Cu3Pt/MgO纳米粒子的制备及甲醛重整制氢性能

以氧化镁(MgO)为载体、H2 PtCl6·6 H2O和CuCl2溶液为催化剂前驱体,通过浸渍还原法制备Cu3 Pt/MgO合金纳米催化剂;采用X射线衍射仪(XRD)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、能量散射X射线(EDX)和电子顺磁共振(EPR)等对催化剂的形貌、晶型和结构进行表征;考察了Cu3...     

纳米CuInSe_2的溶剂热合成与表征

以乙二胺为溶剂,CuCl2.2H2O、InCl3.4H2O和Se粉末为反应物,采用低温溶剂热工艺制备了铜铟硒(CuInSe2,简称为CIS)纳米粉末。通过X射线衍射、扫描电镜、X射线光电子能谱等测试分析方法对产物进行测试和表征。研究结果表明,反应温度、反应物超声预处理等工艺条件对产物形貌有很大的影响。降低反应温度有利于获得均匀的CuInSe2粉末,反应物超声预处理可以获得分散性较好的球形CuInSe2纳米粉末。所得产物为具有黄铜矿构型的CIS纯相。     

采用水热法制备磁性Fe_3O_4纳米棒

以FeCl3·6H2O、2-氨基-2-甲基-1-丙醇、水合肼为主要反应物,水热法制备Fe3O4纳米棒。通过扫描电子显微镜(SEM)、X射线衍射分析仪(XRD)和振动磁强计(VSM)等表征手段进行表征,并对Fe3O4纳米棒的形成机理进行探讨。结果表明,制得的Fe3O4纳米棒,具有较高的饱和磁化强度。     

纳米γ-Fe2O3粉体的合成及其气敏特性研究

以分析纯还原 Fe粉、Fe Cl3· 6 H2 0等为原料 ,以沉淀反应法制备了纳米γ- Fe2 O3粉体 ,采用 X射线衍射、扫描电镜对其晶相和形貌进行了分析 ,并初步检测了 γ- Fe2 O3厚膜对还原性气体的敏感性。结果表明 ,该合成方法工艺简单 ,由此制得的纳米γ- Fe2 O3粉在 2 0 0～ 30 0℃低温条件下对还原性气体具有良好的气敏特性     

金属-有机骨架[Cu(INA)2·H2O]n 纳米晶的超声制备及其催化性质研究

在 EtOH/DMF/H2O (2∶2∶ 1 ) 的混合溶剂中,以硝酸铜(Cu(NO3)2·3H2O)和异烟酸(HINA)为原料,超声制备了具有三维结构的金属-有机骨架(MOF)[Cu(INA)2· H2O]n 纳米晶,并利用粉末 X -射线衍射(XRD)、红外光谱(IR)、透射电子显微镜(TEM)等分别对目标产物的结构和形貌进行了表征.研究结果表明,与传统的水热/溶剂热等制备方法相比较,超声制备方法具有合成时间短(5-60 min)、反应条件温和(常温常压)和反应产率高(50.9%-60.2%)等优点.相关催化动力学研究表明,所制备 MOF纳米晶在乙腈和水的混合溶剂中能够选择性催化氧化苯甲醇为苯甲醛,分别研究了不同的反应温度、催化剂量以及空气流量对催化反应的影响,并初步探讨了催化反应机理.     

类球状和棒状Eu_2O_3和Sm_2O_3纳米粒子的合成与表征

采用表面活性剂和超声波辅助的沉淀法合成了类球状和棒状多晶Eu2O3和Sm2O3纳米粒子,并用透射电镜(TEM)、选区电子衍射(SAED)、X射线衍射(XRD)、N2吸附-脱附和紫外-可见漫反射(UV-Vis DRS)技术表征了其物理性质.结果表明,以十二烷基硫酸钠作表面活性剂所得产物为类球状体心立方晶相Eu2O3和单斜晶相Sm2O3纳米粒子,比表面积为44~49 m2/g;而以聚乙烯吡咯烷酮作表面活性剂所得产物则是棒状正交晶相Eu2O3和体心立方晶相Sm2O3纳米粒子,比表面积为34~37 m2/g.除了在紫外光区(λ390 nm)有较强的吸收外,类球状和棒状Eu2O3和Sm2O3纳米粒子在可见光区(390 nmλ535 nm)也有不同程度的吸收.该吸光性能差异与所得稀土氧化物的表面形貌和晶体结构有关.     

Cr2WO6纳米晶的水热法制备及其对亚甲基蓝的选择性吸附性能

以Cr(NO3)3·6H2O、Na2WO4·2H2O为原料,去离子水为溶剂,采用水热法在不同pH条件下成功制备出颗粒状结构的Cr2WO6纳米晶。采用X-射线衍射仪(XRD)、扫描电子显微镜(SEM)、能谱分析(EDS)和Lambda 950分光光度计分别对产物的物相、形貌和光学性能进行表征,讨论了不同pH对Cr2WO6纳米晶的结构的影响,并对合成粉体的选择性吸附性能进行了研究.结果表明:在水热条件下,前驱体的酸碱性对合成Cr2WO6纳米晶的结构有很明显的影响,只有在弱酸条件下才可以得到Cr2WO6纳米晶.此外,与传统固相法得到的产物相比,水热条件下制备的Cr2WO6纳米晶对亚甲基蓝具有明显优越的选择性吸附性能.     

