Cu掺杂WO3纳米棒的制备及其对正丁醇的气敏响应

通过水热法简易的制备出Cu掺杂WO3纳米棒材料,并运用XRD、SEM、BET等手段对其物相、形貌和比表面积等进行了表征,并研究了其对正丁醇的气敏性能.气敏测试结果表明,所制备的Cu掺杂WO3纳米棒材料对正丁醇具有良好气敏性能.当工作温度为400 ℃时,Cu掺杂WO3材料对100ppm的正丁醇的响应达到了29,约为纯WO3的3倍.同时,Cu掺杂WO3材料对正丁醇的检测限可低至0.1ppm,并且对正丁醇还具有良好的选择性.最后对所制备的Cu掺杂WO3材料进行了气敏机理解释.     

多孔硅基WO3气敏传感器的制备与性能研究

以钨酸钠和氯化钠为原料,采用水热法在硅基多孔硅上原位生长WO3纳米棒薄膜,制成p型多孔硅基-n型WO3复合结构气敏传感器.为了获得最大比表面积的复合形貌,详细研究了水热反应时间和温度对多孔硅基WO3复合结构显微组织表面形貌的影响.利用扫描电镜、粉末衍射等表征手段测试并分析了多孔硅基表面WO3纳米棒薄膜的形貌以及晶体结构,并测试了复合结构传感器在不同工作温度下的气敏响应特性,结果表明:该气敏传感器在室温下便对有毒气体NO2具有高灵敏度以及稳定的重复性.     

石墨烯/WO3纳米片的制备及对H2S气敏性能的研究

为了改善WO3基材料的气敏性能,通过水热法制备出石墨烯添加量为0.5;、0.8;、1.0;、1.5;(质量分数)的石墨烯/WO3纳米片复合材料.利用XRD和FE-SEM对材料的物相、形貌进行表征,并研究其对H2S的气敏性能.结果表明,复合石墨烯对WO3的结构和形貌产生了较大的影响,石墨烯复合使材料对H2S的灵敏度提高,工作温度降低,石墨烯(0.5wt;)/WO3纳米片复合材料在110 ℃对100 ppm H2S气体灵敏度可达8.3,且响应-恢复时间短.     

多级结构CuO微球的制备及室温NOx气敏性能研究

采用一步水热合成方法制备具有多级结构的CuO微球.以聚乙二醇为结构导向剂,通过改变水热温度控制表面形貌.结果表明:制备的CuO微球的直径约为2.1μm,并且球体表面是由纳米棒疏松排列的.这种多级结构增大了材料的比表面积和活性位点.室温下,水热温度为120.C的样品CuO120对NOx表现出优异的气敏性能,最低检测限可达到1 ppm.CuO120对100 ppm NOx的灵敏度为74.4;,响应时间仅为2.6s.同时,CuO120气敏传感器具有很好的选择性和稳定性.     

无机盐添加剂对纳米WO3/rGO气敏性能的影响

通过微波辅助气-液界面法制备了WO3/rGO复合纳米材料,并以无机盐KCl、NaCl、MgCl2、AlCl3为添加剂,将无机盐离子(K+、Na+、Mg2+、Al3+)成功地添加到WO3/rGO纳米材料当中,无机盐离子有效地改变了WO3/rGO纳米颗粒的尺寸,提高了WO3/rGO纳米材料的气敏性能.含有MgCl2添加剂的WO3/rGO的气敏性能最好,在180℃时其对5 ppm NOx的灵敏度值可达301.1,响应/恢复时间仅为3 s/21 s,并且将WO3/rGO的最佳工作温度由210℃降低到了180℃.     

