Volume 35,Issue 2,2006 Table of Contents
2006, 35(2):169-171.
Abstract:
This summarized thesis began to write in 1996 and has been written in every year. In this year, it consists of (1) magnetic super-thin film, (2) giant magnetoresistive material, (3) magnetic microscopic technique and application, (4) soft magnetic ferrite, (5) magnetic fluid material.
This summarized thesis began to write in 1996 and has been written in every year. In this year, it consists of (1) magnetic super-thin film, (2) giant magnetoresistive material, (3) magnetic microscopic technique and application, (4) soft magnetic ferrite, (5) magnetic fluid material.
2 A Set of Models for Microstructure Evolution of Titanium Alloy during High Temperature Deformation
2006, 35(2):172-175.
Abstract:
以钛合金在高温变形过程中的物理机制为基础，建立了钛合金高温变形时的位错密度和晶粒尺寸模型。将该微观组织模型应用于TC6合金的高温变形，并用遗传算法（GA）确定了模型中的8个材料常数。TC6合金的热模拟实验结果和定量金相实验结果证实：初生α相晶粒尺寸的计算值与实验值的平均误差小于15．3％。
以钛合金在高温变形过程中的物理机制为基础，建立了钛合金高温变形时的位错密度和晶粒尺寸模型。将该微观组织模型应用于TC6合金的高温变形，并用遗传算法（GA）确定了模型中的8个材料常数。TC6合金的热模拟实验结果和定量金相实验结果证实：初生α相晶粒尺寸的计算值与实验值的平均误差小于15．3％。
2006, 35(2):176-180.
Abstract:
为了研究Inconel 706合金宏观偏析“黑斑”区相变行为及析出相的形成特征，对黑斑区和正常区的相析出特征进行了系统的对比分析，并用热力学相计算手段对合金黑斑区的相变规律和元素的热力学平衡分配进行了计算分析。结果认为，Inconel 706合金宏观偏析黑斑主要是由富Nb的Laves相和富Ti的η，δ相的严重偏聚粗化导致的。从黑斑的组织行为分析及热力学相计算可以认为，Nb在凝固过程中发生了极为明显的枝晶间液态偏聚，同时Ti和Al也有一定程度的偏聚，这些元素不同程度的液态偏聚行为是造成合金黑斑区相富集的主要原因。
为了研究Inconel 706合金宏观偏析“黑斑”区相变行为及析出相的形成特征，对黑斑区和正常区的相析出特征进行了系统的对比分析，并用热力学相计算手段对合金黑斑区的相变规律和元素的热力学平衡分配进行了计算分析。结果认为，Inconel 706合金宏观偏析黑斑主要是由富Nb的Laves相和富Ti的η，δ相的严重偏聚粗化导致的。从黑斑的组织行为分析及热力学相计算可以认为，Nb在凝固过程中发生了极为明显的枝晶间液态偏聚，同时Ti和Al也有一定程度的偏聚，这些元素不同程度的液态偏聚行为是造成合金黑斑区相富集的主要原因。
2006, 35(2):181-185.
Abstract:
Ni/n-SiO2 compositional coatings were electrodeposited by brush-plating with pulse-reverse current. Morphology, hardness, and tribological properties of the coatings were investigated and compared with those of Ni and composite coatings electrodeposited by brush-plating with direct current. The test results obtained indicate that Ni/n-SiO2 composite coatings electrodeposited by brush-plating with pulse-reverse current, because of the pulse-reverse current and the nano powders, possesses the fine crystal grains, high hardness and low friction coefficient, so it is a better wear-resistant coatings.
Ni/n-SiO2 compositional coatings were electrodeposited by brush-plating with pulse-reverse current. Morphology, hardness, and tribological properties of the coatings were investigated and compared with those of Ni and composite coatings electrodeposited by brush-plating with direct current. The test results obtained indicate that Ni/n-SiO2 composite coatings electrodeposited by brush-plating with pulse-reverse current, because of the pulse-reverse current and the nano powders, possesses the fine crystal grains, high hardness and low friction coefficient, so it is a better wear-resistant coatings.
2006, 35(2):186-188.
