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Solvothermal Synthesis, Structure and the Secondorder NLO Properties of a Novel Non-metal 3-D Borophosphate:（NH4）2[B2P2O8（OH）2]

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Chinese Journal of Structural Chemistry 2019年第11期38卷 1909-1915页

作者：冯玉全赵茜毕冬琴 College of Chemistry and Pharmacy Engineering Nanyang Normal University

A new non-metal 3-D borophosphate compound formulated as(NH4)2[B2P2O8(OH)2](1)has been synthesized by a Solvothermal method and characterized by elemental analysis,energy-dispersive X-ray spectroscopy(EDS),IR spectrum and single-crystal X-ray diffraction.The borophosphate(NH4)2[B2P2O8(OH)2]crystallizes in the cubic system,space group P213 with Z=2,a=b=c=7.586(4)?,V=436.6(4)?3,Mr=281.64,Dc=2.127 g/cm^3,λ=0.71073?,μ=0.551 mm^-1,F(000)=284,R=0.0277 and wR=0.0758 for 262 observed reflections with I>2σ(I)and S=1.082.Its structure is constructed by the connection of PO4 and BO3(OH)tetrahedra to form a 3-D anionic framework containing 4-and 8-membered rings(MRs),with two NH4+cations located in the channels of the 8-membered rings.The N–H…O hydrogen bonds are observed in its packing structure and enhanced the stability of crystal structure.In addition,its thermal stability,UV spectrum and second-order NLO properties have been also investigated.

关键词： Solvothermal synthesis borophosphate UV spectrum second-order NLO properties

Layered double hydroxide nanosheets via Solvothermal delamination

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Journal of Energy Chemistry 2019年第8期28卷 88-94,I0004页

作者： Katarina Cermelj Kanittika Ruengkajorn Jean-Charles Buffet Dermot O’Hare Chemistry Research Laboratory Department of Chemistry University of Oxford

A new Solvothermal post-synthesis treatment for preparing high aspect ratio magnesium aluminium layered double hydroxides(Mg Al–LDHs) has been developed. Treating laurate-intercalated Mg Al–LDHs in pure ethanol in an autoclave for 48 h at 150 °C was found to produce delaminated MgA l–LDH nanosheets with a thickness of ~2.6 nm and an aspect ratio of ~105. It is proposed that the high pressure Solvothermal process promotes the insertion of ethanol molecules into the LDH interlayer space, thereby facilitating delamination. This new post-synthesis treatment provides the opportunity for a facile, large scale route to highly delaminated high aspect ratio LDHs, which might be of interest towards novel nanomaterials for energy conversion and storage.

关键词： Layered double hydroxide Hydrophobicity Aspect ratio Solvothermal treatment Delamination

Solvothermal Synthesis of ZnIn2S4 by Alcohol Solvents and Visible Light Photocatalytic Activity on Selective Oxidation and Dye Degradation

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Chinese Journal of Structural Chemistry 2018年第5期37卷 753-762页

作者：何运慧陈志鑫许静静吴艳肖光参 Analysis and Test Center Fuzhou University State Key Laboratory of Photocatalysis on Energy and Environment Fuzhou University Key Laboratory of Ecological Environment and Information Atlas Fujian Provincial University

A series of hexagonal ZnIn2S4 samples with different morphologies have been successfully prepared via a facile Solvothermal approach using different alcohol solvents with the optimum synthesis time and temperature. X-ray diffraction, field emission scanning electron microscopy, UV-vis diffuse reflection spectroscopy and photoelectrochemical measurements are employed to determine the properties of the samples. It is found that the solvent has a significant influence on the morphology, optical properties and electronic nature of the samples. The photocatalytic activities of the samples have been evaluated by selective oxidation of benzyl alcohol to benzaldehyde to benzaldehyde and the degradation of methyl orange（MO） under visible light irradiation. The results reveal that the photocatalytic activities of ZnIn2S4 are closely related to the reaction solvent. The ethanol-mediated ZnIn2S4 exhibits the best photocatalytic performance toward selective oxidation of benzyl alcohol to benzaldehyde and the degradation of dye MO compared to the samples prepared in other solvents, which can be attributed to the integrative effect of the enhanced light absorption intensity and the prolonged lifetime of photogenerated carriers. In addition, a possible mechanism is proposed and discussed. It is expected that our current research could promote further interest on the synthesizing efficient ternary chalcogenides semiconducting materials for environment remediation and organic transformation.

