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Preparation of Cu(In,Al)(Se,S)2 Thin Films by Low-Cost Non-vacuum Hybrid Process

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Chinese Journal of Chemical Physics 2015年第6期28卷 -页

作者： Zhao-fan Liu Wei Xia Chen-chen Yuan Pai-feng Luo Department of Materials Science and Engineering Hefei University of Technology Hefei 230009China CAS Key Laboratory of Materials for Energy Conversion University of Science and Technology of China Hefei 230026 China

Cu(In,Al)(Se,S)2 thin films were successfully obtained through a simple low-cost non-vacuum process. The Cu(In,Al)Se2 raw material powder was firstly synthesized by a traditional solvothermal route. Then, the precursor coatings were prepared by drop-coating Cu(In, Al)Se2 slurry. Finally, the Cu(In,Al)Se2 and Cu(In,Al)(Se,S)2 films were achieved by the selenization and/or sulfuration process. Through X-ray diffraction (XRD), scanning electron microscope, X-ray fluorescence, and absorption spectroscopy measurement, it was found that all the films show the single chalcopyrite phase structure and have the preferred (112) orientation. Meanwhile, after substituting selenium by sulfur, the main XRD peaks shift to higher 2θ degrees and the porous films become more compact. The energy band gap also increases to a suitable range for light absorption from 1.21 eV to 1.33 eV, which indicates that the additional sulfuration process is much more favorable for improving the quality of Cu(In,Al)(Se,S)2 films.

关键词： Non-vacuum solvothermal X-ray diffraction Sulfuration

Construction of [Cu_nI_n]-based coordination polymers via flexible benzimidazolyl-based ligands

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Science China Chemistry 2010年第10期53卷 2083-2090页

作者： LI LingLing, REN ZhiGang, Lü Xue, WANG HeMing, CHANG YuJie, LI HongXi, WU Bing & LANG JianPing College of Chemistry, Chemical Engineering and Materials Science, Suzhou University, Suzhou 215123, China College of Chemistry Chemical Engineering and Materials Science Suzhou University Suzhou China

Four new [CunIn]-based coordination polymers, [{Cu4(μ3-I)4(mbbm)2}·2DMF]n (1), [(CuI)2(mbbm)2]n (2), [{Cu2(μ-I)2-(ebbm)2}·2MeCN]n (3), and [Cu2(μ-I)2(prbbm)2]n (4), were prepared from solvothermal reactions of CuI with three flexible ligands [(bzim)(CH2)n(bzim)] (bzim = benzimidazole; n = 1, mbbm; n = 2, ebbm; n = 3, prbbm). These compounds were characterized by elemental analysis, IR and X-ray crystallography. 1 consists of cubanelike [Cu4(μ3-I)4] fragments that link the neighboring ones via mbbm bridges to form a 1D ladder-type chain. 2 contains mononuclear [CuI] fragments that are bridged by mbbm ligands to yield a 1D zigzag chain. 3 or 4 contains a [Cu2(μ-I)2] dimeric fragment, which works as a four-connecting node to link its four equivalent ones to form a 2D (4,4) network (3) or acts as a two-connecting node to connect its two equivalent ones via two pairs of prbbm bridges to form a 1D double chain (4). The photoluminescent properties of 1-4 in the solid state at ambient temperature were investigated.

关键词： coordination polymers assembly flexible ligands solvothermal reactions photoluminescent properties

A Unique 2D Layered FeⅢ Coordination Polymer with only Formate Ligand as Bridges: Synthesis, Crystal Structure and Magnetic Properties

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Chinese Journal of Structural Chemistry 2019年第11期38卷 1963-1969页

作者：张琳琳申斌赵炯鹏高素华刘福臣 School of Chemistry and Chemical Engineering Tianjin University of Technology

