简单的溶胶–凝胶法制备致密的铜锌锡硫硒薄膜

采用溶胶–凝胶后硒化法制备了铜锌锡硫硒薄膜, 其薄膜表面平整、无裂纹。通过简化铜锌锡硫前驱体溶胶的制备以及后退火时避免使用硫化氢气体（H₂S）等方法使铜锌锡硫硒薄膜的制备工艺得到简化。选用低毒有机物乙二醇为溶剂,Cu(CH₃COO)₂、Zn(CH₃COO)₂、SnCl₂•2H₂O和硫脲为原料, 制备铜锌锡硫前驱体溶胶。XRD、Raman、EDX和SEM 分析表明制备的铜锌锡硫硒薄膜为锌黄锡矿结构, 所有薄膜均贫铜富锌, 用0.2 g硒粉、硒化20 min得到的铜锌锡硫硒薄膜其结晶较好, 表面晶粒可达1.0 μm左右。透射光谱分析结果表明, 随硒含量的增加, 铜锌锡硫硒薄膜的光学带隙从1.51 eV减小到1.14 eV。     

MgCl2对锌在干湿交替环境中腐蚀行为的影响

使用腐蚀失重、X射线衍射(XRD)、扫描电子显微镜与能谱(SEM-EDS)等手段研究了干湿交替环境中MgCl₂对锌腐蚀行为的影响。结果表明,MgCl₂对锌的腐蚀有显著的抑制作用;在沉积NaCl条件下锌表面的腐蚀产物为Zn₅(OH)₈Cl₂·H₂O、Zn₄CO₃(OH)₆·H₂O和Zn(OH)₂,而在沉积MgCl₂条件下锌表面的腐蚀产物只有Zn₅(OH)₈Cl₂·H₂O。在干湿交替环境中MgCl₂对锌腐蚀行为的影响主要是Mg²⁺与氧还原反应产生的OH^-结合使阴极区的pH值降低造成的。     

酚醛树脂原位催化裂解制备低维碳纳米结构

以Ni（NO₃）₂·6H₂O为催化剂前躯体,原位催化裂解酚醛树脂制备了碳洋葱、竹节碳和碳纳米管等低维碳纳米结构;用粉体X-射线衍射（XRD）、扫描电镜（SEM）和透射电镜（TEM）等手段对低维碳纳米结构进行了表征。结果表明;当Ni（NO₃）₂·6H₂O与苯酚物质量比小于0.01时,Ni催化剂易分散,碳纳米管易生成,管径均一、分布稠密;当Ni（NO₃）₂·6H₂O与苯酚物质量比大于0.04时,Ni催化剂易团聚,碳纳米管管径分布较宽,分布稀疏;当Ni（NO₃）₂·6H₂O与苯酚物质量比为0.10时,Ni催化剂团聚现象严重,难以生成碳纳米管;提出了碳洋葱、竹节碳和碳纳米管不同碳纳米结构可能的形成机理。     

碱式碳酸镁焙烧法制备多孔氧化镁晶体

【目的】实现多孔MgO晶体的可控制备。【方法】以菱镁矿为镁源,采用水化碳化-低温水溶液法,热解Mg(HCO₃)₂溶液合成平均直径为10.0μm、平均长度为50.0μm的多孔棒状碱式碳酸镁(4MgCO₃·Mg(OH)₂·4H₂O);通过焙烧法制备多孔MgO晶体,分别探讨焙烧温度、时间对前驱体4MgCO₃·Mg(OH)₂·4H₂O分解率、 MgO物相组成和形貌的影响,探究4MgCO₃·Mg(OH)₂·4H₂O热分解机制。【结果】在焙烧温度为700℃、时间为3.0 h时,制得平均直径为20.0μm、平均长度为50.0μm、比表面积为76.12 m²/g的介孔棒状MgO晶体;在4MgCO₃·Mg(OH)₂·4H₂O分解过程中,随着温度升高,结晶水失去,—OH的分离和C—...     

