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2015 Volume 31 Issue 1
2015, (1): 1-6
doi: 10.11862/CJIC.2015.027
Abstract:
The water soluble and nitrogen doped carbon quantum dots (N-CDs) with excellent fluorescence performance were fabricated by one step hydrothermal method. The size of N-CDs is homogeneous and about 7 nm. The fluorescent intensity of N-CDs changed with the content of N, reaction temperature and pHvalue. In the optimal condition, the fluorescence quantum yield of N-CDs reached 24.4%. The N-CDs was found to be a simple,lowcost, high selective and sensitive fluorescent probe for the detection of Hg2+ ions with a detection limit as low as 0.02 μmol·L-1 (4.012 ng).
The water soluble and nitrogen doped carbon quantum dots (N-CDs) with excellent fluorescence performance were fabricated by one step hydrothermal method. The size of N-CDs is homogeneous and about 7 nm. The fluorescent intensity of N-CDs changed with the content of N, reaction temperature and pHvalue. In the optimal condition, the fluorescence quantum yield of N-CDs reached 24.4%. The N-CDs was found to be a simple,lowcost, high selective and sensitive fluorescent probe for the detection of Hg2+ ions with a detection limit as low as 0.02 μmol·L-1 (4.012 ng).
2015, (1): 7-14
doi: 10.11862/CJIC.2015.035
Abstract:
Kaolinite-stearic acid intercalation compound was synthesized via intercalation and displacement using kaolinite from Zhangjiakou as raw material. The new intercalation compounds were characterized by X-ray diffraction(XRD), Fourier transform infrared spectracopy(FTIR),Thermal Gravity Analysis(TG/DTG) and Transmission Electron Microscope(TEM). Experimental results show that the basal spacing of kaolinite-stearic acid intercalation compound is 4.05~4.37 nm and the intercalationrate of the product reaches to 86.9%. The intercalation time and the pHvalue of the solution have influence on the basal spacing and intercalationrate.The methoxy groups which were grafted with iner surface OH groups and the stearic acid molecules are inside the interlayers of the kaolinite.The TG/DTG Analyses were to conform that the activity of kaolinite hydroxyl increased after methanol modified. Some sheets of the kaolinite-stearic acid compound have rolled up from the edge and formed nanoscrolls which is similar with halloysite. The possible intercalation mechanism is analyzed. A model was provided by structural computation in theory. The results show that the reason about the changed spacings of the compounds in different conditions is explained by the model.
Kaolinite-stearic acid intercalation compound was synthesized via intercalation and displacement using kaolinite from Zhangjiakou as raw material. The new intercalation compounds were characterized by X-ray diffraction(XRD), Fourier transform infrared spectracopy(FTIR),Thermal Gravity Analysis(TG/DTG) and Transmission Electron Microscope(TEM). Experimental results show that the basal spacing of kaolinite-stearic acid intercalation compound is 4.05~4.37 nm and the intercalationrate of the product reaches to 86.9%. The intercalation time and the pHvalue of the solution have influence on the basal spacing and intercalationrate.The methoxy groups which were grafted with iner surface OH groups and the stearic acid molecules are inside the interlayers of the kaolinite.The TG/DTG Analyses were to conform that the activity of kaolinite hydroxyl increased after methanol modified. Some sheets of the kaolinite-stearic acid compound have rolled up from the edge and formed nanoscrolls which is similar with halloysite. The possible intercalation mechanism is analyzed. A model was provided by structural computation in theory. The results show that the reason about the changed spacings of the compounds in different conditions is explained by the model.
2015, (1): 15-22
doi: 10.11862/CJIC.2015.001
Abstract:
The related properties of intrinsic, Ga-, F-doped and Ga-Fcodoped ZnO are calculated after making geometry optimization using first principles plane-wave ultrasoft pseudopotential method based on the density functional theory. The results show that every doped ZnO has its own advantages and disadvantages, so there is different doping scheme according to specific requirement. The lattice distortion in Ga doped ZnO is smaller than Fdoped ZnO. And Ga doped ZnO has more stable structure than Fdoped ZnO, since Ga atoms are more likely to enter the ZnO lattice than Fatoms under the same environment. Doping Ga and Fimproves the conductivity of ZnO. Compared with intrinsic ZnO, the carrier concentration of doped ZnO is increased by three orders of magnitude. And doping Ga can produce more carriers than doping Fin the same concentration. Ga-Fcodoped ZnO reaches a compromise between merits and demerits of these properties above in Ga-doped and F-doped ZnO. In addition, the optical absorptions of doped ZnO generate a blue shift. The optical transmittance of Ga-Fcodoped ZnO is the biggest in ultraviolet region, and it is higher than 90% in 280~380 nm range.
The related properties of intrinsic, Ga-, F-doped and Ga-Fcodoped ZnO are calculated after making geometry optimization using first principles plane-wave ultrasoft pseudopotential method based on the density functional theory. The results show that every doped ZnO has its own advantages and disadvantages, so there is different doping scheme according to specific requirement. The lattice distortion in Ga doped ZnO is smaller than Fdoped ZnO. And Ga doped ZnO has more stable structure than Fdoped ZnO, since Ga atoms are more likely to enter the ZnO lattice than Fatoms under the same environment. Doping Ga and Fimproves the conductivity of ZnO. Compared with intrinsic ZnO, the carrier concentration of doped ZnO is increased by three orders of magnitude. And doping Ga can produce more carriers than doping Fin the same concentration. Ga-Fcodoped ZnO reaches a compromise between merits and demerits of these properties above in Ga-doped and F-doped ZnO. In addition, the optical absorptions of doped ZnO generate a blue shift. The optical transmittance of Ga-Fcodoped ZnO is the biggest in ultraviolet region, and it is higher than 90% in 280~380 nm range.
2015, (1): 23-28
doi: 10.11862/CJIC.2015.024
Abstract:
The Pd-Fe/C catalyst was prepared by the complexing reduction method using NH4Cl as the complex agent at the low temperature. The high alloy Pd-Fe/C catalyst Pd and Fe could be prepared at low temperature due to the complex formation by NH4Cl and Pd, which leads to a negative shift for the reduction potential of PdCl2, making the reduction potential of PdCl2 closer to that of FeCl3. The XPS results show that the alloying of Pd with Fe could affect the binding energies of Pd and increase the content of Pd0 in the catalyst. Thus, the electrocatalytic activity of the Pd-Fe/C catalyst obtained for the oxygen reduction is higher than that of the Pd/C catalyst prepared with the same method. Furthermore, this Pd-Fe/C catalyst has no electrocatalytic activity for the methanol oxidation.
The Pd-Fe/C catalyst was prepared by the complexing reduction method using NH4Cl as the complex agent at the low temperature. The high alloy Pd-Fe/C catalyst Pd and Fe could be prepared at low temperature due to the complex formation by NH4Cl and Pd, which leads to a negative shift for the reduction potential of PdCl2, making the reduction potential of PdCl2 closer to that of FeCl3. The XPS results show that the alloying of Pd with Fe could affect the binding energies of Pd and increase the content of Pd0 in the catalyst. Thus, the electrocatalytic activity of the Pd-Fe/C catalyst obtained for the oxygen reduction is higher than that of the Pd/C catalyst prepared with the same method. Furthermore, this Pd-Fe/C catalyst has no electrocatalytic activity for the methanol oxidation.
