In order to achieve effective, economic, and easily achievable photocatalyst for the degradation of dye methyl orange(MeO), ZnO, ZnO/ZnS and ZnO/ZnS/α-Fe2O3 nanocomposites were prepared by simple chemical synthetic...In order to achieve effective, economic, and easily achievable photocatalyst for the degradation of dye methyl orange(MeO), ZnO, ZnO/ZnS and ZnO/ZnS/α-Fe2O3 nanocomposites were prepared by simple chemical synthetic route in the aqueous medium. Phase, crystallinity, surface structure and surface behavior of the synthesized materials were determined by X-ray diffraction(XRD) and Brunauer-Emmett-Teller analysis(BET) techniques. XRD study established formation of good crystalline ZnO, ZnO/ZnS and ZnO/ZnS/α-Fe2O3 nanomaterials. By using intensity of constituent peaks in the XRD pattern, the compositions of nanocomposites were determined. From the BET analysis, the prepared materials show mesoporous behavior, type Ⅳ curves along with H4 hysteresis. The ZnO/ZnS/α-Fe2O3 composite shows the largest surface area among three materials. From the UV-visible spectra, the band gap energy of the materials was determined. Photoluminescence spectra(PL) were used to determine the emission behavior and surface defects in the materials. In PL spectra, the intensity of UV peak of ZnO/ZnS is lowered than that of ZnO while in case of ZnO/ZnS/α-Fe2O3, the intensity further decreased. The visible emission spectra of ZnO/ZnS increased compared with ZnO while in ZnO/ZnS/α-Fe2O3 it is further increased compared with ZnO/ZnS. The as-synthesized materials were used as photocatalysts for the degradation of dye MeO. The photo-degradation data revealed that the ZnO/ZnS/α-Fe2O3 is the best photocatalyst among three specimens for the degradation of dye MeO. The decrease of intensity of UV emission peak and the increase of intensity of visible emission cause the decrease of recombination of electrons and holes which are ultimately responsible for the highest photocatalytic activity of ZnO/ZnS/α-Fe2O3.展开更多
目的:检测γ-Fe2O3纳米粒表面油酸的残留量,考察油酸残留量对纳米粒磁共振T1造影效果的影响。方法:采用热分解法制备γ-Fe2O3纳米粒,使用mPEG-P取代γ-Fe2O3纳米粒表面的油酸,得到水溶性的γ-Fe2O3-PEG纳米粒,采用高效液相色谱法测定纳...目的:检测γ-Fe2O3纳米粒表面油酸的残留量,考察油酸残留量对纳米粒磁共振T1造影效果的影响。方法:采用热分解法制备γ-Fe2O3纳米粒,使用mPEG-P取代γ-Fe2O3纳米粒表面的油酸,得到水溶性的γ-Fe2O3-PEG纳米粒,采用高效液相色谱法测定纳米粒表面残留的油酸,并在7T磁共振成像仪下考察油酸残留量与纳米粒T1造影效果的关联。最后,对体外造影效果最优的样品进行了体内磁共振成像测试。结果:建立了油酸的高效液相色谱检测方法,油酸在10~400 μg/mL浓度范围内具有良好的线性关系(r2 = 1),平均回收率为99.86%。通过改变γ-Fe2O3与mPEG-P的投料比,得到γ-Fe2O3-PEG纳米粒表面油酸残留个数分别为100、83、56、33的样品。体外磁共振成像结果表明,油酸残留量较少的纳米粒拥有更好的T1加权成像性能。小鼠体内血管造影显示,本研究制备的γ-Fe2O3-PEG纳米粒与临床使用的钆类造影剂相比,拥有更好的血管成像效果。结论:本研究成果为热分解法制备的氧化铁纳米粒表面油酸的定量分析提供了一种有效的检测方法,以促进该类纳米粒在生物医学领域的应用。Objective: Detection of residual oleic acid on the surface of γ-Fe2O3 nanoparticles and investigation of its impact on magnetic resonance T1 imaging. Method: We prepared γ-Fe2O3 nanoparticles via thermal decomposition, with mPEG-P replacing the oleic acid on the surface of the nanoparticles to yield water-soluble γ-Fe2O3-PEG nanoparticles. The residual oleic acid on the surface of the nanoparticles was quantified using High-Performance Liquid Chromatography, and the relationship between the amount of residual oleic acid and the T1 contrast effect of the nanoparticles was investigated using a 7T magnetic resonance imaging system. Finally, the vivo magnetic resonance imaging of the sample exhibiting the optimal in vitro contrast effect was conducted. Results: We developed a High-Performance Liquid Chromatography method for the detection of oleic acid, demonstrating a strong linear correlation in the concentration range of 10~400 μg/mL (r² = 1) with an average recovery rate of 99.86%. By varying