Abstract:
Indentation microhardness testing was used to assess the microhardness of an EB-PVD thermal barrier coatings (TBCs) deposited on a single crystal Ni-base superalloy substrate. Tests performed using a Knoop indenter geometry reveal that there is an indentation size effect (ISE), namely that the apparent microhardness decrease significantly with increasing indentation test load. An energy balance analysis based on elastic/plastic indentation model was applied to analyze the apparent ISE and to extract the load-independent hardness from the experimental measurements.
Indentation microhardness testing was used to assess the microhardness of an EB-PVD thermal barrier coatings (TBCs) deposited on a single crystal Ni-base superalloy substrate. Tests performed using a Knoop indenter geometry reveal that there is an indentation size effect (ISE), namely that the apparent microhardness decrease significantly with increasing indentation test load. An energy balance analysis based on elastic/plastic indentation model was applied to analyze the apparent ISE and to extract the load-independent hardness from the experimental measurements.
2006, 35(2):189-194.
Abstract:
从高温氧化动力学、组织的微观进化及高温氧化机理3部分对Al4SiC4陶瓷在1200℃-1700℃的高温氧化行为进行了系统的研究。研究结果表明，Al4SiC4陶瓷具有优异的高温抗氧化性能。氧化动力学符合抛物线规律，其氧化活化能经计算为220kJ／mol。XRD及SEM研究结果表明：Al4SiC4陶瓷在1200～1500℃的氧化表面物相为Al2O3和铝硅酸盐玻璃；而高温氧化表面（1600℃～1700℃）的物相由Al2O3，莫来石和铝硅酸盐玻璃构成。由氧化试样横截面观察得知氧化层按其特征的不同分为3个部分：具有较多细小尺寸孔洞的反应层；具有较大尺寸孔洞的中间层和致密的外氧化层。在高温抗氧化机理部分中首先从热力学上计算了氧化过程中各反应的生成焓和吉布斯自由能；然后对高温氧化过程进行了推理和分析；最后根据上述试验及推理结果建立了Al4SiC4陶瓷的高温抗氧化模型。
从高温氧化动力学、组织的微观进化及高温氧化机理3部分对Al4SiC4陶瓷在1200℃-1700℃的高温氧化行为进行了系统的研究。研究结果表明，Al4SiC4陶瓷具有优异的高温抗氧化性能。氧化动力学符合抛物线规律，其氧化活化能经计算为220kJ／mol。XRD及SEM研究结果表明：Al4SiC4陶瓷在1200～1500℃的氧化表面物相为Al2O3和铝硅酸盐玻璃；而高温氧化表面（1600℃～1700℃）的物相由Al2O3，莫来石和铝硅酸盐玻璃构成。由氧化试样横截面观察得知氧化层按其特征的不同分为3个部分：具有较多细小尺寸孔洞的反应层；具有较大尺寸孔洞的中间层和致密的外氧化层。在高温抗氧化机理部分中首先从热力学上计算了氧化过程中各反应的生成焓和吉布斯自由能；然后对高温氧化过程进行了推理和分析；最后根据上述试验及推理结果建立了Al4SiC4陶瓷的高温抗氧化模型。
2006, 35(2):195-199.
Abstract:
采用光学金相(OM)和电子背散射衍射(EBSD)技术研究了高纯铝轧制变形的微观组织、晶界角度分布和取向的关系。结果表明:平行于轧向的形变微观组织可分为具有明显特征取向且包含的晶界以小于5°为主的带状组织(OAB)和取向散布宽度较大且包含的晶界以大于15°为主的带状组织(OSB);<5°,5°~10°,10°~15°和>15°4个级别的晶界角度水平面积率既与形变微观组织的形貌相关,也与其取向有关。
采用光学金相(OM)和电子背散射衍射(EBSD)技术研究了高纯铝轧制变形的微观组织、晶界角度分布和取向的关系。结果表明:平行于轧向的形变微观组织可分为具有明显特征取向且包含的晶界以小于5°为主的带状组织(OAB)和取向散布宽度较大且包含的晶界以大于15°为主的带状组织(OSB);<5°,5°~10°,10°~15°和>15°4个级别的晶界角度水平面积率既与形变微观组织的形貌相关,也与其取向有关。
2006, 35(2):200-204.