2015, (1): 29-36
doi: 10.11862/CJIC.2015.003
Abstract:
Hierarchical structured CuAPO-5 molecular sieve has been ionothermally synthesized by microwave irradiation and using eutectic mixture based on succinic acid, choline chloride and tetraethyl ammonium bromide as solvent and template. The effects of the ratio of P2O5/Al2O3, HF/Al2O3 and CuO/Al2O3, aluminum and copper sources on the crystallization of CuAPO-5 were systematically investigated. The resulting CuAPO-5 molecular sieve was characterized by X-ray diffraction (XRD), Scanning electron microscope (SEM), Transmission electron microscopy (TEM), and N2 physical adsorption-desorption, respectively. SEM analysis reveals that CuAPO-5 molecular sieve with hexagonal nanometer-disc morphology can be synthesized under specific synthesis conditions. N2 physisorption, SEM and TEM characterizations show that the resultant material is one kind of hierarchical structured aluminophosphate molecular sieve possesses both micropore and mesopore.
Hierarchical structured CuAPO-5 molecular sieve has been ionothermally synthesized by microwave irradiation and using eutectic mixture based on succinic acid, choline chloride and tetraethyl ammonium bromide as solvent and template. The effects of the ratio of P2O5/Al2O3, HF/Al2O3 and CuO/Al2O3, aluminum and copper sources on the crystallization of CuAPO-5 were systematically investigated. The resulting CuAPO-5 molecular sieve was characterized by X-ray diffraction (XRD), Scanning electron microscope (SEM), Transmission electron microscopy (TEM), and N2 physical adsorption-desorption, respectively. SEM analysis reveals that CuAPO-5 molecular sieve with hexagonal nanometer-disc morphology can be synthesized under specific synthesis conditions. N2 physisorption, SEM and TEM characterizations show that the resultant material is one kind of hierarchical structured aluminophosphate molecular sieve possesses both micropore and mesopore.
2015, (1): 37-44
doi: 10.11862/CJIC.2015.013
Abstract:
This paper focuses on the long-term storage (in-shelf) stability issues of controllable silver nanoparticle hydrocolloids (AgNPs). Two controllable AgNPs were prepared from two different precursors: silver nitrate (AgNO3) and silver diamminohydroxide ([Ag(NH3)2]OH). The important characteristics of the AgNPs were measured by means of UV-Vis, SEM, EDS, ZETA electric potential techniques as well as mathematical simulations. The comparative studies show that the AgNPs obtained from the [Ag(NH3)2]OH precursor exhibited superior controlla-bility in particle size, size-distribution and dispensability in one month storage, compared to those obtained from AgNO3.
This paper focuses on the long-term storage (in-shelf) stability issues of controllable silver nanoparticle hydrocolloids (AgNPs). Two controllable AgNPs were prepared from two different precursors: silver nitrate (AgNO3) and silver diamminohydroxide ([Ag(NH3)2]OH). The important characteristics of the AgNPs were measured by means of UV-Vis, SEM, EDS, ZETA electric potential techniques as well as mathematical simulations. The comparative studies show that the AgNPs obtained from the [Ag(NH3)2]OH precursor exhibited superior controlla-bility in particle size, size-distribution and dispensability in one month storage, compared to those obtained from AgNO3.
2015, (1): 45-53
doi: 10.11862/CJIC.2015.012
Abstract:
Three zinc complexes [Zn(bptc)0.5]n (1), [Zn2(bptc)(H2O)3]n·nH2O (2), [Zn2(bptc)(H2O)(bipy)1.5]n·nH2O (3), were synthesized under hydrothermal reactions by using biphenyl-2,4,4',6-tetracarboxylic acid (H4bptc) and 4,4'-Bipyridine (bipy). They were characterized by elemental analysis, IR spectra. Crystal structures of the complexes were determined by single crystal X-ray diffraction method. Complex 1 is binuclear structure, eight ring metal clusters with (4,4) topology. Complex 2 is a (4,5,6) topology construction. Complex 3 is a 3D network structure formed by ligand and auxiliary ligand. The interaction between three complexes and DNA were studied by EtBr fluorescence probe. Add the rigid auxiliary ligand, the interaction of complex 3 to the DNA is stronger than complex 1 and 2. CCDC: 952957, 1; 952958, 2; 952959, 3.
Three zinc complexes [Zn(bptc)0.5]n (1), [Zn2(bptc)(H2O)3]n·nH2O (2), [Zn2(bptc)(H2O)(bipy)1.5]n·nH2O (3), were synthesized under hydrothermal reactions by using biphenyl-2,4,4',6-tetracarboxylic acid (H4bptc) and 4,4'-Bipyridine (bipy). They were characterized by elemental analysis, IR spectra. Crystal structures of the complexes were determined by single crystal X-ray diffraction method. Complex 1 is binuclear structure, eight ring metal clusters with (4,4) topology. Complex 2 is a (4,5,6) topology construction. Complex 3 is a 3D network structure formed by ligand and auxiliary ligand. The interaction between three complexes and DNA were studied by EtBr fluorescence probe. Add the rigid auxiliary ligand, the interaction of complex 3 to the DNA is stronger than complex 1 and 2. CCDC: 952957, 1; 952958, 2; 952959, 3.
2015, (1): 54-60
doi: 10.11862/CJIC.2015.029
Abstract:
The multilayer dehydrated reduced graphenes oxide (DRGO) were prepared by a simple and fast treatment of graphene oxide(GO) with sulfuric acid and were used as electrode materials for supercapacitor. Areduction process was devised through a two-step reduction of graphene oxide: first in aqueous sulfuric acid and then in concentrated sulfuric acid at 70 ℃, 30 min. The results showed that the type, amount of oxygen functionalities and newly formed sp2 domains were different for one-pot and two-step reduction of graphene oxide. The high reduction degree DRGOelectrode with less restacked layers and smaller size sp2 domains exhibits a high specific capacitance of 321.8 F·g-1 at a scan rate of 10 mV·s-1, and an excellent cycling stability along with 89.7% specific capacitane retained after 1000 cycle tests. This facile and low cost method makes the DRGOa potential candidate in applications of electrochemical capacitors.
The multilayer dehydrated reduced graphenes oxide (DRGO) were prepared by a simple and fast treatment of graphene oxide(GO) with sulfuric acid and were used as electrode materials for supercapacitor. Areduction process was devised through a two-step reduction of graphene oxide: first in aqueous sulfuric acid and then in concentrated sulfuric acid at 70 ℃, 30 min. The results showed that the type, amount of oxygen functionalities and newly formed sp2 domains were different for one-pot and two-step reduction of graphene oxide. The high reduction degree DRGOelectrode with less restacked layers and smaller size sp2 domains exhibits a high specific capacitance of 321.8 F·g-1 at a scan rate of 10 mV·s-1, and an excellent cycling stability along with 89.7% specific capacitane retained after 1000 cycle tests. This facile and low cost method makes the DRGOa potential candidate in applications of electrochemical capacitors.
