Efficient Preparation and Electrochemical Properties of BiOCl/Graphite by One-step Solvothermal Method

We used the surface-pretreated graphite paper(Gp)as a carrier and loaded BiOCl with high selectivity to Cl^(-)on its surface by solvothermal method to form BiOCl@Gp electrode.The morphology,structure,and composition of the materials were characterized by scanning electron microscopy and nitrogen adsorption/desorption,and the results showed that the spherical BiOCl particles were uniformly dispersed on the surface of the Gp,forming a mesoporous BiOCl@Gp composite with a specific surface area of 22.82 m^(2)/g and a pore volume of 0.043 cm3/g.Furthermore,cyclic voltammetry and electrochemical impedance spectroscopy were used to test the electrochemical properties of the composites,and the stability of BiOCl and the high conductivity of Gp were synergistic,the BiOCl@Gp exhibited a specific capacitance of 30.2 F·g^(-1) at a current density of 0.5 A·g^(-1),and the selectivity of the BiOCl@Gp materials for Cl^(-)was significantly higher than that of SO_(4)^(2-),NO_(2)^(-),and HCO_(3)^(-).Therefore,BiOCl@Gp composite electrode materials can be used for the selective adsorption of Cl^(-)in wastewater,in order to achieve efficient wastewater recycling.

Investigation on the coordination mechanism of Pt-containing species and qualification of the alkaline content during Pt/C preparation via a solvothermal polyol method

A solvothermal assisted ethylene glycol reduction method is a common technology for Pt/C catalysts preparation. Here, the coordination mechanism of the Pt-containing species is deeply studied by innovatively adopting the ultraviolet-visible spectroscopy technology and H+ concentration detector. Moreover, the amount of Na OH that effectively coordinates Pt4+ has been tentatively qualified and the heating parameters during the preparation process of Pt/C have also been optimized. As investigated, the optimized 20-(1/22)-140-2 Pt/C(20 wt%Pt;m(Pt):m(Na OH)=1/22;heating temperature: 140 °C, heating time: 2 h) exhibits higher electrocatalytic activity towards oxygen reduction reaction(ORR) than the commercial 20 wt% Pt/C(E-TEK) in acidic media. This work provides a theoretical reserve and technical accumulation for industrialized mass production of highly efficient Pt/C catalysts for ORR in proton exchange membrane fuel cells.

Catalytic performance and synthesis of a Pt/graphene-TiO_2 catalyst using an environmentally friendly microwave-assisted solvothermal method

A Pt/graphene‐TiO2catalyst was prepared by a microwave‐assisted solvothermal method and was characterized by X‐ray diffraction,scanning electron microscopy,transmission electron microscopy,cyclic voltammetry,and linear sweep voltammetry.The cubic TiO2particles were approximately60nm in size and were distributed on the graphene sheets.The Pt nanoparticles were uniformly distributed between the TiO2particles and the graphene sheet.The catalyst exhibited a significant improvement in activity and stability towards the oxygen reduction reaction compared with Pt/C,which resulted from the high electronic conductivity of graphene and strong metal‐support interactions.

Facile Synthesis of Long,Straight and Uniform Copper Nanowires via a Solvothermal Method

Copper nanowires were facilely prepared via a solvothermal method.In this method,cetyitrimethylammonium bromide (CTAB) was used as a soft template,copper nitrate was an inorganic precursor,and absolute ethanol served as a reducing agent as well as a solvent.X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to characterize the as-prepared copper nanowires.The as-prepared copper nanowires are fairly uniform and long.The majority of them are longer than 100μm and some even longer than 200μm.Furthermore,most nanowires are quite straight.In addition, The mechanism of the growth process of copper nanowires was discussed.