几种改性剂对稻草纤维/ABS复合材料挥发性有机化合物释放的影响

以稻草纤维及丙烯腈-丁二烯-苯乙烯（ABS）为原料,分别以活性炭、Al₂O₃、SiO₂为改性剂,通过混炼-模压工艺制备了稻草纤维/ABS复合材料,采用热重-质谱联用仪对复合材料的挥发性有机化合物（VOC）释放情况进行对比分析,探讨了几种改性剂对稻草纤维/ABS复合材料VOC释放的影响。研究发现:ABS及稻草纤维均能在热解过程中释放CH₂O、C₂H₄O及C₃H₄O,而C₆H₆、C₇H₈、C₈H₈等苯类及烷烃类物质的释放源则主要为ABS;活性炭的添加能够显著降低稻草纤维/ABS复合材料的VOC释放,其VOC释放总量降低了55.5%;Al₂O₃和SiO₂虽然能比较明显地降低复合材料中苯类物质的释放含量,分别降低了32.4%和30.9%,但是其中的Fe、Cu等金属杂质却能够催化醛类物质的产生,导致VOC释放总量分别增加了11.8%和235.7%。      

空气浴条件下三水醋酸钠相变材料的储热性能实验

三水醋酸钠（CH₃COONa3H₂O）作为一种无机相变储能材料,具有潜热值高、导热性能好等优点,但是其在凝固过程中过冷度大制约了CH₃COONa3H₂O的应用。为了调节CH₃COONa3H₂O在空气浴条件下的过冷度,本文选用Na₂HPO₄12H₂O、Na₂CO₃10H₂O、Na₄P₂O₇10H₂O、Na₃PO₄12H₂O、Na₂SiO₃9H₂O、Na₂S₂O₃9H₂O和Na₂B₄O₇10H₂O这7种无机水合盐材料作为成核剂,采用步冷曲线法在高低温试验箱中进行过冷度调节实验和热循环实验。结果表明：在空气浴条件下,质量分数为96% CH₃COONa3H₂O+2% Na₂HPO₄12H₂O+2%羧甲基纤维素的复合相变材料过冷度最小,为5.6℃;将复合相变材料进行25、50和75次热循环后,其相变点温度几乎维持不变,过冷度随循环次数增加而逐渐增大,相变潜热值随循环次数的增加逐渐减小。本研究丰富了CH₃COONa3H₂O相变材料的过冷度调节方案,为其工程化应用提供了参考。     

静电纺丝技术制备NiOZnTiO3TiO2同轴三层纳米电缆及其形成机制

采用静电纺丝技术, 通过改进实验装置, 在最佳的纺丝条件下制备了 [Ni(CH₃COO)₂+PVP]-[Zn(CH₃COO)₂+PVP]-[Ti(OC₄H₉)₄+CH₃COOH+PVP] 前驱体复合电缆, 在600℃下将其进行热处理, 制备出了NiO-ZnTiO₃-TiO₂同轴三层纳米电缆。采用热重-差热 (TG-DTA)、 X射线衍射(XRD)、 傅里叶变换红外光谱(FTIR)、 扫描电子显微镜(SEM)和透射电子显微镜(TEM)等分析技术对样品进行了表征。对NiO-ZnTiO₃-TiO₂ 同轴三层纳米电缆的形成机制进行了讨论。结果表明, 所得产物为NiO-ZnTiO₃-TiO₂同轴三层纳米电缆。芯层为NiO, 直径大约为(42.024±4.405) nm; 中间层为ZnTiO₃, 厚度大约为(55.385±7.681) nm; 壳层为TiO₂, 厚度大约为(70.747±7.373) nm。      