2015, (1): 61-68
doi: 10.11862/CJIC.2015.004
Abstract:
Hierarchical structure ZnO samples with different morphologies were synthesized by sol-gel assisted hydrothermal method, using Zn(NO3)2·6H2O, citric acid and NaOH as raw materials. Nanosheets flower-like ZnO, nanorods flower-like ZnO and spind-like ZnO microstructures could be synthesized only by controlling the time of hydrothermal reaction. The as-prepared samples were characterized by XRD, SEM, UV-Vis, DRS, photoluminescence (PL) and low temperature nitrogen adsorption-desorption. The formation mechanism of different morphologies of ZnO hierarchical structures was proposed. The photocatalytic activities of the samples were evaluated by the degradation of Reactive Blue 14 (KGL) under UV irradiation. The results demonstrated that different morphologies of ZnO samples all showed good photocatalytic performance, with the degradation degree of KGL exceeding 78% after 120 min. But the sample prepared at 120 ℃ for 4 h exhibited superior photocatalytic activity to other ZnO samples, and the degradation rate of KGL can reach 99%. It might be attributed to the morphology, larger specific surface area, more oxygen surface defect and surface polarity.
Hierarchical structure ZnO samples with different morphologies were synthesized by sol-gel assisted hydrothermal method, using Zn(NO3)2·6H2O, citric acid and NaOH as raw materials. Nanosheets flower-like ZnO, nanorods flower-like ZnO and spind-like ZnO microstructures could be synthesized only by controlling the time of hydrothermal reaction. The as-prepared samples were characterized by XRD, SEM, UV-Vis, DRS, photoluminescence (PL) and low temperature nitrogen adsorption-desorption. The formation mechanism of different morphologies of ZnO hierarchical structures was proposed. The photocatalytic activities of the samples were evaluated by the degradation of Reactive Blue 14 (KGL) under UV irradiation. The results demonstrated that different morphologies of ZnO samples all showed good photocatalytic performance, with the degradation degree of KGL exceeding 78% after 120 min. But the sample prepared at 120 ℃ for 4 h exhibited superior photocatalytic activity to other ZnO samples, and the degradation rate of KGL can reach 99%. It might be attributed to the morphology, larger specific surface area, more oxygen surface defect and surface polarity.
2015, (1): 69-73
doi: 10.11862/CJIC.2015.048
Abstract:
β-AgVO3 nanowires with monoclinic structure were synthesized by hydrothermal method. C nanotube (CNT) as an effective cocatalyst was loaded onto β-AgVO3 photocatalyst. The photocatalytic activity of CNT/β-AgVO3 was performed by its O2 evolution performance under UV-Vis irradiation while KIO3 was used as electron acceptor, and the photocatalyst was characterized by XRD, SEM, TEM and UV-Vis absorption spectrum. The results showed that the photocatalytic activity of CNT/β-AgVO3 was superior to that of pure β-AgVO3, and loaded CNT can improve the interfacial electron transfer and the O2 evolution. When the amount of loaded CNT was 1%(wt), the stable average oxygen evolution rate was about 250 μmol·g-1·h-1.
β-AgVO3 nanowires with monoclinic structure were synthesized by hydrothermal method. C nanotube (CNT) as an effective cocatalyst was loaded onto β-AgVO3 photocatalyst. The photocatalytic activity of CNT/β-AgVO3 was performed by its O2 evolution performance under UV-Vis irradiation while KIO3 was used as electron acceptor, and the photocatalyst was characterized by XRD, SEM, TEM and UV-Vis absorption spectrum. The results showed that the photocatalytic activity of CNT/β-AgVO3 was superior to that of pure β-AgVO3, and loaded CNT can improve the interfacial electron transfer and the O2 evolution. When the amount of loaded CNT was 1%(wt), the stable average oxygen evolution rate was about 250 μmol·g-1·h-1.
2015, (1): 74-80
doi: 10.11862/CJIC.2015.033
Abstract:
The nickel(Ⅱ) and copper(Ⅱ) complexes [NiL2] (1) and [Cu(Ac)L] (2) were synthesized by reaction of 2-acetylpyridine isonicotinoyl hydrazone Schiff base(HL) with metal acetate, and characterized by elemental analysis, IR, UV-Vis, FLspectra, TGA and X-ray crystal diffraction. The crystal of 1 belongs to the orthorhombic system,space group Aba2 with cell parameters a=1.2059 (3) nm, b=2.0741(5) nm, c=0.9115 (2) nm, V=2.2798 (10) nm3, Z=4, Mr=537.21, Dc=1.565 g·cm-3, F(000)=1113 and the crystal of 2 belongs to the monoclinic system,space group P21/c with cell parameters a=0.86477(13) nm, b=1.3383(2) nm, c=1.3631(2) nm, β=105.650 (4)°, V=1.5190(4) nm3, Z=4, Mr=361.85, Dc=1.582 g·cm-3, F(000)=740. The tests showed the two complexes displayed good thermal stability below 340 ℃(1)和296 ℃(2), respectively. The complexes exhibits blue luminescence with emission maximum at 430 and 428 nm at room temperature, respectively. CCDC: 952992, 1; 993273, 2.
The nickel(Ⅱ) and copper(Ⅱ) complexes [NiL2] (1) and [Cu(Ac)L] (2) were synthesized by reaction of 2-acetylpyridine isonicotinoyl hydrazone Schiff base(HL) with metal acetate, and characterized by elemental analysis, IR, UV-Vis, FLspectra, TGA and X-ray crystal diffraction. The crystal of 1 belongs to the orthorhombic system,space group Aba2 with cell parameters a=1.2059 (3) nm, b=2.0741(5) nm, c=0.9115 (2) nm, V=2.2798 (10) nm3, Z=4, Mr=537.21, Dc=1.565 g·cm-3, F(000)=1113 and the crystal of 2 belongs to the monoclinic system,space group P21/c with cell parameters a=0.86477(13) nm, b=1.3383(2) nm, c=1.3631(2) nm, β=105.650 (4)°, V=1.5190(4) nm3, Z=4, Mr=361.85, Dc=1.582 g·cm-3, F(000)=740. The tests showed the two complexes displayed good thermal stability below 340 ℃(1)和296 ℃(2), respectively. The complexes exhibits blue luminescence with emission maximum at 430 and 428 nm at room temperature, respectively. CCDC: 952992, 1; 993273, 2.
2015, (1): 81-86
doi: 10.11862/CJIC.2015.017
Abstract:
A multifunctional composite microspheres were prepared based on NaYF4:Yb3+,Er3+ upconversion nanoparticles (UCNPs), zinc phthalocyanine (ZnPc) and poly(maleic anhydride-alt-1-Octadecene) (PMAO) via a one step self-assembly process in microemulsion droplets. The UCNPs as fluorescence imaging agent can be used for biological imaging, and can also use the up-convering luminescence sensitization photosensitive molecules for the research of photosensitive activity. PMAO molecules provide anhydride functional groups for immobilization of biomolecules. The morphologies and property were characterized by transition electron microscopy (TEM), Zeta potential and photoluminescence (PL) spectroscopy. The fluorescence confocal cell imaging confirms that the NaYF4-ZnPc-PMAO are suitable for potential biological labeling. Photodynamic cancer cell killing ability was evaluated using a MTT assay with Hela cells under different time irradiations. The results indicating that the NaYF4-ZnPc-PMAO composite microspheres have highly killing ability to Hela cells under 980 nm light irradiation.
