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Solvothermal Preparation of Mn_3O_4 Nanoparticles and Effect of Temperature on Particle Size

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Chemical Research in Chinese Universities 2012年第4期28卷 577-580页

作者： SONG Rui WANG Hong-jun feng shou-hua State Key Laboratory of lnorganic Synthesis and Preparative Chemistry College of ChemistryJilin UniversityChangchun 130012P R.China PetroChina Jilin Petrochemical Company Research Institute Jilin 132021P.1L China PetroChina Jilin Petrochemical Company Jilin 132002P.R.China

Hausmannite Mn3O4 nanoparticles were successfully prepared via a facile one-step solvothermal route with Mn（CH3COO）2·4H2O as manganese source in the mixed solvent of acetone and *** X-ray diffraction（XRD）,Fourier transform infrared（FTIR） spectrometry and transmission electron microscopy（TEM） were used to characterize Mn3O4 *** was found that the particle size could be tailored by varying the synthesis *** the whole,the particle size becomes larger with the rising of solvothermal reaction *** there is no linear relation between *** to the different temperatures（60―140 °C）,the average particle size is from about 9 nm to 15 *** properties of Mn3O4 samples prepared at 60,100 and 140 °C were studied via a superconducting quantum interference device（SQUID）,respectively.

关键词： Solvothermal preparation MnO Nanoparticle Particle size

Hydrothermal Synthesis and Structural Characterization of Three-dimensional Metal-organic Framework [Zn_3(C_2H_2N_3)_2(C_7H_5O_2)_4]

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Chemical Research in Chinese Universities 2009年第1期25卷 1-4页

作者： SONG Zhe LI Guang-hua YU Yang SHI Zhan feng shou-hua College of Chemistry State Key Laboratory of Inorganic Synthesis and Preparative Chemistry Jilin University Changchun 130012 P. R. China

Hydrothermal reaction between mixed ligand（1,2,4-triazole and benzoic acid） and Zn（NO3）2·6H2O afforded a three-dimensional（3D） metal-organic framework Zn3（C2H2N3）2（C7H5O2）4（C2H2N3=1,2,4-triazole, C7H5O2=benzoic acid）. The compound was crystallized in the hexagonal system with space group R3： a=2.90234（9） nm, b=2.90234（9） nm, c=1.08597（5） nm, γ=120°, V=7.9222（5） nm^3, Mr=816.68, Dc=1.541 g/cm^3, Z=9, F（000）=3708, R=0.0636, and wR=0. 1777. Its structure consists of ZnN2O2 tetrahedron and ZnN204 octahedron, which are connected by 1,2,4-triazole and benzoic acid ligands to form a 3D framework with helical units. This compound forms an interpenetrated NbO topology. The compound was characterized by single-crystal X-ray diffraction, elemental analysis, FTIR spectra, and TGA measurements.

关键词： Hydrothermal synthesis Metal-organic framework 1,2,4-Triazole Benzoic acid Helical units

Synthesis,Proton Conductivity and Humidity Sensing Property ofγ-Type Zirconium Hydrogen Phosphate,Zr(HPO_4)_2·2H_2O

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Chemical Research in Chinese Universities 1999年第1期15卷 7-11页

作者： feng shou-hua ZHAO Hui LI Lian-sheng Martha Greenblatt Key Laboratory of Inorganic Synthesis and Preparative Chemistry Jilin UniversityChangchun 130023 Department of Chemistry Rutgersthe State University of New JerseyPiscatawayNJ 08855USA

A γ - type of layered zirconium hydrogen phosphate, Zr(HPO 4) 2·2H 2O( γ ZrP), was synthesized under hydrothermal conditions and characterized by powder X ray diffraction and thermogravimetric analysis. The temperature dependence of the proton conductivity in γ ZrP was investigated in a temperature range of 23￣413 ℃ by ac impedance spectroscopy. The variation of the conductivity with water loss and phase transitions was observed. The best proton conductivity in γ ZrP is 6×10 -4 S·cm -1 at 60 ℃. The proton conductivities in the dehydrated sample are ￣10 -5 at 150 ℃ and ￣10 -4 S·cm -1 at 350 ℃, respectively. The conductivities as a function of humidity in the temperature range of 120￣200 ℃ were measured.