Preparation,Growth Mechanisms and Characterizations of ZnSe Films via the Solvothermal Method

With diethylamine as a solvent, ZnSe films were formed on the Si substrate directly from zinc and selenium through the modified solvothermal method. The effects of holding temperature, deposition time and substrate surface treatment on the quality and morphologies of the ZnSe films were investigated. The growth mechanism of ZnSe films was proved to be a layer-nucleation growth process, which was tied in with the Stranski-Krastanov （SK） model. ZnSe films were identified by the X-ray diffraction pattern （XRD）, the scanning electron microscope （SEM）, the X-ray photoelectron spectroscope （XPS） and the photoluminescence （PL） techniques. The results indicate that the modified solvothermal method with diethylamine as a solvent is suitable to prepare high quality ZnSe films.

Effect of pH Value on the Micro-structures and Optical Properties of Nano-crystalline CuInS_2 by Solvothermal Method

Copper indium disulfide（CuInS2） nano-particles were synthesized by solvothermal method at 150 ℃ using copper（？） chloride,indium（Ш） chloride,thiourea and ethanol as raw materials,and characterized by X-ray diffraction（XRD）,field-emission scanning electron microscope（FESEM）,and UV-Vis spectra.The effects of pH value on its micro-structures and optical properties were investigated.The results show that,with the pH value increasing,the particle size of the nano-crystalline CuInS2 increases,and its band gap becomes narrower under alkaline condition.The band gaps of CuInS2 nano-particles are from 1.52 eV to 1.93 eV,which makes them promising candidates as absorber materials for photovoltaic applications.

Controlled Synthesis of Sea-urchin-like ZnO Nanomaterials with the Aid of Ethylene Glycol Using a Solvothermal Method

Sea-urchin-like ZnO nanomaterials were successfully synthesized by decomposition of zinc acetate precursor in the presence of sodium hydroxide and ethylene glycol（EG） in an ethanol solution using a solvothermal method at 180 ℃ for 12 h.The crystalline phase and morphology of the resultant nanomaterials were characterized by X-ray diffraction（XRD）,scanning electron microscopy（SEM）,transmission electron microscopy（TEM）,selected-area electronic diffraction（SAED） and high-resolution electron microscopy（HRTEM）.Interestingly, the sizes and prod length of the samples can be easily tuned by changing the amount of directing agent EG and keeping other reaction conditions unchangeable. On the basis of our experimental outcomes, EG-controlled-nucleation-growth formation mechanism was proposed to correspond for the sea-urchin-like ZnO growth processes. And the photoluminescence （PL） spectra of the as-selected samples were measured at room temperature, 480 nm. presenting two emission peaks centered at - 388 and

Exciton emissions of CdS nanowire array fabricated on Cd foil by the solvothermal method

Nanowires have recently attracted more attention because of their low-dimensional structure, tunable optical and electrical properties for next-generation nanoscale optoelectronic devices. Cd S nanowire array, which is(002)-orientation growth and approximately perpendicular to Cd foil substrate, has been fabricated by the solvothermal method. In the temperature-dependent photoluminescence, from short wavelength to long wavelength, four peaks can be ascribed to the emissions from the bandgap, the transition from the holes being bound to the donors or the electrons being bound to the acceptors, the transition from Cd interstitials to Cd vacancies, and the transition from S vacancies to the valence band,respectively. In the photoluminescence of 10 K, the emission originated from the bandgap appears in the form of multiple peaks. Two stronger peaks and five weaker peaks can be observed. The energy differences of the adjacent peaks are close to 38 me V, which is ascribed to the LO phonon energy of Cd S. For the multiple peaks of bandgap emission, from low energy to high energy, the first, second, and third peaks are contributed to the third-order, second-order, and first-order phonon replica of the free exciton A, respectively;the fourth peak is originated from the free exciton A;the fifth peak is contributed to the first-order phonon replica of the excitons bound to neutral donors;the sixth and seventh peaks are originated from the excitons bound to neutral donors and the light polarization parallel to the c axis of hexagonal Cd S, respectively.