the ratio of γ-Fe2O3 to mPEG-P, samples with oleic acid on the surface of γ-Fe2O3-PEG nanoparticles were obtained, with respective counts of 100, 83, 56, and 33. In vitro magnetic resonance imaging demonstrated that nanoparticles with lower residual oleic acid exhibited enhanced T1-weighted imaging performance. In vivo vascular imaging in mice demonstrated that the γ-Fe2O3-PEG nanoparticles prepared in this study provided better imaging results compared to commercially available gadolinium-based contrast agents. Conclusions: This study presents an effective detection method for the quantitative analysis of oleic acid on the surface of iron oxide nanoparticles synthesized via a thermolytic approach, thereby facilitating the application of such nanoparticles in the biomedical field.展开更多
The ferrites of Cuo-ZnO-Fe2o3 solid solution series near the molar ratio of ZnxCu1-x were prepared by direct heating of their coprecipitated hydroxides using NH4OH as precipitating agent where x=0.0, 0.2, 0.5, 0.8 and...The ferrites of Cuo-ZnO-Fe2o3 solid solution series near the molar ratio of ZnxCu1-x were prepared by direct heating of their coprecipitated hydroxides using NH4OH as precipitating agent where x=0.0, 0.2, 0.5, 0.8 and 1.0. Additional amounts of Cu and Zn sulphates were added to compensate the loss during the coprecipitation of the hydroxides. The ferritized samples were characterized by chemical analysis, XRD. DTA, TGA and SEM. XRD of both Zn0.2Cu0.8Fe2O4 and Zn0.5Cu0.5 Fe2O4 that indicates the formation of a heterogeneous ferrite material of ZnFe2O4 and CuFe2O4 mixed with variable amounts of α-Fe2O3. Zn and Cu ferrites were observed only in Zn0.8Cu0.2Fe2O4.From TGA-time relation, the activation energy of the different transformation phases were calculated. It is found that, the activation energy of ZnFe2O4 is slightly equal to 3/2 of that for CuFe2O4. Dielectric measurements show that the electrical behaviour depends on the ordering and disordering of the phases.展开更多
Two-step steam reforming of methane (SRM) is a novel chemical looping process towards the production of pure hydrogen and syngas (synthesis gas), consisting of a syngas production step and a water-splitting step. Rene...Two-step steam reforming of methane (SRM) is a novel chemical looping process towards the production of pure hydrogen and syngas (synthesis gas), consisting of a syngas production step and a water-splitting step. Renewable energy can be used to drive this process for hydrogen production, especially solar energy. CeO2-Fe2O3 complex oxide oxygen carrier was prepared by the impregnation method and characterized by means of X-ray diffractometer (XRD), Raman spectroscopy (Raman) and hydrogen programmed reduction (H2-TPR). CH4 temperature programmed and isothermal reactions were adopted to test syngas production reactivity, and water splitting reaction was employed to investigate water-splitting activity. Moreover, two-step SRM performance was evaluated by a successive redox cycle. The results showed that CO-uncontaminated H2 and highly selective syngas (with H2/CO ratio close to 2) could be respectively obtained from two steps, and CeFeO3 formation was found in the first redox cycle and proved to be enhanced by the redox treatment. After 10 successive cycles, obvious CeFeO3 phase was detected, which may be responsible for favorable successive redox cycle performances.展开更多