Al2 O3晶型对K2 WO4/Al2 O3物化性质及催化合成甲硫醇的影响

采用等体积浸渍法改性制备了K2 WO4/Al2 O3催化剂,研究了载体Al2 O3晶型对K2 WO4/Al2 O3催化剂物化性质及催化合成甲硫醇的影响.借助XRD、SEM、EDS、BET及NH3/CO2-TPD等手段对不同催化剂的晶相组成、微观形貌、孔结构及表面酸碱性质进行了表征分析.结果表明,Al2 O3晶型对K2 WO4/Al2 O3催化剂晶相组成及微观形貌影响较小,但对孔结构及表面酸碱性质影响较大.与K2 WO4/η-Al2 O3和K2 WO4/θ-Al2 O3催化剂相比,K2 WO4/γ-Al2 O3催化剂具有更大比表面积及孔容(介孔比表面积为226.75 m2·g-1,总孔容为0.557 cm3·g-1),且表面仅有弱酸和弱碱中心(弱酸浓度为0.42521 mmol·g-1,弱碱浓度为0.44184 mmol·g-1).在反应温度370℃,反应压力1.0 MPa,H2 S流速4.9 mL·min-1,CH3 OH流速0.03 mL·min-1反应条件下,K2 WO4/γ-Al2 O3催化剂表现出优良催化性能,甲醇转化率和甲硫醇选择性分别达81.58;和87.05;,与K2 WO4/η-Al2 O3和K2 WO4/θ-Al2 O3催化剂相比,甲醇转化率分别提高了4.23;和19.42;,甲硫醇选择性分别提高了14.68;和7.85;.     

纳米WO3中空球的制备及其气敏性能研究

采用液相沉淀法在乙二醇/水混合体系中以钨酸钠、盐酸及水合肼为反应物制备了WO3纳米中空微球,通过XRD、FTIR、SEM等分析手段对产物的晶型结构、结构官能团和形貌进行了表征,探讨了WO3纳米中空球的形成机理,并对其气敏性能进行了研究.结果表明,制备的具有中空结构的纳米WO3为以单斜WO3和正交WO3为主的多晶相,晶粒度为25.93 nm,水合肼的添加为其中空结构的形成起到了重要作用,气敏性能研究表明,纳米WO3中空球对H2S具有很好的选择性,在工作电压为5.00V时,其灵敏度可达40.90.     

纳米结构WO3薄膜气致变色特性研究进展及应用

三氧化钨(WO3)薄膜具有许多特性,是一种优良的致色材料.纳米结构WO3薄膜的着色效率高、可逆性好、响应时间短、光学调制高.综述纳米结构WO3薄膜的化学沉积法和物理沉积法.化学沉积法可制备出多孔、片状和特殊形貌纳米结构WO3薄膜.掠射角磁控溅射作为一种物理沉积方法,能够可控制备纳米柱状结构WO3薄膜.其次,介绍WO3薄膜的气致变色特性在气体传感器和智能窗等领域的应用.最后,对纳米结构WO3薄膜气致变色特性改善提出展望,并指出其目前存在的问题及未来发展趋势.     

MnO2/NiO纳米复合微球的制备及室温NOx气敏性能研究

采用低温沉淀法合成含有Mn和Ni的碳酸盐前驱体.经焙烧处理制备了MnO2/NiO纳米复合微球.采用SEM和XRD研究了复合材料的形貌和结构.结果表明:所制备的MnO2/NiO复合微球直径约为2μm.微球表面纳米粒子稀松的排列,且粒子端口呈介孔结构.在室温下,MnO2/NiO-2薄膜传感器对NOx具有较好的气敏响应.当NOx气体浓度为100 ppm时,灵敏度达36;,响应时间为11s.MnO2/NiO-2传感器对NOx气体的最低检测线为3 ppm.     

聚氨酯增强二氧化硅气凝胶常压干燥制备及其性能

以正硅酸乙酯(TEOS)为硅源,3-氨丙基三乙氧基硅烷(APTES)为偶联剂,聚氨酯为增强相,经水解缩聚形成凝胶后通过常压干燥工艺制备聚氨酯增强二氧化硅复合气凝胶.采用傅立叶红外光谱对样品的化学结构进行表征,并通过扫描电镜、比表面积与孔径分析仪,万能试验机和接触角仪等对所制得气凝胶的微观形貌、孔结构,力学和疏水性性能进行了分析.结果表明,所制备的气凝胶的孔径分布范围为2.0～25.0 nm,是一种具有三维网状结构的介孔材料,并且具有良好的力学性能,15wt;聚氨酯增强的气凝胶的压缩模量达到4MPa,同时疏水性也得到了提高,其接触角为77.73°.     