A multifunctional composite microspheres were prepared based on NaYF4:Yb3+,Er3+ upconversion nanoparticles (UCNPs), zinc phthalocyanine (ZnPc) and poly(maleic anhydride-alt-1-Octadecene) (PMAO) via a one step self-assembly process in microemulsion droplets. The UCNPs as fluorescence imaging agent can be used for biological imaging, and can also use the up-convering luminescence sensitization photosensitive molecules for the research of photosensitive activity. PMAO molecules provide anhydride functional groups for immobilization of biomolecules. The morphologies and property were characterized by transition electron microscopy (TEM), Zeta potential and photoluminescence (PL) spectroscopy. The fluorescence confocal cell imaging confirms that the NaYF4-ZnPc-PMAO are suitable for potential biological labeling. Photodynamic cancer cell killing ability was evaluated using a MTT assay with Hela cells under different time irradiations. The results indicating that the NaYF4-ZnPc-PMAO composite microspheres have highly killing ability to Hela cells under 980 nm light irradiation.
2015, (1): 87-96
doi: 10.11862/CJIC.2015.011
Abstract:
Co-polymerization of [2Fe2S] model complex [Fe2(μ-SCH2C≡CH)2(CO)6] (A), diazide 2,6-(N3CH2)Py (B, Py=pyridine) and diyne compound (2-PyCH2)N(CH2C≡CH)2 (C, Py=pyridine) led to the formation of six functionalized Polymers Polymer-1~Polymer-6 via "click reaction" by varying the ratio of the three components. These Polymers were characterized by IR spectroscopy, sulfur elemental analysis, thermal gravimetric analysis, scanning electron microscopy and electrochemistry. IR spectroscopic data and electrochemical investigations suggested that diiron hexacarbonyl complex A exists as diiron pentacarbonyl unit in these Polymers. In the co-polymerizing process, increasing the content of monomer C can significantly change the morphologies of these Polymers and improve their solubility in organic solvents and thermal stability. Electrochemistry of these Polymers in acetic acid-DMF indicated that the secondary coordination atmosphere established by introducing alkaline group provided by the monomer C can significantly enhance the catalytic performance of the diiron units in these Polymers.
Co-polymerization of [2Fe2S] model complex [Fe2(μ-SCH2C≡CH)2(CO)6] (A), diazide 2,6-(N3CH2)Py (B, Py=pyridine) and diyne compound (2-PyCH2)N(CH2C≡CH)2 (C, Py=pyridine) led to the formation of six functionalized Polymers Polymer-1~Polymer-6 via "click reaction" by varying the ratio of the three components. These Polymers were characterized by IR spectroscopy, sulfur elemental analysis, thermal gravimetric analysis, scanning electron microscopy and electrochemistry. IR spectroscopic data and electrochemical investigations suggested that diiron hexacarbonyl complex A exists as diiron pentacarbonyl unit in these Polymers. In the co-polymerizing process, increasing the content of monomer C can significantly change the morphologies of these Polymers and improve their solubility in organic solvents and thermal stability. Electrochemistry of these Polymers in acetic acid-DMF indicated that the secondary coordination atmosphere established by introducing alkaline group provided by the monomer C can significantly enhance the catalytic performance of the diiron units in these Polymers.
2015, (1): 97-102
doi: 10.11862/CJIC.2015.010
Abstract:
The nano-MnO2 was prepared by hydrothermal method, and then super thermite Al/MnO2 was prepared by ultrasonic dispersion method using nano-MnO2 and Al nanoparticles as raw materials. The physical phase, composition, morphology and structure of products were characterized by X-ray diffraction (XRD) and scanning electron microscope-energy dispersive spectrometer (SEM-EDS). The catalytic effect of MnO2 nanotube and the super thermite on the thermal decomposition of cyclotrimethylene trinitramine were investigated by differential scanning colorimetry (DSC). The results indicate that nano-MnO2 is in tubular structure, and the globose nano-Al particles are homodispersed on the surface of MnO2 nanotube. MnO2 nanotube and its super thermite influence the thermal decomposition behavior and decomposition process of cyclotrimethylene trinitramine. They can change the primary decomposition of liquid phase to the reaction of secondary gas phase and can change the shape of main decomposition peak obviously.
The nano-MnO2 was prepared by hydrothermal method, and then super thermite Al/MnO2 was prepared by ultrasonic dispersion method using nano-MnO2 and Al nanoparticles as raw materials. The physical phase, composition, morphology and structure of products were characterized by X-ray diffraction (XRD) and scanning electron microscope-energy dispersive spectrometer (SEM-EDS). The catalytic effect of MnO2 nanotube and the super thermite on the thermal decomposition of cyclotrimethylene trinitramine were investigated by differential scanning colorimetry (DSC). The results indicate that nano-MnO2 is in tubular structure, and the globose nano-Al particles are homodispersed on the surface of MnO2 nanotube. MnO2 nanotube and its super thermite influence the thermal decomposition behavior and decomposition process of cyclotrimethylene trinitramine. They can change the primary decomposition of liquid phase to the reaction of secondary gas phase and can change the shape of main decomposition peak obviously.
2015, (1): 103-108
doi: 10.11862/CJIC.2015.032
Abstract:
Honeycomb-like hierarchical porous carbon was prepared and employed as substrate to support nickel nanparticles via an impregnation-chemical reduction method. The synthesized carbon-supported nickel (denoted as Ni/C) was used as catalysts for hydrogen generation from hydrolysis of ammonia borane (AB). Results of XRD, BET, SEM, Raman, and TEM measurements showed that the synthesized carbon possessed high specific surface area of 737 m2·g-1 and partially graphited structure; the supported amorphous Ni nanoparticles had an average particle size of 10 nm and were uniformly dispersed on the porous carbon substrate. The synthesized Ni/C exhibited high catalytic activity towards the hydrolysis of AB. At hydrolysis temperature of 298 K, Ni/C with 30wt% Ni loading was the most active, resulting in a high hydrogen release rate of 1304.67 mL·min-1·g-1 and a low activation energy of 29.1 kJ·mol-1. In addition, the Ni/C catalyst could be repeatedly utilized with respectable activity reservation for several times. The results indicate that Ni/C is a promising low-cost catalyst for hydrolytic dehydrogenation of AB.
Honeycomb-like hierarchical porous carbon was prepared and employed as substrate to support nickel nanparticles via an impregnation-chemical reduction method. The synthesized carbon-supported nickel (denoted as Ni/C) was used as catalysts for hydrogen generation from hydrolysis of ammonia borane (AB). Results of XRD, BET, SEM, Raman, and TEM measurements showed that the synthesized carbon possessed high specific surface area of 737 m2·g-1 and partially graphited structure; the supported amorphous Ni nanoparticles had an average particle size of 10 nm and were uniformly dispersed on the porous carbon substrate. The synthesized Ni/C exhibited high catalytic activity towards the hydrolysis of AB. At hydrolysis temperature of 298 K, Ni/C with 30wt% Ni loading was the most active, resulting in a high hydrogen release rate of 1304.67 mL·min-1·g-1 and a low activation energy of 29.1 kJ·mol-1. In addition, the Ni/C catalyst could be repeatedly utilized with respectable activity reservation for several times. The results indicate that Ni/C is a promising low-cost catalyst for hydrolytic dehydrogenation of AB.