High proton conductivity in metalloring-cluster based metal-organic nanotubes

Two novel anionic single-walled metal-organic nanotubes(MONTs),[(CH₃)₂NH₂][ln(cdc)(thb)].2DMF.9.5H₂O(FJU-105)and[(CH₃)₂NH₂][ln(cdc)(H-btc)]-2DMA·11H₂O(FJU-106)(H₂cdc=9H-carbazole-3,6-dicarboxylic acid,H₂thb=2,5-thiophene dicarboxylic acid,H3btc=1,3,5-benzene tricarboxylic acid),are achieved by employing[ln₆(cdc)₆]⁶⁺metalloring cluster with largest diameter as the secondary building blocks(SBUs).The inner surface of FJU-106 is functionalized by uncoordinated-COOH groups of the H-btc linkers,leading to a higher proton conduction than FJU-105.At 70℃,FJU-106 displays the proton conduction performances among MONTs,up to 1.80×10^-2S·cm(^-1).And FJU-105 and FJU-106 are the first examples of MONT proton conductors operating at subzero temperature.     

Ag-ZnO/生物质炭纳米复合材料的制备及协同可见光催化性能

以醋酸锌(Zn(CH₃COO)₂·2H₂O)为锌源、硝酸银(AgNO₃)为掺杂源、纤维素纳米晶体(Cellulose nanocrystal, CNC)为生物模板，通过溶胶-凝胶法结合碳化处理，制备了Ag-ZnO/生物质炭(Biochar)复合材料。采用TEM、XRD、BET、UV-Vis DRS对所制得的Ag-ZnO/Biochar复合材料进行表征。以亚甲基蓝(MB)为模型污染物，评价Ag-ZnO/Biochar复合材料在可见光源照射下的光催化性能，进一步阐明其光催化机制。结果表明:碳化后纳米ZnO仍保持良好的分散性，球形Ag纳米粒子均匀分散在ZnO表面，形成Ag-ZnO/Biochar三元复合材料。与Ag-ZnO和ZnO/Biochar复合材料相比，Ag-ZnO/Biochar复合材料在可见光下的光催化降解率显著提高。这是由于生物质炭赋予复合体系良好的吸附性能，使MB的光催化降解反应持续发生；而Ag纳米粒子的表面等离子体共振(Surface plasmon resonance, SRP)效应则增强了复合体系在可见光区的吸收。其中，当AgNO₃、CNC、Zn(CH₃COO)₂·2H₂O的质量比为0.01:0.25:1时，制得的Ag-ZnO/Biochar复合材料在可见光下具有最佳的光吸收性能和MB降解效率:室温条件下，黑暗中吸附30 min，再用可见光照射120 min，即可达到99%的MB降解率，显著高于Ag-ZnO(约23%)和ZnO/Biochar复合材料(约64%)。      

凹凸棒土负载CeO2-La2O3复合材料制备表征及催化性能

以凹凸棒土(ATP)为载体, 以Ce(NO₃)₃·6H₂O和La(NO₃)₃·6H₂O为原料, 以C₆H₁₂N₄(HMT)为沉淀剂, 采用均相沉淀法制备了不同铈镧比的CeO₂-La₂O₃/ATP(Ce:La=9:1~3:7, 摩尔比, 下同)复合材料。用TG-DSC、 TEM、 XRD和FTIR对所制备复合材料的微观结构和形貌进行表征, 并分别考察不同铈镧比和H₂O₂添加量对酸性品红模拟废水脱色降解的影响。结果表明, 当Ce:La=5:5时, CeO₂-La₂O₃固溶体颗粒均匀分布在ATP表面, 颗粒尺寸为5~10 nm。随着铈镧摩尔比的增加, 酸性品红的降解率呈先增后减的趋势, 且当Ce:La=5:5、 H₂O₂为10 mL、 酸性品红浓度为100 mg/L时, 降解效果最好, 300 min后的最大降解率达82%。     

Estimation of Parameters of Universal Distribution of Moments of Failure of Products

A method is proposed for estimating the parameters of a mixture of exponential and Weibull distributions for which the accuracy of preliminary estimates obtained by graphical analysis is refined in accordance with the criterion of maximum likelihood. The efficiency of the proposed method is supported by the results of statistical modeling.     

