomposition reaction of （NH4...The thermal decomposition process of （NH4）3AlF6 was studied by DTA-TGA method and the related thermodynamic data were obtained. The results show that AlF3 is obtained after three-step decomposition reaction of （NH4）3AlF6, and the solid products of the first two decomposition reactions are NH4AlF4 and AlF3（NH4F）0.69, respectively. The three reactions occur at 194.9, 222.5 and 258.4 ℃, respectively. Gibbs free energy changes of pertinent materials at the reaction temperatures were calculated. Enthalpy and entropy changes of the three reactions were analyzed by DSC method. Anhydrous aluminum fluoride was prepared. The XRD analysis and mass loss calculation show that AlF3 with high purity can be obtained by heating （NH4）3AlF6 at 400 ℃ for 3 h.展开更多
Cubic boron nitride（c-BN） was synthesized through benzene thermal method at a lower temperature of （300℃） by selecting liquid（（C2H5）2O·）BF3 and Li3N as reactants. Hexagonal boron nitride（h-BN） and orth...Cubic boron nitride（c-BN） was synthesized through benzene thermal method at a lower temperature of （300℃） by selecting liquid（（C2H5）2O·）BF3 and Li3N as reactants. Hexagonal boron nitride（h-BN） and orthorhombic boron nitride（o-BN） were also obtained. The samples were characterized by X-ray powder diffractometry and Fourier transformation infrared spectroscopy. The results show that all the BF3, BCl3 and BBr3 in the same family compounds can react with Li3N to synthesize BN since the strongest bond of B—F can be broken. Compared with BBr3, liquid （C2H5）2O·BF3 is cheaper, less toxic and more convenient to operate. Li3N not only provides nitrogen source but also has catalytic effect on accelerating the formation of c-BN at low temperature and pressure.展开更多
TiO2hollow microspheres(TiO2‐HMSs)have attracted much attention because of their high photoreactivity,low density,and good permeability.However,anatase TiO2‐HMSs have poor thermal stability.In this study,surface‐fl...TiO2hollow microspheres(TiO2‐HMSs)have attracted much attention because of their high photoreactivity,low density,and good permeability.However,anatase TiO2‐HMSs have poor thermal stability.In this study,surface‐fluorinated TiO2‐HMSs were assembled from hollow nanoparticles by the hydrothermal reaction of the mixed Ti(SO4)2–NH4HF–H2O2solution at180°C.The effect of the calcination temperature on the structure and photoreactivity of the TiO2‐HMSs was systematically investigated,which was evaluated by photocatalytic oxidation of acetone in air under ultraviolet irradiation.We found that after calcination at300°C,the photoreactivity of the TiO2‐HMSs decreases from1.39×10?3min?1(TiO2‐HMS precursor)to0.82×10?3min?1because of removal of surface‐adsorbed fluoride ions.With increasing calcination temperature from300to900°C,the building blocks of the TiO2‐HMSs evolve from truncated bipyramidal shaped hollow nanoparticles to round solid nanoparticles,and the photoreactivity of the TiO2‐HMSs steady increases from0.82×10?3to2.09×10?3min?1because of enhanced crystallization.Further increasing the calcination temperature to1000and1100°C results in a decrease of the photoreactivity,which is ascribed to a sharp decrease of the Brunauer–Emmett–Teller surface area and the beginning of the anatase–rutile phase transformation at1100°C.The effect of surface‐adsorbed fluoride ions on the thermal stability of the TiO2‐HMSs is also discussed.展开更多
Fluorosilicone oil is polysiloxane with alkyl side chains containing fluorine, and because of its excellent thermal oxidation stability, cold flow property and cryogenic property, it can be widely used as a high tempe...Fluorosilicone oil is polysiloxane with alkyl side chains containing fluorine, and because of its excellent thermal oxidation stability, cold flow property and cryogenic property, it can be widely used as a high temperature lubricant in the field of military aerospace industry. Two kinds of fluorosilicone oils, FSiO-a and FSiO-b, were synthesized by different pro- cessing means. FTICR MS was used to collect the information on composition and structure of the two polymers, respec- tively. The test results show that the two fluorosilicone oils have different contents of fluorine-containing chain segments (m/ n value), the maximum distribution of m/n value of FSiO-a oil ranges from 0.22 to 0.25, and that of FSiO-b oil ranges from 0.4 to 0.67. Difference in synthesis techniques makes this discrepancy and affects the quality and thermal stability of the fluoro- silicone oils.展开更多
