The influence of cathodic pulse parameters was evaluated on plasma electrolytic oxidation(PEO)coatings grown on 7075 aluminum alloy in a silicate-based electrolyte containing potassium titanyl oxalate(PTO)using pulsed...The influence of cathodic pulse parameters was evaluated on plasma electrolytic oxidation(PEO)coatings grown on 7075 aluminum alloy in a silicate-based electrolyte containing potassium titanyl oxalate(PTO)using pulsed bipolar waveforms with various cathodic duty cycles and cathodic current densities.The coatings were characterized by SEM,EDS,and XRD.EIS was applied to investigate the electrochemical properties.It was observed that the increase of cathodic duty cycle and cathodic current density from 20%and 6 A/dm^(2) to 40%and 12 A/dm^(2) enhances the growth rate of the inner layer from 0.22 to 0.75μm/min.Adding PTO into the bath showed a fortifying effect on influence of the cathodic pulse and the mentioned change of cathodic pulse parameters,resulting in an increase of the inner layer growth rate from 0.25 to 1.10μm/min.Based on EDS analysis,Si and Ti were incorporated dominantly in the upper parts of the coatings.XRD technique merely detectedγ-Al_(2)O_(3),and there were no detectable peaks related to Ti and Si compounds.However,the EIS results confirmed that the incorporation of Ti^(4+)into alumina changed the electronic properties of the coating.The coatings obtained from the bath containing PTO using the bipolar waveforms with a cathodic duty cycle of 40%and current density values higher than 6 A/dm^(2) showed highly appropriate electrochemical behavior during 240 d of immersion due to an efficient repairing mechanism.Regarding the effects of studied parameters on the coating properties,the roles of cathodic pulse parameters and PTO in the PEO process were highlighted.展开更多
Silane coupling agent KH560 was used to modify the surface of nano-α-Al<sub>2</sub>O<sub>3</sub> in ethanol-aqueous solution with different proportions. The particle size of nano-α-Al<sub&...Silane coupling agent KH560 was used to modify the surface of nano-α-Al<sub>2</sub>O<sub>3</sub> in ethanol-aqueous solution with different proportions. The particle size of nano-α-Al<sub>2</sub>O<sub>3</sub> was determined by nano-particle size analyzer, and the effects of nano-α-Al<sub>2</sub>O<sub>3</sub> content, ethanol-aqueous solution ratio and KH560 dosage on the dispersion and particle size of nano-α-Al<sub>2</sub>O<sub>3</sub> were investigated. The material structure before and after modification was determined by Fourier transform infrared spectroscopy (FTIR). Aqueous polyurethane resin and inorganic components are combined with modified nano-α-Al<sub>2</sub>O<sub>3</sub> dispersion to form chromium-free passivation solution. The solution is coated on the galvanized sheet, the adhesion and surface hardness are tested, the bonding strength of the coating and the surface hardness of the substrate are discussed. The corrosion resistance and surface morphology of the matrix were investigated by electrochemical test, neutral salt spray test and scanning electron microscope test. The chromium-free passivation film formed after the modification of nano-α-Al<sub>2</sub>O<sub>3</sub> increases the surface hardness of galvanized sheet by about 85%. The corrosion resistance of the film is better than that of a single polyurethane film. The results show that the surface hardness and corrosion resistance of polyurethane resin composite passivation film are significantly improved by the introduction of nano-α-Al<sub>2</sub>O<sub>3</sub>.展开更多
