酸蒸气水热免洗法制备前驱物ZrMo2-xWxO7(OH,Cl)2·2H2O和立方ZrMo2-xWxO8热收缩化合物

采用酸蒸气水热免洗方法合成了立方ZrW2O8类型化合物的系列前驱物ZrMo2-xWxO7(OH, Cl)2·2H2O(x=0, 0.2, 0.4, 0.6, 0.8, 1.0, 1.2, 1.4, 1.6, 1.8), 并由此制备了纯立方相ZrMo2-xWxO8(x=0.6, 0.8, 1.0, 1.2, 1.4, 1.6, 1.8). 提出了用X射线粉末衍射相对积分强度表征有序-无序介稳态晶体有序度的方法, 发现在制备条件下, 随着Mo/W摩尔比的减小, 立方相ZrMo2-xWxO8有序-无序介稳态的饱和有序度增加的规律. 讨论了原料选择以及中间产物的形貌对合成目标产物的影响, 探讨了以铵盐为原料制备前驱物反应的微观过程.     

Nd:GSAG纳米粉体的合成、晶体结构及光谱

采用共沉淀法,以NH4OH为沉淀剂制备了1％(原子分数)Nd3+:Gd3 Se2 Al3 O12前驱体,并在不同的温度下对前驱体进行煅烧.用X射线衍射(XRD)和红外光谱(FT-IR)技术对前驱体及煅烧后粉体的结构、微观形貌进行了研究.结果表明,前驱体在1000℃下煅烧n获得纯GSAG多晶相粉体.用X射线衍射宽化法估算粉体的平均晶粒尺寸为25 nm.通过X射线粉末衍射,用Rietveld全谱拟合方法对晶体结构进行了精修,得到1000℃下煅烧所得Nd:GSAG粉体的晶胞参数为a=b=c=1.24164(5)nm,α=β=y=90°.在室温下,测定了激发波长为808m的发射谱和检测波长为942 nm的激发谱.另外,测定了 942和1064 nm处的荧光衰减曲线,并用单指数函数进行了拟合,得到对应的荧光寿命分别为0.529和0.512 ms.     

机械力化学反应法制备纳米金红石型二氧化钛的研究

以Ti (C4H9O)4 和 C2H2O4·2H2O 为原料在室温下利用机械力化学反应法制备前驱体,利用热重-微商热重法(TG-DTG)决定前驱体的分解温度,通过在特定温度下对前驱体进行热分解得到TiO2.利用XRD,SEM,ZETA 电位粒度分析仪以及紫外光谱仪对所得样品物相,形貌,粒度和光学性能进行分析和表征.结果显示所得粉体微观形貌为球形,其直径(＞ 95%)小于60nm,粒径较小的粉体对紫外线UVA波段的吸收效果较好.     

立方形貌ITO粉体的水热法制备及光电性能

以金属In和SnCl_4·5H_2O为原料,采用水热法在120~140℃得到In(OH)_3前驱体,该前驱体在550℃下煅烧得到立方体形貌的氧化铟锡粉体.研究了水热反应温度和反应时间对粉体形貌和晶型的影响.通过热分析仪(TG-DSC)、X射线衍射仪(XRD)、拉曼光谱仪(Raman)、透射电子显微镜(TEM)、四探针电阻仪、X射线光电子能谱仪(XPS)、紫外-可见-近红外分光光度计以及荧光光谱仪对粉体进行了表征,并对水热反应条件为140℃及12 h下制备的c-ITO的光电性能进行了分析.结果表明,随着水热反应温度的升高,ITO粉体形貌由立方体向不规则形貌转变,粉体晶型出现少量的六方相.在水热反应条件为140℃,12 h,铟离子与尿素的摩尔比为1∶5时,得到平均粒径为230 nm的立方体ITO粉体,其电阻率为1.247Ω·cm,光学能带间隙为3.685 e V,与c-In2O3相比其能带间隙更高,室温下260 nm激发波长下粉体出现光致发光,发射峰位于蓝光区域.     