热喷涂法制备Sb掺杂的SnO_2薄膜

以SnCl4·5H2O和SbCl3为原料,采用喷雾热分解法在管状石英玻璃基材上制备出Sb掺杂的SnO透明导电薄膜,并采用X射线衍射仪(XRD)和原子力显微镜(AFM)对薄膜的结构和表面形貌进行了分析,研究了Sb掺杂量和喷涂温度对薄膜方阻及结构的影响.结果表明:当Sb掺杂量为6 mol%、成膜温度为500℃时,薄膜的方阻达到最低(65Ω/□),结构最致密.     

尖晶石型ZnGa_2O_4纳米晶的制备及光催化性能

采用共沉淀法合成了尖晶石型ZnGa2O4纳米晶,利用X射线衍射(XRD)、氮吸附、紫外-可见漫反射光谱(UV-Vis DRS)、电子自旋共振谱(ESR)、扫描电镜(SEM)和透射电镜(TEM)对样品进行了详细的表征。共沉淀法合成的Zn-Ga2O4纳米晶紫外光下降解水杨酸的活性明显高于高温固相法合成的ZnGa2O4。对不同方法合成的ZnGa2O4活性差异的原因进行了探讨,提出了ZnGa2O4降解水杨酸的反应机理。     

纳米钒酸铋的水热合成及其可见光光催化降解罗丹明B

以Bi(NO3)3·5H2O和NH4VO3为原料,采用水热法合成了BiVO4纳米颗粒,X射线衍射(XRD)表征结果显示所制备的BiVO4颗粒为单斜晶结构.紫外-可见漫反射(DRS)测定结果表明,BiVO4的禁带宽度为2.46 eV.以罗丹明B为目标降解物,研究了样品在可见光下的光催化性能,最佳反应条件为:罗丹明B的初始...     

Sol-gel preparation and characterization of Co_3O_4 nanocrystals

A new citrate acid-hydrazine sol-gel route for preparation of Co3O4 nanoparticles has been developed. Co3O4 nanoparticles with different particle-sizes and morphology were prepared at different heat-treatment temperatures and the pure cubic nanocrystals of Co3O4 were obtained at 600℃. The synthesis process was monitored by infrared spectroscopy (IR), thermal gravimetric and differential thermal analysis (TG-DTA). The structure and morphology of Co3O4 nanocrystals were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and X-ray-photoelectron spectroscopy (XPS). The infrared absorption bands blue-shifted with particle size decreasing, which could be attributed to increasing surface effect. XPS results showed that predominant species at surface layers of Co3O4 nanocrystals are octahedral Co (Ⅲ).     

铌酸锶铋粉体的水热法制备及表征

以SrCl2·6H2O、Bi（NO2）。·5H2O和Nb2O5为原料,以NaOH为矿化剂,采用水热法在较低温度和较短时间内合成出纯相的SrBi。Nb2O9陶瓷粉体,比传统固相法的合成温度降低了1000℃左右;同时,通过x射线衍射仪（X-raydiffraction,XRD）、扫描式电子显微镜（scanningelectronmicroscope,SEM）等分析手段对粉体的物相、微观形貌进行研究,并分析反应温度、时间和矿化剂浓度对粉体制备结果的影响。结果表明,纯相的SrBizNb2O9粉体合成的最佳工艺条件为240℃,4h,2mol／L,其显微结构较为均匀,平均粒径为1μm,该研究工艺简单,周期较短。     

一种基于钕离子的金属有机框架化合物的合成与发光性质分析

以一种V型3,5-二（4-羧基苯基）-4-苯基-1,2,4-三唑（H2PhTz）为有机配体通过溶剂热法合成出一种金属-有机框架化合物[Nd（PhTz）3/2（H2O）2]n（MOF_Nd）,其中,PhTz是3,5-二（4-羧基苯基）-4-苯基-1,2,4-三唑的二价阴离子。利用单晶X-射线衍射、粉未X-射线衍射及红外吸收光谱等分析手段表征了MOF_Nd的分子结构与纯度。X-射线单晶衍射分析表明含有1维孔道结构的MOF_Nd单晶属于的三斜晶系的P1空间群。MOF_Nd的固体粉末在紫外光的激发下,能发出位于385nm的半峰宽为48nm的荧光峰,该荧光发射被归为配体的π*→π电子跃迁。     

Enhanced photocatalytic activity of (La, N) co-doped TiO_2 by TiCl_4 sol-gel autoigniting synthesis

(La, N) co-doped TiO2 photocatalysts were synthesized using TiCl4 sol-gel autoigniting synthesis (SAS) starting from a complex compound system of TiCl4-La(NO3)3-citric acid-NH4NO3-NH3?H2O, in which the (La, N) co-doped process was accom- plished in the formation of TiO2 nanocrystals. The prepared samples were characterized by using X-ray diffraction (XRD), X-ray photoemission spectroscopy (XPS) and UV-vis diffuse reflectance spectra. The results indicated that nitrogen and lanthanum were incorporated into the lattice and interstices of titania nanocrystals, which resulted in narrowing the band gap and promoting the sepa- ration of photoexcited hole-electron pairs, respectively, and showing expected red-shifts and enhanced photocatalytic activity under visible light. The mechanism on nitrogen doping and enhancement in photocatalytic activity of (La, N) co-doped titania by SAS was discussed in detail.     