关键词： Synthesis γ-Type zirconium hydrogen phosphate Proton conductivity Humidity sensing property

New Zincophosphite with Infinite One-dimensional [Zn(HPO_3)(H_2PO_3)]~– Chains: Synthesis, Characterizations and Spectral Properties

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Chemical Research in Chinese Universities 2011年第1期27卷 19-22页

作者： WANG Lei LUO Yan-ling WEN Yong-hong LI Guang-hua feng shou-hua Key Laboratory of Eco-chemical Engineering Ministry of Education College of Chemistry and Molecular Engineering Qingdao University of Science and Technology Qingdao 266042 P. R. China State Key Laboratory of Inorganic Synthesis and Preparative Chemistry College of Chemistry Jilin University Changchun 130012 P. R. China

With dimethylamine as a template, a new one-dimensional zincophosphite （C2H8N）·[Zn（HPO3）（H2PO3）] was prepared under hydrothermal conditions and characterized by single-crystal X-ray diffraction, FTIR spectrametry, elemental analysis, powder X-ray diffraction, and thermogravimetric analysis. The compound crystallized in the Monoclinic space group P2（1）/c, with cell parameters, a=0.78410（9） nm, b=1.54744（2） nm, c=0.81418（1） nm, β=105.8150（1）°, V=0.95049（2） nm3 and Z=4. The connectivity of the ZnO4 tetrahedron and HPO3 pseudo pyramid resulted in inifinite corner-sharing 4-membered ring chains, which were further linked by the protonated amine molecules to form a 3D structure via hydrogen bonds. To the best of our knowledge, this is the first existence of a zincophosphite with the anionic framework composition of [Zn（HPO3）（H2PO3）]-. The compound exhibits intense photoluminescence at room temperature.

关键词： Hydrothermal synthesis Organically-templated Zincophosphite Structural characterization

Hydrothermal Synthesis and Characterization of Perovskite Oxide AgTaO_3

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Chemical Research in Chinese Universities 2012年第5期28卷 760-763页

作者： HE Li-jie ZHANG Dong feng shou-hua ZOU Bo CHEN Gang Yingkou University Zone Yingkou 115000P.R.China State Key Laboratory of Superhard Materials College of Physics State Key Laboratory of Inorganic Synthesis and Preparative Chemistry College of ChemistryJilin UniversityChangchun 130012P.R.China

The perovskite-type AgTaO3 crystals were prepared by mild hydrothermal method and determined by powder X-ray diffraction. Rietveld refinement indicates that AgTaO3 crystallized in an orthorhombic system with the space group Pcmn. The lattice parameters are a=5.5822（1） nm, b=7.8522（2） nm and c=5.5347（1） nm, with α=β=γ= 90.0o. The compound was characterized by scanning electron microscopy（SEM）, X-ray photoelectron spectroscopy （XPS）, high resolution transmission electron microscopy（HR-TEM） and UV-Vis diffuse reflectance spectrometry （UV-Vis DRS）. The photocatalytic activity of AgTaO3 powder was evaluated by the degradation of Congo red under UV-light irradiation. The result shows that the titled compound has a high photocatalytic activity at room temperature and potential application in photocatalysis.

关键词： Hydrothermal synthesis Perovskite structure Photocatalytic activity

Synthesis and Characterization of a One-dimensional Coordination Polymer Generated from Unsymmetrical Bridging Organosulfur Ligand

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Chemical Research in Chinese Universities 2008年第4期24卷 389-391页

作者： WANG Lei ZHANG Hui DONG Wen-jun SHI Zhan feng shou-hua Key Laboratory of Eco-chemical Engineering Ministry of Education College of Chemistry and Molecular Engineering Qingdao University of Science and Technology Qingdao 266042 P. R. China State Key Laboratory of lnorganic Synthesis and Preparative Chemistry College of Chemistry Jilin University Changchun 130012 P. R. China

A new one-dimensional（1D） coordination polymer [Zn（MMTA）2]n（MMTA=5-mercapto-l-methyl-tetrazole） was synthesized under solvothermal conditions and characterized by single crystal X-ray diffraction. This compound crystallizes in the monoclinic space group C2/c, with cell parameters： a=1.4938（7） nm, b=1.3599（5） nm, c=1.2180（4） nm, fl=120.84（3）^＊, V=2.1243（2） nm^3, and Z=8. The deprotonated HMMTA molecule as a/a2-1igand links the zinc center, forming ID chains, which are luther linked by weak C--H...N hydrogen bonds, forming a three-dimensional supramolecular framework. The compound exhibits intense photoluminescence at room temperature. On the basis of the results of TG/DTA analyses, the structure is thermally stable up to -280 ℃.