Abstract:
The microscopic structure and evolution of ordered interphase boundary of Ni-Al-V alloy was investigated using microscopic phase-field model. The results show that three kinds of interphase boundaries are formed between LI2 phases, the width of the interphase boundaries are narrower, and of which one kind of interphase boundary is in equilibrium for the occupation probability of Al atoms. According to the different orientation variants of [ 10] and [01 ] of the projection of D022, there form eight kinds of interphase boundaries structure, in which the interphase boundaries are wider with the same orientation variants, and the occupation probability of V atoms reach the equilibrium value with different orientation variants. There are four kinds of interphase boundaries between the different phases. The occupation probability of atoms in the interphase boundaries reach the equilibrium value and two phase transit continuously, for one phase precipitate from the interphase boundary of another. With the precipitation process, the interphase boundaries formed in [01] direction of D022 transform from disordered to ordered and become narrower firstly and then dissolve into disordered phase.
The microscopic structure and evolution of ordered interphase boundary of Ni-Al-V alloy was investigated using microscopic phase-field model. The results show that three kinds of interphase boundaries are formed between LI2 phases, the width of the interphase boundaries are narrower, and of which one kind of interphase boundary is in equilibrium for the occupation probability of Al atoms. According to the different orientation variants of [ 10] and [01 ] of the projection of D022, there form eight kinds of interphase boundaries structure, in which the interphase boundaries are wider with the same orientation variants, and the occupation probability of V atoms reach the equilibrium value with different orientation variants. There are four kinds of interphase boundaries between the different phases. The occupation probability of atoms in the interphase boundaries reach the equilibrium value and two phase transit continuously, for one phase precipitate from the interphase boundary of another. With the precipitation process, the interphase boundaries formed in [01] direction of D022 transform from disordered to ordered and become narrower firstly and then dissolve into disordered phase.
2006, 35(2):205-208.
Abstract:
合成了3种新的多金属氧酸盐(CTMA)5BW12O40·8H2O,(CTMA)4SiW12O40·3H2O,(CTMA)3PW12O40·2H2O,利用元素分析、IR光谱和TG-DTA技术对其进行了表征.IR光谱表明这些化合物不仅含有Keggin型结构,而且存在有机大阳离子的特征吸收峰;TG-DTA曲线显示它们的热行为是一个多步分解过程,首先这些化合物在大约269℃以下脱去水分子,然后它们的无水多金属氧酸盐经历了两步或3步的分解过程,分别脱去CTMA分子及其碎片,并伴随Keggin型结构的塌陷.通过XRD和IR光谱确证其最终分解产物是一个含有WO3与B2O3,SiO2或P2O5的混合物.同时还提出了这些化合物可能的热分解过程.
合成了3种新的多金属氧酸盐(CTMA)5BW12O40·8H2O,(CTMA)4SiW12O40·3H2O,(CTMA)3PW12O40·2H2O,利用元素分析、IR光谱和TG-DTA技术对其进行了表征.IR光谱表明这些化合物不仅含有Keggin型结构,而且存在有机大阳离子的特征吸收峰;TG-DTA曲线显示它们的热行为是一个多步分解过程,首先这些化合物在大约269℃以下脱去水分子,然后它们的无水多金属氧酸盐经历了两步或3步的分解过程,分别脱去CTMA分子及其碎片,并伴随Keggin型结构的塌陷.通过XRD和IR光谱确证其最终分解产物是一个含有WO3与B2O3,SiO2或P2O5的混合物.同时还提出了这些化合物可能的热分解过程.
2006, 35(2):209-212.