Evaluation of optical properties of highly scattering media by moments of distributions of times of flight of photons

A novel method for the determination of the optical properties of tissue from time-domain measurements is presented. The data analysis is based on the evaluation of the first moment and the second centralized moment, i.e., the mean time of flight and the variance of the measured distribution of times of flight (DTOF) of photons injected by short (picosecond) laser pulses. Analytical expressions are derived for calculation of absorption and of reduced scattering coefficients from these moments by application of diffusion theory for infinite and semi-infinite homogeneous media. The proposed method was tested on experimental data obtained with phantoms, and results for absorption and reduced scattering coefficients obtained by the proposed method are compared with those obtained by fitting of the same data with analytical solutions of the diffusion equation. Furthermore, the accuracy of the moment analysis was investigated for a range of integration limits of the DTOF. The moment analysis may serve as a comparatively fast method for evaluating optical properties with sufficient accuracy and can be used, e.g., for on-line monitoring of optical properties of biological tissue.     

Analysis of the rate of propagation of the wave of change of boiling modes

An approximate analytical expression is derived for the velocity of the front of the wave of change of boiling modes on a rod and on a plate. The impact of the Thomson effect and of the heater orientation in the gravity field is included. Adequate agreement is demonstrated between the derived relations and experimental data.     

Estimation of potentialities of methods of summation of direct measurement errors

Conventional methods for summation of direct measurement errors are considered. Conditions under which these methods provide consistent results are stated. It is proposed to utilize for characteristic of the total error, its interval estimator or the half-sum of the value obtained by adding up its arithmetic and geometric random errors.Translated from Izmeritel'naya Tekhnika, No. 4, pp. 10–12, April, 1995.     

空压机轴承箱蜗壳温度探头油封改造

由于空压机进气侧轴承箱蜗壳温度探头密封效果不好,使空压机及其后续管道受到油污染。后将温度探头的O形圈密封改为骨架油封,杜绝了轴承箱漏油问题。文章简介空压机的结构和技术参数,详细介绍了骨架油封的制作和优点。     

Characteristics of mechanical properties of materials in studies of conditions of attainment of marginal states

It is shown that conditions of attainment of marginal states in the material of structural components are formulated on the basis of analysis of force and deformation criteria of formation and development of destruction. The parameters of these criteria are data on types of structural materials, standard and special characteristics of their mechanical properties, structural forms of considered elements of the equipment, and their operating stress loading. In this case, the construction of a system of state equations for describing interrelation of current damage, external actions, and responses to them is based on the concept of calculating variations in properties of materials at all stages of the design life cycle.     

Determination of parameters of microstructural inhomogeneity of deformation of metals by the method of modeling

The article suggests a method of evaluating the microstructural inhomogeneity of deformation of metals by modeling. The method includes the measurement of deformations of metal according to meshes of a dividing grid with small base and the calculation of the distribution parameters of microdeformations in model representation. It is shown that the modeling method makes it possible objectively to evaluate the microinhomogeneity of deformation of metals independently of the chosen mesh size of the dividing grid. New structural characteristics are introduced: the base and wave of variation expressing the degree of crumbling or amalgamation of metal grains by inhomogeneity of deformation.Translated from Problemy Prochnosti, No. 7, pp. 40–44, July, 1991.     

水三相点复现的不确定度评定

水三相点是开尔文热力学温度的唯一基准点，也是ITS-90国际温标重要的定义固定点。因此，水三相点不确定度分析对整个温标的建立、温度量值传递起着至关重要的作用。近3年来，中国计量科学研究院研制出一系列高质量的水三相点容器，加强了水三相点的研究，为不确定度的分析提供了更为可靠的实验依据。同时，不确定度的分析也是客观评价新研制容器性能的一个重要指标。因此，根据实验结果对新研制容器所复现的水三相点进行了不确定度评定。评定结果表明，其扩展不确定度为0．16mK(k=2．69，P=0．99)。