溶剂热法制备纳米晶Sb2O3

以 SbCl3为锑源,采用溶剂热法制备了纳米Sb2O3(1),其结构经XRD和SEM表征.溶剂的种类和体系 pH可以控制1的晶型及形貌.水作溶剂时,1为板状斜方晶型;乙醇作溶剂时,1为单一斜方晶型或立方和斜方混合晶型;用乙醇和乙二醇混合溶剂时,1为斜方晶型;用乙醇和异丙醇混合溶剂时1为单一立方晶型.     

溶剂热法制备纳米MnOOH

MnOOH在常温常压下为黑色固体粉末,经氧化或还原可制成电子工业中生产锰锌铁氧体软磁材料的重要原料.以KMnO4与MnSO4为原料,在水与正丙醇混合溶剂中反应制备了MnOOH纳米棒;采用X射线粉末衍射仪(XRD)、差热-热重(DTA-TG)分析系统、红外光谱仪(IR),以及扫描电镜(SEM)、透射电镜(TEM)、X射线...     

溶剂热法制备球状Cu2ZnSnS4纳米晶及其表征

通过简单的溶剂热法合成了锌黄锡矿结构的Cu2ZnSnS4(CZTS)纳米晶,使用L-半胱氨酸作硫源和络合剂,以金属氯化物作前驱体,在180°C下反应16h成功获得了CZTS微球.使用X射线衍射(XRD)仪,场发射扫描电子显微镜(FESEM)、能量色散谱(EDS)、高分辨透射电子显微镜(HRTEM)、多功能X射线光电子能谱仪(XPS)、紫外-可见(UV-Vis)分光光度计对产物的物相、结构、形貌及光学性能进行表征.结果表明:所得的产物为纯相锌黄锡矿结构的CZTS纳米颗粒,CZTS微球直径为400-800nm,并可观察到微球是由大量厚度约20nm的纳米片构成;将CZTS颗粒均匀分散在异丙醇中,测试后估算其禁带宽度约1.58eV,与薄膜太阳能电池所需的最佳禁带宽度相近.并对其形成机理进行了初步探讨.     

简捷溶剂热技术制备纳米棒基PbS树枝晶

以氯化铅和硫氰酸钾为原料,乙二醇为溶剂,采用简捷溶剂热技术制备了半导体PbS纳米棒基树枝晶。粉体用XRD、XPS、FESEM、TEM和ED进行了表征。单个PbS树枝晶具有三维空间结构,由一个主干和四个相互垂直侧枝组成。主干长2～10 μm,直径150～300 μm,每组侧枝纳米棒相互平行,沿主干垂直生长,棒长0.1～1.5 μm,直径80～180 nm。并对生长过程进行了探讨。     

溶剂热法合成锐钛矿型二氧化钛纳米晶的形状演化规律

以钛酸四丁酯为前驱体,乙醇为溶剂,月桂酸和十二胺为共同稳定剂,采用溶剂热法制备了不同形状的锐钛矿型二氧化钛纳米晶。利用透射电子显微镜(TEM)、选区电子衍射(SAED)、X射线衍射(XRD)、傅里叶变换红外(FTIR)光谱和热失重-差热分析(TG-DTA)等技术对纳米晶的结构、尺寸、形貌及形状进行了系统的表征,并探讨了月桂酸与十二胺不同配比时纳米晶的形状演化规律。结果表明:用溶剂热法在不同配比情况下获得的二氧化钛均为锐钛矿相;在月桂酸与十二胺总摩尔量不变的情况下,随着十二胺含量的增加,二氧化钛纳米晶的形状由球形逐渐演化为棒状,且结晶化程度在两者摩尔比为1:1时最好;月桂酸与十二胺稳定剂与纳米晶内核之间以桥接配位体的形式结合,且稳定剂在样品中的含量约为5%。     

溶剂热合成单分散硫化镉纳米晶

在双表面活性剂十八胺和油酸存在条件下, 以氯化镉和硫粉作为反应前驱物, 通过简单的溶剂热方法合成单分散性闪锌矿硫化镉纳米晶, 粒径大小在13 nm. 用X射线衍射(XRD)、透射电子显微镜(TEM)对产物的结构和形貌进行了表征, 同时对硫化镉纳米晶的紫外吸收谱和光致发光谱(PL)性能进行了表征. 实验结果表明合成的样品具有很好的发光性能, 此外溶剂热反应的温度对纳米晶的单分散性有重要影响. 并对硫化镉纳米晶的形成机理做了初步的研究.     