Mesoporous superacids S2O82–-Fe2O3/SBA-15(SFS)with active nanoparticles are prepared by ultrasonic adsorption method.This method is adopted to ensure a homo-dispersed nanoparticle active phase,large specific surface ...Mesoporous superacids S2O82–-Fe2O3/SBA-15(SFS)with active nanoparticles are prepared by ultrasonic adsorption method.This method is adopted to ensure a homo-dispersed nanoparticle active phase,large specific surface area and many acidic sites.Compared with bulk S2O82–-Fe2O3,Br?nsted acid catalysts and other reported catalysts,SFS with an Fe2O3 loading of 30%(SFS-30)exhibits an outstanding activity in the probe reaction of alcoholysis of styrene oxide by methanol with 100%yield.Moreover,SFS-30 also shows a more excellent catalytic performance than bulk S2O82–-Fe2O3 towards the alcoholysis of other ROHs(R=C2H5-C4H9).Lewis and Bronsted acid sites on the SFS-30 surfaces are confirmed by pyridine adsorbed infrared spectra.The highly efficient catalytic activity of SFS-30 may be attributed to the synergistic effect from the nano-effect of S2O82–-Fe2O3 nanoparticles and the mesostructure of SBA-15.Finally,SFS-30 shows a good catalytic reusability,providing an 84.1%yield after seven catalytic cycles.展开更多
In this study,Ag/γ-Al_(2)O_(3)catalysts were synthesized by an Ar dielectric barrier discharge plasma using silver nitrate as the Ag source andγ-alumina(γ-Al_(2)O_(3))as the support.It is revealed that plasma can r...In this study,Ag/γ-Al_(2)O_(3)catalysts were synthesized by an Ar dielectric barrier discharge plasma using silver nitrate as the Ag source andγ-alumina(γ-Al_(2)O_(3))as the support.It is revealed that plasma can reduce silver ions to generate crystalline silver nanoparticles(Ag NPs)of good dispersion and uniformity on the alumina surface,leading to the formation of Ag/γ-Al_(2)O_(3)catalysts in a green manner without traditional chemical reductants.Ag/γ-Al_(2)O_(3)exhibited good catalytic activity and stability in CO oxidation reactions,and the activity increased with increase in the Ag content.For catalysts with more than 2 wt%Ag,100%CO conversion can be achieved at 300°C.The catalytic activity of the Ag/γ-Al_(2)O_(3)catalysts is also closely related to the size of theγ-alumina,where Ag/nano-γ-Al_(2)O_(3)catalysts demonstrate better performance than Ag/micro-γ-Al_(2)O_(3)catalysts with the same Ag content.In addition,the catalytic properties of plasma-generated Ag/nano-γ-Al_(2)O_(3)(Ag/γ-Al_(2)O_(3)-P)catalysts were compared with those of Ag/nano-γ-Al_(2)O_(3)catalysts prepared by the traditional calcination approach(Ag/γ-Al_(2)O_(3)-C),with the plasma-generated samples demonstrating better overall performance.This simple,rapid and green plasma process is considered to be applicable for the synthesis of diverse noble metal-based catalysts.展开更多
Eu-doped GaOOH nanoparticles with size of 5-8 nm were prepared by hydrothermal method using sodium dodecylbenzene sulfonate (SDBS) as surfactant. Eu-doped α-Ga2O3 and β-Ga2O3 were further fabricated by annealing G...Eu-doped GaOOH nanoparticles with size of 5-8 nm were prepared by hydrothermal method using sodium dodecylbenzene sulfonate (SDBS) as surfactant. Eu-doped α-Ga2O3 and β-Ga2O3 were further fabricated by annealing GaOOH:Eu and then characterized by X-ray diffraction(XRD), transmission electron microscopy (TEM) and photoluminescence (PL). The TEM results show that monodisperse Eu^3+-doped GaOOH nanoparticles form and then transform into Eu^3+-doped a-Ga2O3 and β-Ga2O3 through annealing the GaOOH:Eu nanoparticles at 600 and 900℃, respectively. PL studies indicate that GaOOH:Eu has the highest intensity at 618 nm. Luminescence quenching is observed at higher Eu3+concentration in all samples.展开更多
Highly pure active γ-Al2O3 nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studi...Highly pure active γ-Al2O3 nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studied. The properties of γ-Al2O3 nanoparticles were characterized by DTA, XRD, BET, TEM, laser granularity analysis and impurity content analysis. The results show that the amorphous precursor AI(OH)3 sols are produced by using 0.1 mol/L Al(NO3)3·9H2O and 0.16 mol/L (NH4)2CO3·H2O reaction solutions, according to the volume ratio 1.33, adding 0.024%(volume fraction) surfactant PEG600, and reacting at 40℃, 1000 r/min stirring rate for 15min. Then, after stabilizing for 24 h, the precursors were extracted and filtrated by vacuum, washed thoroughly with deionized water and dehydrated ethanol, dried in vacuum at 80℃ for 8h, final calcined at 800℃ for 1h in the air, and high purity active γ-Al2O3 nanoparticles can be prepared with cubic in crystal system, OH^7-FD3M in space group, about 9 nm in crystal grain size, about 20 nm in particle size and uniform size distribution, 131.35 m^2/g in BET specific surface area, 7 - 11 nm in pore diameter, and not lower than 99.93% in purity.展开更多