Abstract:
利用XRD，SEM，EDS及TEM对TiAl／TiB2复合材料在静止空气中高温氧化后的氧化膜结构及其形成机制进行了研究。结果表明：TiAl／TiB2复合材料的氧化膜主要由TiO2外层与由TiO2和Al2O3混合内层构成。TiO2和Al2O3混合内层为孔洞较多的疏松状结构。TiO2外层亦可分为内外两层，TiO2的内层部分存在一些与TiB2的轮廓相似的“孔洞”，TiO2的外层部分没有此类孔洞。由于TiAl／TiB2复合材料中的TiB2被氧化后生成的B2O3在高温下蒸发掉，使氧化膜中TiB2所处的位置留下了孔洞。因此，氧化膜中的部分孔洞是由于TiB2被氧化后产生的；氧化温度达到1000℃时，TiAl／TiB2复合材料中的TiB2使氧化膜中的孔洞数量增加，复合材料的抗氧化性能急剧下降。
利用XRD，SEM，EDS及TEM对TiAl／TiB2复合材料在静止空气中高温氧化后的氧化膜结构及其形成机制进行了研究。结果表明：TiAl／TiB2复合材料的氧化膜主要由TiO2外层与由TiO2和Al2O3混合内层构成。TiO2和Al2O3混合内层为孔洞较多的疏松状结构。TiO2外层亦可分为内外两层，TiO2的内层部分存在一些与TiB2的轮廓相似的“孔洞”，TiO2的外层部分没有此类孔洞。由于TiAl／TiB2复合材料中的TiB2被氧化后生成的B2O3在高温下蒸发掉，使氧化膜中TiB2所处的位置留下了孔洞。因此，氧化膜中的部分孔洞是由于TiB2被氧化后产生的；氧化温度达到1000℃时，TiAl／TiB2复合材料中的TiB2使氧化膜中的孔洞数量增加，复合材料的抗氧化性能急剧下降。
11 Study on the Microstructures and Mechanical Properties of Mg-xCa-5Zn-3Al-0.2Mn Sand-Casting Alloy
2006, 35(2):217-222.
Abstract:
研究发现,Mg-5Zn-3Al-0.2Mn合金的砂型铸造组织相组成为δ-Mg基体和τ(Mg32(Al,Zn)49)化合物。在343℃固溶17h后淬火,合金组织完全转变为固溶体,力学性能最佳,σb=245MPa,δ=12%。合金中加入xCa后,组织发生变化。当x=0.43%(质量分数)时,相组成为δ-Mg+Mg-Zn-Al-Ca复杂化合物相。当x=0.95%和1.80%时,相组成为Mg-Zn-Al-Ca相+δ-Mg+Al2Ca。随着x增加,铸态合金室温力学性能呈下降趋势。加Ca合金在350℃固溶17h后淬火,室温力学性能有所提高,而σb250o和σ02.520o则随x增加而稳步提高。
研究发现,Mg-5Zn-3Al-0.2Mn合金的砂型铸造组织相组成为δ-Mg基体和τ(Mg32(Al,Zn)49)化合物。在343℃固溶17h后淬火,合金组织完全转变为固溶体,力学性能最佳,σb=245MPa,δ=12%。合金中加入xCa后,组织发生变化。当x=0.43%(质量分数)时,相组成为δ-Mg+Mg-Zn-Al-Ca复杂化合物相。当x=0.95%和1.80%时,相组成为Mg-Zn-Al-Ca相+δ-Mg+Al2Ca。随着x增加,铸态合金室温力学性能呈下降趋势。加Ca合金在350℃固溶17h后淬火,室温力学性能有所提高,而σb250o和σ02.520o则随x增加而稳步提高。
2006, 35(2):223-226.
Abstract:
分别以碳毡和二维碳纤维为预制体，采用化学液相气化渗入法结合熔融渗硅反应法快速制备了C／C-SiC陶瓷复合材料。对这种材料的密度和气孔率进行了表征，并通过XRD，OM和SEM等方法对其相组成、显微结构和反应机理进行了研究。结果表明：不同预制体制备的C／C—SiC材料密度和气孔率分别为～2．0g／cm^3和～1．0％。其相组成包括反应生成β-SiC以及未反应的游离Si和C。C／C—SiC中纤维被环状的沉积碳包裹，生成SiC的反应只发生在Si与沉积碳之间，纤维没有损伤。Si，C和SiC各相分布和含量因预制体的不同而有明显差异。
分别以碳毡和二维碳纤维为预制体，采用化学液相气化渗入法结合熔融渗硅反应法快速制备了C／C-SiC陶瓷复合材料。对这种材料的密度和气孔率进行了表征，并通过XRD，OM和SEM等方法对其相组成、显微结构和反应机理进行了研究。结果表明：不同预制体制备的C／C—SiC材料密度和气孔率分别为～2．0g／cm^3和～1．0％。其相组成包括反应生成β-SiC以及未反应的游离Si和C。C／C—SiC中纤维被环状的沉积碳包裹，生成SiC的反应只发生在Si与沉积碳之间，纤维没有损伤。Si，C和SiC各相分布和含量因预制体的不同而有明显差异。
2006, 35(2):227-231.