Although the traditional Fenton reaction is considered an effective strategy for solving problems caused by environmental pollution,construction of an efficient photocatalytic system by coordinating the Fenton reactio...Although the traditional Fenton reaction is considered an effective strategy for solving problems caused by environmental pollution,construction of an efficient photocatalytic system by coordinating the Fenton reaction is challenging.In this study,2D/2D step-schemeα-Fe2O3/Bi2WO6(FO/BWO)heterostructure photo-Fenton catalysts were successfully fabricated by a facile hydrothermal method.The as-prepared materials were characterized by XRD,FT-IR,TEM,XPS,UV-vis DRS,PL,I-t,EIS,and BET analyses.Under visible light irradiation,FO/BWO exhibited remarkably high and stable photo-Fenton catalytic activity for the degradation of methyl blue(MB)at low concentrations of H2O2.It was noted that FO/BWO(0.5)displayed a significantly enhanced photo-Fenton catalytic activity,which was 11.06 and 3.29 times those of FO nanosheets and BWO nanosheets,respectively.The notably improved photo-Fenton catalytic activity of FO/BWO was mainly due to the combination of H2O2 and FO under light illumination and the presence of the 2D/2D S-scheme heterostructure,with the large contact surface,abundant active sites,and efficient separation rate of photogenerated carriers playing contributory roles.Additionally,a possible catalytic mechanism for the FO/BWO composite was preliminarily proposed via active species trapping experiments.In summary,this study provided new insights into the synthesis of an effectively heterogeneous 2D/2D S-scheme photo-Fenton catalyst for degradation of organic pollutants in wastewater.展开更多
A facile hydrothermal method was developed for the preparation of Fe_2O_3@C nanocomposites using FeCl_3·6H_2O as iron source and glucose as carbon source under alkaline condition. The morphology and structure of ...A facile hydrothermal method was developed for the preparation of Fe_2O_3@C nanocomposites using FeCl_3·6H_2O as iron source and glucose as carbon source under alkaline condition. The morphology and structure of the as-prepared product were identified by transmission electron microscopy(TEM), high resolution transmission electron microscopy(HRTEM), field-emission scanning electron microscopy(FESEM),X-ray diffraction(XRD), Raman spectroscopy, Fourier Transform infrared spectroscopy(FTIR), and thermogravimetric analysis(TGA). The as-prepare α-Fe_2O_3@C nanocomposites were employed for supercapacitor electrode material. The synergistic combination of carbon electrical double-layer capacitance and α-Fe_2O_3 pseudo-capacitance established such nanocomposites as versatile platform for high performance supercapacitors. The synthesis method developed here is expected to obtain other metal oxide/carbon composite.展开更多
A novel coprecipitation-reduction process has been proposed for preparing highly selective Cu/ZnO/Al 2O 3 catalysts for methanol synthesis from CO 2 hydrogenation. Compared to the catalysts prepared by the conventiona...A novel coprecipitation-reduction process has been proposed for preparing highly selective Cu/ZnO/Al 2O 3 catalysts for methanol synthesis from CO 2 hydrogenation. Compared to the catalysts prepared by the conventional method, the new catalysts prepared via the new method exhibit much higher BET surface area and pore size, much smaller crystallite size and higher catalytic activity and selectivity in CO 2 hydrogenation to methanol. It is also found that the molar ratio of Cu + to Cu 0 on the surface of the catalyst obtained by coprecipitation-reduction is much higher than that on the reduced catalyst obtained by the conventional method, which could be crucial for its high activity and selectivity for catalytic hydrogenation of CO 2 to methanol.展开更多