关键词： photocatalyst Solvothermal selective oxidation methyl orange visible light

Spindle LiFePO_4 particles as cathode of lithium-ion batteries synthesized by Solvothermal method with glucose as auxiliary reductant

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Rare Metals 2015年第10期34卷 731-737页

作者： Li Ren Xing-En Li Fang-Fang Wang Yang Han Polymer Research Institute College of Chemical EngineeringHebei University of Technology

The well-distribution spindle Li Fe PO4(LFP)nanoparticles as cathode of lithium secondary batteries were synthesized by a Solvothermal reaction route at low temperature(180 °C) in which the ascorbic acid was used as reducing agent. In order to guarantee that the p H values of thermal systems were not affected too much and the reducibility of the system was enhanced at the same time,glucose was chosen as an auxiliary reductant in this reaction. The obtained powders were characterized by X-ray diffraction(XRD), scanning electron microscopy(SEM),and laser particle analyzer. The results show that the carbon-coated uniform spindle olivine Li Fe PO4/C-glucose particles(glucose as auxiliary reductant, LFP/C-G) are prepared with the size 500–600 nm and without any impurity phases. Their electrochemical properties were evaluated by electrochemical impedance spectroscopy,cyclic voltammetry, and galvanostatic charge/discharge tests. LFP/C-G has a higher conductivity and better reversible capability than carbon-coated LFP(LFP/C). The highest discharge capacity of LFP/C-G is 161.3 mAh·g-1at0.1C and 108.6 mAh·g-1at 5.0C, respectively. The results imply that the neat crystal nanostructure of LFP/C-G has excellent capacity retention and cycling stability.The adding of glucose is the key factor for the welldistribution and neat crystal structure of nanoparticles,thus the electrochemical performances of materials are improved.

关键词： Lithium-ion battery LiFePO4 Spindle Solvothermal G

Controllable synthesis of metallic Bi from commercial Bi_2O_3 via one-pot Solvothermal reduction method

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Chinese Journal of Chemical Engineering 2017年第9期25卷 1202-1206页

作者： Lei Yang Yangyang Zhang Hua Li Hezhou Liu State Key Laboratory of Metal Matrix Composites School of Materials Science and Engineering Shanghai Jiao Tong University

Metallic bismuth crystal is one important and interesting semimetal that has attracted great attention owing to its unique thermal and electrical properties. Herein, we report a facile, green, cost-effective and sustainable Solvothermal process using ethanol, glycol, isopropanol, phenylcarbinol as solvent and commercial Bi_2O_3 as the starting material to produce high-purity metallic Bi with tunable morphologies on large scale. It is found that all alcohols are capable of reducing Bi_2O_3 to Bi and the reducibility of glycol is proved to be the strongest. The highest purity of the resultant Bi is calculated to be 99.74%. What's more, the morphology of final Bi particles is controllable by adding various types and concentrations of additives. As a consequence, our work lays the root for the large scale Solvothermal production of high-purity Bi particles with various regular morphologies.

关键词： Solvothermal Alcohol Metal Morphology Bismuth Reduction

Preparation and Characterization of Flower-like Cu_2SnS_3 Nanostructures by Solvothermal Route

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Journal of Materials Science & Technology 2013年第3期29卷 231-236页

作者： Xiaojuan Liang Qian Cai Weidong Xiang Zhaopin Chen Jiasong Zhong Yun Wang Mingguo Shao Zhenrong Li College of Chemistry and Materials Engineering Wenzhou University College of Materials Science and Engineering Tongji University College of Light Industry Liaoning University

Flower-like Cu2SnS3 nanostructures composed of nano-flakes were successfully synthesized by Solvothermal technique at 180 ℃ for 16 h. In the preparation process, CuCl2·H2O, SnCl2·2H2O and thiourea were used as raw materials, and ethylene glycol were used as solvent. The results showed that the obtained product was pure phase Cu2SnS3. The average diameter of Cu2SnS3 flowers and the thickness of the nano-flakes were about 1-1.5 μm and 10 nm, respectively. The influence of reaction time and solvents on the morphology, size and structure of the products was investigated by powder X-ray diffraction and field-emission scan electron microscopy （FESEM）. The ultraviolet-visible absorption spectrum measurement indicated that the band gap of the sample was about 1.26 eV and could be applied to the absorbing layer of thin solar cell. The possible formation mechanism of flower-like Cu2SnS3 was also proposed and discussed.

