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2015 Volume 31 Issue 6
2015, (6): 1071-1075
doi: 10.11862/CJIC.2015.173
Abstract:
Rose-like cobalt hydroxide [β-Co(OH)2] microcrystals were synthesized by a facile route without any surfactants. The rose-like β-Co(OH)2 microcrystals, 3~5 μm in width and 2~3 μm in thickness, are composed of nanosheets with an average thickness of 15 nm. The water contact angle (CA) of the rose-like β-Co(OH)2 film is 158.5°±1.2° and the water droplet is firmly pinned on the surfaces without any movement at any tilted angles.
Rose-like cobalt hydroxide [β-Co(OH)2] microcrystals were synthesized by a facile route without any surfactants. The rose-like β-Co(OH)2 microcrystals, 3~5 μm in width and 2~3 μm in thickness, are composed of nanosheets with an average thickness of 15 nm. The water contact angle (CA) of the rose-like β-Co(OH)2 film is 158.5°±1.2° and the water droplet is firmly pinned on the surfaces without any movement at any tilted angles.
2015, (6): 1076-1084
doi: 10.11862/CJIC.2015.164
Abstract:
Two Hg(Ⅱ) (1) and Zn(Ⅱ) (2) complexes with general formulation M(DMP)Cl2 where DMP=1,3-dimorpholinopropane were synthesized and structurally characterized by physicochemical methods and single crystal X-ray diffraction. An X-ray structural analysis shows that in both complexes Hg and Zn are coordinated by two nitrogen and two chlorine atoms in a form of distorted tetrahedron. The ligand and related complexes have antibacterial activity against three Gram-positive bacteria (S. epidermidis ATCC25923, E. faecalis ATCC23212 and S. epidermidis ATCC34384), and also against the three Gram-negative bacteria (E. coli ATCC25922, P. aeruginosa ATCC27853 and K. pneumonia ATCC70063). The results revealed that in some cases the antibacterial activity of Hg(Ⅱ) complex exceeded the one of sulfisoxazole used as a standard.
Two Hg(Ⅱ) (1) and Zn(Ⅱ) (2) complexes with general formulation M(DMP)Cl2 where DMP=1,3-dimorpholinopropane were synthesized and structurally characterized by physicochemical methods and single crystal X-ray diffraction. An X-ray structural analysis shows that in both complexes Hg and Zn are coordinated by two nitrogen and two chlorine atoms in a form of distorted tetrahedron. The ligand and related complexes have antibacterial activity against three Gram-positive bacteria (S. epidermidis ATCC25923, E. faecalis ATCC23212 and S. epidermidis ATCC34384), and also against the three Gram-negative bacteria (E. coli ATCC25922, P. aeruginosa ATCC27853 and K. pneumonia ATCC70063). The results revealed that in some cases the antibacterial activity of Hg(Ⅱ) complex exceeded the one of sulfisoxazole used as a standard.
2015, (6): 1085-1090
doi: 10.11862/CJIC.2015.178
Abstract:
By supported platinum complex to the graphite oxide carrier modified by diphenylphosphine ligands, a GO-P-Pt catalyst was synthesized. The GO-P-Pt catalyst was characterized by means of elemental analysis, FT-IRand XRD, and tested for the hydrosilylation of olefin with triethoxysilane. The catalytic results shows that GO-P-Pt catalyst possessed a high catalytic activity, and 94.6% conversion of 1-octene and 99.4% selectivity of β-adduct in yield were obtained at 100 ℃ after 180 min. And the selectivity of β-adduct was lower when the aromatic olefins were used as reaction substrates. Additionally, GO-P-Pt catalyst can be recycled four times without significant loss of catalytic activity and selectivity.
By supported platinum complex to the graphite oxide carrier modified by diphenylphosphine ligands, a GO-P-Pt catalyst was synthesized. The GO-P-Pt catalyst was characterized by means of elemental analysis, FT-IRand XRD, and tested for the hydrosilylation of olefin with triethoxysilane. The catalytic results shows that GO-P-Pt catalyst possessed a high catalytic activity, and 94.6% conversion of 1-octene and 99.4% selectivity of β-adduct in yield were obtained at 100 ℃ after 180 min. And the selectivity of β-adduct was lower when the aromatic olefins were used as reaction substrates. Additionally, GO-P-Pt catalyst can be recycled four times without significant loss of catalytic activity and selectivity.
2015, (6): 1091-1098
doi: 10.11862/CJIC.2015.155
Abstract:
Hydrothermally synthesized TiO2 nanorod arrays on FTO glass substrates were functionalized with uniform Bi2S3 quantum dots by CBD method combined with self-assembled monolayers(SAMs). The surface morphology, structure, optical and photoelectrochemical behaviors of the TiO2/Bi2S3 nanorod arrays are considered. The results that uniform Bi2S3 thin films were deposited on the surface of TiO2 nanorods modified by APTS SAMs. The key of the technology is that the APTS SAM possessing -NH2 functional groups can be employed to control nucleation. Moreover, the deposition time of Bi2S3 thin film plays a key role in the visible light absorption as well as photoelectric response of TiO2/Bi2S3 nanorod arrays. It reveals that, with the increase of the deposition time, the Jsc of composite thin film first increased and then decreased, and a Jsc maximum value of 0.13 mA·cm-2 reached at 20 min deposition of Bi2S3. The increase of Jsc for the initial deposition time could be interpreted as the result of enhanced absorption in the visible light range. Further increase the deposition time resulted in an obvious decrease in Jsc. This phenomenon might be attributed to Bi2S3 overloading on the surface of TiO2 resulted in aggregations and conglomerations, leading to more surface defects and recombination of photoexcited carrier.
Hydrothermally synthesized TiO2 nanorod arrays on FTO glass substrates were functionalized with uniform Bi2S3 quantum dots by CBD method combined with self-assembled monolayers(SAMs). The surface morphology, structure, optical and photoelectrochemical behaviors of the TiO2/Bi2S3 nanorod arrays are considered. The results that uniform Bi2S3 thin films were deposited on the surface of TiO2 nanorods modified by APTS SAMs. The key of the technology is that the APTS SAM possessing -NH2 functional groups can be employed to control nucleation. Moreover, the deposition time of Bi2S3 thin film plays a key role in the visible light absorption as well as photoelectric response of TiO2/Bi2S3 nanorod arrays. It reveals that, with the increase of the deposition time, the Jsc of composite thin film first increased and then decreased, and a Jsc maximum value of 0.13 mA·cm-2 reached at 20 min deposition of Bi2S3. The increase of Jsc for the initial deposition time could be interpreted as the result of enhanced absorption in the visible light range. Further increase the deposition time resulted in an obvious decrease in Jsc. This phenomenon might be attributed to Bi2S3 overloading on the surface of TiO2 resulted in aggregations and conglomerations, leading to more surface defects and recombination of photoexcited carrier.