Nanocomposites of PAn-DBSA/γ-Fe 2O 3 with electrical and ferromagnetic behavior(σ= 2.18×10 -3-5.00×10 -5 S/cm, M s=3.7-16.6 m 2·A/kg, H c=8 805.2-9 133.1 A/m) were prepared by a chemical modification-...Nanocomposites of PAn-DBSA/γ-Fe 2O 3 with electrical and ferromagnetic behavior(σ= 2.18×10 -3-5.00×10 -5 S/cm, M s=3.7-16.6 m 2·A/kg, H c=8 805.2-9 133.1 A/m) were prepared by a chemical modification-redoping method in a neutral medium. The products were characterized by TEM, XRD, UV-Vis, four-probe method, and magnetometer. The results indicate that the electrical and magnetic properties of the nanocomposites strongly depend on γ-Fe 2O 3 content. With the increase of γ-Fe 2O 3 content, the electrical conductivity is decreased and saturation magnetization is increased.展开更多
摘要In order to achieve effective, economic, and easily achievable photocatalyst for the degradation of dye methyl orange(MeO), ZnO, ZnO/ZnS and ZnO/ZnS/α-Fe2O3 nanocomposites were prepared by simple chemical synthetic route in the aqueous medium. Phase, crystallinity, surface structure and surface behavior of the synthesized materials were determined by X-ray diffraction(XRD) and Brunauer-Emmett-Teller analysis(BET) techniques. XRD study established formation of good crystalline ZnO, ZnO/ZnS and ZnO/ZnS/α-Fe2O3 nanomaterials. By using intensity of constituent peaks in the XRD pattern, the compositions of nanocomposites were determined. From the BET analysis, the prepared materials show mesoporous behavior, type Ⅳ curves along with H4 hysteresis. The ZnO/ZnS/α-Fe2O3 composite shows the largest surface area among three materials. From the UV-visible spectra, the band gap energy of the materials was determined. Photoluminescence spectra(PL) were used to determine the emission behavior and surface defects in the materials. In PL spectra, the intensity of UV peak of ZnO/ZnS is lowered than that of ZnO while in case of ZnO/ZnS/α-Fe2O3, the intensity further decreased. The visible emission spectra of ZnO/ZnS increased compared with ZnO while in ZnO/ZnS/α-Fe2O3 it is further increased compared with ZnO/ZnS. The as-synthesized materials were used as photocatalysts for the degradation of dye MeO. The photo-degradation data revealed that the ZnO/ZnS/α-Fe2O3 is the best photocatalyst among three specimens for the degradation of dye MeO. The decrease of intensity of UV emission peak and the increase of intensity of visible emission cause the decrease of recombination of electrons and holes which are ultimately responsible for the highest photocatalytic activity of ZnO/ZnS/α-Fe2O3.
摘要目的:检测γ-Fe2O3纳米粒表面油酸的残留量,考察油酸残留量对纳米粒磁共振T1造影效果的影响。方法:采用热分解法制备γ-Fe2O3纳米粒,使用mPEG-P取代γ-Fe2O3纳米粒表面的油酸,得到水溶性的γ-Fe2O3-PEG纳米粒,采用高效液相色谱法测定纳米粒表面残留的油酸,并在7T磁共振成像仪下考察油酸残留量与纳米粒T1造影效果的关联。最后,对体外造影效果最优的样品进行了体内磁共振成像测试。结果:建立了油酸的高效液相色谱检测方法,油酸在10~400 μg/mL浓度范围内具有良好的线性关系(r2 = 1),平均回收率为99.86%。通过改变γ-Fe2O3与mPEG-P的投料比,得到γ-Fe2O3-PEG纳米粒表面油酸残留个数分别为100、83、56、33的样品。体外磁共振成像结果表明,油酸残留量较少的纳米粒拥有更好的T1加权成像性能。小鼠体内血管造影显示,本研究制备的γ-Fe2O3-PEG纳米粒与临床使用的钆类造影剂相比,拥有更好的血管成像效果。结论:本研究成果为热分解法制备的氧化铁纳米粒表面油酸的定量分析提供了一种有效的检测方法,以促进该类纳米粒在生物医学领域的应用。Objective: Detection of residual oleic acid on the surface of γ-Fe2O3 nanoparticles and investigation of its impact on magnetic resonance T1 imaging. Method: We prepared γ-Fe2O3 nanoparticles via thermal decomposition, with mPEG-P replacing the oleic acid on the surface of the nanoparticles to yield water-soluble γ-Fe2O3-PEG nanoparticles. The residual oleic acid on the surface of the nanoparticles was quantified using High-Performance Liquid Chromatography, and the relationship between the amount of residual oleic acid and the T1 contrast effect of the nanoparticles was investigated using a 7T magnetic resonance imaging