关键词： Cu2SnS3 nanostructures Solvothermal Semiconductor materials Formation process

Biomolecule-assisted Solvothermal Synthesis of Bismuth Sulfide Nanorods

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Journal of Materials Science & Technology 2010年第5期26卷 417-422页

作者： Jiasong Zhong Weidong Xian Lijun Liu Xinyu Yan Wen Cai Jingfeng Zhang Xiaojuan Liang College of Chemistryand Materials Engineering Wenzhou University Wenzhou 325035 China College of Materials Science and Engineering Tongji University Shanghai 200092 China

A simple biomolecule-assisted synthetic route has been successfully developed to prepare bismuth sulfide（Bi 2 S 3 ） nanorods under Solvothermal conditions.In the synthetic system,pentahydrate bismuth nitrate was employed to supply Bi source and L-cystine was used as sulfide source and complexing agent.The morphology,structure,and phase composition of the as-prepared Bi 2 S 3 products were characterized by X-ray diffraction（XRD）,energy dispersion spectroscopy（EDS）,X-ray photoelectron spectroscopy（XPS）,field-emission scanning electron microscopy（FESEM）,transmission electron microscopy（TEM）,selected area electron diffraction（SAED）,and high-resolution transmission electron microscopy（HRTEM）.The experimental results show that the nanorods have uniform diameter of 100-200 nm and length of 2-4 μm.The possible formation mechanism for the bismuth sulfide nanorods was discussed.

关键词： Bismuth sulfide Solvothermal L-cystine Nanorods

Solvothermal Synthesis and Characterization of Zinc Indium Sulfide Microspheres

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Journal of Materials Science & Technology 2011年第6期27卷 559-562页

作者： Wen Cai Yinsheng Zhao Jie Hu Jiasong Zhong Weiclong Xiang Department of Materials Science and Engineering Tongji University Shanghai 200092 China

ZnIn2S4 microspheres have been Solvothermally prepared at 160℃ for 12 h with ZnCl2.2H2O,InCl3,and thiourea as the starting reagents in ethanol.The morphology,structure,and phase composition of the asprepared product were characterized by means of X-ray powder diffraction（XRD）,field-emission scanning electron microscopy（FE-SEM）,X-ray photoelectron spectra（XPS）,transmission electron microscopy（TEM）,high-resolution TEM（HRTEM）,and selected area electron diffraction（SAED）.Results revealed that the prepared ZnIn2S4 microspheres were composed of sheetlike nanocrystals.The average diameter of the microspheres and the thickness of the nanosheets are about 1-6 μm and 10-50 nm,respectively.A possible growth mechanism of the ZnIn2S4 nanosheet-built microspheres was proposed and briefly discussed.

关键词： Solvothermal Semiconductor Microspheres Zinc indium sulfide

Solvothermal synthesis of nano-CeO_2 aggregates and its application as a high-efficient arsenic adsorbent

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Rare Metals 2019年第1期38卷 73-80页

作者： Jing-Hua Pang Ying Liu Jun Li Xiao-Jiao Yang College of Materials Science and Engineering Sichuan University

Aggregates of cerium dioxide nanoparticles(nano-CeO_2) were successfully prepared via a facile Solvothermal process in this study. The crystallographic information and morphological information of nano-CeO_2 were systematically studied by X-ray diffraction(XRD),transmission electron microscopy(TEM), laser particle size analyzer(LA) and specific surface area and pore size analyzer during the Solvothermal process. Among all the obtained samples, the 18-h Solvothermal-prepared nano-CeO_2 aggregates show the best crystallinity and the largest specific surface area of 110.92 m^2·g^(-1). Owing to the high activity derived from the high specific surface area of the aggregates, the application as arsenic(As) adsorption was also studied. The adsorption efficiency of arsenic by nano-CeO_2 aggregates was established as the function of adsorbent dose, then pH value and at last adsorption time.The results indicate that the nano-CeO_2 aggregates show a high efficiency in removing arsenic from low As concentration solution, from which the nano-CeO_2 adsorbent could be easily separated. In addition, the adsorption kinetics is best fitted to pseudo-second-order model(R^2 = 0.99999).

关键词： Nano-CeO2 Large surface Aggregates Solvothermal Removal of arsenic