A cross-linkable fluorinated poly (ether ether ketone) (FPEEK) was synthesized for the fabrication of arrayed waveguide grating (AWG) multiplexer. The results of thermal gravimetric analysis (TGA) and near-infrared ab...A cross-linkable fluorinated poly (ether ether ketone) (FPEEK) was synthesized for the fabrication of arrayed waveguide grating (AWG) multiplexer. The results of thermal gravimetric analysis (TGA) and near-infrared absorption spectrum show that the materials have high thermal stability and high optical transparency in the infrared communication region. The refractive index of FPEEK can be controlled easily by changing the fluorine content of the materials. The 32-channel AWG multiplexer is fabricated using the FPEEK and oxygen reactive ion etching technology. The AWG multiplexer exhibits that the insertion loss is from 12.8 to 17.8 dB and the channel crosstalk is less than-20 dB. The wavelength channel spacing and the center wavelength are 0.8nm and 1548nm, respectively.展开更多
A set of experimental data obtained at the Institute of Physics and Power Engineering in a vertical bundle cooled with supercritical R-12 was analyzed. The test section was a 7-element bundle installed in a hexagonal ...A set of experimental data obtained at the Institute of Physics and Power Engineering in a vertical bundle cooled with supercritical R-12 was analyzed. The test section was a 7-element bundle installed in a hexagonal flow channel with three grid spacers. Data was collected at pressures of approximately 4.65 MPa for several different combinations of wall and bulk-fluid temperatures that were below, at, or above pseudocritical conditions. Analysis of the data has confirmed that there are three distinct heat-transfer regimes for forced convention in supercritical fluids： （1） normal heat transfer, （2） deteriorated heat transfer, and （3） enhanced heat transfer. It was also confirmed that the effects of spacers are evident which was previously observed in sub-critical experimental data. This work compares the wall and bulk fluid temperature data of the experiments to predictions based upon current 1-D correlations for heat transfer in supercritical fluids.展开更多
A new effective process to improve the utilization of industrial fluorosilicic acid of phosphate fertilizer by-product has been investigated to comprehensive application of the silicon and fluorine source. Two-step am...A new effective process to improve the utilization of industrial fluorosilicic acid of phosphate fertilizer by-product has been investigated to comprehensive application of the silicon and fluorine source. Two-step ammoniation was applied to recover high-quality silica. The recovered silica can be used to hydrothermal synthesize ZSM-5 zeolite without impurity phase contamination, which was confirmed by XRD, TG, SEM, BET and EDS characteristic techniques. It was found that with the increase of SiO_2/Al_2O_3 ratio and the extension of reaction time, the crystal type transform from the orthorhombic to the monoclinic phase. The impurity fluorine content of the recovered SiO_2 from H_2SiF_6 has great influence on the hydrothermal process for ZSM-5 crystal structure formation.Moreover, the increase of fluorine ions content in the hydrothermal process can control the crystal morphology and size of synthesized ZSM-5. Catalytic properties of synthesized HZSM-5 with different SiO_2/Al_2O_3 ratio in transalkylation of toluene and 1,2,4-trimethylbenzene show good and stable catalytic performance. The ZSM-5 synthesized with recovered silica source exhibits similar catalyst life as the performance of small particle size HZSM-5, because the ZSM-5 synthesized with the silica source from industrial hexafluorosilicic acid prefers a thin disk crystal along the b axis direction, which shortens the diffusion distance of generated products.展开更多
TiO2 nanorod arrays （NRAs） were prepared on,fluorine doped tin oxide （FTO） substrates by a facile two-step hydrothermal method. The nanorods were selectively grown on the FTO regions which were covered with TiO2 s...TiO2 nanorod arrays （NRAs） were prepared on,fluorine doped tin oxide （FTO） substrates by a facile two-step hydrothermal method. The nanorods were selectively grown on the FTO regions which were covered with TiO2 seeding layer. It took 5 h to obtain the compact arrays with the nanorod length of -2 μm and diameter of-50 nm. The photoelectrochemical （PEC） properties of TiO2 NRAs are also investigated. It is demonstrated that the TiO2 NRAs indicate the good photoelectric conversion ability with an efficiency of 0.22% at a full-wavelength irradiation. A photocurrent density of 0.21 mA/cm2 is observed at 0,7 V versus the saturated calomel electrode （SCE）. More evidences suggest that the charge transferring resistance is lowered at an irradiation, while the flat-band potential （Vgb） is shifted towards the positive side.展开更多