system. Finally, the vivo magnetic resonance imaging of the sample exhibiting the optimal in vitro contrast effect was conducted. Results: We developed a High-Performance Liquid Chromatography method for the detection of oleic acid, demonstrating a strong linear correlation in the concentration range of 10~400 μg/mL (r² = 1) with an average recovery rate of 99.86%. By varying the ratio of γ-Fe2O3 to mPEG-P, samples with oleic acid on the surface of γ-Fe2O3-PEG nanoparticles were obtained, with respective counts of 100, 83, 56, and 33. In vitro magnetic resonance imaging demonstrated that nanoparticles with lower residual oleic acid exhibited enhanced T1-weighted imaging performance. In vivo vascular imaging in mice demonstrated that the γ-Fe2O3-PEG nanoparticles prepared in this study provided better imaging results compared to commercially available gadolinium-based contrast agents. Conclusions: This study presents an effective detection method for the quantitative analysis of oleic acid on the surface of iron oxide nanoparticles synthesized via a thermolytic approach, thereby facilitating the application of such nanoparticles in the biomedical field.
摘要The ferrites of Cuo-ZnO-Fe2o3 solid solution series near the molar ratio of ZnxCu1-x were prepared by direct heating of their coprecipitated hydroxides using NH4OH as precipitating agent where x=0.0, 0.2, 0.5, 0.8 and 1.0. Additional amounts of Cu and Zn sulphates were added to compensate the loss during the coprecipitation of the hydroxides. The ferritized samples were characterized by chemical analysis, XRD. DTA, TGA and SEM. XRD of both Zn0.2Cu0.8Fe2O4 and Zn0.5Cu0.5 Fe2O4 that indicates the formation of a heterogeneous ferrite material of ZnFe2O4 and CuFe2O4 mixed with variable amounts of α-Fe2O3. Zn and Cu ferrites were observed only in Zn0.8Cu0.2Fe2O4.From TGA-time relation, the activation energy of the different transformation phases were calculated. It is found that, the activation energy of ZnFe2O4 is slightly equal to 3/2 of that for CuFe2O4. Dielectric measurements show that the electrical behaviour depends on the ordering and disordering of the phases.
基金Project support by the National Natural Science Foundation of China (50574046, 50774038)the Natural Science Foundation of Yunnan Prov-ince (2008E030M)+1 种基金the Research Fund for the Doctoral Program of Higher Education of China (20095314120005)2010 Innovation Fund of Kunming University of Science and Technology
摘要Two-step steam reforming of methane (SRM) is a novel chemical looping process towards the production of pure hydrogen and syngas (synthesis gas), consisting of a syngas production step and a water-splitting step. Renewable energy can be used to drive this process for hydrogen production, especially solar energy. CeO2-Fe2O3 complex oxide oxygen carrier was prepared by the impregnation method and characterized by means of X-ray diffractometer (XRD), Raman spectroscopy (Raman) and hydrogen programmed reduction (H2-TPR). CH4 temperature programmed and isothermal reactions were adopted to test syngas production reactivity, and water splitting reaction was employed to investigate water-splitting activity. Moreover, two-step SRM performance was evaluated by a successive redox cycle. The results showed that CO-uncontaminated H2 and highly selective syngas (with H2/CO ratio close to 2) could be respectively obtained from two steps, and CeFeO3 formation was found in the first redox cycle and proved to be enhanced by the redox treatment. After 10 successive cycles, obvious CeFeO3 phase was detected, which may be responsible for favorable successive redox cycle performances.