Mn3O4的溶剂热法制备及晶粒生长动力学研究

非化学计量M n3O4-δ由八面体的M n2O3-δ相与四面体的M nO相组成,结构中的氧空位是其催化活性中心[1]。M n3O4-δ用途广泛,其高催化活性可用于环保领域分解去除废气中的CO、N2O、NO与NH3等气体或从废气中去除有机物等[2~4],高纯四方相M n3O4-δ纳米晶适用于制作软磁性材料如高     

溶剂热法制备小粒径无皂均聚物纳米胶乳粒子

采用溶剂热法，用过硫酸钾引发苯乙烯均聚，制备出分散性好、粒径约30nm的无皂聚苯乙烯肢乳纳米粒子。讨论了引发剂的用量、助溶剂丙酮的含量、反应温度对粒子尺寸及其粒径分布的影响。实验结果表明：在一定范围内，温度改变，粒径变化较快；引发剂、丙酮和单体用量改变时，粒径变化较缓慢。     

溶剂热法制备无皂PMMA纳米粒子

用溶剂热法制备无皂聚甲基丙烯酸甲酯(PMMA)纳米粒子,讨论了温度和丙酮含量对粒子粒径和分散度的影响,用DTA,^1HNMR,TEM,GPC等对产物进行了表征。结果表明无皂PMMA纳米粒子的粒径约60衄,分子量分布较好、以间同结构为主;随着反应温度增高,PMMA的玻璃化温度增加,间同结构含量有所增大,纳米粒子的粒径逐渐减小,粒径分布变差;溶剂中丙酮含量增加时,粒径逐渐减小,粒径的分布变差。     

纳米晶CuLa3Se5微波溶剂热合成及结构研究

采用微波溶剂热法合成纳米晶CuLa3Se5,具有快速,节能、纯度高、粒度小(平均粒径为20～30 nm)等优点.通过X射线粉末衍射(XRD)、透射电子显微镜(TEM)、扫描电镜能谱分析(EDS)和X射线光电子能谱(XPS)等手段表征其组成.讨论了微波溶剂热合成纳米晶的机制.漫反射紫外-可见吸收光谱(UV-Vis)表明标题化合物禁带宽度为2.27 eV,具有优良的半导体性能.     

溶剂热法制备八面体纳米结构四氧化三铁

利用乙二醇溶剂热法成功制备了八面体结构四氧化三铁,利用场发射扫描电子显微镜、透射电子显微镜、选区电子衍射仪、X射线衍射仪及超导量子干涉仪分析了合成产物的形貌、晶体结构及磁学性能,并探讨了多种实验条件对纳米结构形成的影响.结果表明所得八面体四氧化三铁纳米晶粒径均一,棱边尺寸约为120nm,室温下显示铁磁性质.     

Impact of polyvinylpyrrolidone and quantity of silver nitrate on silver nanoparticles sizing via solvothermal method for dye-sensitized solar cells

The multiple sizing of silver nanoparticles (AgNPs) were synthesized from the miscible compound of ethylene glycol (EG), polyvinylpyrrolidone (PVP) and silver nitrate (AgNO3) via the solvothermal method. During the synthesis, the PVP-AgNO3 was contemplated as a paramount parameter. Using the simple method of solvothermal, the sizing of AgNPs was easily controlled in accord with the augmentation of PVP-AgNO3 at secured and moderate temperature. In regards to the sizing of AgNPs, the presence of minimum agglomeration, the absorption capability and chemical structures were highlighted through a series of verification includes ultraviolet–visible (UV–Vis) spectroscopy, Fourier-transform infrared (FTIR) spectroscopy and transmission electron microscopy (TEM) analysis. The effectiveness of the synthesized AgNPs was further investigated and compared with the commercial AgNPs by incorporating the AgNPs into titanium dioxide (TiO2) semiconductor film-based dye-sensitized solar cells (DSSCs). Results signified that the spherical AgNPs with produced sizing within the range of 19.6 to 45.2 nm were greatly impacting by tunable quantities of PVP-AgNO3, which was validated in the forms of linear equations. A larger size promotes a slower nucleation rate that conduces agglomeration. In opposition to this, the smallest size of AgNPs develops a faster formation rate of Ag ions into AgNPs, inducing the deterrent of agglomeration in light of notable particle dispersion. The power conversion efficiency (PCE) contributed by the incorporation of synthesized AgNPs into TiO2 is also 41.2% higher than that of the commercial AgNPs-TiO2. This is because the synthesized AgNPs provides less agglomeration which led to a better surface plasmonic effect towards the nanoparticles.     

溶剂热还原法制备蛋壳状碳材料

Eggshell-like carbon materials with high yields have been synthesized by a solvothermal route in a stainless steel autoclave using metallic zinc and absolute ethanol as starting materials. The products were characterized by X-ray powder diffractometry (XRD)， energy-dispersive X-ray spectroscopy (EDX)， Raman spectroscopy and scanning electron microscopy (SEM). The eggshell-like carbon spheres had diameters ranging from 500 nm to 1 μm. The optimal reaction conditions to obtain eggshell-like carbon materials were 600 ℃ and 12 h.     