Al<sub>2</sub>S<sub>3</sub>/MoS<sub>2</sub> nanocomposite has been synthesized through electrochemical method and characterized by UV-Visible spectroscopy, XRD, SEM and EDAX data. U...Al<sub>2</sub>S<sub>3</sub>/MoS<sub>2</sub> nanocomposite has been synthesized through electrochemical method and characterized by UV-Visible spectroscopy, XRD, SEM and EDAX data. UV-Visible spectroscopy measurements reveal that the Al<sub>2</sub>S<sub>3</sub>/MoS<sub>2</sub> nanocomposite has maximum absorption at 353.04 nm and this peak position reflects the band gap of particles and it is found to be 2.51 eV which was calculated using Tauc plot. X-Ray diffraction (XRD) reveals crystaline size to be 49.85 nm which was calculated using Williamson-Hall (W-H) plot method. Photocatalytic degradation of acetic acid, chloroacetic acid and trichloroacetic acid has been studied by volumetric method using NaOH solution. Photocatalytic degradation of chloroacetic acid and acetic acid follows first order kinetics. The photodegradation efficiency for Al<sub>2</sub>S<sub>3</sub>/MoS<sub>2</sub> nanocomposite was found to be ≈97.8%. A Taft linear free energy relationship is noted for the catalysed reaction with ρ* = 0.233 and indicating electron withdrawing groups enhance the rate. An isokinetic relation is observed with β = 358 K indicating that enthalpy factor controls the reaction rate. The result of this paper suggests the possibility of degradation of organic compounds, industrial effluants and toxic organic compounds by photodegradation process by ecofriendly Al<sub>2</sub>S<sub>3</sub>/ MoS<sub>2</sub>. The antibacterial activity of Al<sub>2</sub>S<sub>3</sub>/MoS<sub>2</sub> nanocomposite was investigated. These particles were shown to have an effective bactericide.展开更多
A method of heating ethanol-aqueous salt solution combined with co-precipitation was used to synthesize Al2O3/ZrO2 nanoparticles. The analysis of DSC and XRD revealed that the transformation temperature from amorphous...A method of heating ethanol-aqueous salt solution combined with co-precipitation was used to synthesize Al2O3/ZrO2 nanoparticles. The analysis of DSC and XRD revealed that the transformation temperature from amorphous to crystal phase was about 850 ℃. The grain size was increased with the raising of calcine temperature. The alcohol-water ratio did not affect the formation of main crystal phases, but affected the agglomeration of nanoparticles based on the results of TEM. When alcohol-water ratio was 5∶1, the dispersion of nanoparticles was good. When there was not alcohol, the dispersion of nanoparticles was poor because there was only pure co-precipitation reaction and the speed of co-precipitation reaction was too high to have enough time of PEG. dispersing particles.展开更多
Attempts had been made to synthesize Al2O3-2SiO2 nanopowders by sol-gel method with tetraethoxysilane(TEOS) and aluminum nitrate(ANN) as the starting materials.DTS,TEM,SEM and BET were employed to study the effect...Attempts had been made to synthesize Al2O3-2SiO2 nanopowders by sol-gel method with tetraethoxysilane(TEOS) and aluminum nitrate(ANN) as the starting materials.DTS,TEM,SEM and BET were employed to study the effects of process parameters on the size,specific surface area and structure(morphology) of powders.The alkali-activation reactivity of the powders was tested for manufacturing geopolymers and their hydrothermal reactions were performed for fabricating zeolites.The results show that the optimum process parameters and drying method for preparing Al2O3-2SiO2 nanopowders are as follows:the molar ratio of water and ethanol to TEOS are 0:1 and 12:1 respectively at synthetic temperature of 50 ℃ and the drying method is azeotropic distillation with microwave drying.The average particle diameters of the powders were about 70 nm and the largest BET specific surface area was up to 669 m^2·g^-1.The compressive strength of the geopolymer and the calcium exchange capacity(by CaCO3) of NaA zeolite prepared with the powders reached to 29 MPa and 366 m^2·g^-1 respectively.展开更多