2015, (6): 1099-1104
doi: 10.11862/CJIC.2015.165
Abstract:
The all-nanoparticle TiO2 films were directly prepared on the flexible transparent conductive oxide substrates by the layer-by-layer (LBL) self assembly method through the crystallized TiO2. During the preparation, the polyelectrolytes were replaced and the calcination is avoided. The TiO2 used in the self assembling process included an anatase TiO2 sol and the Degussa P25. The microstructure of the self assembly films was controlled through the ultrafine TiO2 crystallites of the sol, which could improve the uniformity and density of the films. The TiO2 film was introduced to be the working electrode in a three-electrode photoelectrochemical bulk cell, and the one with the high uniformity and density showed a good photoelectrochemical property. The photocurrent responses obtained from the TiO2 electrodes prepared with the TiO2 sol were about 25% higher than that of the one prepared without the sol.
The all-nanoparticle TiO2 films were directly prepared on the flexible transparent conductive oxide substrates by the layer-by-layer (LBL) self assembly method through the crystallized TiO2. During the preparation, the polyelectrolytes were replaced and the calcination is avoided. The TiO2 used in the self assembling process included an anatase TiO2 sol and the Degussa P25. The microstructure of the self assembly films was controlled through the ultrafine TiO2 crystallites of the sol, which could improve the uniformity and density of the films. The TiO2 film was introduced to be the working electrode in a three-electrode photoelectrochemical bulk cell, and the one with the high uniformity and density showed a good photoelectrochemical property. The photocurrent responses obtained from the TiO2 electrodes prepared with the TiO2 sol were about 25% higher than that of the one prepared without the sol.
2015, (6): 1105-1111
doi: 10.11862/CJIC.2015.152
Abstract:
Zirconia functionalized activated carbon fiber (ACF-Zr) adsorbent was successfully prepared using the post-grafting method and its adsorptions for fluoride ion (F-) uptake were investigated in details. Characterized results demonstrated that zirconia was highly dispersed on the surface of active carbon fiber. Adsorption experiment indicated ACF-Zr has high removal efficiency of F-, because of ion exchange andelectrostatic interaction. The adsorption isotherm could be well described by the Langmuir adsorption model and adsorption kinetics on ACF-Zr followed by pseudo-second-order kinetics. The adsorption capacity decreased with the increase of solution pHvalue. Nearly no influence was observed by solution coexisting ions Cl-, NO3- and SO42-.
Zirconia functionalized activated carbon fiber (ACF-Zr) adsorbent was successfully prepared using the post-grafting method and its adsorptions for fluoride ion (F-) uptake were investigated in details. Characterized results demonstrated that zirconia was highly dispersed on the surface of active carbon fiber. Adsorption experiment indicated ACF-Zr has high removal efficiency of F-, because of ion exchange andelectrostatic interaction. The adsorption isotherm could be well described by the Langmuir adsorption model and adsorption kinetics on ACF-Zr followed by pseudo-second-order kinetics. The adsorption capacity decreased with the increase of solution pHvalue. Nearly no influence was observed by solution coexisting ions Cl-, NO3- and SO42-.
2015, (6): 1112-1118
doi: 10.11862/CJIC.2015.067
Abstract:
Two tri(n-butyl)tin carboxylates (n-Bu)3SnO2CR(H2O) (R: C(OH)Ph2 (1), C5NH3Cl (2)) were synthesized by the reactions of bis[tri(n-butyl)tin] oxide with benzilic acid and 2-chloronicotinic acid under microwave irradia-tion, respectively. Their structures were characterized by IR, 1H and 13C NMR, elemental analysis and X-ray single crystal diffraction. Both of the complexes belong to orthorhombic system, but their space groups are different. One is Pbca and the other is P212121. For each of them, the central tin atom is aberrant trigonal bipyramid with five-coordination. In their crystal structures, there are multi-hydrogen bonds, resulting in the formation of a 2D structure of 1 and a 3D supermolecular network of 2. The preliminary tests showed that both of which displayed strong in vitro anti-tumor activity against five human tumor cell lines, Colo205, HepG2, MCF-7, Hela and NCI-H460, and especially for the later three, the complexes were much stronger than carboplatin, but the activity order was 1>2.
Two tri(n-butyl)tin carboxylates (n-Bu)3SnO2CR(H2O) (R: C(OH)Ph2 (1), C5NH3Cl (2)) were synthesized by the reactions of bis[tri(n-butyl)tin] oxide with benzilic acid and 2-chloronicotinic acid under microwave irradia-tion, respectively. Their structures were characterized by IR, 1H and 13C NMR, elemental analysis and X-ray single crystal diffraction. Both of the complexes belong to orthorhombic system, but their space groups are different. One is Pbca and the other is P212121. For each of them, the central tin atom is aberrant trigonal bipyramid with five-coordination. In their crystal structures, there are multi-hydrogen bonds, resulting in the formation of a 2D structure of 1 and a 3D supermolecular network of 2. The preliminary tests showed that both of which displayed strong in vitro anti-tumor activity against five human tumor cell lines, Colo205, HepG2, MCF-7, Hela and NCI-H460, and especially for the later three, the complexes were much stronger than carboplatin, but the activity order was 1>2.
2015, (6): 1119-1124
doi: 10.11862/CJIC.2015.179
Abstract:
Ni-doped pyrite FeS2 were synthesized through a solvothermal method using FeSO4·7H2O, Na2S2O3·5H2O and NiSO4·6H2O as raw materials. The products were characterized by X-ray diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), field emission scanning electron microscope (FE-SEM), UV-Vis diffuse reflectance spectra (DRS) and Raman spectroscopy. The results showed that appropriate amount of Ni doping facilitated the transformation of the marcasite to pyrite. After Ni2+ doping, the visible-light-driven photocatalytic performance of the FeS2 was greatly enhanced. Methylene blue (MB) was decomposed 62.8% within 210 min using Ni0.125Fe0.875S2 as photocatalyst, which was 26.2% higher than that of the pristine FeS2.
Ni-doped pyrite FeS2 were synthesized through a solvothermal method using FeSO4·7H2O, Na2S2O3·5H2O and NiSO4·6H2O as raw materials. The products were characterized by X-ray diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), field emission scanning electron microscope (FE-SEM), UV-Vis diffuse reflectance spectra (DRS) and Raman spectroscopy. The results showed that appropriate amount of Ni doping facilitated the transformation of the marcasite to pyrite. After Ni2+ doping, the visible-light-driven photocatalytic performance of the FeS2 was greatly enhanced. Methylene blue (MB) was decomposed 62.8% within 210 min using Ni0.125Fe0.875S2 as photocatalyst, which was 26.2% higher than that of the pristine FeS2.
2015, (6): 1125-1130
doi: 10.11862/CJIC.2015.154
Abstract:
Monodisperse core-shell structured Gd2(CO3)3:Eu@SiO2@APTES microsphere was successfully prepared via the stöber method by coating a layer of silica on the surface of Gd2(CO3)3:Eu microspheres which derived from a simple urea assisted coprecipitation method. Their structural, optical and magnetic properties were investigated using SEM, TEM, XRD, FTIR, PL, and MPMS. The results indicated that the microspheres with general 30 nm shell thickness and 150 nm core size has spherical morphology with smooth surface and narrow size distribution. The paramagnetic property of the synthesized Gd2(CO3)3:Eu@SiO2@APTES microspheres were confirmed with its linear hysteresis plot (M-H). The synthesized microspheres can enter into living cancer cells and emit orange-red luminescence light due to the 5D0→7F2 transition of the Eu3+ ions, and Gd2(CO3)3:Eu@SiO2@APTES microspheres showed no cell cytotoxicity or adverse affect on kidney cell growth under high dose up to 400 μg·mL-1. Therefore, Gd2(CO3)3:Eu@SiO2@APTES microspheres provides the dual modality of optical and magnetic resonance imaging.
