A new two-step synthetic method was successfully developed to simplify the recrystallization process of lithium difluoro(oxalate)borate(LiODFB).Meanwhile,the purity of LiODFB as-prepared was determined by NMR,ICP-AES ...A new two-step synthetic method was successfully developed to simplify the recrystallization process of lithium difluoro(oxalate)borate(LiODFB).Meanwhile,the purity of LiODFB as-prepared was determined by NMR,ICP-AES and Karl Fisher measurements,respectively.The as-prepared LiODFB presents a high purity up to 99.95%.Its metal ions and water contents are under good control as well.Besides,its structure information and thermal properties were confirmed by FTIR,Raman and DSC-TGA analyses,respectively.LiODFB exerts fine thermostability and hypo-water-sensitivity and its structure information agrees well with previous literature.Furthermore,a combination of phase diagram and Raman spectroscopy were utilized to study the thermal phase behavior and ions coordination of LiODFB-DMC binary system to optimize the synthesis and recrystallization process.Although there are three types of molecular interaction forms(CIPs,AGG-IIa,AGG-IIIb)in LiODFB-DMC binary system,LiODFB can only be isolated as large single crystal solvate as LiODFB·(DMC)3/2 by slowly cooling subjected to the nucleation kinetics.Therefore,the fundamental information of our work is helpful in accelerating the application of LiODFB in Li-ion secondary batteries.展开更多
The synthetic method of nickel borate acylate (NBA), a kind of rubber steel cord adhesion promoter (AP), through nickel carbonate, borate and mixed carboxylic acid was studied. The preparation of nickel carbonate coul...The synthetic method of nickel borate acylate (NBA), a kind of rubber steel cord adhesion promoter (AP), through nickel carbonate, borate and mixed carboxylic acid was studied. The preparation of nickel carbonate could be performed through reaction of nickel sulfate with sodium carbonate in aqueous solution, in which fractional conversion of nickel was more than 99.9%. The mixed nickel carboxylate was prepared by the reaction of nickel carbonate with isooctanoic acid and acetic acid, under strong stirring for 2 h, the mole ratio of these chemicals were 1∶1∶1.1 respectively, and water should be removed completely by adding of inert organic solvent after reaction was finished so as to avoid hydrolysis of tributyl borate in the second reaction. NBA was synthesized by reaction of mixed nickel carboxylate with tributyl borate under strong stirring at 200 250 ℃ for 6 h. By detection and comparison with 680C product from Manobond Company of England, the NBA synthesized through isooctanoic acid and tributyl borate was very similar to product 680C in IR data, 300% fixed extension strength, tensile strength, hardness and cure curve, and was slightly lower than those of product 680C in tensile failure extensibility and hot air aging. The experimental results show that the prepared NBA can be used as rubber steel cord AP.展开更多
Based on anionic group theory,a computer assisted nonlinear optical(NLO)crystal design system has been developed.This method has proved to be a highly efficient means of discovering NLO crystals.With the help of this ...Based on anionic group theory,a computer assisted nonlinear optical(NLO)crystal design system has been developed.This method has proved to be a highly efficient means of discovering NLO crystals.With the help of this system,a series of new borate crystals,like as KBe 2BO 3F 2(KBBF),Sr 2Be 2B 2O 7(SBBO),Ba 2Be 2B 2O 7(SBBO),BaAl 2B 2O 7(BABO)and K 2Al 2B 2O 7(KABO)have been discovered.Among them KBBF possesses the shortest SHG wavelength output,SBBO has the largest SHG coefficient and KABO is found to have the best optical homogeneity and easy to grow out large size of the crystal.The investigation showed that KABO is a promising NLO crystal for 4 th and 5 th harmonic generations of Nd∶YAG laser.展开更多
Lithium difluoro(axalato)borate (LiODFB) was synthesized in dimethyl carbonate (DMC) solvent and purified by the method of solventing-out crystallization. The structure characterization of the purified LiODFB was perf...Lithium difluoro(axalato)borate (LiODFB) was synthesized in dimethyl carbonate (DMC) solvent and purified by the method of solventing-out crystallization. The structure characterization of the purified LiODFB was performed by Fourier transform infrared (FTIR) spectrometry and nuclear magnetic resonance (NMR) spectrometry. The electrochemical properties of the cells using 1 mol/L LiPF6 and 1 mol/L LiODFB in ethylene carbonate (EC)/DMC were investigated, respectively. The results indicate that LiODFB can be reduced at about 1.5 V and form a robust protective solid electrolyte interface (SEI) film on the graphite surface in the first cycle. The graphite/LiNi1/3Mn1/3Co1/3O2 cells with LiODFB-based electrolyte have very good capacity retention at 55 ℃, and show very good rate capability at 0.5C and 1C charge/discharge rate. Therefore, as a new salt, LiODFB is a most promising alternative lithium salt to replace LiPF6 for lithium ion battery electrolytes in the future.展开更多