掺杂合成纳米WO3

掺杂SiO2的WO3粉体对NOX、NH3等多种气体十分敏感,可用于某些特定场合和环境监测方面[1,2]。本文以钨酸铵和硅酸乙酯为原料,分别采用固相法和沉淀法制备了不同掺杂量的SiO2 WO3纳米粉体,并对其进行了XRD,TEM表征。1　实验部分1 1　仪器与试剂德国布鲁克D8X 射线衍射仪;日本电子公司JEM 100SX型透射电子显微镜;天津卫东电炉厂RJX 5 13型马弗炉;上海司乐仪器厂85-2型恒温磁力搅拌器。钨酸铵(NH4)5H5[H2(WO4)6]H2O(化学纯);硅酸乙酯(C2H5O)4Si(分析纯);无水乙醇CH3CH2OH(分析纯);盐酸HCl(分析纯)。1 2　固相法制备WO3…     

三种纳米片组装的α-4CaO·5B_2O_3·7H_2O纳米结构的可控制备、表征及其阻燃性能

以Ca(NO3)2·4H2O和Na2B4O7·10H2O为原料,水和乙醇为混合溶剂,在水热120℃条件下,可控制备了α-4CaO·5B2O3·7H2O纳米片以及由纳米片组装成的球形和蚕蛹状α-4CaO·5B2O3·7H2O纳米结构,通过X射线粉晶衍射(XRD)、X射线能谱分析(EDS)、红外光谱(FT-IR)和扫描电子显微镜(SEM)等手段对产物进行了表征.考察了反应温度、反应时间、溶剂及表面活性剂等条件对硼酸钙α-4CaO·5B2O3·7H2O形貌及尺寸的影响,提出了α-4CaO·5B2O3·7H2O纳米结构的可能形成机理.通过热分析法研究了三种不同形貌硼酸钙α-4CaO·5B2O3·7H2O样品的阻燃性能,结果表明其阻燃性能比非纳米样品好.     

化学沉淀法制备BaTiO3纳米粉体的研究

以正钛酸(H₄TiO₄)、硝酸钡[Ba(NO₃)₂]为原料, 以双氧水、氨水为溶剂, 采用化学沉淀法制备出晶粒尺寸约20 nm的钛酸钡粉体. 研究了原料种类、煅烧温度、加料方式、反应温度对钛酸钡粉体性能的影响, 确定了最佳的制备条件. 结果表明: 当正钛酸(g)∶双氧水(mL)∶氨水(mL)＝1∶5∶3, 且采用正钛酸的双氧水-氨水溶液缓慢滴加到硝酸钡溶液中的加料方式时, 溶解完全, 制得的BaTiO₃粉体粒径小、纯度高. 用X射线衍射(XRD)和扫描电子显微镜(SEM)表征了颗粒的晶体结构、晶型转变机理以及颗粒的形貌|结果显示: 前驱体的起始晶型转变温度为500, 800 ℃煅烧获得的粒子晶型完整, 形貌呈规则的球形, 当煅烧温度升高到900 ℃时, 粉体晶体结构由立方相转变为四方相.     

ZnO微晶的水热合成及形貌控制研究

以Zn(NH3)4(Ac)2为前驱体,不加任何模板剂和表面活性剂,低温下通过改变反应条件(如前驱体浓度、反应时间及反应温度),实现了对ZnO微晶形貌和尺度的有效控制.所得花状、蜂窝状、柱状ZnO用X射线衍射仪和扫描电镜进行了鉴定和表征,并初步探讨了不同形貌ZnO微晶的生长机理.     

焙烧温度对ZnO粉体结晶及其光学性能的影响

以草酸铵和醋酸锌为原料,采用直接沉淀法制备ZnO粉体,考察了焙烧温度对粉体结晶和光学性能的影响。采用热重分析(TGA-DTA)、X射线衍射、紫外-可见漫反射(UV-Vis)、荧光分光光度计(FS)和扫描电子显微镜(SEM)等方法对样品进行了分析。结果表明,制备的前驱物为C2O4Zn·2H2O,最低焙烧温度400℃,随着焙烧温度的提高,粉体结晶度提高,一次粒径增大;600℃焙烧后有较强紫外发光峰,粉体由200 nm的粒子排列成层叠状;900℃焙烧后有较强可见发光峰,粉体粒子大于500 nm,团聚严重;粉体有较强的紫外吸收,吸收峰有蓝移。     