Monodisperse core-shell structured Gd2(CO3)3:Eu@SiO2@APTES microsphere was successfully prepared via the stöber method by coating a layer of silica on the surface of Gd2(CO3)3:Eu microspheres which derived from a simple urea assisted coprecipitation method. Their structural, optical and magnetic properties were investigated using SEM, TEM, XRD, FTIR, PL, and MPMS. The results indicated that the microspheres with general 30 nm shell thickness and 150 nm core size has spherical morphology with smooth surface and narrow size distribution. The paramagnetic property of the synthesized Gd2(CO3)3:Eu@SiO2@APTES microspheres were confirmed with its linear hysteresis plot (M-H). The synthesized microspheres can enter into living cancer cells and emit orange-red luminescence light due to the 5D0→7F2 transition of the Eu3+ ions, and Gd2(CO3)3:Eu@SiO2@APTES microspheres showed no cell cytotoxicity or adverse affect on kidney cell growth under high dose up to 400 μg·mL-1. Therefore, Gd2(CO3)3:Eu@SiO2@APTES microspheres provides the dual modality of optical and magnetic resonance imaging.
2015, (6): 1131-1138
doi: 10.11862/CJIC.2015.151
Abstract:
Asymmetrical ruthenium complex bearing phosphonic acid was prepared under the microwave irradiation and fully characterized by 1H NMR, ESI-MS and thermo gravimetric(TG) analysis. For the Ru complex, the phosphonic groups were selectively attached to the ITO through covalent interaction, resulting in the hydrophilic surface due to the appearance of the exposed other phosphonic-acid groups on the top. The Layer by layer(LBL) growth of molecular units was used to fabricate redox-active films of Ru complex, which was followed by the formation of Zr4+-phosphonate layer. The buildup of the films was followed by monitoring cyclic voltammetry(CV) and ultraviolet-visible absorption spectrometry(UV-Vis) measurements. The results showed the electrode modified by multilayered film displayed reversible redox processes, and the Ru(Ⅱ/Ⅲ) oxidative peak was observed at +0.53 V. The plots of surface coverage versus number of layers show a linear relationship, which means a uniform layer structure is formed during the LBL process. UV-Vis spectra shows the prepared Ru film have strong absorptions between 300 nm and 600 nm. These findings show the Ru complex has good photoelectric properties.
Asymmetrical ruthenium complex bearing phosphonic acid was prepared under the microwave irradiation and fully characterized by 1H NMR, ESI-MS and thermo gravimetric(TG) analysis. For the Ru complex, the phosphonic groups were selectively attached to the ITO through covalent interaction, resulting in the hydrophilic surface due to the appearance of the exposed other phosphonic-acid groups on the top. The Layer by layer(LBL) growth of molecular units was used to fabricate redox-active films of Ru complex, which was followed by the formation of Zr4+-phosphonate layer. The buildup of the films was followed by monitoring cyclic voltammetry(CV) and ultraviolet-visible absorption spectrometry(UV-Vis) measurements. The results showed the electrode modified by multilayered film displayed reversible redox processes, and the Ru(Ⅱ/Ⅲ) oxidative peak was observed at +0.53 V. The plots of surface coverage versus number of layers show a linear relationship, which means a uniform layer structure is formed during the LBL process. UV-Vis spectra shows the prepared Ru film have strong absorptions between 300 nm and 600 nm. These findings show the Ru complex has good photoelectric properties.
2015, (6): 1139-1144
doi: 10.11862/CJIC.2015.153
Abstract:
LaBiMn2O6(LBM) cathode for IT-SOFCs (intermediate temperature solid oxide fuel cells) has been prepared by solid state reaction and studied by XRDand EISspectrum,respectively. The results show that LBM has no reaction with Ce0.7Bi0.3O1.85(CBO) electrolyte at 1000 ℃ for 12 h. AC impedance spectroscopy and DC polarization measurements are used to study the electrode performances. The polarization resistance decreases with temperature and reaches 0.71 Ω·cm2 at 700 ℃ in air. Oxygen partial pressure study indicated that charge transfer process is the major rate limiting step for LaBiMn2O6 cathode from 600 to 700 ℃. The LaBiMn2O6 cathode exhibits the lowest overpotential of 85 mVunder current density of 216 mA·cm-2 at 700 ℃ in air. This preliminary work showes that LaBiMn2O6 material may be potential cathodes for IT-SOFCs.
LaBiMn2O6(LBM) cathode for IT-SOFCs (intermediate temperature solid oxide fuel cells) has been prepared by solid state reaction and studied by XRDand EISspectrum,respectively. The results show that LBM has no reaction with Ce0.7Bi0.3O1.85(CBO) electrolyte at 1000 ℃ for 12 h. AC impedance spectroscopy and DC polarization measurements are used to study the electrode performances. The polarization resistance decreases with temperature and reaches 0.71 Ω·cm2 at 700 ℃ in air. Oxygen partial pressure study indicated that charge transfer process is the major rate limiting step for LaBiMn2O6 cathode from 600 to 700 ℃. The LaBiMn2O6 cathode exhibits the lowest overpotential of 85 mVunder current density of 216 mA·cm-2 at 700 ℃ in air. This preliminary work showes that LaBiMn2O6 material may be potential cathodes for IT-SOFCs.
2015, (6): 1145-1152
doi: 10.11862/CJIC.2015.171
Abstract:
Multi-walled carbon nano-tube (MWCNT)-supported palladium nano-catalysts (Pd-EDTA/MWCNT, Pd-Gly/MWCNTand Pd-Ls/MWCNT) were prepared by supporting Pd nano-particles on MWCNT. The Pd nano-particles were obtained from reduction of Pd2+ with NaBH4 as the reducing agent in the presence of EDTA, Glycine(Gly), and sodium lignin sulfonate(Ls) as the ligand, separately. The catalysts were characterized by SEM, TEMand XRD. The electrochemical activity of the catalysts towards ethanol oxidation in alkaline media was examined by cyclic voltammetry (CV) and chronoamperometry (CA). The characterization results show that the Pd-EDTA/MWCNTcatalyst exhibits a smaller particle size and a better dispersity of Pd nanoaprticles compared to the Pd-Gly/MWCNTand Pd-Ls/MWCNTcatalysts. As for the ethanol oxidation in alkaline media, the Pd-EDTA/MWCNTcatalyst exhibits a lower onset potential, a higher current density, a smaller electron transfer resistance, a larger reaction rate, and more stable oxidation current, in comparison with the other two catalysts.