Lead-free low melting glasses,ZnO-CuO-Bi_(2)O_(3)-B_(2)O_(3)-SiO_(2)system,with fixed contents of 15 mol%CuO and 20 mol%Bi_(2)O_(3),were prepared by using melt cooling method.Structure and thermal properties of the gl...Lead-free low melting glasses,ZnO-CuO-Bi_(2)O_(3)-B_(2)O_(3)-SiO_(2)system,with fixed contents of 15 mol%CuO and 20 mol%Bi_(2)O_(3),were prepared by using melt cooling method.Structure and thermal properties of the glasses were studied by using X-ray diffractometer(XRD),infrared spectrometer(FIT-IR),thermal dilatometer and differential thermal analyzer(DTA).Chemical durability of the glasses was studied by using dissolution rate method.Wettability of glasses on substrate was tested by using button sintering experiment.It is found that alkaline resistance of the glass solders is lower than that of plate glass and the water resistance is comparable with that of plate glass.The sealing temperatures are Ts=445-490℃,while the average thermal expansion coefficient from room temperature to 300℃is in the range of(65-82)×10^(−7)℃^(−1).At sealing temperature,the glass solders have good wettability on plate glass or alumina substrate.They are not crystallized even sintered at the sealing temperature for 30 min.The solder glasses are suitable for sealing plate glass,alumina and other inorganic non-metallic materials.展开更多
All solid state UV lasers have been in demand for various industrial and medical applications because of the convenient operation procedure and cost effectiveness as alternative to corrosive gas based excimer laser.Th...All solid state UV lasers have been in demand for various industrial and medical applications because of the convenient operation procedure and cost effectiveness as alternative to corrosive gas based excimer laser.The performance of such lasers seems to depend on the capability and reliability of UV frequency converter.In the third decade,CsLiB 6O 10 (CLBO)and Gd xY 1 x Ca 4O(BO 3) 3 (GdYCOB)were developed by the authors group.CLBO is the most effective nonlinear optical crystal to generate high power fourth and fifth harmonics of Nd∶YAG laser.GdYCOB is the first material which can achieve noncritical phase matching (NCPM) condition for THG of Nd∶YAG laser.The NCPM condition is advantageous owing to its large angular acceptance and the elimination of walk off between fundamental and harmonic lights.On the other hand,reliability is very importmat for actual application of these crystals.Here,we will present about techniques to improve durability of NLO crystals for high power UV light generation.For instance,we found that removal of surface polishing compound by means of ion beam etching can imrpove surface durability of CLBO.Also,we will discussed about photo induced damages in GdYCOB and its solution.展开更多
基金Project(51371198)supported by the National Natural Science Foundation of ChinaProject(K1202039-11)supported by the Science and Technology Project of Changsha,China
文摘A new two-step synthetic method was successfully developed to simplify the recrystallization process of lithium difluoro(oxalate)borate(LiODFB).Meanwhile,the purity of LiODFB as-prepared was determined by NMR,ICP-AES and Karl Fisher measurements,respectively.The as-prepared LiODFB presents a high purity up to 99.95%.Its metal ions and water contents are under good control as well.Besides,its structure information and thermal properties were confirmed by FTIR,Raman and DSC-TGA analyses,respectively.LiODFB exerts fine thermostability and hypo-water-sensitivity and its structure information agrees well with previous literature.Furthermore,a combination of phase diagram and Raman spectroscopy were utilized to study the thermal phase behavior and ions coordination of LiODFB-DMC binary system to optimize the synthesis and recrystallization process.Although there are three types of molecular interaction forms(CIPs,AGG-IIa,AGG-IIIb)in LiODFB-DMC binary system,LiODFB can only be isolated as large single crystal solvate as LiODFB·(DMC)3/2 by slowly cooling subjected to the nucleation kinetics.Therefore,the fundamental information of our work is helpful in accelerating the application of LiODFB in Li-ion secondary batteries.
文摘The synthetic method of nickel borate acylate (NBA), a kind of rubber steel cord adhesion promoter (AP), through nickel carbonate, borate and mixed carboxylic acid was studied. The preparation of nickel carbonate could be performed through reaction of nickel sulfate with sodium carbonate in aqueous solution, in which fractional conversion of nickel was more than 99.9%. The mixed nickel carboxylate was prepared by the reaction of nickel carbonate with isooctanoic acid and acetic acid, under strong stirring for 2 h, the mole ratio of these chemicals were 1∶1∶1.1 respectively, and water should be removed completely by adding of inert organic solvent after reaction was finished so as to avoid hydrolysis of tributyl borate in the second reaction. NBA was synthesized by reaction of mixed nickel carboxylate with tributyl borate under strong stirring at 200 250 ℃ for 6 h. By detection and comparison with 680C product from Manobond Company of England, the NBA synthesized through isooctanoic acid and tributyl borate was very similar to product 680C in IR data, 300% fixed extension strength, tensile strength, hardness and cure curve, and was slightly lower than those of product 680C in tensile failure extensibility and hot air aging. The experimental results show that the prepared NBA can be used as rubber steel cord AP.