2015, (1): 109-113
doi: 10.11862/CJIC.2015.051
Abstract:
Two complexes [CdL(NO3)2·H2O] (1) and [ZnL2] (2) were synthesized by the reaction of Schiff base ligand (2-acetylpyridine-o-aminobenzoylhydrazone) (L) with Cd(NO3)2·4H2O or Zn(CH3COO)2·2H2O respectively. The compounds are characterized by 1H NMR, FTIR, and elemental analysis. The structures of the two complexes are analyzed via single crystal X-ray diffraction. The results show that the complex 1 crystallizes in monoclinic, space group P21/n, and the complex 2 crystallizes in monoclinic, space group P21/c. The antibacterial activities of the ligand and complexes were measured in vitro, and the results show that the ligand Land complex 1 possess inhibiting effects to bacteria. CCDC: 1012633, 1; 1012634, 2.
Two complexes [CdL(NO3)2·H2O] (1) and [ZnL2] (2) were synthesized by the reaction of Schiff base ligand (2-acetylpyridine-o-aminobenzoylhydrazone) (L) with Cd(NO3)2·4H2O or Zn(CH3COO)2·2H2O respectively. The compounds are characterized by 1H NMR, FTIR, and elemental analysis. The structures of the two complexes are analyzed via single crystal X-ray diffraction. The results show that the complex 1 crystallizes in monoclinic, space group P21/n, and the complex 2 crystallizes in monoclinic, space group P21/c. The antibacterial activities of the ligand and complexes were measured in vitro, and the results show that the ligand Land complex 1 possess inhibiting effects to bacteria. CCDC: 1012633, 1; 1012634, 2.
2015, (1): 114-120
doi: 10.11862/CJIC.2015.036
Abstract:
In order to overcome the brittleness of hydroxyapatite (HA) bioceramics, it is suggested to be an efficient approach to fabricate carbon nanotubes (CNTs)/HA composites by compounding CNTs with HA for the clinic applications in bone tissue engineering. CNTs/HA composites had been fabricated by three different methods, that was CNTs dispersing into HA with the addition of surfactant, CNTs coprecipitating with HA via an acid-base reaction, and HA growing on CNTs by a mineralization approach. The results showed that CNTs/HA composites exhibited a certain plastic deformation under the compress load condition and the compressive mechanical properties had been increased owing to the existence of CNTs in these composites. For the uniform distribution and network array of CNTs with slightly damaged structure in HA matrix and good interfacial bonding between CNTs and HA, CNTs/HA composites prepared by CNTs dispersing into HA with the addition of surfactant have the best compressive mechanical properties. However, CNTs/HA composites prepared by CNTs coprecipitating with HA via an acid-base reaction have the worst compressive mechanical properties for the uneven distribution and aggregating array of CNTs with greatly damaged structure in HA matrix.
In order to overcome the brittleness of hydroxyapatite (HA) bioceramics, it is suggested to be an efficient approach to fabricate carbon nanotubes (CNTs)/HA composites by compounding CNTs with HA for the clinic applications in bone tissue engineering. CNTs/HA composites had been fabricated by three different methods, that was CNTs dispersing into HA with the addition of surfactant, CNTs coprecipitating with HA via an acid-base reaction, and HA growing on CNTs by a mineralization approach. The results showed that CNTs/HA composites exhibited a certain plastic deformation under the compress load condition and the compressive mechanical properties had been increased owing to the existence of CNTs in these composites. For the uniform distribution and network array of CNTs with slightly damaged structure in HA matrix and good interfacial bonding between CNTs and HA, CNTs/HA composites prepared by CNTs dispersing into HA with the addition of surfactant have the best compressive mechanical properties. However, CNTs/HA composites prepared by CNTs coprecipitating with HA via an acid-base reaction have the worst compressive mechanical properties for the uneven distribution and aggregating array of CNTs with greatly damaged structure in HA matrix.
2015, (1): 121-126
doi: 10.11862/CJIC.2015.009
Abstract:
The extraction behavior of Th4+ from nitric acid solution with N,N,N',N'-tetraoctyldiglycolamide(TODGA) dissolved in hydrophobic ionic liquid [C2mim][NTf2] was studied. The effect of contact time, acidity, Th4+ concentration,TODGAconcentration and temperature on the extraction performance of TODGA/[C2mim][NTf2] system were investigated. For comparison, the same experiment in TODGA/isooctane system was also done. The results showed that the extraction of TODGA/[C2mim][NTf2] system against Th4+ was endothermic reaction and could balance within5 min at 50 ℃. The extraction efficiency decreased first and then increased with the increasing of acidity and Th4+concentration as well as decreasing of TODGAconcentration. It was found that TODGA/[C2mim][NTf2] system had better extraction efficiency than TODGA/isooctane system especially at low acidity. The extraction mechanism was suggested that at low acidity the extraction proceed via ion exchange mechanism to a coordination compound,and the mechanism at the high acidity was neutral complex.
The extraction behavior of Th4+ from nitric acid solution with N,N,N',N'-tetraoctyldiglycolamide(TODGA) dissolved in hydrophobic ionic liquid [C2mim][NTf2] was studied. The effect of contact time, acidity, Th4+ concentration,TODGAconcentration and temperature on the extraction performance of TODGA/[C2mim][NTf2] system were investigated. For comparison, the same experiment in TODGA/isooctane system was also done. The results showed that the extraction of TODGA/[C2mim][NTf2] system against Th4+ was endothermic reaction and could balance within5 min at 50 ℃. The extraction efficiency decreased first and then increased with the increasing of acidity and Th4+concentration as well as decreasing of TODGAconcentration. It was found that TODGA/[C2mim][NTf2] system had better extraction efficiency than TODGA/isooctane system especially at low acidity. The extraction mechanism was suggested that at low acidity the extraction proceed via ion exchange mechanism to a coordination compound,and the mechanism at the high acidity was neutral complex.
2015, (1): 127-132
doi: 10.11862/CJIC.2015.023
Abstract:
Acyclam-based ligand: tetratert-butyl ((4,11-dimethyl-1,4,8,11-tetraazacyclotetradecane-1,8-diyl)bis (propane-3,2,1-triyl)) tetracarbamatev (L1), and its metal complexes [Zn(L1)Cl2] (1), [Ni(L1)Cl2] (2) and [Cu(L1)Cl2] (3) were designed and synthesized. L1 has a C2 symmetrical structure and the 1H chemical shift of the same carbon was different because of the influence of cyclam ring. The metal binding site of the L1 was confirmed by 2D [1H, 15N] HSQC by comparing the chemical shift of N of the branched chains of the ligand that of with the corresponding metal complex. The co-existence of two configuration was characterized by 13C VT NMR combined with 2D [1H, 15N] HSQC NMR and trans-Ⅲ was confirmed to be the main configuration for complex 1. The cleavage activity of the ligand L1 and the complexes 1~3 was investigated in detail under physiological conditions. Agarose gel electrophoresis experiments showed that the complex 3 possesses interesting nuclease activity in the present of ascorbate; No matter the hydrolysis or oxidation, the ligand L1 and complex 1, and 2 were negative to DNA at the experimental conditions.
