沉淀剂对共沉淀法制备 Lu2O3发光粉体形貌的影响

研究了共沉淀法制备Eu³⁺掺杂氧化镥(Lu₂O₃)发光粉体过程中三种不同的沉淀剂(氨水、碳酸氢铵以及NH₃·H₂O+NH₄HCO₃两者的混合溶液)对所得粉体形貌的影响. 通过差热热重质谱联用(DTA-TG-MS)和红外光谱研究了不同沉淀剂所得沉淀前驱体的热分解行为, 结合显微结构观察、粒度分布和比表面积测试, 对三种沉淀剂影响Lu₂O₃晶粒尺寸和团聚状态的规律进行了探讨. 研究发现: 采用NH₃·H₂O+NH₄HCO₃混合沉淀剂得到的Lu₂O₃粉体具有最佳的显微结构和粒径分布状态, 沉淀前驱体经1000℃煅烧2h, 粉体的平均晶粒尺寸为35nm, 中位粒径(D₅₀)为0.48μm.     

不同沉淀剂对Nd3+:Lu2O3纳米粉体性能的影响

采用湿化学共沉淀法合成了Nd3+掺杂的氧化镥纳米晶粉体,研究了三种不同沉淀剂(NH4OH、NH4HCO3、NH4OH+NH4HCO3)对Nd3+:Lu2O3纳米晶粉体性能的影响.采用NH4OH+NH4HCO3混合溶液作复合沉淀剂所得粉体具有比表面积高(13.37m2/g)、颗粒尺寸小(～30nm)、粒度分布窄(60～160nm)的优点.该粉体经过干压和等静压成型后,素坯从室温至1400℃获得的线性收缩率可达17%,其烧结活性明显高于其它两种沉淀剂所得的粉体.在流动H:气氛下,经1880℃/8h烧结可获得具有优良光学透明性的Nd3+:Lu2O3透明陶瓷,在1080nm波长处的直线透过率超过75%.     

化学沉淀法制备纳米氧化铝过程中的防团聚研究

分别以无水乙醇、去离子水为溶剂,以NH3·H2O、NH4HCO3为沉淀剂,采用化学沉淀法制备了纳米Al2O3粉体.利用TEM、XRD、FT-IR和激光粒度仪研究了溶剂、沉淀剂、浓度、前驱体等因素对纳米Al2O3粉体制备过程中的团聚程度的影响.结果表明:当NH4HCO3和Al(NO3)3水溶液浓度分别为3.0mol/L和0.3mol/L时,借助超声分散和微波干燥,得到的纳米Al2O3粉体粒度均匀、分散良好,1100℃煅烧所得粉体平均粒径为20nm.     

醇-水法制备纳米晶NiO粉体

Ni(NO3 ) 2 ·6H2 O和NH4HCO3 在醇 水溶液中反应合成NiCO3 · 2Ni(OH) 2 ·2H2 O前驱体 ,经煅烧后得到大约 10nmNiO粉体。同传统的水溶液法相比 ,醇 水法得到的NiO粉体粒径尺寸小、分布范围窄和团聚少 ,PEG的添加能够减少团聚     

无团聚ZrO2-HfO2-Y2O3复合纳米粉体的制备

以分析纯ZrOCl2·8H2O、HfOCl2·8H2O和Y(NO3)3·6H2O为原料,采用反向滴定共沉淀-共沸蒸馏法成功地制备出无团聚的ZrO2-HfO2-Y2O3复合纳米粉体.借助XRD、TEM、BET等手段分析了制备工艺对粉体粒径和团聚状态的影响.研究表明,分散剂PEG的加入量及前驱体湿凝胶的处理方式对最终制备的ZrO2-HfO2-Y2O3复合粉体的晶粒度影响不大,但显著影响粉体的分散状态.分散剂加入量为1%(质量分数)并对湿凝胶共沸蒸馏处理条件下最终获得的粉体的分散性最好.前驱体沉淀经500℃焙烧1h后,生成了具有高氧离子电导率的立方晶型ZrO2基ZrO2-HfO2-Y2O3固溶体,粉体的平均粒径约为15nm.     