不同酸掺杂聚苯胺电极材料的制备及其导电性能研究

本文使用(NH_4)_2S_2O_8为氧化剂,用HCl、H_2SO_4和磷钨酸作为掺杂剂配制前驱体溶液,然后采用氧化还原法制备了聚苯胺电极材料。通过红外(FT-IR)、X射线衍射(XRD)、热重分析(TGA0)及扫描电子显微镜(SEM)对电极材料的结构和形貌进行表征,并利用四探针方法测定聚苯胺电极材料在控制氧化剂的量、酸的浓度和不同温度条件下的电导率。结果表明,磷钨酸掺杂聚苯胺(PANI)的结构和形貌优于HCl和H_2SO_4掺的PANI,过硫酸铵(APS)与苯胺(An)的摩尔比为1∶1、酸的浓度为2 mol·L~(-1)、合成温度为0℃的条件下,PANI具有高电导率,分别达到10.27、9.62和8.79S·cm~(-1)。     

Preparation and characterization of ZrWMoO<Subscript>8</Subscript> powders with different morphologies

ZrWMoO₈ powders with different morphologies were obtained using ammonium tungstate, molybdate tungstate and zirconium tungstate as the starting materials by dehydrating the precursor ZrWMoO₇(OH)₂(H₂O)₂. The precursor was studied by thermo-gravimetric and differential scanning calorimetry (TG-DSC). The influence of the gelling agents (HCl, HClO₄, HNO₃, H₂SO₄ and H₃PO₄) on the crystallization process and crystal morphology of the products prepared was investigated by X-ray powder diffraction (XRD), scanning electron micrograph (SEM) and X-ray fluorescence spectrometer (XRF). Results showed that the morphology of the ZrWMoO₈ particles can be simply adjusted by changing the gelling agents, and the thermal expansion coefficients of cubic ZrWMoO₈ prepared in HCl solution are −3.84 × 10⁻⁶ K⁻¹ from 100°C to 700°C. __________ Translated from Chemical Journal of Chinese University, 2007, 28(3): 397–401 [译自: 高等学校化学学报]     

Fabrication and morphology control of BaWO4 thin films by microwave assisted chemical bath deposition

Highly crystallized barium tungstate (BaWO₄) thin films with dumbbell-like, kernel-like, bowknot-like and cauliflower-like microstructure were synthesized from an aqueous solution containing barium nitrate, ethylenediamine tetraacetate acid disodium and sodium tungstate, via mild microwave assisted chemical bath deposition process. The resulting BaWO₄ films with different morphologies were characterized by X-ray diffraction spectrum, scanning electron microscope, Raman and photoluminescence spectra. The results indicate that the morphologies of final products significantly depend on the reaction conditions including the reaction time, the initial concentration of precursor reagent and the physicochemical characteristics of the substrates. Furthermore, the oriented aggregation mechanism is proposed as a possible formation mechanism of the films with specific morphologies.     

柠檬酸钠与碳酸钙晶型和形貌的控制

晶体的晶型和形貌是碳酸钙制备中的关键问题之一。 采用尿素水解均匀沉淀法来控制碳酸钙的晶型和形貌。 利用XRD和SEM等技术手段对CaCO₃晶体的结构和形貌进行了表征。 结果表明,高温条件下(90 ℃)水溶液中得到均匀的针状结构的文石晶体。 添加适量柠檬酸钠后,则得到的是特殊形貌的方解石晶体。 在乙醇/水混合溶剂中,柠檬酸钠对CaCO₃晶体的形貌也有重要影响,通过改变乙醇体积分数,得到了中空绒毛球状的球霰石。     

Controllable synthesis of organic-inorganic hybrid MoOx/polyaniline nanowires and nanotubes