Acyclam-based ligand: tetratert-butyl ((4,11-dimethyl-1,4,8,11-tetraazacyclotetradecane-1,8-diyl)bis (propane-3,2,1-triyl)) tetracarbamatev (L1), and its metal complexes [Zn(L1)Cl2] (1), [Ni(L1)Cl2] (2) and [Cu(L1)Cl2] (3) were designed and synthesized. L1 has a C2 symmetrical structure and the 1H chemical shift of the same carbon was different because of the influence of cyclam ring. The metal binding site of the L1 was confirmed by 2D [1H, 15N] HSQC by comparing the chemical shift of N of the branched chains of the ligand that of with the corresponding metal complex. The co-existence of two configuration was characterized by 13C VT NMR combined with 2D [1H, 15N] HSQC NMR and trans-Ⅲ was confirmed to be the main configuration for complex 1. The cleavage activity of the ligand L1 and the complexes 1~3 was investigated in detail under physiological conditions. Agarose gel electrophoresis experiments showed that the complex 3 possesses interesting nuclease activity in the present of ascorbate; No matter the hydrolysis or oxidation, the ligand L1 and complex 1, and 2 were negative to DNA at the experimental conditions.
2015, (1): 133-139
doi: 10.11862/CJIC.2015.037
Abstract:
TiO2 nanotube array was prepared by anodic oxidation method on the titanium substrate, and Fe2O3 nanoparticles was successfully deposited on TiO2 nanotube array by a chemical bath method. Scanning electron microscopy (SEM), X-ray diffraction (XRD) and UV-Vis diffuse reflectance spectroscopy was applied to characterize their properties and the photoelectrochemical properties and the performance of photocatalytic degradation of methylene blue was investigated. The results indicated that the Fe2O3 modification not only broadened the absorption spectrum of TiO2 nanotube arrays to the visible light region, but also increased the photocurrent. The photocurrent response of Fe2O3 modified TiO2 nanotube arrays was 9 times higher than undecorated TiO2 nanotube arrays. In the photocatalytic reaction, the highest methylene blue degradation rate can reach 80%, which was 30% higher than the bare TiO2 nanotube arrays.
TiO2 nanotube array was prepared by anodic oxidation method on the titanium substrate, and Fe2O3 nanoparticles was successfully deposited on TiO2 nanotube array by a chemical bath method. Scanning electron microscopy (SEM), X-ray diffraction (XRD) and UV-Vis diffuse reflectance spectroscopy was applied to characterize their properties and the photoelectrochemical properties and the performance of photocatalytic degradation of methylene blue was investigated. The results indicated that the Fe2O3 modification not only broadened the absorption spectrum of TiO2 nanotube arrays to the visible light region, but also increased the photocurrent. The photocurrent response of Fe2O3 modified TiO2 nanotube arrays was 9 times higher than undecorated TiO2 nanotube arrays. In the photocatalytic reaction, the highest methylene blue degradation rate can reach 80%, which was 30% higher than the bare TiO2 nanotube arrays.
2015, (1): 140-146
doi: 10.11862/CJIC.2015.022
Abstract:
Pt/C catalysts were prepared using a new modified polyol method with different heat treatment temperatures of Vulcan XC-72 carbon support. The oxygen containing functional group and the specific surface area of carbon black were characterized by pH meter and physical adsorption instrument. The composition, morphology and the electrochemical properties of the Pt/C catalyst were characterized by coupled plasma atomic emission spectroscopy, Transmission electron microscopy, X-ray diffraction and cyclic voltammograms, respectively. The results indicate that the Pt/C catalyst with 400 ℃ heat treatment for carbon black has an electrochemical specific surface area of 83 m2·g-1, and the quality of the current density of 49.03 A·g-1, while the corresponding parameters for imported commercial JM 20% Pt/C catalyst are 77 m2·g-1 and 11.13 A·g-1, respectively. The Pt loading in the present work is decreased by 3wt%~4wt% and the electric catalytic activity for the catalyst obtained in this work is better than that of commercial JM 20% Pt/C catalyst.
Pt/C catalysts were prepared using a new modified polyol method with different heat treatment temperatures of Vulcan XC-72 carbon support. The oxygen containing functional group and the specific surface area of carbon black were characterized by pH meter and physical adsorption instrument. The composition, morphology and the electrochemical properties of the Pt/C catalyst were characterized by coupled plasma atomic emission spectroscopy, Transmission electron microscopy, X-ray diffraction and cyclic voltammograms, respectively. The results indicate that the Pt/C catalyst with 400 ℃ heat treatment for carbon black has an electrochemical specific surface area of 83 m2·g-1, and the quality of the current density of 49.03 A·g-1, while the corresponding parameters for imported commercial JM 20% Pt/C catalyst are 77 m2·g-1 and 11.13 A·g-1, respectively. The Pt loading in the present work is decreased by 3wt%~4wt% and the electric catalytic activity for the catalyst obtained in this work is better than that of commercial JM 20% Pt/C catalyst.
2015, (1): 147-152
doi: 10.11862/CJIC.2015.005
Abstract:
Gd2O3:Er3+ up-conversion luminescent powder was synthesized by precipitation-calcination method, and characterized by X-ray diffraction, scanning electron microscope, energy dispersive spectrometry and fluorescence spectroscopy. The luminescent powder was added to the TiO2 photoanode of dye-sensitized solar cells to make use of up-conversion luminescent character. The results indicate that Gd2O3:Er3+ up-conversion luminescent powder with tubular morphology improves the light harvesting via a conversion luminescence process and increases absorption efficiency by light scattering, resulting in the increment of photocurrent and photovoltage. When TiO2 is doped by 5wt% Gd2O3:Er3+, the overall light-to-electric conversion efficiency is enhanced from 5.93% to 7.55%, i.e. about 27% increase.
Gd2O3:Er3+ up-conversion luminescent powder was synthesized by precipitation-calcination method, and characterized by X-ray diffraction, scanning electron microscope, energy dispersive spectrometry and fluorescence spectroscopy. The luminescent powder was added to the TiO2 photoanode of dye-sensitized solar cells to make use of up-conversion luminescent character. The results indicate that Gd2O3:Er3+ up-conversion luminescent powder with tubular morphology improves the light harvesting via a conversion luminescence process and increases absorption efficiency by light scattering, resulting in the increment of photocurrent and photovoltage. When TiO2 is doped by 5wt% Gd2O3:Er3+, the overall light-to-electric conversion efficiency is enhanced from 5.93% to 7.55%, i.e. about 27% increase.
2015, (1): 153-158
doi: 10.11862/CJIC.2015.014
Abstract:
5%ZrO2/MCM-41 and 5%ZrO2-5%M2O3/MCM-41(M=La,Ce,Sm,Gd)were prepared by the impregnation method. The hydrogen transfer reduction of acetophenone with 2-propanol was investigated over these catalysts. The catalysts were characterized with XRD, N2 adsorption-desorption and FTIR spectra of adsorbed pyridine. The results show that ZrO2 and rare-earth metal oxides disperse on the surface of MCM-41 supports in an amorphous phase or as tiny crystal particles lower than the detection limit of XRD. The catalytic activity obviously varies upon loading rare-earth metal oxides on5%ZrO2-MCM-41, The activities of the catalysts decrease in the order of 5%ZrO2-5%La2O3/MCM-41 > 5%ZrO2-5%Sm2O3/MCM-41 > 5%ZrO2-5%Gd2O3/MCM-41 > 5%ZrO2/MCM-41 > 5%ZrO2-5%Ce2O3/MCM-41. Addition of rare-earth metal oxides leads to strengthening the acidity of Zr-OH, Lewis acid sites and Brönsted acid sites on the catalyst surface. On the other hand, the addition of La2O3 can obviously enhance the number of acid sites on the catalyst surface. On the contrary, the loading of Sm2O3、Gd2O3 results in the slight decrease in the number of acid sites on the catalyst surface, especially, the addition of Ce2O3 leads to a significant drop in the number of acid sites.