HFC-227ea(1,1,1,2,3,3,3-heptafluoropropane) is considered as a promising refrigerant alternative, especially as a component in mixtures, to replace to CFC-12, HCFC-22 and R502. But reliable transport properties data f...HFC-227ea(1,1,1,2,3,3,3-heptafluoropropane) is considered as a promising refrigerant alternative, especially as a component in mixtures, to replace to CFC-12, HCFC-22 and R502. But reliable transport properties data for HFC-227ea are very limited. In this paper, experimental data of viscosity along the saturation line and gaseous thermal conductivity of HFC-227ea are given. The viscosity of HFC-227ea was measured with a capillary viscometer at temperatures between 263.15 K and 333.15 K along the saturation line and its uncertainty of the results is estimated to be no more than ±3%. The thermal conductivity of gaseous HFC-227ea was also measured with a transient hot-wire instrument at temperatures between 259.28 K and 341.75 K and pressures up to 1.289MiPa, and its uncertainty of the results is estimated to be less than ±1%.展开更多
A new silicate fluoride,NaBa3 Si207 F,has been successfully synthesized by a high-temperature solution method.It crystallizes in the orthorhombic space group Cmcm(No.63).NaBa3 Si2 O7 F is the first barium-containing a...A new silicate fluoride,NaBa3 Si207 F,has been successfully synthesized by a high-temperature solution method.It crystallizes in the orthorhombic space group Cmcm(No.63).NaBa3 Si2 O7 F is the first barium-containing alkali metal silicate fluoride with the[NaO6]polyhedra,the[BaO8 F]polyhedra and isolated[Si2 O7]units.The optical characterizations indicate that NaBa3 Si2 O7 F possesses wide transparent window and available luminescence properties.To confirm the coordination surroundings of anionic groups and its thermostability,infrared spectroscopy and thermal behaviors were also analyzed,which proved the existence of tetrahedronly coordinated silicium atoms and the good stability of NaBa3 Si2 O7 F at high temperature.First-principles calculation was also implemented for better understanding the relationship between the structure of NaBa3 Si207 F and its property.Additionally,to further explore the structural novelty of NaBa3 Si2 O7 F,the comparison of the anionic structures was carried out in mixed alkali and alkaline-earth metal silicate fluorides.Interestingly,the result indicates the isolated[Si2 O7]dimer is rare among the above systems,which enriches the structural chemistry of silicate fluorides.展开更多
基金Project(51004034)supported by the National Natural Science Foundation of ChinaProject(N090302009)supported by the Fundamental Research Funds for the Central Universities,China
文摘The thermal decomposition process of （NH4）3AlF6 was studied by DTA-TGA method and the related thermodynamic data were obtained. The results show that AlF3 is obtained after three-step decomposition reaction of （NH4）3AlF6, and the solid products of the first two decomposition reactions are NH4AlF4 and AlF3（NH4F）0.69, respectively. The three reactions occur at 194.9, 222.5 and 258.4 ℃, respectively. Gibbs free energy changes of pertinent materials at the reaction temperatures were calculated. Enthalpy and entropy changes of the three reactions were analyzed by DSC method. Anhydrous aluminum fluoride was prepared. The XRD analysis and mass loss calculation show that AlF3 with high purity can be obtained by heating （NH4）3AlF6 at 400 ℃ for 3 h.
基金Projects(2027300750372006) supported by the National Natural Science Foundation of China
文摘Cubic boron nitride（c-BN） was synthesized through benzene thermal method at a lower temperature of （300℃） by selecting liquid（（C2H5）2O·）BF3 and Li3N as reactants. Hexagonal boron nitride（h-BN） and orthorhombic boron nitride（o-BN） were also obtained. The samples were characterized by X-ray powder diffractometry and Fourier transformation infrared spectroscopy. The results show that all the BF3, BCl3 and BBr3 in the same family compounds can react with Li3N to synthesize BN since the strongest bond of B—F can be broken. Compared with BBr3, liquid （C2H5）2O·BF3 is cheaper, less toxic and more convenient to operate. Li3N not only provides nitrogen source but also has catalytic effect on accelerating the formation of c-BN at low temperature and pressure.