Multi-walled carbon nano-tube (MWCNT)-supported palladium nano-catalysts (Pd-EDTA/MWCNT, Pd-Gly/MWCNTand Pd-Ls/MWCNT) were prepared by supporting Pd nano-particles on MWCNT. The Pd nano-particles were obtained from reduction of Pd2+ with NaBH4 as the reducing agent in the presence of EDTA, Glycine(Gly), and sodium lignin sulfonate(Ls) as the ligand, separately. The catalysts were characterized by SEM, TEMand XRD. The electrochemical activity of the catalysts towards ethanol oxidation in alkaline media was examined by cyclic voltammetry (CV) and chronoamperometry (CA). The characterization results show that the Pd-EDTA/MWCNTcatalyst exhibits a smaller particle size and a better dispersity of Pd nanoaprticles compared to the Pd-Gly/MWCNTand Pd-Ls/MWCNTcatalysts. As for the ethanol oxidation in alkaline media, the Pd-EDTA/MWCNTcatalyst exhibits a lower onset potential, a higher current density, a smaller electron transfer resistance, a larger reaction rate, and more stable oxidation current, in comparison with the other two catalysts.
2015, (6): 1153-1158
doi: 10.11862/CJIC.2015.167
Abstract:
Using FeSO4·7H2O, NH4H2PO4, H2O2, Li2CO3, C6H12O6 and GO as raw materials, LiFePO4/C/G-2 composite cathode material prepared by mixing FePO4·2H2O, Li2CO3 and GO and LiFePO4/C/G-1 by mixing FePO4·2H2O/GO and Li2CO3 were compared. Crystal structure, morphology and electrochemical performance of the two samples were investigated by X-ray diffraction(XRD), scanning electron microscope(SEM), Transmission Electron Microscope (TEM),electrochemical impedance spectroscopy (EIS) test and charge-discharge test. LiFePO4/C/G-1 showed better electrochemical performances compared to LiFePO4/C/G-2. When the chemical synthesis method product (LiFePO4/C/G-1) was charged-discharged in 2.5~4.1 V, the initial discharge capacity was 158.15 and 150.5 mAh·g-1 at 0.1Cand 1Crate, respectively. After cycling for 500 times at 1Crate, the retention of discharge capacity was 98.3%.
Using FeSO4·7H2O, NH4H2PO4, H2O2, Li2CO3, C6H12O6 and GO as raw materials, LiFePO4/C/G-2 composite cathode material prepared by mixing FePO4·2H2O, Li2CO3 and GO and LiFePO4/C/G-1 by mixing FePO4·2H2O/GO and Li2CO3 were compared. Crystal structure, morphology and electrochemical performance of the two samples were investigated by X-ray diffraction(XRD), scanning electron microscope(SEM), Transmission Electron Microscope (TEM),electrochemical impedance spectroscopy (EIS) test and charge-discharge test. LiFePO4/C/G-1 showed better electrochemical performances compared to LiFePO4/C/G-2. When the chemical synthesis method product (LiFePO4/C/G-1) was charged-discharged in 2.5~4.1 V, the initial discharge capacity was 158.15 and 150.5 mAh·g-1 at 0.1Cand 1Crate, respectively. After cycling for 500 times at 1Crate, the retention of discharge capacity was 98.3%.
2015, (6): 1159-1164
doi: 10.11862/CJIC.2015.158
Abstract:
The graphite composite (G/C) anode was prepared by spray drying and high temperature sintering using natural spherical graphite as raw material and citric acid as carbon source. X-ray diffraction (XRD), scanning electron microscope (SEM) and high-resolution transmission electron microscope (HRTEM) were used to characterize crystal structure and morphology of samples. Galvanostatic charge-discharge tests and cyclic voltammentry (CV) were utilized to study the effect of heat treatment temperature on electrochemical performance of G/C anode. With typical voltage feature of graphite anode, G/C-2900 sample shows higher capacity than commercial graphite anode. The charge capacity of the G/C-2900 after the first activation is 423 mAh·g-1, and the 100th charge capacity is 416 mAh·g-1 with capacity retention rate of 98%.
The graphite composite (G/C) anode was prepared by spray drying and high temperature sintering using natural spherical graphite as raw material and citric acid as carbon source. X-ray diffraction (XRD), scanning electron microscope (SEM) and high-resolution transmission electron microscope (HRTEM) were used to characterize crystal structure and morphology of samples. Galvanostatic charge-discharge tests and cyclic voltammentry (CV) were utilized to study the effect of heat treatment temperature on electrochemical performance of G/C anode. With typical voltage feature of graphite anode, G/C-2900 sample shows higher capacity than commercial graphite anode. The charge capacity of the G/C-2900 after the first activation is 423 mAh·g-1, and the 100th charge capacity is 416 mAh·g-1 with capacity retention rate of 98%.
2015, (6): 1165-1170
doi: 10.11862/CJIC.2015.150
Abstract:
Fe3O4 nanoparticles were prepared by coprecipitation, which were modified by polyethyleneimine(PEI). Au nanoparticles were composited in situ, and then the Fe3O4/PEI/Au microspheres were obtained. CdSe/CdS QDs was modified with thioglycolic acid, and connected to magnetic nanoparticles. Fe3O4/PEI/Au@CdSe/CdS multifunctional composite microspheres were prepared successfully. Fourier transform infrared spectroscopy (FTIR), Fluorescence spectrophotometer, Fluorescence microscopy, X-ray diffraction (XRD), Transmission electron microscopy (TEM) and Vibrating sample magnetometer (VSM) are used for characterizing. The results shows that: the multifunctional composite microspheres with the size about 40 nm were superparamagnetic and remanence; the coercivity is near zero; the saturated magnetization is 28.83 A·m2·kg-1. What's more, the microspheres have both superior fluorescence and gold nanoparticles' properties.
Fe3O4 nanoparticles were prepared by coprecipitation, which were modified by polyethyleneimine(PEI). Au nanoparticles were composited in situ, and then the Fe3O4/PEI/Au microspheres were obtained. CdSe/CdS QDs was modified with thioglycolic acid, and connected to magnetic nanoparticles. Fe3O4/PEI/Au@CdSe/CdS multifunctional composite microspheres were prepared successfully. Fourier transform infrared spectroscopy (FTIR), Fluorescence spectrophotometer, Fluorescence microscopy, X-ray diffraction (XRD), Transmission electron microscopy (TEM) and Vibrating sample magnetometer (VSM) are used for characterizing. The results shows that: the multifunctional composite microspheres with the size about 40 nm were superparamagnetic and remanence; the coercivity is near zero; the saturated magnetization is 28.83 A·m2·kg-1. What's more, the microspheres have both superior fluorescence and gold nanoparticles' properties.