均相共沉淀法制备钇铝石榴石(YAG)纳米粉末

以Y2O3、Al(NO3)3·9H2O、(NH4)2SO4为原料,尿素为沉淀剂,正硅酸乙酯作为添加剂,采用均相共沉淀法制备出YAG前驱体粉末,在沉淀过程中采用静电稳定、聚合物位阻以及共沸方法相结合有效地防止了纳米颗粒硬团聚的形成,前驱体颗粒尺寸小于100nm.采用DTA/TG、IR、XRD和TEM测试手段对粉末材料进行了表征,根据Scherrer公式计算出晶粒大小,研究了晶粒尺寸分布及其变化情况.研究结果表明前驱体粉末经过1200℃温度烧结后,全部转化YAG相,其晶粒尺寸小于50nm,随着烧结温度提高,晶粒平均尺寸增大.     

共沉淀法合成制备Ce^3＋掺杂Lu3Al5O12纳米粉体

用碳酸氢铵作为沉淀剂,将硝酸镥、硝酸铝和硝酸铈配成混合溶液,采用反滴定共沉淀及低温煅烧前驱体的方法制备 Lu3Al5O12(Ce)纳米发光粉体.采用热分析(TG-DTA)、傅立叶红外光谱(FTIR)、X射线衍射(XRD)、透射电镜(TEM)和光致发光(PL)等分析测试方法对Lu3Al5O12(Ce)粉体制备过程中的物理化学变化及粉体的激发发射发光性能进行了研究.结果表明,采用反滴定共沉淀法制备工艺,经过1000℃煅烧2h,可以得到晶粒尺寸为30nm左右,仅有轻微团聚,单一石榴石相的Lu3Al5O12(Ce)粉体.并且在1000℃处理得到的粉体的光致发光最强.     

CaMoO_4:Eu~(3+)红色荧光粉化学共沉淀合成与表征

以NH4HCO3-NH3·H2O为混合沉淀剂,采用化学共沉淀法制备CaMoO4:Eu3+红色荧光粉.通过TG-DTA和XRD研究CaMoO4:Eu3+前驱体的热分解和晶相形成过程;采用SEM和PL表征了该荧光粉的表面形貌和发光性能,并与NH4HCO3沉淀剂、NH3·H2O沉淀剂合成的CaMoO4:Eu3+荧光粉以及高温固相法制备的荧光粉进行对比.结果表明,煅烧温度700℃时,前驱体能够完全转换成单一CaMoO4:Eu3+白钨矿结构;煅烧温度900℃制备的荧光粉发光强度达到最大值;采用混合沉淀剂制备的荧光粉大小均匀、无团聚、呈类球型,平均粒径0.9μm.与高温固相法比较,其激发光谱中的Eu-O电荷迁移带向长波方向微小移动,而7F0→5L6(394nm)和7F0→5D2(465nm)的强电子吸收能有效改善红色荧光粉使用性能;与单独的NH4HCO3或NH3·H2O沉淀剂或高温固相法相比,该荧光粉发光性能显著改善,发光强度为传统固相法的2倍.     

共沉淀法制备纯相钇铝石榴石(YAG)纳米粉体中的若干影响因素

探讨了影响生成纯相YAG纳米粉体的各种因素,并通过优化工艺参数,得到了纯相并具有单分散、无团聚、颗粒尺寸分布窄且近似球形特点的YAG纳米粉体.实验中,配制不同浓度的NH4HCO3水溶液作为沉淀剂,配制不同浓度的Y(NO3)3和NH4Al(SO4)2混合水溶液作为母液,在不同的的温度下,采用不同的滴定速度,得到不同的前驱体,前驱体在900℃以上的温度焙烧2h即可获得不同的粉体.主要采用X射线衍射(XRD)对这些粉体进行了物相分析,同时结合红外光谱法(F-IR)对部分前驱体进行了定性分析,用透射电子显微镜(TEM)对纯相粉体进行了形貌观察.结果表明,在共沉淀过程中,混合溶液和沉淀剂的浓度直接决定了是否生成YAG为主相的粉体,环境温度和滴定速度则对是否生成纯相粉体有较大的影响.     

化学沉淀法制备纳米氧化铝过程中的防团聚研究

分别以无水乙醇、去离子水为溶剂，以NH3·H2O、NH4HCO3为沉淀剂，采用化学沉淀法制备了纳米Al2O3粉体。利用TEM、XRD、nIR和激光粒度仪研究了溶剂、沉淀剂、浓度、前驱体等因素对纳米Al2O3粉体制备过程中的团聚程度的影响。结果表明：当NHaHCO3和Al（NO3）3水溶液浓度分别为3．0mol／L和0．3mol／L时，借助超声分散和微波干燥，得到的纳米Al2O3粉体粒度均匀、分散良好，1100℃煅烧所得粉体平均粒径为20nm。     

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)。