基金supported by the National Natural Science Foundation of China(51672312,21373275)the Science and Technology Program of Wuhan,China(2016010101010018,2015070504020220)the Dean’s Research Fund–04257 from the Education University of Hong Kong~~
文摘TiO2hollow microspheres(TiO2‐HMSs)have attracted much attention because of their high photoreactivity,low density,and good permeability.However,anatase TiO2‐HMSs have poor thermal stability.In this study,surface‐fluorinated TiO2‐HMSs were assembled from hollow nanoparticles by the hydrothermal reaction of the mixed Ti(SO4)2–NH4HF–H2O2solution at180°C.The effect of the calcination temperature on the structure and photoreactivity of the TiO2‐HMSs was systematically investigated,which was evaluated by photocatalytic oxidation of acetone in air under ultraviolet irradiation.We found that after calcination at300°C,the photoreactivity of the TiO2‐HMSs decreases from1.39×10?3min?1(TiO2‐HMS precursor)to0.82×10?3min?1because of removal of surface‐adsorbed fluoride ions.With increasing calcination temperature from300to900°C,the building blocks of the TiO2‐HMSs evolve from truncated bipyramidal shaped hollow nanoparticles to round solid nanoparticles,and the photoreactivity of the TiO2‐HMSs steady increases from0.82×10?3to2.09×10?3min?1because of enhanced crystallization.Further increasing the calcination temperature to1000and1100°C results in a decrease of the photoreactivity,which is ascribed to a sharp decrease of the Brunauer–Emmett–Teller surface area and the beginning of the anatase–rutile phase transformation at1100°C.The effect of surface‐adsorbed fluoride ions on the thermal stability of the TiO2‐HMSs is also discussed.
文摘Fluorosilicone oil is polysiloxane with alkyl side chains containing fluorine, and because of its excellent thermal oxidation stability, cold flow property and cryogenic property, it can be widely used as a high temperature lubricant in the field of military aerospace industry. Two kinds of fluorosilicone oils, FSiO-a and FSiO-b, were synthesized by different pro- cessing means. FTICR MS was used to collect the information on composition and structure of the two polymers, respec- tively. The test results show that the two fluorosilicone oils have different contents of fluorine-containing chain segments (m/ n value), the maximum distribution of m/n value of FSiO-a oil ranges from 0.22 to 0.25, and that of FSiO-b oil ranges from 0.4 to 0.67. Difference in synthesis techniques makes this discrepancy and affects the quality and thermal stability of the fluoro- silicone oils.
文摘A cross-linkable fluorinated poly (ether ether ketone) (FPEEK) was synthesized for the fabrication of arrayed waveguide grating (AWG) multiplexer. The results of thermal gravimetric analysis (TGA) and near-infrared absorption spectrum show that the materials have high thermal stability and high optical transparency in the infrared communication region. The refractive index of FPEEK can be controlled easily by changing the fluorine content of the materials. The 32-channel AWG multiplexer is fabricated using the FPEEK and oxygen reactive ion etching technology. The AWG multiplexer exhibits that the insertion loss is from 12.8 to 17.8 dB and the channel crosstalk is less than-20 dB. The wavelength channel spacing and the center wavelength are 0.8nm and 1548nm, respectively.
文摘A set of experimental data obtained at the Institute of Physics and Power Engineering in a vertical bundle cooled with supercritical R-12 was analyzed. The test section was a 7-element bundle installed in a hexagonal flow channel with three grid spacers. Data was collected at pressures of approximately 4.65 MPa for several different combinations of wall and bulk-fluid temperatures that were below, at, or above pseudocritical conditions. Analysis of the data has confirmed that there are three distinct heat-transfer regimes for forced convention in supercritical fluids： （1） normal heat transfer, （2） deteriorated heat transfer, and （3） enhanced heat transfer. It was also confirmed that the effects of spacers are evident which was previously observed in sub-critical experimental data. This work compares the wall and bulk fluid temperature data of the experiments to predictions based upon current 1-D correlations for heat transfer in supercritical fluids.