2015, (6): 1171-1176
doi: 10.11862/CJIC.2015.159
Abstract:
α-Fe2O3 nanoparticles with uniform size were synthesized via a complex-precursor strategy. First, iron ion-based coordination polymer was synthesized via a solvothermal method by using p-benzene-dicarboxylic acid (p-H2bdc) as ligand. Second, α-Fe2O3 nanoparticles with uniform size were prepared via a solid state pyrolysis procedure. The synthesized coordination polymer and Fe2O3 product were characterized by XRD, FT-IR, SEM and TEM respectively. When used as anode material for lithium-ion batteries, the Fe2O3 electrode can deliever a stable reversible capacity of 530 mAh·g-1 after 50 charge-discharge cycles at a current density of 0.1 A·g-1, which showed a higher specific capacity and superior cycle stability.
α-Fe2O3 nanoparticles with uniform size were synthesized via a complex-precursor strategy. First, iron ion-based coordination polymer was synthesized via a solvothermal method by using p-benzene-dicarboxylic acid (p-H2bdc) as ligand. Second, α-Fe2O3 nanoparticles with uniform size were prepared via a solid state pyrolysis procedure. The synthesized coordination polymer and Fe2O3 product were characterized by XRD, FT-IR, SEM and TEM respectively. When used as anode material for lithium-ion batteries, the Fe2O3 electrode can deliever a stable reversible capacity of 530 mAh·g-1 after 50 charge-discharge cycles at a current density of 0.1 A·g-1, which showed a higher specific capacity and superior cycle stability.
2015, (6): 1177-1184
doi: 10.11862/CJIC.2015.144
Abstract:
Hydrothermal reactions of CdSO4 and NaN3 with 4-cyanopyridine or 3-cyanopyridine yielded two three-dimensional layered-pillared inorganic-organic hybrid materials based on mixed ligands of sulfate and in situ synthesized 5-(4-pyridyl)tetrazolate(4-ptz-) or 5-(3-pyridyl)tetrazolate(3-ptz-), respectively, namely, [Cd2(H2O)(OH)(SO4)(4-ptz)]n (1) and [Cd2(OH)(SO4)(3-ptz)]n (2), which have been structurally characterized by elemental analysis (EA), infrared spectroscopy (IR), thermogravimetric analysis (TGA), single-crystal and powder X-ray diffraction. In 1 and 2, each Cd(Ⅱ) ion is six-coordinated with a distorted octahedral coordination geometry, which are connected through SO42- and OH-, leading to an infinite two-dimensional cation layer structure of [Cd2(H2O)(OH)(SO4)]nn+(1) or [Cd2(OH)(SO4)]nn+(2). These adjacent two-dimensional cation layers are further linked by 4-ptz- (1) or 3-ptz- (2) pillared ligands to form infinite three-dimensional layered-pillared inorganic-organic hybrid frameworks architecture of 1 and 2, respectively. In addition, the results of photoluminescent measurements in the solid state at room temperature indicate that 1 and 2 all exhibit intense fluorescent emissions at λmax=481 nm and 489 nm when excited at 350 nm, respectively.
Hydrothermal reactions of CdSO4 and NaN3 with 4-cyanopyridine or 3-cyanopyridine yielded two three-dimensional layered-pillared inorganic-organic hybrid materials based on mixed ligands of sulfate and in situ synthesized 5-(4-pyridyl)tetrazolate(4-ptz-) or 5-(3-pyridyl)tetrazolate(3-ptz-), respectively, namely, [Cd2(H2O)(OH)(SO4)(4-ptz)]n (1) and [Cd2(OH)(SO4)(3-ptz)]n (2), which have been structurally characterized by elemental analysis (EA), infrared spectroscopy (IR), thermogravimetric analysis (TGA), single-crystal and powder X-ray diffraction. In 1 and 2, each Cd(Ⅱ) ion is six-coordinated with a distorted octahedral coordination geometry, which are connected through SO42- and OH-, leading to an infinite two-dimensional cation layer structure of [Cd2(H2O)(OH)(SO4)]nn+(1) or [Cd2(OH)(SO4)]nn+(2). These adjacent two-dimensional cation layers are further linked by 4-ptz- (1) or 3-ptz- (2) pillared ligands to form infinite three-dimensional layered-pillared inorganic-organic hybrid frameworks architecture of 1 and 2, respectively. In addition, the results of photoluminescent measurements in the solid state at room temperature indicate that 1 and 2 all exhibit intense fluorescent emissions at λmax=481 nm and 489 nm when excited at 350 nm, respectively.
2015, (6): 1185-1193
doi: 10.11862/CJIC.2015.160
Abstract:
Polyethyleneimine modified graphite oxide (PEI-GO) were prepared by grafting polyethyleneimine (PEI) on the surface of graphite after oxidation and esterification. The structure and surface properties of synthesized composites were characterized by Fourier-transformed infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscope (TEM), Rraman spectroscopy (RS) and X-ray photoelectron spectroscopy (XPS) analysis, and its adsorption and desorption capability for aqueous Cr(Ⅵ) was also conducted. Characterization results indicated that polyethyleneimine has been successfully grafted on the surface of graphite oxide, and the content of the amino groups of PEI-GOis 4.36 mmol·g-1. PEI-GOexhibits high adsorption capacity for aqueous Cr(Ⅵ). Adsorption isotherm of Cr(Ⅵ) onto PEI-GO could be described better by Freundlich model than Langmuir model. The pseudo-second-order kinetics followed the adsorption data very well. Adsorption amount of Cr(Ⅵ) onto PEI-GOdecreased with increasing pH. The presence of anions in solution resulted in the suppressed Cr(Ⅵ) adsorption, and the effect of different anions was in the order of PO43- > SO42- > NO3- > Cl-. XPSanalysis indicates that adsorption coupled chemical reduction mechanism contributes to enhanced Cr(Ⅵ) adsorption on PEI-GO. After four successive desorption-regeneration cycles, PEI-GO still possesses high adsorption capacity for Cr(Ⅵ), which indicates that the adsorbent has good regeneration capability and can be used repeatedly.
Polyethyleneimine modified graphite oxide (PEI-GO) were prepared by grafting polyethyleneimine (PEI) on the surface of graphite after oxidation and esterification. The structure and surface properties of synthesized composites were characterized by Fourier-transformed infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscope (TEM), Rraman spectroscopy (RS) and X-ray photoelectron spectroscopy (XPS) analysis, and its adsorption and desorption capability for aqueous Cr(Ⅵ) was also conducted. Characterization results indicated that polyethyleneimine has been successfully grafted on the surface of graphite oxide, and the content of the amino groups of PEI-GOis 4.36 mmol·g-1. PEI-GOexhibits high adsorption capacity for aqueous Cr(Ⅵ). Adsorption isotherm of Cr(Ⅵ) onto PEI-GO could be described better by Freundlich model than Langmuir model. The pseudo-second-order kinetics followed the adsorption data very well. Adsorption amount of Cr(Ⅵ) onto PEI-GOdecreased with increasing pH. The presence of anions in solution resulted in the suppressed Cr(Ⅵ) adsorption, and the effect of different anions was in the order of PO43- > SO42- > NO3- > Cl-. XPSanalysis indicates that adsorption coupled chemical reduction mechanism contributes to enhanced Cr(Ⅵ) adsorption on PEI-GO. After four successive desorption-regeneration cycles, PEI-GO still possesses high adsorption capacity for Cr(Ⅵ), which indicates that the adsorbent has good regeneration capability and can be used repeatedly.