关键词： Solvothermal synthesis Coordination polymer Crystal structure Organosulfur ligand

Hydrothermal Synthesis,Structure Characterization and Magnetic Studies of Perovskite-type Fluorides K_2 NaVF_6 and(NH_4)_3VF_6

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Chemical Research in Chinese Universities 2012年第3期28卷 371-374页

作者： HE Li-jie ZHANG Dong feng shou-hua CHEN Gang ZOU Bo College of Chemistry Yingkou University ZoneYingkou 115000P.R.China State Key Laboratory of Superhard Materials College of Physics State Key Laboratory of Inorganic Synthesis and Preparative Chemistry College of ChemistryJilin UniversityChangehun 130012P.R.China

Two perovskite-type fluorides K2NaVF6 and （NH4）3VF6 were synthesized under mild hydrothermal con- ditions. The structures of the compounds were determined by means of powder X-ray diffraction analysis. The Riet- veld refinement indicates that K2NaVF6 has a cubic elpasolite-type structure and crystallizes in space group Fm3m with lattice constant a=8.3180（2） nm. （NH4）3VF6 has a cubic cryolite-type structure and crystallizes in space group Fm3m with lattice parameter a=9.090（1） rim. The compounds were further characterized by scanning electron micro- scopy（SEM）, thermogravimetric（TG） and differential thermal analysis（DTA）. The variable temperature magnetic susceptibility of these two compounds was characterized for the first time and the result shows that the magnetic or- dering is related to the crystallographic features and isolated magnetic unit with the temperature decreasing.

关键词： Hydrothermal Fluoride Perovskite-type Magnetic property

Synthesis and Ferrimagnetic Behaviour of Mn Doped Rare Earth Iron Garnets

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Chemical Research in Chinese Universities 2012年第3期28卷 391-394页

作者： GUO Li YUAN Lin PENG Wen YUAN Hong-ming feng shou-hua State Key Laboratory of Inorganic Synthesis and Preparative Chemistry College of ChemistryJilin UniversityChangchun 130012R R.China

Rare earth iron garnets R3Fe5-xMnxO12（R=Pr, Nd, Sm, Eu） were prepared through mild hydrothermal me- thod. The initial alkalinity of solutions was thought to play an important role in governing the content of Mn. The effect of substitution Fe^3＋ ions by Mn^3＋ ions on magnetic properties was investigated. The saturation magnetizations of Mn-doped samples are larger than that of corresponding parent compounds due to the moment of Mn^3＋ ion being smaller than that of Fe^3＋. It is clearly shown that incorporation of Mn^3＋ gives rise to significant variations in the Curie temperature. With increasing of Mn content x, Curie temperatures reduced sharply for the garnets, which could be explained by the exchange interaction between a-d Fe^3＋ being reduced in these compounds.

关键词： Hydrothermal synthesis Garnet Substitution Ferrimagnetism

Magnetic and Transport Properties of Bi_(0.5)Ca_(0.5–x)La_xFe_(0.3)Mn_(0.7)O_3(x=0, 0.05, 0.10, 0.15, 0.20, 0.25) Prepared by Molten Salt Method

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Chemical Research in Chinese Universities 2011年第1期27卷 15-18页

作者： DONG Zhong-ping HU Bin CHEN Yan YUAN Hong-ming feng shou-hua State Key Laboratory of Inorganic Synthesis ＆ Preparative Chemistry College of Chemistry Jilin University Changchun 130012 P. R. China

Polycrystallines Bi0.5Ca0.5-xLaxFe0.3Mn0.7O3（x=0, 0,05, 0.10, 0.15, 0.20, 0.25） were prepared by molten salt method and showed perovskite orthorhombic structure with space group Pnma. The magnetic measurements indicate that the compounds exhibit antiferromagnetic behavior in a temperature range of 4-300 K. The measurements of transport properties suggest that the substitution of La for Ca enhanced the conductivity, and a kink appeared on the curve of temperature dependence of resistivity at 275 K, which is related to the spin-reorientation in the samples.

关键词： Perovskite Doping Magnetism Spin-reorientation