Thermoelectric Properties of n-type Poly(nickel 1,1,2,2-ethenetetrathiolate)Prepared by a New One-step Solvothermal Method

Poly(nickel 1,1,2,2-ethenetetrathiolate)(poly[Na_(x)(Ni-ett)])is one of the most promising n-type organic thermoelectric materials which can be used in wearable devices.However,the conventional solution method is time-consuming and the prepared poly[Na_(x)(Ni-ett)]usually has poor crystallinity,which does not benefit for achieving high thermoelectric performance.Here,a new one-step solvothermal method under the high reaction temperature and high vapor pressure was developed to prepare poly[Na_(x)(Ni-ett)]with a quite short period.The experimental results show crystallinity and electrical conductivity are greatly enhanced as compared with those prepared by conventional solution method.As a result,a maximum ZT value of 0.04 was achieved at 440 K,which is about four times of the polymer prepared by the conventional solution method.This study may provide a new route to enhance the TE properties of n-type organic thermoelectric materials.

Framework-solvent interactional mechanism and effect of NMP/DMF on solvothermal synthesis of [Zn_4O(BDC)_3]_8

In order to explore the effect mechanism of solvent on the synthesis of the metal organic framework materials, the microscopic interaction between solvent and framework and the effects of N,N-dimethyl-formamide(DMF) or N-methyl- 2-pyrrolidone(NMP) on solvothermal synthesis of [Zn4O(BDC)3]8 were investigated through a combined DFT and experimental study. XRD and SEM showed that the absorbability of NMP in the pore of [Zn4O(BDC)3]8 was weaker than that of DMF. The thermal decomposition temperature of [Zn4O(BDC)3]8 synthesized in DMF was higher than that in NMP according to TG and FT-IR. In addition, the nitrogen sorption isotherms indicated that NMP improved gas sorption property of [Zn4O(BDC)3]8. The COSMO optimized calculations indicated that the total energy of Zn4O(BDC)3 in NMP was higher than that in DMF, and compared with non-solvent system, the charge of zinc atoms decreased and the charge value was the smallest in NMP. Furthermore, the interaction of DMF, NMP or DEF in [Zn4O(BDC)3]8 crystal model was calculated by DFT method. The results suggested that NMP should be easier to be removed from pore of materials than DMF from the point of view of energy state. It can be concluded that NMP was a favorable solvent to synthesize [Zn4O(BDC)3]8 and the microscopic mechanism was that the binding force between Zn4O(BDC)3 and NMP molecule was weaker than DMF.

Alcohol Solvent Effect on Fluorescence Properties in the Solvothermal Synthesis of Carbon Quantum Dots

Highly monodisperse carbon quantum dots(CQDs)were synthesized by a solvothermal method using L-ascorbic acid as carbon source and different simple alcohols(methanol,ethanol,ethylene glycol,and isopropanol)as reaction solvents at 180℃for 4 hours.The performance of CQDs was characterized by transmission electron microscope(TEM),Fourier infrared spectrometer(FTIR),UV-visible spectrophotometer,and fluorescence spectrophotometer.The results show that the prepared CQDs are wavelength-dependent,and have good hydrophilicity and similar surface compositions.However,there are more carbon and oxygen-containing functional groups on the surface of CQDs prepared with ethanol(CQDs-ET),and the type and number of functional groups will directly affect the fluorescence emission of CQDs.Also,it is found that the luminescence mechanisms of CQDs prepared by this solvothermal method are mainly based on the defect state of the oxygen group surface.And alcohol solvents do not directly participate in the formation of carbon nuclei during the reaction process,but it will affect the number and type of surface groups.Therefore,the influence of surface groups on the CQDs performance is greater than that of carbon nuclei in this experiment.

A Facile Solvothermal Synthesis of Monodisperse Ni Nanoparticles

A simple solvothermal approach was developed to synthesize uniform spherical monodisperse Ni nanoparticles, which can easily disperse in nonpolar solvents to form homogenous colloidal solution. The as-prepared sample was characterized by XRD, TEM, and FTIR. The results indicate that Ni nanoparticles have the structure of face-centered cube and a narrow distribution with a diameter of （3.5±0.5） nm. The FTIR spectrum reveals that the nanoparticles are coated with oleic acid. In the synthetic process, N2H4·H2O was used as a reducing agent and oleic acid as a surfactant. The probable formation mechanism of the spherical nanoparticles was also discussed.