2015, (6): 1194-1200
doi: 10.11862/CJIC.2015.157
Abstract:
The tetra(o-fluorobenzyl)tin (1) and the tribenzyltin ferrocenecarboxylate (2) have been synthesized. The crystal structures of the complexes were determined by X-ray diffraction. The crystal 1 belongs to tetragonal space group I41/a with a=1.96794(16) nm, b=1.96794(16) nm, c=0.59316(5) nm, V=2.2972(3) nm3, Z=4, Dc= 1.605 g·cm-3, μ(MoKα)=11.58 cm-1,F(000)=1112, R1=0.0208, wR2=0.0576. The crystal 2 belongs to monoclinic space group P21/n with a=1.59354(12) nm, b=1.00723(8) nm, c=1.70026(13) nm, β=91.001(10)°, V=2.7286(4) nm3, Z=4, Dc=1.521 g·cm-3, μ(MoKα)=14.74 cm-1, F(000)=1256, R1=0.0384, wR2=0.0952. The stabilities, some frontier molecular orbital energies and composition characteristics of some frontier molecular orbital of the complexes have been investigated by quantum chemistry calculation. Further more, thermal stability and anticancer activity of the complexes were tested.
The tetra(o-fluorobenzyl)tin (1) and the tribenzyltin ferrocenecarboxylate (2) have been synthesized. The crystal structures of the complexes were determined by X-ray diffraction. The crystal 1 belongs to tetragonal space group I41/a with a=1.96794(16) nm, b=1.96794(16) nm, c=0.59316(5) nm, V=2.2972(3) nm3, Z=4, Dc= 1.605 g·cm-3, μ(MoKα)=11.58 cm-1,F(000)=1112, R1=0.0208, wR2=0.0576. The crystal 2 belongs to monoclinic space group P21/n with a=1.59354(12) nm, b=1.00723(8) nm, c=1.70026(13) nm, β=91.001(10)°, V=2.7286(4) nm3, Z=4, Dc=1.521 g·cm-3, μ(MoKα)=14.74 cm-1, F(000)=1256, R1=0.0384, wR2=0.0952. The stabilities, some frontier molecular orbital energies and composition characteristics of some frontier molecular orbital of the complexes have been investigated by quantum chemistry calculation. Further more, thermal stability and anticancer activity of the complexes were tested.
2015, (6): 1201-1206
doi: 10.11862/CJIC.2015.136
Abstract:
The green-emitting Ca3Y2-x-ySi3O12:xTb3+, yCe3+ silicate phosphors were synthesized by a high temperature solid-state method. The principal crystalline of the samples is Ca3Y2Si3O12, which is belonging to the monoclinic system. All the phosphors can be effectively excited in the range of 300 nm to 450 nm, and emit green light. Excited by 370 nm, the emission peaks mainly locate at 490 nm (5D4→7F6) 544 nm(5D4→7F5), 585 nm(5D4→7F4) and 621 nm(5D4→7F3). The effect of sintering conditions, doping concentration and Ce3+ co-doping was studied on the luminescence properties of the phosphors. The sample twice sintered for 6 h at 1400 ℃ shows the best performance. The optimum doping content of Tb3+ is x(Tb3+)=20mol%. The emission intensity of the phosphors can be increased by the Ce3+ ion co-doping, and the test shows that the best doping amount is 4mol%. The result confirms the presence of Ce3+→Tb3+ energy transfer.
The green-emitting Ca3Y2-x-ySi3O12:xTb3+, yCe3+ silicate phosphors were synthesized by a high temperature solid-state method. The principal crystalline of the samples is Ca3Y2Si3O12, which is belonging to the monoclinic system. All the phosphors can be effectively excited in the range of 300 nm to 450 nm, and emit green light. Excited by 370 nm, the emission peaks mainly locate at 490 nm (5D4→7F6) 544 nm(5D4→7F5), 585 nm(5D4→7F4) and 621 nm(5D4→7F3). The effect of sintering conditions, doping concentration and Ce3+ co-doping was studied on the luminescence properties of the phosphors. The sample twice sintered for 6 h at 1400 ℃ shows the best performance. The optimum doping content of Tb3+ is x(Tb3+)=20mol%. The emission intensity of the phosphors can be increased by the Ce3+ ion co-doping, and the test shows that the best doping amount is 4mol%. The result confirms the presence of Ce3+→Tb3+ energy transfer.
2015, (6): 1207-1214
doi: 10.11862/CJIC.2015.172
Abstract:
Based on the versatile ligand 1H-3-(3-pyridyl)-5-(3'-pyridyl)-1,2,4-triazole (3,3'-Hbpt, (1), a coordination polymer, [Co(3,3'-Hbpt)2(H2O)4]·(ad)·6H2O (2), has been hydrothermally isolated (ad=adipate). The crystal structure of ligand has been investigated. Density functional theory (DFT) is employed to explicate the optimized geometry, preferred conformation and electronic properties of 3,3'-Hbpt ligand. Structural analysis reveals that compound 2 is a zero-dimensional mononuclear molecule, and the 3D supramolecular network is constructed through hydrogen-bonding interactions, in which the rectangular channels are filled by free adipate anions. Notably, the geometry and conformation of the ligand in compound 2 are corresponding with the calculated results. In addition, thermostability of compound 2 is investigated by TG.
Based on the versatile ligand 1H-3-(3-pyridyl)-5-(3'-pyridyl)-1,2,4-triazole (3,3'-Hbpt, (1), a coordination polymer, [Co(3,3'-Hbpt)2(H2O)4]·(ad)·6H2O (2), has been hydrothermally isolated (ad=adipate). The crystal structure of ligand has been investigated. Density functional theory (DFT) is employed to explicate the optimized geometry, preferred conformation and electronic properties of 3,3'-Hbpt ligand. Structural analysis reveals that compound 2 is a zero-dimensional mononuclear molecule, and the 3D supramolecular network is constructed through hydrogen-bonding interactions, in which the rectangular channels are filled by free adipate anions. Notably, the geometry and conformation of the ligand in compound 2 are corresponding with the calculated results. In addition, thermostability of compound 2 is investigated by TG.
2015, (6): 1215-1223
doi: 10.11862/CJIC.2015.145
Abstract:
The reaction of copper(Ⅱ) nitrate with flexible bis(1,2,4-triazol-1-yl)alkanes and rigid ligand 5-sulfoisophthalic acid monosodium salt (NaH2sip) affords three complexes [Cu0.5(btm)(H2O)](H2sip)·H2O}n (1, btm=bis(1,2,4-triazol-1-yl)methane), {[Cu(btp)2(H2sip)(H2O)](NO3)·4H2O}n (2, btp=1,3-bis(1,2,4-triazol-1-yl)propane), and {[Cu(btb)2(Hsip)]n (3, btb=1,4-bis(1,2,4-triazol-1-yl)butane). Compound 1 contains one-dimensional (1D) double-strained chains. Compound 2 contains two-dimensional (2D) rectangular networks with (4,4) topology, in which the 2D planar nanogrid networks stacked in a step stacking fashion.3 is also 2D layers, in which double-strained chains [Cu(btb)]n are connected into 2D layer architectures by the μ2-Hsip2- linkers. The three compounds also are characterized by Elemental analysis, EPR, and thermal stability.