A novel two-dimensional layered FeⅢ formate, Fe(HCO2)2ClH2O, has been synthesized by solvothermal reaction. The structure of complex is characterized by single-crystal X-ray diffraction. The complex crystallizes in tetragonal space group P4/nmm with a = 5.9588(6), c = 8.3831(17) ?, V = 297.66(7) ?3, Z = 2, F(000) = 198, Dc = 2.224 g/cm3, Mr = 199.35, μ = 2.927 mm-1, the final R = 0.0231 and w R = 0.0585(I > 2σ(I)) for all data. Single-crystal structure analysis indicates that the complex has a 2D metal formate structure with only formate anions as bridges. The anti-anti formats link the FeⅢ ions to form a(4, 4) net, while the chlorine ions and water molecules coordinate to FeⅢ on both sides of the layer. Magnetic study have shown that an antiferromagnetic interactions between the FeⅢ ions in the complex. And a field induced spin-flop was detected at low temperature.

关键词： formate solvothermal reaction low-dimensional materials antiferromagnetism

solvothermal Syntheses and Characterizations of Two Quaternary Copper Sulfides BaCu3MS4(M=In, Ga)

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Solvothermal Syntheses and Characterizations of Two Quaterna...

Design and synthesis of nitrogen-doped hexagonal NiCoO nanoplates derived from Ni-Co-MOF for high-performance electrochemical energy storage

中国化学会第十届全国无机化学学术会议

作者： Yan Liu Ren-Chun Zhang Min Ji Yong-Lin An Department of Chemistry Dalian University of Technology College of Chemistry and Chemical Engineering Anyang Normal University

In the past,the syntheses of quaternary copper sulfides containing alkaline earth metal ions were mainly concentrated on high temperature solid state method,while they were rarely synthesized under mild hydro(solvo)thermal conditions. In this work,by using excess sulfur as mineralizer we successfully prepared two quaternary sulfides BaCuMS (M=In,Ga,1 and 2) through solvothermal technique at relatively low temperature.Particularly,this is not only the first time to synthesize quaternary sulfides in theⅡA-Cu-ⅢA-S system using solvothermal method,but also the first time to synthesize quaternary sulfides with high-proportion of copper under this condition. BaCuInS(1) crystallizes in the orthorhombic space group Ama2 and possesses a novel 3-D anionic[CuInS]framework composed of 8-membered ring ([CuS]and[CuInS]alternatively) channels with Balocated in the channels.BaCuGaS(2) crystallizes in the orthorhombic space group P321 and adopts a unique 3-D anionic[CuGaS]framework assembled by 8-membered ring ([CuS]and[CuGaS]alternatively)and[CuGaS]anionic chains with Balocated in the 8-membered ring.Our success in synthesizing the two quaternary sulfides demonstrate that solvothermal method is an effective way to explore multinary alkaline earth metal sulfides with novel structures and fascinating properties.

关键词： solvothermal alkaline earth metal ions excess sulfur high-proportion of copper

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Chinese Chemical Letters 2020年第9期31卷 2280-2286页

作者： Yan Li Yuying Shan Huan Pang School of Chemistry and Chemical Engineering Institute for Innovative Materials and EnergyYangzhou UniversityYangzhou 225009China

In order to further improve the potential application of nickel-cobalt oxide(NiCoO) in supercapacitors,we use controlled calcination of diffe rent Ni-Co-MOF([NiCo(HBTC)(4,4’-bipy)]) composites to obtain five kinds of nickel doped NiCoO(N-NiCoO) with different Ni/Co molar ratio.These N-NiCoO materials with unique hexagonal nanoplates structure,high specific surface area and high porosity indicate high and stable electrochemical activity.In particular,N-NiCoO-2 with a Ni/Co molar ratio of 2:1 exhibits the highest 945.79 F/g specific capacitance at 1 A/g and a high cycle stability of only 6.7% attenuation after 5000 cycles.Apart from the certain percentage of NiCoO with higher conductivity,nitrogen doping provides more reactive sites and the specific porous hexagonal nanoplates structure of the product itself accelerate electron transfer and promote electrolyte diffusion can more effectively enhance the electrochemical performance.Therefore,N-NiCoO synthesized via a simple method exhibit exciting potential and can be used as an electrode material for supercapacitors with good performance.