文摘The influence of cathodic pulse parameters was evaluated on plasma electrolytic oxidation(PEO)coatings grown on 7075 aluminum alloy in a silicate-based electrolyte containing potassium titanyl oxalate(PTO)using pulsed bipolar waveforms with various cathodic duty cycles and cathodic current densities.The coatings were characterized by SEM,EDS,and XRD.EIS was applied to investigate the electrochemical properties.It was observed that the increase of cathodic duty cycle and cathodic current density from 20%and 6 A/dm^(2) to 40%and 12 A/dm^(2) enhances the growth rate of the inner layer from 0.22 to 0.75μm/min.Adding PTO into the bath showed a fortifying effect on influence of the cathodic pulse and the mentioned change of cathodic pulse parameters,resulting in an increase of the inner layer growth rate from 0.25 to 1.10μm/min.Based on EDS analysis,Si and Ti were incorporated dominantly in the upper parts of the coatings.XRD technique merely detectedγ-Al_(2)O_(3),and there were no detectable peaks related to Ti and Si compounds.However,the EIS results confirmed that the incorporation of Ti^(4+)into alumina changed the electronic properties of the coating.The coatings obtained from the bath containing PTO using the bipolar waveforms with a cathodic duty cycle of 40%and current density values higher than 6 A/dm^(2) showed highly appropriate electrochemical behavior during 240 d of immersion due to an efficient repairing mechanism.Regarding the effects of studied parameters on the coating properties,the roles of cathodic pulse parameters and PTO in the PEO process were highlighted.
文摘Silane coupling agent KH560 was used to modify the surface of nano-α-Al<sub>2</sub>O<sub>3</sub> in ethanol-aqueous solution with different proportions. The particle size of nano-α-Al<sub>2</sub>O<sub>3</sub> was determined by nano-particle size analyzer, and the effects of nano-α-Al<sub>2</sub>O<sub>3</sub> content, ethanol-aqueous solution ratio and KH560 dosage on the dispersion and particle size of nano-α-Al<sub>2</sub>O<sub>3</sub> were investigated. The material structure before and after modification was determined by Fourier transform infrared spectroscopy (FTIR). Aqueous polyurethane resin and inorganic components are combined with modified nano-α-Al<sub>2</sub>O<sub>3</sub> dispersion to form chromium-free passivation solution. The solution is coated on the galvanized sheet, the adhesion and surface hardness are tested, the bonding strength of the coating and the surface hardness of the substrate are discussed. The corrosion resistance and surface morphology of the matrix were investigated by electrochemical test, neutral salt spray test and scanning electron microscope test. The chromium-free passivation film formed after the modification of nano-α-Al<sub>2</sub>O<sub>3</sub> increases the surface hardness of galvanized sheet by about 85%. The corrosion resistance of the film is better than that of a single polyurethane film. The results show that the surface hardness and corrosion resistance of polyurethane resin composite passivation film are significantly improved by the introduction of nano-α-Al<sub>2</sub>O<sub>3</sub>.
文摘Mesoporous superacids S2O82–-Fe2O3/SBA-15(SFS)with active nanoparticles are prepared by ultrasonic adsorption method.This method is adopted to ensure a homo-dispersed nanoparticle active phase,large specific surface area and many acidic sites.Compared with bulk S2O82–-Fe2O3,Br?nsted acid catalysts and other reported catalysts,SFS with an Fe2O3 loading of 30%(SFS-30)exhibits an outstanding activity in the probe reaction of alcoholysis of styrene oxide by methanol with 100%yield.Moreover,SFS-30 also shows a more excellent catalytic performance than bulk S2O82–-Fe2O3 towards the alcoholysis of other ROHs(R=C2H5-C4H9).Lewis and Bronsted acid sites on the SFS-30 surfaces are confirmed by pyridine adsorbed infrared spectra.The highly efficient catalytic activity of SFS-30 may be attributed to the synergistic effect from the nano-effect of S2O82–-Fe2O3 nanoparticles and the mesostructure of SBA-15.Finally,SFS-30 shows a good catalytic reusability,providing an 84.1%yield after seven catalytic cycles.