The reaction of copper(Ⅱ) nitrate with flexible bis(1,2,4-triazol-1-yl)alkanes and rigid ligand 5-sulfoisophthalic acid monosodium salt (NaH2sip) affords three complexes [Cu0.5(btm)(H2O)](H2sip)·H2O}n (1, btm=bis(1,2,4-triazol-1-yl)methane), {[Cu(btp)2(H2sip)(H2O)](NO3)·4H2O}n (2, btp=1,3-bis(1,2,4-triazol-1-yl)propane), and {[Cu(btb)2(Hsip)]n (3, btb=1,4-bis(1,2,4-triazol-1-yl)butane). Compound 1 contains one-dimensional (1D) double-strained chains. Compound 2 contains two-dimensional (2D) rectangular networks with (4,4) topology, in which the 2D planar nanogrid networks stacked in a step stacking fashion.3 is also 2D layers, in which double-strained chains [Cu(btb)]n are connected into 2D layer architectures by the μ2-Hsip2- linkers. The three compounds also are characterized by Elemental analysis, EPR, and thermal stability.
2015, (6): 1224-1230
doi: 10.11862/CJIC.2015.156
Abstract:
Two silver(Ⅰ) complexes with heterocyclic thione, [AgBr(PPh3)2(BTZT)]2 (1) and [Ag2Cl2(PPh3)2(BTZT)2]·CH3OH (2) (PPh3=triphenylphosphine; BTZT=benzothiazoline-2-thione) have been synthesized and characterized by IR, single-crystal X-ray diffraction, fluorescence spectrum and 1H NMR spectroscopy. 1 and 2 are obtained by the reactions of AgX (X=Cl, Br) with PPh3 in the presence of 2-mercaptobenzothiazole (MBT) in mixed solvent (CH3OH/CH2Cl2). The MBTligand possesses chemically active groups (-N=C(-SH)), so MBTligand can transform into BTZTligand. Structure analysis shows that there exist two same molecular structures in complex 1, but they have different bond lengths and bond angles. Complex 2 consists of inversion symmetric dimers with a diamond-shaped Ag2Cl2 group at the center, and two adjacent [AgCl(PPh3)(BTZT)] units are bridged by two Cl atoms.
Two silver(Ⅰ) complexes with heterocyclic thione, [AgBr(PPh3)2(BTZT)]2 (1) and [Ag2Cl2(PPh3)2(BTZT)2]·CH3OH (2) (PPh3=triphenylphosphine; BTZT=benzothiazoline-2-thione) have been synthesized and characterized by IR, single-crystal X-ray diffraction, fluorescence spectrum and 1H NMR spectroscopy. 1 and 2 are obtained by the reactions of AgX (X=Cl, Br) with PPh3 in the presence of 2-mercaptobenzothiazole (MBT) in mixed solvent (CH3OH/CH2Cl2). The MBTligand possesses chemically active groups (-N=C(-SH)), so MBTligand can transform into BTZTligand. Structure analysis shows that there exist two same molecular structures in complex 1, but they have different bond lengths and bond angles. Complex 2 consists of inversion symmetric dimers with a diamond-shaped Ag2Cl2 group at the center, and two adjacent [AgCl(PPh3)(BTZT)] units are bridged by two Cl atoms.
2015, (6): 1231-1238
doi: 10.11862/CJIC.2015.132
Abstract:
Two Ni(Ⅱ)-organic frameworks, namely, {[Ni3(BPT)2(bpe)2(H2O)6]·2DMF·7H2O}n (1) and {[Ni3(BPT)2(bpea)2(H2O)6]·2DMF·5H2O}n (2) (H3BPT = biphenyl-3,4',5-tricarboxylic acid, bpe = 1,2-bis(4-pyridyl)ethylene, bpea=1,2-bis(4-pyridyl)ethane, DMF=N,N-dimethylformamide), were solvothermally synthesized and characterized. In the two isostructural complexes, BPTligand and N-containing ligand bpea or bpe connect adjacent Ni centers to form a bilayer structure. The whole topology could be represented as (3,4)-connected (63)(65.8) with the tricarboxylate ligands and Ni atoms as 3-connected T-shaped and 4-connected tetrahedral nodes, respectively. Each bilayer polycatenates two other identical bilayers, giving rise to a 2D→3D polycatenating network with polyrotaxane moieties. Gas adsorptive measurements indicated compound 1 exhibited adsorption of CO2 and N2.
Two Ni(Ⅱ)-organic frameworks, namely, {[Ni3(BPT)2(bpe)2(H2O)6]·2DMF·7H2O}n (1) and {[Ni3(BPT)2(bpea)2(H2O)6]·2DMF·5H2O}n (2) (H3BPT = biphenyl-3,4',5-tricarboxylic acid, bpe = 1,2-bis(4-pyridyl)ethylene, bpea=1,2-bis(4-pyridyl)ethane, DMF=N,N-dimethylformamide), were solvothermally synthesized and characterized. In the two isostructural complexes, BPTligand and N-containing ligand bpea or bpe connect adjacent Ni centers to form a bilayer structure. The whole topology could be represented as (3,4)-connected (63)(65.8) with the tricarboxylate ligands and Ni atoms as 3-connected T-shaped and 4-connected tetrahedral nodes, respectively. Each bilayer polycatenates two other identical bilayers, giving rise to a 2D→3D polycatenating network with polyrotaxane moieties. Gas adsorptive measurements indicated compound 1 exhibited adsorption of CO2 and N2.
2015, (6): 1239-1244
doi: 10.11862/CJIC.2015.169
Abstract:
The bis(2,4-tBu2-pentadienyl)lanthanide complexes (η5-Pdl')2Yb(THF) (1) and (η5-Pdl')2Sm(DME) (2) were successfully prepared in high yield by direct salt metathesis between LnI2 and 2,4-di-butyl-pentadienyl potassium(K(Pdl')). Complexes 1 and 2 could also be obtained smoothly from the reaction of LnCl3 and K(Pdl') through oxidation-reduction reaction. These two compounds were characterized and the X-ray single crystal analysis revealed a predominantly η5-pentadienyl-metal bonding. Both two compounds could initiate ring-opening polymerization of ε-caprolactone rapidly at room temperature and led to narrow polydispersities with high activity.
The bis(2,4-tBu2-pentadienyl)lanthanide complexes (η5-Pdl')2Yb(THF) (1) and (η5-Pdl')2Sm(DME) (2) were successfully prepared in high yield by direct salt metathesis between LnI2 and 2,4-di-butyl-pentadienyl potassium(K(Pdl')). Complexes 1 and 2 could also be obtained smoothly from the reaction of LnCl3 and K(Pdl') through oxidation-reduction reaction. These two compounds were characterized and the X-ray single crystal analysis revealed a predominantly η5-pentadienyl-metal bonding. Both two compounds could initiate ring-opening polymerization of ε-caprolactone rapidly at room temperature and led to narrow polydispersities with high activity.