基金Supported by the National Natural Science Foundation of China(21306143)the Educational Commission of Hubei Province of China(D20161503)the Hubei Province Phosphorus Resource and Ethylene Project Downstream Exploitation Collaborative Innovation Center
文摘A new effective process to improve the utilization of industrial fluorosilicic acid of phosphate fertilizer by-product has been investigated to comprehensive application of the silicon and fluorine source. Two-step ammoniation was applied to recover high-quality silica. The recovered silica can be used to hydrothermal synthesize ZSM-5 zeolite without impurity phase contamination, which was confirmed by XRD, TG, SEM, BET and EDS characteristic techniques. It was found that with the increase of SiO_2/Al_2O_3 ratio and the extension of reaction time, the crystal type transform from the orthorhombic to the monoclinic phase. The impurity fluorine content of the recovered SiO_2 from H_2SiF_6 has great influence on the hydrothermal process for ZSM-5 crystal structure formation.Moreover, the increase of fluorine ions content in the hydrothermal process can control the crystal morphology and size of synthesized ZSM-5. Catalytic properties of synthesized HZSM-5 with different SiO_2/Al_2O_3 ratio in transalkylation of toluene and 1,2,4-trimethylbenzene show good and stable catalytic performance. The ZSM-5 synthesized with recovered silica source exhibits similar catalyst life as the performance of small particle size HZSM-5, because the ZSM-5 synthesized with the silica source from industrial hexafluorosilicic acid prefers a thin disk crystal along the b axis direction, which shortens the diffusion distance of generated products.
基金supported by the Science and Technology Projects of Xuzhou City(No.KC14SM088)the Natural Science Fund for Colleges and Universities in Jiangsu Province(No.15KJB430031)
文摘TiO2 nanorod arrays （NRAs） were prepared on,fluorine doped tin oxide （FTO） substrates by a facile two-step hydrothermal method. The nanorods were selectively grown on the FTO regions which were covered with TiO2 seeding layer. It took 5 h to obtain the compact arrays with the nanorod length of -2 μm and diameter of-50 nm. The photoelectrochemical （PEC） properties of TiO2 NRAs are also investigated. It is demonstrated that the TiO2 NRAs indicate the good photoelectric conversion ability with an efficiency of 0.22% at a full-wavelength irradiation. A photocurrent density of 0.21 mA/cm2 is observed at 0,7 V versus the saturated calomel electrode （SCE）. More evidences suggest that the charge transferring resistance is lowered at an irradiation, while the flat-band potential （Vgb） is shifted towards the positive side.
基金National NatUralScience Foundahon of China (Grant No.59706012).
文摘HFC-227ea(1,1,1,2,3,3,3-heptafluoropropane) is considered as a promising refrigerant alternative, especially as a component in mixtures, to replace to CFC-12, HCFC-22 and R502. But reliable transport properties data for HFC-227ea are very limited. In this paper, experimental data of viscosity along the saturation line and gaseous thermal conductivity of HFC-227ea are given. The viscosity of HFC-227ea was measured with a capillary viscometer at temperatures between 263.15 K and 333.15 K along the saturation line and its uncertainty of the results is estimated to be no more than ±3%. The thermal conductivity of gaseous HFC-227ea was also measured with a transient hot-wire instrument at temperatures between 259.28 K and 341.75 K and pressures up to 1.289MiPa, and its uncertainty of the results is estimated to be less than ±1%.
基金supported by the National Natural Science Foundation of China(U1703132,51872325 and 61835014)Tianshan Innovation Team Program(2018D14001)+5 种基金Xinjiang International Science&Technology Cooperation Program(2017E01014)the National Key Research Project(2016YFB0402104)the Science and Technology Project of Urumqi(P161010002)Xinjiang Key Research and Development Program(2016B02021)Major Program of Xinjiang Uygur Autonomous Region of China during the 13th Five-Year Plan Period(2016A02003)West Light Foundation of the Chinese Academy of Sciences(2016-YJRC-2)
文摘A new silicate fluoride,NaBa3 Si207 F,has been successfully synthesized by a high-temperature solution method.It crystallizes in the orthorhombic space group Cmcm(No.63).NaBa3 Si2 O7 F is the first barium-containing alkali metal silicate fluoride with the[NaO6]polyhedra,the[BaO8 F]polyhedra and isolated[Si2 O7]units.The optical characterizations indicate that NaBa3 Si2 O7 F possesses wide transparent window and available luminescence properties.To confirm the coordination surroundings of anionic groups and its thermostability,infrared spectroscopy and thermal behaviors were also analyzed,which proved the existence of tetrahedronly coordinated silicium atoms and the good stability of NaBa3 Si2 O7 F at high temperature.First-principles calculation was also implemented for better understanding the relationship between the structure of NaBa3 Si207 F and its property.Additionally,to further explore the structural novelty of NaBa3 Si2 O7 F,the comparison of the anionic structures was carried out in mixed alkali and alkaline-earth metal silicate fluorides.Interestingly,the result indicates the isolated[Si2 O7]dimer is rare among the above systems,which enriches the structural chemistry of silicate fluorides.