Solvothermal Synthesis of α-Fe2O3 Porous Nanobelts and Their Enhanced Acetone-sensing Properties

Porous α-Fe2O3 nanobelts have been prepared via a solvothermal route and subsequent calcination. The as-prepared nanostructure was characterized by XRD, FESEM, TEM, N2 adsorption-desorption isotherms, etc. The α-Fe2O3 nanobelts presented obvious porous structures with the length of ca. 1~2μm, width of ca. 200~350 nm and thickness of ca. 30~60 nm. It was found that the assistance of inorganic additives played an important role in the shape control of α-Fe2O3 nanostructure. The gas-sensing performance of the fabricated sensor based on α-Fe2O3 nanobelts sample was also investigated, and the response towards 1000 ppm acetone can reach 24.4. In addition, the gas-sensing conductive mechanism of the sensor was also proposed.

溶剂热法制备磷酸锰锂的优化研究

橄榄石结构的磷酸锰锂(LiMnPO_(4))具有比容量高､热稳定性好和原料来源广泛等特点,与同为橄榄石结构的磷酸铁锂相比具有更高的放电电压。采用溶剂热法制备了高性能的磷酸锰锂正极材料,通过对过程参数进行优化实现材料性能的提升,以柠檬酸为添加剂优化颗粒形貌得到纳米级颗粒,并对碳层包覆进行优化。结果表明,柠檬酸添加量为1 mmol时,椭球状颗粒平均尺寸为42.3 nm;当以蔗糖为碳源且与LiMnPO_(4)质量比为1∶2时得到的碳层包覆颗粒尺寸较小､碳层石墨化程度更高;在最优参数下制备的LiMnPO_(4)材料具有更高的首次放电容量(126.9 mAh/g)及更优的倍率性能。

β-In_(2)Se_(3)的溶剂热合成及其光催化性能研究

β-In_(2)Se_(3)由于良好的迁移率和优异的光响应而被广泛应用于各个领域。然而,由于In_(2)Se_(3)有多种复杂的晶体结构和铟易水解,导致溶液法难以制备出层状β-In_(2)Se_(3)。采用氯化铟、硒粉和乙二胺为原料,通过溶剂热法制备了β-In_(2)Se_(3)粉体。利用拉曼光谱仪、傅里叶红外光谱仪、热重分析仪、扫描电子显微镜和荧光分光光度计等仪器对粉体的结构、形貌和光学性能进行了表征。以甲基橙溶液为降解物,研究了粉体的光催化性能。结果表明,所制备的粉体主要成分为β-In_(2)Se_(3),呈片层状结构;粉体在紫外光区和可见光区具有较好的吸光度,光学带隙约为2.01 eV,具有很好的荧光特性;β-In_(2)Se_(3)对甲基橙具有光催化性能,经过5 h的紫外线照射,对甲基橙的降解率可达到81%。该结果拓展了β-In_(2)Se_(3)在降解有机物污染物方面的应用。

纳米TiO_(2)微球的制备及光催化降解气相苯特性

以四氯化钛和尿素为原料,通过溶剂热法制备了纳米TiO_(2)微球。利用XRD、FE-SEM、TEM、UV-Vis、BET测试手段对样品的组成、结构、形貌、光学性能、比表面特性进行分析,以气相苯为目标降解物,研究不同溶剂热时间所制备的微球对光催化活性的影响。结果表明,随溶剂热时间的延长,TiO_(2)微球结构经历了实心-核壳-空心的演变过程,但均由20 nm以下的颗粒组成。此类微球的光吸收带边出现明显“蓝移”现象,且光吸收性能较P25 TiO_(2)要高,比表面积是其3~5倍。其中溶剂热时间为6 h所制备的核壳结构微球光催化活性最佳,降解气相苯的矿化率高达93%,高于P25 TiO_(2)近3倍,分析表明,该优异性能得益于核壳结构对光的充分反射吸收和高比表面积导致的吸附协同光催化特性。