摘要Although the traditional Fenton reaction is considered an effective strategy for solving problems caused by environmental pollution,construction of an efficient photocatalytic system by coordinating the Fenton reaction is challenging.In this study,2D/2D step-schemeα-Fe2O3/Bi2WO6(FO/BWO)heterostructure photo-Fenton catalysts were successfully fabricated by a facile hydrothermal method.The as-prepared materials were characterized by XRD,FT-IR,TEM,XPS,UV-vis DRS,PL,I-t,EIS,and BET analyses.Under visible light irradiation,FO/BWO exhibited remarkably high and stable photo-Fenton catalytic activity for the degradation of methyl blue(MB)at low concentrations of H2O2.It was noted that FO/BWO(0.5)displayed a significantly enhanced photo-Fenton catalytic activity,which was 11.06 and 3.29 times those of FO nanosheets and BWO nanosheets,respectively.The notably improved photo-Fenton catalytic activity of FO/BWO was mainly due to the combination of H2O2 and FO under light illumination and the presence of the 2D/2D S-scheme heterostructure,with the large contact surface,abundant active sites,and efficient separation rate of photogenerated carriers playing contributory roles.Additionally,a possible catalytic mechanism for the FO/BWO composite was preliminarily proposed via active species trapping experiments.In summary,this study provided new insights into the synthesis of an effectively heterogeneous 2D/2D S-scheme photo-Fenton catalyst for degradation of organic pollutants in wastewater.
基金the National Natural Science Foundation of China (nos. 21403091 and 51473070)the Natural Science Foundation of Jiangsu Province (no. BK20140557)+1 种基金a project funded by Jiangsu University for Senior Intellectuals (grant no. 12JDG093)the Jiangsu Province for support under the innovation/entrepreneurship program (Suzutong [2012]19)
摘要A facile hydrothermal method was developed for the preparation of Fe_2O_3@C nanocomposites using FeCl_3·6H_2O as iron source and glucose as carbon source under alkaline condition. The morphology and structure of the as-prepared product were identified by transmission electron microscopy(TEM), high resolution transmission electron microscopy(HRTEM), field-emission scanning electron microscopy(FESEM),X-ray diffraction(XRD), Raman spectroscopy, Fourier Transform infrared spectroscopy(FTIR), and thermogravimetric analysis(TGA). The as-prepare α-Fe_2O_3@C nanocomposites were employed for supercapacitor electrode material. The synergistic combination of carbon electrical double-layer capacitance and α-Fe_2O_3 pseudo-capacitance established such nanocomposites as versatile platform for high performance supercapacitors. The synthesis method developed here is expected to obtain other metal oxide/carbon composite.
摘要A novel coprecipitation-reduction process has been proposed for preparing highly selective Cu/ZnO/Al 2O 3 catalysts for methanol synthesis from CO 2 hydrogenation. Compared to the catalysts prepared by the conventional method, the new catalysts prepared via the new method exhibit much higher BET surface area and pore size, much smaller crystallite size and higher catalytic activity and selectivity in CO 2 hydrogenation to methanol. It is also found that the molar ratio of Cu + to Cu 0 on the surface of the catalyst obtained by coprecipitation-reduction is much higher than that on the reduced catalyst obtained by the conventional method, which could be crucial for its high activity and selectivity for catalytic hydrogenation of CO 2 to methanol.
摘要Nanocomposites of PAn-DBSA/γ-Fe 2O 3 with electrical and ferromagnetic behavior(σ= 2.18×10 -3-5.00×10 -5 S/cm, M s=3.7-16.6 m 2·A/kg, H c=8 805.2-9 133.1 A/m) were prepared by a chemical modification-redoping method in a neutral medium. The products were characterized by TEM, XRD, UV-Vis, four-probe method, and magnetometer. The results indicate that the electrical and magnetic properties of the nanocomposites strongly depend on γ-Fe 2O 3 content. With the increase of γ-Fe 2O 3 content, the electrical conductivity is decreased and saturation magnetization is increased.