A review of measurement of thermophysical properties of silicon melt

Measurements of thermophysical properties of Si melt and supplementary study of X-ray scattering/diffraction by the authors' group were reviewed. The values obtained differed variously from those of literature. Density was 2–3% larger, surface tension 20–30% smaller, viscosity up to 40% larger, electrical conductivity 8% smaller, spectral emissivity more or less in good agreement with literature values, and thermal diffusivity a few percent larger. An anomalous density jump was found near the melting point. Surface tension and viscosity also showed anomaly. A strange time-dependent change of density was observed over 3 h after melting. X-ray analyses suggested a slight change in local atom ordering, but showed no sign of cluster formation. An addition of 0.1 at% gallium caused the density jump to disappear, while that of boron caused no change. An EXAFS study of the former melt indicated a strong interaction between Ga and Si atoms as if molecules of GaSi₃ existed. The implications of the measured properties are a possibility of soft-turbulence in an Si melt in a relatively large crucible, a more complicated manner of intake of oxygen depleted molten Si from the free surface region to underneath the growing crystal, and a relaxation of the melt after melting arising from trapped gas species.     

原位氮化法制备TiN纳米粉体

用溶胶凝胶法合成的纳米TiO2粉体作为原料,将该粉体在氨气中进行原位氮化制备了TiN纳米粉体.用XRD,TEM,化学分析等手段对合成的TiN纳米粉体的物相组成、形貌、成分进行了分析.实验分析表明:在1000℃和1100℃下分别氮化5h,可以制备粒径大约为40nm和80nm的TiN粉体,其TiN的含量分别为95.40;和98.37;;而在1000℃条件下氮化时间减少到2h时,TiN的含量仅为58.36;.氮化温度和氮化时间是合成纳米TiN的重要因素,提高合成温度和延长氮化时间均可形成纯度较高的TiN纳米粉体,但延长氮化时间更有利于获得粒径小的氮化钛粉体.     

Mesomorphism Dependence on the Position of Substitution of a Pair of Esters

A novel homologous series of ethylene derivatives of thermotropic liquid crystals has been synthesized. The methoxy to octyloxy derivatives are nematogenic, the decyloxy to tetradecyloxy derivatives are smectogenic, in addition to nematogenic, and the hexadecyloxy homologue is smectogenic only. All the members of the series are enantiotropically mesogenic. Thermotropic behavior was determined by an optical polarizing microscope equipped with a heating stage and Differential Scanning Calorimetry (DSC) study. Analytical and spectral data confirm the molecular structures of homologues (infrared, nuclear magnetic resonance, mass spectra, X-ray, and DSC data). Textures of the nematic phase are threaded or Schlieren and that of smectic phase are focal conic fan-shaped of smectic A or C. Transition curves of the phase diagram behave in a normal manner except one or two deviations from the normal trend. The mesophase range (Sm+N) varies from 3°C to 44°C. The average thermal stability for smectic is 93°C and that for nematic 117.4°C. The LC behavior of the novel series is compared with a structurally similar known series.     

Effect of alumina on enthalpy of mixing of mixed alkali silicate glasses

The enthalpy of mixing of mixed alkali (Na₂O and K₂O) silicate glasses containing various concentrations of alumina was determined using an ion-exchange equilibrium method. For glasses with a constant alkali concentration, the enthalpy of mixing was found to become less negative with alumina addition. Consistent with our previous results on the enthalpy of mixing of alumina-free mixed alkali silicate glasses, the magnitude of enthalpy of mixing exhibited a good correlation with the molar volume mismatch of the corresponding two single alkali glasses as well as with the extent of conductivity mixed alkali effect, e.g. excess activation energy of conductivity, ΔE. The reduction of the magnitude of the enthalpy of mixing with alumina addition can be attributed to the reduction of non-bridging oxygen and ionic field strength. Combining the present results with results obtained earlier, the magnitude of the enthalpy of mixing for all mixed alkali (Na₂O and K₂O) silicate glasses with and without alumina was expressed by a simple function of a modified Tobolsky parameter, which takes into account the alkali concentration and the difference in cation-to-effective anion distances. The enthalpy of mixing data of the mixed alkali glasses was then compared with reported experimental data on the conductivity of mixed alkali aluminosilicate glasses. What appears to be conflicting experimental data can be understood in terms of the magnitude of the enthalpy of mixing and we can conclude that the mixed alkali effect is closely correlated with the negative enthalpy of mixing.     