基金financial support from National Natural Science Foundation of China(Nos.52004102 and 22078125)Postdoctoral Science Foundation of China(No.2021M690068)+2 种基金Fundamental Research Funds for the Central Universities(Nos.JUSRP221018 and JUSRP622038)Key Laboratory of Green Cleaning Technology and Detergent of Zhejiang Province(No.Q202204)Open Project of Key Laboratory of Green Chemical Engineering Process of Ministry of Education(No.GCP202112)。
文摘In this study,Ag/γ-Al_(2)O_(3)catalysts were synthesized by an Ar dielectric barrier discharge plasma using silver nitrate as the Ag source andγ-alumina(γ-Al_(2)O_(3))as the support.It is revealed that plasma can reduce silver ions to generate crystalline silver nanoparticles(Ag NPs)of good dispersion and uniformity on the alumina surface,leading to the formation of Ag/γ-Al_(2)O_(3)catalysts in a green manner without traditional chemical reductants.Ag/γ-Al_(2)O_(3)exhibited good catalytic activity and stability in CO oxidation reactions,and the activity increased with increase in the Ag content.For catalysts with more than 2 wt%Ag,100%CO conversion can be achieved at 300°C.The catalytic activity of the Ag/γ-Al_(2)O_(3)catalysts is also closely related to the size of theγ-alumina,where Ag/nano-γ-Al_(2)O_(3)catalysts demonstrate better performance than Ag/micro-γ-Al_(2)O_(3)catalysts with the same Ag content.In addition,the catalytic properties of plasma-generated Ag/nano-γ-Al_(2)O_(3)(Ag/γ-Al_(2)O_(3)-P)catalysts were compared with those of Ag/nano-γ-Al_(2)O_(3)catalysts prepared by the traditional calcination approach(Ag/γ-Al_(2)O_(3)-C),with the plasma-generated samples demonstrating better overall performance.This simple,rapid and green plasma process is considered to be applicable for the synthesis of diverse noble metal-based catalysts.
基金Project(50772133) supported by the National Natural Science Foundation of ChinaProject(LA 09014) supported by Innovation Projects for Graduates of Center South University,China
文摘Eu-doped GaOOH nanoparticles with size of 5-8 nm were prepared by hydrothermal method using sodium dodecylbenzene sulfonate (SDBS) as surfactant. Eu-doped α-Ga2O3 and β-Ga2O3 were further fabricated by annealing GaOOH:Eu and then characterized by X-ray diffraction(XRD), transmission electron microscopy (TEM) and photoluminescence (PL). The TEM results show that monodisperse Eu^3+-doped GaOOH nanoparticles form and then transform into Eu^3+-doped a-Ga2O3 and β-Ga2O3 through annealing the GaOOH:Eu nanoparticles at 600 and 900℃, respectively. PL studies indicate that GaOOH:Eu has the highest intensity at 618 nm. Luminescence quenching is observed at higher Eu3+concentration in all samples.
文摘Highly pure active γ-Al2O3 nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studied. The properties of γ-Al2O3 nanoparticles were characterized by DTA, XRD, BET, TEM, laser granularity analysis and impurity content analysis. The results show that the amorphous precursor AI(OH)3 sols are produced by using 0.1 mol/L Al(NO3)3·9H2O and 0.16 mol/L (NH4)2CO3·H2O reaction solutions, according to the volume ratio 1.33, adding 0.024%(volume fraction) surfactant PEG600, and reacting at 40℃, 1000 r/min stirring rate for 15min. Then, after stabilizing for 24 h, the precursors were extracted and filtrated by vacuum, washed thoroughly with deionized water and dehydrated ethanol, dried in vacuum at 80℃ for 8h, final calcined at 800℃ for 1h in the air, and high purity active γ-Al2O3 nanoparticles can be prepared with cubic in crystal system, OH^7-FD3M in space group, about 9 nm in crystal grain size, about 20 nm in particle size and uniform size distribution, 131.35 m^2/g in BET specific surface area, 7 - 11 nm in pore diameter, and not lower than 99.93% in purity.