关键词： Ni-Co-MOF N-NiCoO solvothermal Supercapacitors Electrochemical performance

Mesocrystalline TiO2/sepiolite composites for the effective degradation of methyl orange and methylene blue

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Frontiers of Materials Science 2018年第3期12卷 292-303页

作者： Ruirui LIU Zhijiang JI Jing WANG Jinjun ZHANG State Key Laboratory of Green Building Materials China Building Materials Academy Beijing 100024 China

Mesocrystalline TiO2/sepiolite （TiS） composites with the function of adsorption and degradation of liquid organic pollutants were successfully fabricated via a facile and low-cost solvothermal reaction. The prepared TiS composites were characterized by FESEM, HRTEM, XRD, XPS, N2 adsorption-desorption, UV-vis DRS, and EPR. Results revealed the homogeneous dispersion of highly reactive TiO2 mesocrystals on the sepiolite nanofibers. Thereinto each single-crystal-like TiO2 mesocrystal comprised many [001]-oriented anatase nanoparticles about 10-20 nm in diameter. The photocatalytic activity was further evaluated by the degradation of anionic dye （methyl orange） and cationic dye （methylene blue） under the UV-vis light （350≤λ≤780 nm） irradiation. By selecting appropriate experimental conditions, we can easily manipulate the photocatalytic performance of TiS composites. The optimal TiS catalyst （the sepiolite content of 28.5 wt.%, and the reaction time of 24 h） could efficiently degrade methyl orange to 90.7% after 70 min, or methylene blue to 97.8% after 50 min, under UV-vis light irradiation. These results can be attributed to their synergistic effect of high crystallinity, large specific surface area, abundant hydroxyl radicals, and effective photogenerated charge separation.

关键词： TiO2/sepiolite mesocrystal solvothermal composites photocatalysis

Template-free Polyoxometalate-assisted Synthesis of Au/ZnO Hollow Sphere Hererostructures for Photocatalytic Water Purification

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Chinese Journal of Structural Chemistry 2018年第6期37卷 924-936页

作者：陈彬彬刘思奇翁孙贤 Department of Practice and Education Fuzhou University Zhicheng College State Key Laboratory of Photocatalysis College of Chemistry Fuzhou University

The controlled synthesis of ZnO hollow spheres is successfully achieved through a facile solvothermal method using a Keggin-type silicotungstic acid（H_4 Si（W_3 O_（10））_4：HSW） as structure directing agent. The formation process of these hollow spheres is proposed based on a variety of controlled experiments. In addition, Au nanoparticles are loaded onto the surface of ZnO hollow spheres. It is found that the Au-loaded ZnO（Au/ZnO） composites exhibit greatly enhanced activity on oxidizing Rhodamine B（Rh B） under simulated UV or visible light irradiation, compared to the pristine ZnO hollow spheres. The improved performance of Au/ZnO heterostructures is mainly attributed to the enhanced optical absorption and the accelerated separation and migration of photogenerated charge carriers. Moreover, the photocatalytic reaction mechanisms are proposed based on the results of electron spin resonance（ESR） analysis, photoelectrochemical measurements, and photocatalytic evaluation. The results and findings are expected to provide significance to the synthesis of noble metal-semiconductor hybrids towards water purification.

关键词： ZnO hollow spheres Au nanoparticles solvothermal photocatalyst

Three Two-dimensional Heterometallic Chalcogenides[TM(tren)][InSbSe_3S](TM = Fe, Co, Mn): Syntheses,Crystal Structures, and Properties

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Chinese Journal of Structural Chemistry 2019年第1期38卷 128-136,5页

作者：陈娟杜翠霞娜米拉阿古拉萨嘎拉白音孟和 College of Chemistry & Environmental Science Innner Mongolia Normal University Key Laboratory for Physics and Chemistry of Functional Materials Inner Mongolia