两种不同形貌纳米Cu_(2)(Salen)_(2)的制备与表征综合实验设计

分别采用反溶剂沉淀法和溶剂热法制备了两种不同形貌的Cu_(2)(Salen)_(2)纳米材料,通过红外光谱(IR)、X射线粉末衍射(XRD)和扫描电子显微镜(SEM)等手段对其进行了结构和形貌表征,并利用Olex2软件对该配合物的分子结构和配位情况进行了展示。本实验内容涉及有机合成、配位化学、纳米材料制备与表征、晶体结构分析软件应用等,将基础理论知识与现代科技手段有机统一,兼顾基础的同时,注重创新能力和综合素质的培养。本实验将前沿科研成果转化到实验教学实践中,使二者相互促进,形成良性循环。

Al掺杂硫铟锌光催化剂的制备综合实验教学设计与实践

结合化学工程与工艺专业人才培养方案和实践教学体系的要求,设计了硫铟锌(ZnIn2S4)基光催化剂的制备综合性实验。实验采用溶剂热法制备了Al掺杂硫铟锌光催化剂,系统地表征分析了光催化剂的晶体结构、形貌以及光电化学特性。该实验是将典型的科研成果转化为实验教学内容,有助于学生了解该领域的前沿科学成果和研究方法,掌握光催化剂的制备技术,进而深入理解光电化学性能相关专业理论知识。科研反哺教学有利于创新实验教学内容,激发和培养学生的创新意识和专业综合实践能力。

TiO_(2)/石墨烯基复合材料的制备及光催化降解染料研究

采用改进Hummers法制备氧化石墨烯(GO)和水解法制备的TiO_(2)及溶剂热法制备了还原氧化石墨烯(rGO)和一系列不同浓度的rGO/TiO_(2)纳米复合材料(0、5%、10%、15%、20%质量分数),并对合成产物进行SEM、XRD、XPS、DRS、Raman等表征,研究不同实验条件下纯TiO_(2)和rGO/TiO_(2)复合催化剂对亚甲基蓝染液(MB)的降解效果。结果表明,复合光催化剂中TiO_(2)主要为锐钛矿相,溶剂热合成引入的还原氧化石墨烯(rGO)对TiO_(2)的物相没有产生影响,rGO的引入使得rGO/TiO_(2)吸收带发生一定红移,TiO_(2)禁带宽度由3.23降低至3.09 eV;合成的(15%质量分数)rGO/TiO_(2)具有最佳的光催化效果,光催化活性最高,在100 W高压汞灯照射下70 min对20 mg/L的亚甲基蓝染料的降解率达97.6%;在500 W氙灯光源下照射70 min对20 mg/L亚甲基蓝染料的降解率达到93.2%,(15%质量分数)rGO/TiO_(2)复合光催化剂具有良好的光催化降解性及循环稳定性,5次循环光催化降解后,rGO/TiO_(2)有86.1%的降解效率。表现出了优异的吸附和光催化性能,这可为光催化处理废液提供了一种有效的方法。

TpBD-3COOH COF的制备及对废水中罗丹明B吸附性能研究

研究了以三醛基间苯三酚(Tp)、4,4-二氨基联苯-2,2-二羧酸(DBd)和联苯二胺(BD)为原料,通过溶剂热法制备新型羧基官能化的二维共价有机框架材料TpBD-3COOH COF,并用于吸附罗丹明B染料废水,采用XRD、FT-IR、SEM对其形貌进行了表征。结果表明:在pH=4、TpBD-3COOH COF用量8 mg、废水中罗丹明B质量浓度10 mg/L条件下吸附60 min,罗丹明B去除率可达95%;5次重复试验后,TpBD-3COOH COF对罗丹明B的去除率仍可达70%以上,且吸附过程与准二级动力学模型和Langmuir等温吸附模型相吻合。