文摘Al<sub>2</sub>S<sub>3</sub>/MoS<sub>2</sub> nanocomposite has been synthesized through electrochemical method and characterized by UV-Visible spectroscopy, XRD, SEM and EDAX data. UV-Visible spectroscopy measurements reveal that the Al<sub>2</sub>S<sub>3</sub>/MoS<sub>2</sub> nanocomposite has maximum absorption at 353.04 nm and this peak position reflects the band gap of particles and it is found to be 2.51 eV which was calculated using Tauc plot. X-Ray diffraction (XRD) reveals crystaline size to be 49.85 nm which was calculated using Williamson-Hall (W-H) plot method. Photocatalytic degradation of acetic acid, chloroacetic acid and trichloroacetic acid has been studied by volumetric method using NaOH solution. Photocatalytic degradation of chloroacetic acid and acetic acid follows first order kinetics. The photodegradation efficiency for Al<sub>2</sub>S<sub>3</sub>/MoS<sub>2</sub> nanocomposite was found to be ≈97.8%. A Taft linear free energy relationship is noted for the catalysed reaction with ρ* = 0.233 and indicating electron withdrawing groups enhance the rate. An isokinetic relation is observed with β = 358 K indicating that enthalpy factor controls the reaction rate. The result of this paper suggests the possibility of degradation of organic compounds, industrial effluants and toxic organic compounds by photodegradation process by ecofriendly Al<sub>2</sub>S<sub>3</sub>/ MoS<sub>2</sub>. The antibacterial activity of Al<sub>2</sub>S<sub>3</sub>/MoS<sub>2</sub> nanocomposite was investigated. These particles were shown to have an effective bactericide.
基金The authors acknowledges the financial support of Tianjin University Youth FoundationTangshan Ceramics Limited
文摘A method of heating ethanol-aqueous salt solution combined with co-precipitation was used to synthesize Al2O3/ZrO2 nanoparticles. The analysis of DSC and XRD revealed that the transformation temperature from amorphous to crystal phase was about 850 ℃. The grain size was increased with the raising of calcine temperature. The alcohol-water ratio did not affect the formation of main crystal phases, but affected the agglomeration of nanoparticles based on the results of TEM. When alcohol-water ratio was 5∶1, the dispersion of nanoparticles was good. When there was not alcohol, the dispersion of nanoparticles was poor because there was only pure co-precipitation reaction and the speed of co-precipitation reaction was too high to have enough time of PEG. dispersing particles.
基金Supported by the National Natural Science Foundation of China (50962002,50602006)Opening Funds of State Key Laboratory of Chemical Resource Engineering of Beijing University of Chemical Technology (201008)
文摘Attempts had been made to synthesize Al2O3-2SiO2 nanopowders by sol-gel method with tetraethoxysilane(TEOS) and aluminum nitrate(ANN) as the starting materials.DTS,TEM,SEM and BET were employed to study the effects of process parameters on the size,specific surface area and structure(morphology) of powders.The alkali-activation reactivity of the powders was tested for manufacturing geopolymers and their hydrothermal reactions were performed for fabricating zeolites.The results show that the optimum process parameters and drying method for preparing Al2O3-2SiO2 nanopowders are as follows:the molar ratio of water and ethanol to TEOS are 0:1 and 12:1 respectively at synthetic temperature of 50 ℃ and the drying method is azeotropic distillation with microwave drying.The average particle diameters of the powders were about 70 nm and the largest BET specific surface area was up to 669 m^2·g^-1.The compressive strength of the geopolymer and the calcium exchange capacity(by CaCO3) of NaA zeolite prepared with the powders reached to 29 MPa and 366 m^2·g^-1 respectively.