Three two-dimensional(2-D) heterometallic chalcogenides [TM(tren)][InSbSe_3S](TM = Fe(1), Co(2), Mn(3); tren = tris(2-aminoethyl)-amine) have been solvothermally synthesized in this paper. Single-crystal X-ray analysis indicates that they are isostructural to each other except the different transition metal ions. These compounds contain an unsaturated complex cation [TM(tren)]^(2+), which can be further coordinated by the 2-D [InSbSSe_3]_n^(2n-) anion, resulting in a new neutral organic-decorated heterometallic chalcogenide. These compounds crystallize in monoclinic space group P21/c, with a = 11.768(12), b = 13.884(14), c = 11.095(11) ?, Z = 4, D_c =2.910 Mg·m^(-3), F(000) = 1304, M_r = 707.60 for 1; a = 11.843(9), b = 14.064(10), c = 10.979(8) ?, Z= 4, Dc = 2.875 Mg·m^(-3), F(000) = 1308, M_r = 710.68 for 2; a = 11.969(10), b = 14.191(11), c =11.112(9) ?, Z = 4, D_c = 2.779 Mg·m^(-3), F(000) = 1300, Mr = 706.69 for 3. The maximum and minimum peaks of compounds 1～3 are 6.996 and –2.880 e·?^(-3), 2.242 and –3.066 e·?^(-3), 3.655 and –3.569 e·?^(-3), respectively. These compounds were structurally characterized by powder X-ray diffraction measurement, thermal analysis, infrared spectroscopy and UV-Vis diffuse reflectance spectroscopy. A solid-state UV/Vis reflectance spectroscopy measurement on 1, 2 and 3 confirmed that these compounds are semiconductor materials.

关键词： heterometallic chalcogenides solvothermal synthesis crystal structure

[N-ethyl-4,4'-bipyridinium][ZnX_4](X = Cl or Br) with N-ethyl-4,4'-bipyridinium Generated In Situ:Syntheses, Structures, Fluorescence and TDDFT Calculations

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Chinese Journal of Structural Chemistry 2014年第8期33卷 1141-1146页

作者：陈文通胡荣华罗志刚陈华龙张娴刘娟 Institute of Applied Chemistry School of Chemistry and Chemical Engineering Jiangxi Province Key Laboratory of Coordination Chemistry Jinggangshan University State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences

Two new zinc bipyridinium compounds, [N-ethyl-4,4＂-bipyridinium][ZnX4] （X = CI （1） or Br （2）） with N-ethyl-4,4＂-bipyridinium generated in situ, have been synthesized through solvothermal reactions and structurally characterized by single-crystal X-ray diffraction analyses. Both compounds are isostructural and crystallize in the P2/c space group of monoclinic system. Compound 1： a = 8.4397（5）, b = 21.988（1）, c = 8.8777（5） А, β = 106.490（1）°, V = 1579.7（2） A3, C2H15C14N2Zn, Mr = 394.43, Z = 4, Dc = 1.658 g/cm3, S = 1.068,/a（MoKa） = 2.218 mm-1, F（000） = 796, R = 0.0295 and wR = 0.0766. Compound 2： a = 8.4154（6）, b = 22.844（2）, c = 9.0308（7） A, fl = 106.026（1）°, V = 1668.6（2） A3, Cj/HjsBraN2Zn, Mr = 572.27, Z = 4, Dc = 2.278 g/cm3, S = 1.033, /l（MoKa） = 11.038 mm＂1, F（000） = 1084, R = 0.0427 and wR = 0.1175. Both of them are characteristic of an isolated structure with the zinc atoms locating at a tetrahedral environment. In both compounds, the N-ethyl-4,4＂-bipyridinium2＋ cations and ZnX42- anions interconnect together via hydrogen bonding interactions to construct a three-dimensional （3-D） supramolecular framework. Fluorescent studies reveal that both compounds exhibit a strong emission in the green region. In combination with the theoretical calculations, we can draw a conclusion that the emissions should result from ligand-to- ligand charge-transfer （LLCT） transition.

关键词： fluorescence LLCT solvothermal TDDFT zinc