A novel chemical oxidative polymerization approach has been proposed for the controllable preparation of organic-inorganic hybrid MoO(x)/polyaniline (PANI) nanocomposites based on the nanowire precursor of Mo(3)O(10)(C(6)H(8)N)(2)·2H(2)O with sub-nanometer periodic structures. The nanotubes, nanowires, and rambutan-like nanoparticles of MoO(x)/PANI were successfully obtained through simply modulating the pH values to 2.5-3.5, ≈2.0 and ≈1.0, respectively. Through systematic physicochemical characterization, such as scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, Raman spectroscopy, and so forth, the composition and structure of MoO(x)/PANI hybrid nanocomposites are well confirmed. It is found that the nanowire morphology of the precursor is the key to achieve the one-dimensional (1D) structures of final products. A new polymerization-dissolution mechanism is proposed to explain the formation of such products with different morphologies, in which the match between polymerization and dissolution processes of the precursor plays the important role. This approach will find a new way to controllably prepare various organic-inorganic hybrid 1D nanomaterials especially for polymer-hybrid nanostructures.     

Conductivity and chemical stability of SrCe0.92Nb0.03Tm0.05O3-δ membrane prepared by modified sol-gel method

SrCe0.92 Nb 0.03 Tm0.05 O 3-δ powders were synthesized by a modified sol-gel method using citrate as a chelating agent.X-ray diffraction(XRD) analysis verified SrCe 0.92 Nb 0.03 Tm 0.05 O 3-δ powders and membranes consisting of a single perovskite phase.The morphologies of the sintered membranes were investigated by using scanning electron microscopy(SEM) technique.Stability tests demonstrated that the Nb introduction into doped strontium cerate greatly enhanced the chemical stability.Electrical conductivities of SrCe 0.92 Nb 0.03 Tm 0.05 O 3-δ and SrCe 0.95 Tm 0.05 O 3-δ were measured by the four-point DC method under 10% H 2 /He atmosphere and temperatures(700-900℃).With a maximum conductivity of 0.0067 S cm-1 at 900℃,the total electrical conductivity of SrCe 0.92 Nb 0.03 Tm 0.05 O 3-δ increases with increasing temperature.The H 2 permeation flux of SrCe 0.92 Nb 0.03 Tm 0.05 O 3-δ is 0.035 mL cm-2 min-1 when 40% H 2 /He and Ar were used respectively as the feed and sweeping gases at 900℃.     

氧化铜纳米片及其自组装球状纳米结构的制备及催化作用

氧化铜具有独特的光电和光化学性能,可被用来制作太阳能电池或高能锂电池~([1,2]).纳米氧化铜还可以作为催化剂、载体以及电极活性材料等~([3-7]).在实际应用中,纳米材料的结构和形貌对其性能有很大影响.     

不同形貌WO3的水热合成及其在水处理中的应用研究

三氧化钨(WO₃)以其较窄的带隙,成为继二氧化钛(TiO₂)之后颇具发展潜力的n型半导体光催化剂.本文采用水热合成法,通过调控反应参数,如原料组成、沉淀时间等,合成了不同形貌和晶型的WO₃;采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、傅里叶变换红外光谱(FT-IR)、氮气吸附-脱附(N₂ adsorption-desorption)等表征了所合成的WO₃产品,发现原料组成、沉淀时间等条件对WO₃的晶型和形貌都有影响;研究了所合成的WO₃产品去除水中亚甲基蓝染料污染物的性能,结果表明,所制备的WO₃对水中亚甲基蓝具有较好的去除效果,去除率可达97%.     

镀锌扁钢电力接地材料在NaCl介质中的腐蚀特性

应用极化曲线、电化学阻抗谱和中性盐雾腐蚀试验法,研究电力接地材料镀锌扁钢在5%NaCl溶液中的腐蚀行为,扫描电子显微镜（SEM）、X射线衍射仪（XRD）观察与表征镀锌扁钢样品腐蚀的表面形貌及其产物性质.结果表明,在20～60℃温度范围内,镀锌扁钢腐蚀电流随温度升高而增大,60℃时腐蚀速率达到0.8408mA.cm-2（...     

A Solvothermal Route to Cu2O Nanocubes and Cu Nanoparticles

IntroductionSynthesis of Cu2O and Cu nanostructures has beenactively researched for many decades because bothCu2O and Cu are important industrial materials on ac-count of their novel physical and chemical properties.In particular,Cu2O is a p-type metal ox…