5%ZrO2/MCM-41 and 5%ZrO2-5%M2O3/MCM-41(M=La,Ce,Sm,Gd)were prepared by the impregnation method. The hydrogen transfer reduction of acetophenone with 2-propanol was investigated over these catalysts. The catalysts were characterized with XRD, N2 adsorption-desorption and FTIR spectra of adsorbed pyridine. The results show that ZrO2 and rare-earth metal oxides disperse on the surface of MCM-41 supports in an amorphous phase or as tiny crystal particles lower than the detection limit of XRD. The catalytic activity obviously varies upon loading rare-earth metal oxides on5%ZrO2-MCM-41, The activities of the catalysts decrease in the order of 5%ZrO2-5%La2O3/MCM-41 > 5%ZrO2-5%Sm2O3/MCM-41 > 5%ZrO2-5%Gd2O3/MCM-41 > 5%ZrO2/MCM-41 > 5%ZrO2-5%Ce2O3/MCM-41. Addition of rare-earth metal oxides leads to strengthening the acidity of Zr-OH, Lewis acid sites and Brönsted acid sites on the catalyst surface. On the other hand, the addition of La2O3 can obviously enhance the number of acid sites on the catalyst surface. On the contrary, the loading of Sm2O3、Gd2O3 results in the slight decrease in the number of acid sites on the catalyst surface, especially, the addition of Ce2O3 leads to a significant drop in the number of acid sites.
2015, (1): 159-165
doi: 10.11862/CJIC.2015.020
Abstract:
The precursor Co0.9Ni0.05Mn0.05(OH)2 of the high-voltage cathode material for lithium ion batteries was synthesized by hydroxide co-precipitation method using the transition metal sulphate as the raw material, NaOH and NH3·H2Oas the precipitate agents. Then the corresponding Li(Co0.9Ni0.05Mn0.05)O2 was obtained when mixing the precursor with Li2CO3 by high solid method. Crystal structure, morphology and electrochemical performance of the sample were investigated by XRD, SEM, Cyclic voltammetry (C-V) method, electrochemical impedance spectroscopy (EIS) test and charge-discharge test. Mixed doping Ni-Mn material Li(Co0.9Ni0.05Mn0.05)O2 shows better electrochemical performance compared to LiCoO2 as confirmed by the results of C-V, XRD and EIS. When the co-doped product Li(Co0.9Ni0.05Mn0.05)O2 was charged to 4.4 and 4.5 V, the initial discharge capacity is 162.5 mAh·g-1 and 185 mAh·g-1 at 0.5Crate, respectively. After cycling for 100 times, the retention of discharge capacity was 94.4% and 93.7%, respectively.
The precursor Co0.9Ni0.05Mn0.05(OH)2 of the high-voltage cathode material for lithium ion batteries was synthesized by hydroxide co-precipitation method using the transition metal sulphate as the raw material, NaOH and NH3·H2Oas the precipitate agents. Then the corresponding Li(Co0.9Ni0.05Mn0.05)O2 was obtained when mixing the precursor with Li2CO3 by high solid method. Crystal structure, morphology and electrochemical performance of the sample were investigated by XRD, SEM, Cyclic voltammetry (C-V) method, electrochemical impedance spectroscopy (EIS) test and charge-discharge test. Mixed doping Ni-Mn material Li(Co0.9Ni0.05Mn0.05)O2 shows better electrochemical performance compared to LiCoO2 as confirmed by the results of C-V, XRD and EIS. When the co-doped product Li(Co0.9Ni0.05Mn0.05)O2 was charged to 4.4 and 4.5 V, the initial discharge capacity is 162.5 mAh·g-1 and 185 mAh·g-1 at 0.5Crate, respectively. After cycling for 100 times, the retention of discharge capacity was 94.4% and 93.7%, respectively.
2015, (1): 166-176
doi: 10.11862/CJIC.2015.002
Abstract:
Barium oxide was developed to modify palladium catalysts supported on CeO2-ZrO2-La2O3-Al2O3 (CZLA) compound oxides by impregnation/co-precipitation methods. Low temperature N2 adsorption-desorption, X-ray diffraction (XRD), H2-temperature-programmed reduction (H2-TPR), NH3-temperature programmed desorption (NH3-TPD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) were employed to characterize the influence of the preparation method on physicochemical properties of the catalyst. Catalytic activity performance for methanol, CO, C3H8 and NO conversion was evaluated. Catalytic activity results show that the addition of BaO has a positive effect on the conversion of all pollutants, and the best results are achieved by the impregnation method. The light-off temperature decreases by 43, 31, 45 and 35 ℃, respectively. The XRD, H2-TPR and XPS results confirm that the impregnation method is mainly based on the surface modification. The enrichment of Ba2+ strengthens the Pd-Ce interaction in Pd-Ce interface, promoting the reductive ability, thus increasing the catalytic activity at low temperature. The co-precipitation method results in structure disorder and additional anion vacancies accompanied by the formation of more Ce3+, which may be beneficial to the conversion of CO.
Barium oxide was developed to modify palladium catalysts supported on CeO2-ZrO2-La2O3-Al2O3 (CZLA) compound oxides by impregnation/co-precipitation methods. Low temperature N2 adsorption-desorption, X-ray diffraction (XRD), H2-temperature-programmed reduction (H2-TPR), NH3-temperature programmed desorption (NH3-TPD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) were employed to characterize the influence of the preparation method on physicochemical properties of the catalyst. Catalytic activity performance for methanol, CO, C3H8 and NO conversion was evaluated. Catalytic activity results show that the addition of BaO has a positive effect on the conversion of all pollutants, and the best results are achieved by the impregnation method. The light-off temperature decreases by 43, 31, 45 and 35 ℃, respectively. The XRD, H2-TPR and XPS results confirm that the impregnation method is mainly based on the surface modification. The enrichment of Ba2+ strengthens the Pd-Ce interaction in Pd-Ce interface, promoting the reductive ability, thus increasing the catalytic activity at low temperature. The co-precipitation method results in structure disorder and additional anion vacancies accompanied by the formation of more Ce3+, which may be beneficial to the conversion of CO.
2015, (1): 177-182
doi: 10.11862/CJIC.2015.006
Abstract:
The electrochemical behavior of Ho(Ⅲ) in LiCl-KCl eutectic melts and the alloying mechanism of Ho-Ni alloys were investigated by cyclic voltammetry, square wave voltammetry and open circuit chronopotentiometry. On an inert Welectrode, the electroreduction of Ho(Ⅲ) proceeds in a one-step process involving three electrons at -2.06 V (vs Ag/AgCl). Compared with the cyclic voltammograms on an inert Welectrode, three reduction peaks are observed which indicates the under-potential deposition of Ho(Ⅲ) on the reactive Ni electrode due to the formation of Ho-Ni intermetallic compounds. Three alloy samples were produced by potentiostatic electrolysis at various potentials and characterized by X-ray diffraction (XRD), scanning electron microscopy and energy dispersive spectrometer (SEM-EDS), respectively. The results confirm the three alloy samples of Ho2Ni17, HoNi5 and HoNi2 intermetallic compounds, respectively.