One-pot synthesis of Sb-Fe-carbon-fiber composites with in situ catalytic growth of carbon fibers

A Sb-Fe-carbon-fiber (CF) composite was prepared by a chemical vapor deposition (CVD) method with in situ growth of CFs us-ing Sb2O3/Fe2O3 as the precursor and acetylene (C2H2) as the carbon source. The Sb-Fe-CF composite was characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM), and its electrochemical per-formance was investigated by galvanostatic charge-discharge cycling and electrochemical impedance spectroscopy. The Sb-Fe-CF composite shows a better cycling stability than the Sb-amorphous-carbon composite prepared by the same CVD method but using Sb2O3 as the precur-sor. Improvements in cycling stability of the Sb-Fe-CF composite can be attributed to the formation of three-dimensional network structure by CFs, which can connect Sb particles firmly. In addition, the CF layer can buffer the volume change effectively.     

Eu2Zr2O7纳米晶的硬脂酸法制备

以硝酸锆和硝酸铕作为原材料,硬脂酸作为溶剂和分散剂,通过硬脂酸燃烧法制备了具有立方晶系的萤石型Eu2Zr2O7纳米晶.通过热重和红外光谱对其反应过程进行跟踪.产物经X-射线粉末衍射、透射电镜、高分辨电子显微镜、能谱以及荧光光谱进行了表征.热处理温度对产物的形成有较大的影响,在800℃单一相的Eu2Zr2O7纳米晶已完全形成.所制得的纳米晶由平均粒径为5~20 nm的球状粒子组成.从透射电镜上（222）面的晶面距分别为0.307 nm,与理论值一致.实验检测到Eu2Zr2O7具有较强的荧光性质.     

PbSe纳米晶的溶剂热法制备与表征

以Pb(Ac)2、Na2SeSO3分别作为铅源和硒源,自制的月桂酸硫脲咪唑啉季铵盐(SUDEI)作为表面活性剂,采用溶剂热法在醇水混合溶剂中得到不同形貌的PbSe纳米晶。通过透射电镜(TEM)、X射线衍射(XRD)、X射线光电子能谱(XPS)对PbSe纳米晶进行了表征。探讨了制备PbSe纳米晶的最佳条件,当月桂酸硫脲咪唑啉季铵盐浓度0.05 mol.L-1,反应温度150℃,反应时间12h,可制得分散较好的粒径约50~100 nm的四方形硒化铅纳米晶。     

Synthesis and Characterization of Vanadium Substituted Dawson-Type Heteropoly Acid （Mo, As）

SubstitutedDawson typepolyoxometalateshave beencalledinorganicmetalloprophyrinbecauseof analogousstructureofmetalloprophyrinandstronger antioxidantthanmetalloprophyrin.Theywerealso usedaseffectivenovelcatalystsofalkeneepoxyring reactions[1].Becausevanadiu…     

湿化学法制备ATO/TiO2导电复合粉体包覆机制的研究

采用湿化学共沉淀法,通过在TiO2颗粒表面包覆Sb掺杂SnO2（ATO）制备ATO/TiO2导电粉.运用TG-DSC、XRD、XPS、SEM、BET和电导率等手段对ATO/TiO2导电粉进行了表征.研究结果表明：锡锑混合物xSn（Sb）O2·yH2O以非晶态的形态靠范德华力与静电引力吸附在TiO2表面,煅烧过程中,xSn（Sb）O2·yH2O脱去结晶水吸附或鍵合在TiO2表面.随着TiO2颗粒表面包覆层ATO厚度逐渐增加,ATO/TiO2粉体的电导率逐渐增加.     

Preparation and Composition—Structure—Thermal Stability Relation of a Novel Open—framework Vanadium Phosphate （H3NCH2CH2NH3）3[（VO）4（PO4）2（HPO4）4]

A novel open-franmework vanadium(IV) phosphate (H3NCH2CH2NH3)3[(VO)4(PO4)2(HPO4)4](short for V2P3-en)has been prepared.It is synthesized hydrothermally in the presence of ethylenediamine(en)at 170℃ for 5 days by self-assembly form sturcturally simple precursors V2O5,H3PO4and H2O.The compound is characterized by means of Fourier transform-infrared spectroscopy(FT-IR),Thermogravimetry-differenti8al thermal analysis(TG-DTA),X-ray powder diffraction analysis(XRD) and Scanning electron microscopy (SEM) \.Furthermore,the composition-structure-thermal stability relation of V2P3-en is exploed in terms of crystal chemistry,and the potential approach to the enhancement of its thermal stability is proposed.