Abstract:
用在（Ms＋30℃）温度下的拉伸实验和差示扫描量热仪（DSC）较系统地研究了Ti44Ni47Nb9宽滞后形状记忆合金应力诱发马氏体的相变行为。研究结果表明：当形变量达到14％左右时，应力诱发马氏体相变过程基本完成。应力诱发马氏体的逆相变温度间隔要比热诱发马氏体约小一个数量级。形变对该合金应力诱发马氏体的逆转变开始温度、逆转变温度间隔以及相变潜热均有明显影响，随着拉伸变形量的增加而增加。而在随后的冷却循环中，相变潜热和马氏体相变开始温度均随着形变的增加缓慢降低。
用在（Ms＋30℃）温度下的拉伸实验和差示扫描量热仪（DSC）较系统地研究了Ti44Ni47Nb9宽滞后形状记忆合金应力诱发马氏体的相变行为。研究结果表明：当形变量达到14％左右时，应力诱发马氏体相变过程基本完成。应力诱发马氏体的逆相变温度间隔要比热诱发马氏体约小一个数量级。形变对该合金应力诱发马氏体的逆转变开始温度、逆转变温度间隔以及相变潜热均有明显影响，随着拉伸变形量的增加而增加。而在随后的冷却循环中，相变潜热和马氏体相变开始温度均随着形变的增加缓慢降低。
2006, 35(2):232-236.
Abstract:
Based on life prediction of fatigue crack growth in a powder metallurgy, the residual strength interference model and life interference model are proposed to analyze the reliability of the fatigue crack growth. The reliability of the fatigue crack growth life of single inclusion is analyzed by the advanced first order and second moment method. In order to obtain the crack growth reliability of multiple inclusions existed in the structure, a new model, where the mean value of the random inclusion position is distributed uniformly, is presented. Comparing with the available model, where the mean value of the random inclusion position is at the center of the volume occupied by the corresponding inclusion, the new position distribution model is more safe and more suitable for engineering application. In the illustration, the above reliability method is applied to analyze the reliability of a powder metallurgy turbine disk. The results show that the position of the inclusion in the turbine disk has significant effect on the failure probability of the crack growth.
Based on life prediction of fatigue crack growth in a powder metallurgy, the residual strength interference model and life interference model are proposed to analyze the reliability of the fatigue crack growth. The reliability of the fatigue crack growth life of single inclusion is analyzed by the advanced first order and second moment method. In order to obtain the crack growth reliability of multiple inclusions existed in the structure, a new model, where the mean value of the random inclusion position is distributed uniformly, is presented. Comparing with the available model, where the mean value of the random inclusion position is at the center of the volume occupied by the corresponding inclusion, the new position distribution model is more safe and more suitable for engineering application. In the illustration, the above reliability method is applied to analyze the reliability of a powder metallurgy turbine disk. The results show that the position of the inclusion in the turbine disk has significant effect on the failure probability of the crack growth.
2006, 35(2):237-241.
Abstract:
The pure Mg2Ni intermetallic was synthesized by self-propagating combustion mode and thermal explosion mode respectively. And the reaction process of thermal explosion was researched under different preheat temperatures. The results show that solid combustion exists at lower temperatures, and the degree of reaction increase with the decrease of preheat rate. A further experiment of Combustion Front Quenching (CFQ) was carried out successfully in cylindrical steel mould by adding some Al-Ti-C powder that is accepted as a high exothermic system on the top of Mg-Ni samples. The physical and chemical changes of all region in the quenched samples during the combustion synthesis were examined by scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS) and x-ray diffraction (XRD). The results show that the Mg2Ni is directly synthesized rather than through other intermediates and the synthesis process of Mg2Ni can be express as: (1) solid combustion in the pre-combustion stage; (2) liquid combustion in the combustion process; (3) nucleation and crystallization of the product after the reaction; (4) uniformizing of the composition in the heat preservation stage.