Preparation of submicrometer-sized copper and silver crystallites by a facile solvothermal complexation-reduction route

Pure submicrometer-sized copper and silver crystallites have been directly synthesized via solvothermal treatment of CuCl₂·2H₂O or AgNO₃ in ethylenediamine (EDA) at 80-180 °C for 15-20 h, and characterized by means of X-ray powder diffraction, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and transmission electron microscopy. It was suggested that the formation of copper and silver crystallites in this solvothermal system be through a typical complexation-reduction process, in which EDA serves not only as a reducing reagent, but also as a complexing solvent.     

基于纳米Ag粒子的表面等离子体共振光谱测定CN-的研究

利用UV-辐照光化学还原法制备了平均直径为20 nm的黄色胶体银溶液,银粒子的表面等离子体共振(SPR)光谱的最大吸收波长位于399 nm处,摩尔吸光系数为1.3×104 L·mol-1·cm-1.利用Ag粒子与CN-反应的动力学特性,研究了SPR光谱的λMAX吸光与CN-浓度的关系及其影响因素,拟定了检测环境水样中隐色、有毒CN-离子的方法.标准工作曲线的线性相关系数0.9995,测定下限0.05 μg/mL, 相对标准偏差RSD(%)≤6.1 (n=5).对Ag粒子与CN-反应的机理进行了探讨.     

溶剂热法合成CuInS2微球及表征

以CuCl2·2H2O为铜源,InCl3·4H2O为铟源,硫脲为硫源,乙醇为溶剂在160℃水热反应12h合成了花状CuInS2,利用SEM、EDX、X射线和ICP对其形貌及结构进行表征,并讨论了不同溶剂对产物形貌的影响.     

Synthesis of beltlike CdS nanocrystals via solvothermal route

CdS nanocrystals with a beltlike morphology were prepared via a low-temperature solvothermal route in ethylenediamine. The obtained nanocrystals were characterized by X-ray powder diffraction, transmission electron microscopic, ultraviolet-visible and fluorescence spectroscopy. In the mixed solvents of ethylenediamine and distilled water, CdS nanocrystals with various morphologies were obtained with the change of the volume ratio of the two constituents.     

乙二胺溶剂热还原法制备碳纳米管

以乙二胺作为溶剂和碳源,用KBH4还原NiCl2得到的镍作为催化剂,于300℃制备碳纳米管。X-射线衍射(XRD)、透射电子显微镜(TEM)、选区电子衍射(SAED)和Raman光谱分析证明,产品为多壁碳纳米管,直径约为100nm,长度达几微米。该方法具有反应温度低、反应时间短、操作简便等特点。     

Preparation and lithium doping of gallium oxynitride by ammonia nitridation via a citrate precursor route

Gallium oxynitride, isostructural to hexagonal gallium nitride (h-GaN), was obtained by ammonia nitridation of a precursor prepared from the addition of citric acid to an aqueous solution of gallium nitrate. Gallium oxynitride produced at 750 °C had a small amount of gallium vacancies, and was formulated as (Ga_0.89□_0.11) (N_0.66O_0.34) where the symbol □ stands for gallium vacancy. Both the gallium vacancies and oxygen substituted for nitrogen were randomly distributed within the structure. The amount of vacancies decreased with nitridation temperatures in the range of 750-850 °C. Approximately, 10 at% Li⁺ was doped into the gallium oxynitride, using a similar preparation with the additional presence of lithium nitrate, resulted in the random substitution of Ga³⁺ in an atomic ratio of Li/Ga<1 at 750 °C. Oxygen was codoped with lithium and substituted nitrogen in the wurtzite-type crystal lattice. These substitutions reduced the electrical conductivity in the gallium oxynitride semiconductor. A new oxynitride, Li₂Ga₃NO₄, was also obtained with Li₂CN₂ impurity using similar preparations from a mixture of Li/Ga?1. The crystal structure was isostructural with h-GaN, and was refined as P6₃mc with a=0.31674(1) nm, and c=0.50854(2) nm. The Ga and Li occupancies at the 2b site were refined to be 0.6085 and 0.3915, respectively, assuming that the other 2b site was randomly occupied with 1/5O and 4/5N. When the new compound was washed for over 1 min for the removal of Li₂CN₂ impurities, it was decomposed to a mixture of α-GaOOH and α-LiGaO₂. The as-prepared product with Li/Ga=1 showed the highest intensity in yellow luminescence among the products under excitation at 254 nm.