2015, (6): 1245-1251
doi: 10.11862/CJIC.2015.168
Abstract:
Two cadmium(Ⅱ) complexes based on 2-(pyridin-4-yl)-1H-imidazole-4,5-dicarboxylic acid (H3PIDC) and 1,10-phenanthroline's derivatives mixed ligands, namely, {[Cd3(HPIDC)3(DPPZ)3]·7H2O}n (1) and [Cd(HPIDC)(Imphen)(H2O)]2 (2) (DPPZ=dipyrido[3,2-a:2',3'-c]phenazine, Imphen=imidazo[4,5-f ][1,10]phenanthroline), have been synthesized under hydrothermal conditions and characterized by elemental analysis, infrared spectrum and single-crystal X-ray diffraction. Complexes 1 and 2 are one-dimensional chain and zero-dimensional structures, respectively. Two complexes exhibit excellent thermal stabilities and photoluminescent properties.
Two cadmium(Ⅱ) complexes based on 2-(pyridin-4-yl)-1H-imidazole-4,5-dicarboxylic acid (H3PIDC) and 1,10-phenanthroline's derivatives mixed ligands, namely, {[Cd3(HPIDC)3(DPPZ)3]·7H2O}n (1) and [Cd(HPIDC)(Imphen)(H2O)]2 (2) (DPPZ=dipyrido[3,2-a:2',3'-c]phenazine, Imphen=imidazo[4,5-f ][1,10]phenanthroline), have been synthesized under hydrothermal conditions and characterized by elemental analysis, infrared spectrum and single-crystal X-ray diffraction. Complexes 1 and 2 are one-dimensional chain and zero-dimensional structures, respectively. Two complexes exhibit excellent thermal stabilities and photoluminescent properties.
2015, (6): 1252-1260
doi: 10.11862/CJIC.2015.161
Abstract:
The synthesis and characterization of carbon foam supported silica aerogel (SiO2/Carbon foam) and silicon carbide composite (SiC/Carbon foam) are presented in this study. The phase composition, microstructure, thermal and mechanical properties are investigated by XRD, SEM, LFA Laser Flashmeasurements, and Universal Material Testing.The resulting SiO2/Carbon foam composite shows a higher compressive strength (14.95 MPa) and a smaller thermal conductivity (0.44 W·m-1·K-1) at room temperature, in comparison with the pristine carbon foam. The SiC/Carbon foam composite maintains a compressive strength of 14.66 MPa, and possesses a low high-temperature thermal conductivity (2.18 W·m-1·K-1 at 1200 ℃). Mass loss does not begin until 610 ℃ for the SiC/Carbon foam composite, and complete carbon combustion does not occur until 844 ℃, indicating a much better thermal stability than the pristine carbon foam in oxidizing atmosphere.
The synthesis and characterization of carbon foam supported silica aerogel (SiO2/Carbon foam) and silicon carbide composite (SiC/Carbon foam) are presented in this study. The phase composition, microstructure, thermal and mechanical properties are investigated by XRD, SEM, LFA Laser Flashmeasurements, and Universal Material Testing.The resulting SiO2/Carbon foam composite shows a higher compressive strength (14.95 MPa) and a smaller thermal conductivity (0.44 W·m-1·K-1) at room temperature, in comparison with the pristine carbon foam. The SiC/Carbon foam composite maintains a compressive strength of 14.66 MPa, and possesses a low high-temperature thermal conductivity (2.18 W·m-1·K-1 at 1200 ℃). Mass loss does not begin until 610 ℃ for the SiC/Carbon foam composite, and complete carbon combustion does not occur until 844 ℃, indicating a much better thermal stability than the pristine carbon foam in oxidizing atmosphere.
2015, (6): 1261-1268
doi: 10.11862/CJIC.2015.170
Abstract:
Two coordination polymers, [Ni(BDOA)(BIDPE)(H2O)]n (1) and [Cd(BDOA)0.5(BIDPE)Cl]n (2), (H2BDOA=benzene-1,4-dioxydiacetic acid and BIDPE=4,4'-bis(imidazole-l-yl)diphenyl ether), have been synthesized and characterized by IRspectroscopy, elemental analysis and single-crystal X-ray diffraction. Complex 1 crystallizes in triclinic, space group P1 with a=0.93497(8) nm, b=1.03231(9) nm, c=1.35291(12) nm, α=96.3980(10)°, β=90.7290(10)°, γ=102.0270(10) °, V=1.26831(19) nm3, Z=2, Mw=603.22, Dc=1.580 g·cm-3, μ=0.827, F(000)=624, R1=0.0395, wR2=0.0895(I>2σ(I)). Complex 2 belongs to triclinic, space group P1 with a=1.01751(7) nm, b=1.04299(7) nm, c=1.17338(8) nm, α=68.7230(10)°, β=71.8260(10)°, γ=76.0910(10)°, V=1.09105(13) nm3, Z=2, Mw=562.26, Dc=1.711 g·cm-3, μ=1.163, F(000)=562, R1=0.0210, wR2=0.0537(I>2σ(I)). Structural analyses reveal that complex 1 exhibits a two-dimensional (2D) corrugated layer structure, whereas complex 2 possesses a one-dimensional (1D) chain structure which is generated by joining binuclear Cd2 units by BIDPEand BDOAligands. The results show that the nature of metal ions plays an important role in governing the molecular frameworks. The photochemical properties of two complexes have also been studied.
Two coordination polymers, [Ni(BDOA)(BIDPE)(H2O)]n (1) and [Cd(BDOA)0.5(BIDPE)Cl]n (2), (H2BDOA=benzene-1,4-dioxydiacetic acid and BIDPE=4,4'-bis(imidazole-l-yl)diphenyl ether), have been synthesized and characterized by IRspectroscopy, elemental analysis and single-crystal X-ray diffraction. Complex 1 crystallizes in triclinic, space group P1 with a=0.93497(8) nm, b=1.03231(9) nm, c=1.35291(12) nm, α=96.3980(10)°, β=90.7290(10)°, γ=102.0270(10) °, V=1.26831(19) nm3, Z=2, Mw=603.22, Dc=1.580 g·cm-3, μ=0.827, F(000)=624, R1=0.0395, wR2=0.0895(I>2σ(I)). Complex 2 belongs to triclinic, space group P1 with a=1.01751(7) nm, b=1.04299(7) nm, c=1.17338(8) nm, α=68.7230(10)°, β=71.8260(10)°, γ=76.0910(10)°, V=1.09105(13) nm3, Z=2, Mw=562.26, Dc=1.711 g·cm-3, μ=1.163, F(000)=562, R1=0.0210, wR2=0.0537(I>2σ(I)). Structural analyses reveal that complex 1 exhibits a two-dimensional (2D) corrugated layer structure, whereas complex 2 possesses a one-dimensional (1D) chain structure which is generated by joining binuclear Cd2 units by BIDPEand BDOAligands. The results show that the nature of metal ions plays an important role in governing the molecular frameworks. The photochemical properties of two complexes have also been studied.