文摘Based on anionic group theory,a computer assisted nonlinear optical(NLO)crystal design system has been developed.This method has proved to be a highly efficient means of discovering NLO crystals.With the help of this system,a series of new borate crystals,like as KBe 2BO 3F 2(KBBF),Sr 2Be 2B 2O 7(SBBO),Ba 2Be 2B 2O 7(SBBO),BaAl 2B 2O 7(BABO)and K 2Al 2B 2O 7(KABO)have been discovered.Among them KBBF possesses the shortest SHG wavelength output,SBBO has the largest SHG coefficient and KABO is found to have the best optical homogeneity and easy to grow out large size of the crystal.The investigation showed that KABO is a promising NLO crystal for 4 th and 5 th harmonic generations of Nd∶YAG laser.
基金Project(2007BAE12B01) supported by the National Key Technology Research and Development Program of ChinaProject(20803095) supported by the National Natural Science Foundation of China
文摘Lithium difluoro(axalato)borate (LiODFB) was synthesized in dimethyl carbonate (DMC) solvent and purified by the method of solventing-out crystallization. The structure characterization of the purified LiODFB was performed by Fourier transform infrared (FTIR) spectrometry and nuclear magnetic resonance (NMR) spectrometry. The electrochemical properties of the cells using 1 mol/L LiPF6 and 1 mol/L LiODFB in ethylene carbonate (EC)/DMC were investigated, respectively. The results indicate that LiODFB can be reduced at about 1.5 V and form a robust protective solid electrolyte interface (SEI) film on the graphite surface in the first cycle. The graphite/LiNi1/3Mn1/3Co1/3O2 cells with LiODFB-based electrolyte have very good capacity retention at 55 ℃, and show very good rate capability at 0.5C and 1C charge/discharge rate. Therefore, as a new salt, LiODFB is a most promising alternative lithium salt to replace LiPF6 for lithium ion battery electrolytes in the future.
基金National Natural Science Foundation of China(52172070)Jiangxi Provincial Natural Science Foundation(20242BAB25222)Jiangxi Provincial Graduate Innovation Special Fund Project(YC2022-S882 and YC2023-S808).
文摘Lead-free low melting glasses,ZnO-CuO-Bi_(2)O_(3)-B_(2)O_(3)-SiO_(2)system,with fixed contents of 15 mol%CuO and 20 mol%Bi_(2)O_(3),were prepared by using melt cooling method.Structure and thermal properties of the glasses were studied by using X-ray diffractometer(XRD),infrared spectrometer(FIT-IR),thermal dilatometer and differential thermal analyzer(DTA).Chemical durability of the glasses was studied by using dissolution rate method.Wettability of glasses on substrate was tested by using button sintering experiment.It is found that alkaline resistance of the glass solders is lower than that of plate glass and the water resistance is comparable with that of plate glass.The sealing temperatures are Ts=445-490℃,while the average thermal expansion coefficient from room temperature to 300℃is in the range of(65-82)×10^(−7)℃^(−1).At sealing temperature,the glass solders have good wettability on plate glass or alumina substrate.They are not crystallized even sintered at the sealing temperature for 30 min.The solder glasses are suitable for sealing plate glass,alumina and other inorganic non-metallic materials.
文摘All solid state UV lasers have been in demand for various industrial and medical applications because of the convenient operation procedure and cost effectiveness as alternative to corrosive gas based excimer laser.The performance of such lasers seems to depend on the capability and reliability of UV frequency converter.In the third decade,CsLiB 6O 10 (CLBO)and Gd xY 1 x Ca 4O(BO 3) 3 (GdYCOB)were developed by the authors group.CLBO is the most effective nonlinear optical crystal to generate high power fourth and fifth harmonics of Nd∶YAG laser.GdYCOB is the first material which can achieve noncritical phase matching (NCPM) condition for THG of Nd∶YAG laser.The NCPM condition is advantageous owing to its large angular acceptance and the elimination of walk off between fundamental and harmonic lights.On the other hand,reliability is very importmat for actual application of these crystals.Here,we will present about techniques to improve durability of NLO crystals for high power UV light generation.For instance,we found that removal of surface polishing compound by means of ion beam etching can imrpove surface durability of CLBO.Also,we will discussed about photo induced damages in GdYCOB and its solution.