电子显微分析在表征纳米晶体化学组分中的应用

纳米材料的化学组分及含量影响其光、电、声、热、磁等物理性能,电子显微分析是表征纳米晶体化学组分的重要方法之一.本文综述了X-射线能谱(EDS)、X-射线波谱(WDS)、电子能量损失谱(EELS)和选区电子衍射(SAED)等现代电子显微分析技术在表征纳米晶体化学组分、形貌、尺寸和结构等方面的应用及其研究进展,并比较了这些分析方法存在的差异,提出了其应用中存在的不足及今后的研发方向.     

Ni-ZrO2纳米复合电铸层的制备及纳米颗粒分布均匀性研究

研究了在复合电铸过程中,当其它工艺参数一定时,复合电铸层的沉积速率及其厚度随时间的变化趋势, 以及复合电铸层表面微观形貌随电沉积时间的变化趋势.测定了复合电铸层的组织成分,并就纳米颗粒在复合电铸层表面和横截面上分布的均匀性进行了评价.结果表明,复合电铸层表面平整,组织均匀致密,其组成主要是镍和所复合的纳米颗粒,纳米颗粒较为均匀地分散在复合电铸层中.     

Evolution of the Defect Structure of Zinc-Oxide as a Consequence of Tribophysical Activation

Zinc-oxide powder was tribophysically activated in a high-energy vibro mill in a continual regime in air for 3, 30 and 300 minutes with the purpose of modifying the powders physico-chemical properties. By analyzing of data obtained by X-ray powder diffraction, electron diffraction and transmission electron microscopy, the values of distances between corresponding crystallographic planes, average domain sizes of coherent scattering, i.e. crystallites, width of diffraction lines due to the existence of microstrains, and microstrain values, minimal dislocation densities, dislocation density due to microstrain and real dislocation density, and also average distances between dislocations were determined. The dependence of these values on the activation time was established, which enabled analysis of the evolution of the defect structure of zinc-oxide powders during tribophysical activation by grinding in the described regime.     

Some peculiarities of spectral proprieties of leukocytes

This article presents the results of spectral investigations of white blood human cells including absorption, fluorescence and phosphorescence (using low-temperature measurements). For this research, the main optical centres were identified and local distribution of emitting and absorbing centres into white blood human cells was determined. In addition, the spectra of normal and pathological (B-cell chronic lymphocytic leukemia, B-CLL) cells were compared.     

立方晶系晶体本征铁弹相变序参量的选取

在本征铁弹相变的软模理论的基础上,依据弹性本构关系和居里原理,给出了立方晶系晶体所有可能的自发应变的种类,研究了立方晶系晶体本征铁弹相变序参量的选取问题.以Th群和Oh群为例,阐明了不同类的序参量导致晶体对称性变化相同的的原因,提出了该情况下序参量选取的“就少不就多”的原则.得到了发生本征铁弹相变时所有可能的序参量及晶体的对称性的变化.     

Features of transformations in REE-containing systems of nitrate precursors in preparatory processes of formation of multifunctional oxide materials

Abstract

The complex study provides a reliable idea of ??the trends in the joint behavior of structural components in the water-salt systems of nitrate precursors of REE, alkaline, alkaline earth metals in the preparatory stages of the processes of forming multicomponent oxide polyfunctional materials on their basis with thermal activation. Stages of such transformations are revealed; The regularities of complex and phase formation in systems and factors influencing them are determined; A number of physicochemical properties of the intermediate phases formed - coordination lanthanides nitrates: their composition, types of compounds, atomic-crystalline structure, regularities of transformations during heat treatment were studied.