The electrochemical behavior of Ho(Ⅲ) in LiCl-KCl eutectic melts and the alloying mechanism of Ho-Ni alloys were investigated by cyclic voltammetry, square wave voltammetry and open circuit chronopotentiometry. On an inert Welectrode, the electroreduction of Ho(Ⅲ) proceeds in a one-step process involving three electrons at -2.06 V (vs Ag/AgCl). Compared with the cyclic voltammograms on an inert Welectrode, three reduction peaks are observed which indicates the under-potential deposition of Ho(Ⅲ) on the reactive Ni electrode due to the formation of Ho-Ni intermetallic compounds. Three alloy samples were produced by potentiostatic electrolysis at various potentials and characterized by X-ray diffraction (XRD), scanning electron microscopy and energy dispersive spectrometer (SEM-EDS), respectively. The results confirm the three alloy samples of Ho2Ni17, HoNi5 and HoNi2 intermetallic compounds, respectively.
2015, (1): 183-190
doi: 10.11862/CJIC.2015.034
Abstract:
Two new complex [Mn(NIPH)(mbix)]n (1) and [Co(NIPH)(mbix)(H2O)3]2n·2nH2O (2) (H2NIPH=5-nitroiso-phthalic acid, mbix=1,3-bis(imidazol-1-ylmethyl)benzene) have been hydrothermally synthesized and structurally characterized by elemental analysis, IRspectrum, UVspectrum, TGand single-crystal X-ray diffraction. They are further extended into a three-dimensional supramolecular network structure through hydrogen bonds and π-π interactions. CCDC: 979616, 1; 1011701, 2.
Two new complex [Mn(NIPH)(mbix)]n (1) and [Co(NIPH)(mbix)(H2O)3]2n·2nH2O (2) (H2NIPH=5-nitroiso-phthalic acid, mbix=1,3-bis(imidazol-1-ylmethyl)benzene) have been hydrothermally synthesized and structurally characterized by elemental analysis, IRspectrum, UVspectrum, TGand single-crystal X-ray diffraction. They are further extended into a three-dimensional supramolecular network structure through hydrogen bonds and π-π interactions. CCDC: 979616, 1; 1011701, 2.
2015, (1): 191-197
doi: 10.11862/CJIC.2015.021
Abstract:
The CeO2/γ-Al2O3 supports were prepared and pretreated in different atmospheres to adjust the valence state of surface Ce element, then Cu(CH3COO)2 was impregnated as the precursor to prepare CuCeAl samples. XRD and H2-TPR results indicate that the CeO2/γ-Al2O3 support pretreated by reducing atmosphere has more active oxygen atoms, consequently has more dispersed Cu2+/Cu+ species on the surface. The "NO+CO" reaction tests reveal that the dispersed Cu2+/Cu+ are the active species for NO conversion, while crystalline Cu0 promotes the N2 selectivity at low temperatures. Hence, the catalysts containing both dispersed Cu2+/Cu+ and a few crystalline Cu0 have the optimal catalytic efficiency.
The CeO2/γ-Al2O3 supports were prepared and pretreated in different atmospheres to adjust the valence state of surface Ce element, then Cu(CH3COO)2 was impregnated as the precursor to prepare CuCeAl samples. XRD and H2-TPR results indicate that the CeO2/γ-Al2O3 support pretreated by reducing atmosphere has more active oxygen atoms, consequently has more dispersed Cu2+/Cu+ species on the surface. The "NO+CO" reaction tests reveal that the dispersed Cu2+/Cu+ are the active species for NO conversion, while crystalline Cu0 promotes the N2 selectivity at low temperatures. Hence, the catalysts containing both dispersed Cu2+/Cu+ and a few crystalline Cu0 have the optimal catalytic efficiency.
2015, (1): 198-204
doi: 10.11862/CJIC.2015.038
Abstract:
Via thermal reactions of the substituted tetramethylcyclopentadienes [C5Me4HR] [R=4-BrPh (1), (MeC5H3N)CH2 (2)] with Mo(CO)6, Ru3(CO)12 and Fe(CO)5, respectively in refluxing xylene, the responding dinuclear metal carbonyl complexes trans-[η5-C5Me4R]2Mo2(CO)6 (3, 4), trans-[(η5-C5Me4R)Ru(CO)(μ-CO)]2 (5, 6), and trans-[η5-(C5Me4R)Fe(CO)(μ-CO)]2 (7, 8) have been obtained. These complexes have been characterized by elemental analysis, IR, and 1H NMR spectra. The crystal structures of 3, 5, 6 and 8 have been determined by X-ray crystallography. CCDC: 934733, 3; 944267, 5; 926404, 6; 926405, 8.
Via thermal reactions of the substituted tetramethylcyclopentadienes [C5Me4HR] [R=4-BrPh (1), (MeC5H3N)CH2 (2)] with Mo(CO)6, Ru3(CO)12 and Fe(CO)5, respectively in refluxing xylene, the responding dinuclear metal carbonyl complexes trans-[η5-C5Me4R]2Mo2(CO)6 (3, 4), trans-[(η5-C5Me4R)Ru(CO)(μ-CO)]2 (5, 6), and trans-[η5-(C5Me4R)Fe(CO)(μ-CO)]2 (7, 8) have been obtained. These complexes have been characterized by elemental analysis, IR, and 1H NMR spectra. The crystal structures of 3, 5, 6 and 8 have been determined by X-ray crystallography. CCDC: 934733, 3; 944267, 5; 926404, 6; 926405, 8.
2015, (1): 205-212
doi: 10.11862/CJIC.2015.007
Abstract:
Two manganese complexes, [Mn2L2(μ-CH3OH)2(CH3OH)2] (1) and {[MnL(μ-CH3OH)]·CH3OH·CHCl3}n (2) (H2L=N-(1-phenyl-3-benzyl-4-propylene-5-pyrazolone)-isonicotinic hydrazide) were synthesized and structurally characterized by elemental analyses, IR spectra, UV-Vis spectra, thermogravimetric analyses and single crystal X-ray diffraction. The results show that the pHvalue of the reaction system has significant effect on the coordination mode of the ligand, which results in a dinuclear structure of 1 and a 2D network of 2. The thermal gravimetric analyses show that 1 is more stable than 2. CCDC: 997907, 1; 997908, 2.
Two manganese complexes, [Mn2L2(μ-CH3OH)2(CH3OH)2] (1) and {[MnL(μ-CH3OH)]·CH3OH·CHCl3}n (2) (H2L=N-(1-phenyl-3-benzyl-4-propylene-5-pyrazolone)-isonicotinic hydrazide) were synthesized and structurally characterized by elemental analyses, IR spectra, UV-Vis spectra, thermogravimetric analyses and single crystal X-ray diffraction. The results show that the pHvalue of the reaction system has significant effect on the coordination mode of the ligand, which results in a dinuclear structure of 1 and a 2D network of 2. The thermal gravimetric analyses show that 1 is more stable than 2. CCDC: 997907, 1; 997908, 2.