The pure Mg2Ni intermetallic was synthesized by self-propagating combustion mode and thermal explosion mode respectively. And the reaction process of thermal explosion was researched under different preheat temperatures. The results show that solid combustion exists at lower temperatures, and the degree of reaction increase with the decrease of preheat rate. A further experiment of Combustion Front Quenching (CFQ) was carried out successfully in cylindrical steel mould by adding some Al-Ti-C powder that is accepted as a high exothermic system on the top of Mg-Ni samples. The physical and chemical changes of all region in the quenched samples during the combustion synthesis were examined by scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS) and x-ray diffraction (XRD). The results show that the Mg2Ni is directly synthesized rather than through other intermediates and the synthesis process of Mg2Ni can be express as: (1) solid combustion in the pre-combustion stage; (2) liquid combustion in the combustion process; (3) nucleation and crystallization of the product after the reaction; (4) uniformizing of the composition in the heat preservation stage.
2006, 35(2):242-246.
Abstract:
The aging behavior of Ni-Cr-Al ternary alloy are studied at temperature 1123 K, the early ordering process are simulated at atomic-scale with microscopic phase-field model. Precipitation mechanism of low supersaturated alloy Ni-15at.%Cr-10.5at.%Al is non-classical nucleation and growth, the precipitation process include three stages, i.e. the nucleation and growth of D022 ordering phase, nucleation of L12 ordering phase and transmit of L12 ordering phase from D022 ordering phase. The occupation possibilities of Al and Cr in L12 ordering phase are similar because of substitution behavior of Cr atom, Ni3(CrxAl1-x) structure are formed and coexist with D022 ordering phase. high supersaturated alloys show the congruent ordering and spinodal decomposition mechanism and the process of the ordering and clustering are precedent to low supersaturated alloys.
The aging behavior of Ni-Cr-Al ternary alloy are studied at temperature 1123 K, the early ordering process are simulated at atomic-scale with microscopic phase-field model. Precipitation mechanism of low supersaturated alloy Ni-15at.%Cr-10.5at.%Al is non-classical nucleation and growth, the precipitation process include three stages, i.e. the nucleation and growth of D022 ordering phase, nucleation of L12 ordering phase and transmit of L12 ordering phase from D022 ordering phase. The occupation possibilities of Al and Cr in L12 ordering phase are similar because of substitution behavior of Cr atom, Ni3(CrxAl1-x) structure are formed and coexist with D022 ordering phase. high supersaturated alloys show the congruent ordering and spinodal decomposition mechanism and the process of the ordering and clustering are precedent to low supersaturated alloys.
2006, 35(2):247-252.
Abstract:
采用第一原理赝势平面波方法——CASTEP程序计算了4种B2型Y基金属间化合物YH（X=Ag，Cu，In，Rh）的部分弹性性质，计算结果与文献报道值基本一致。通过Pugh定律、Cauchy压力和泊松比等经验判据，分析并预测了它们的脆性／延性，其延性高低次序为：YRh〉YAg〉YCu〉YIn。电子结构分析表明：这4种金属间化合物良好的延性源于其较强的金属键，而不同程度的Y（d）-X（p）电子杂化则导致了其延性的差异。YIn中因In的P电子较多，杂化程度高，共价键方向性强，因而延展性最低，而YRh则由于存在Y（d）-Rh（d）电子间强的相互作用，增强了其金属键作用，因而延性最好。
采用第一原理赝势平面波方法——CASTEP程序计算了4种B2型Y基金属间化合物YH（X=Ag，Cu，In，Rh）的部分弹性性质，计算结果与文献报道值基本一致。通过Pugh定律、Cauchy压力和泊松比等经验判据，分析并预测了它们的脆性／延性，其延性高低次序为：YRh〉YAg〉YCu〉YIn。电子结构分析表明：这4种金属间化合物良好的延性源于其较强的金属键，而不同程度的Y（d）-X（p）电子杂化则导致了其延性的差异。YIn中因In的P电子较多，杂化程度高，共价键方向性强，因而延展性最低，而YRh则由于存在Y（d）-Rh（d）电子间强的相互作用，增强了其金属键作用，因而延性最好。
2006, 35(2):253-256.
Abstract:
Based on test data from hot process simulator, a Kumar type constitutive equation for TC11 ahoy is established in this paper. Applying this cortstitutive equation in commercial FEM software of MSC /Autoforge, hot die forging process of TC11 alloy turbine disc is then simulated. The results show that the Kumar-type constitutive relationship meets the practical need to a great extent.
Based on test data from hot process simulator, a Kumar type constitutive equation for TC11 ahoy is established in this paper. Applying this cortstitutive equation in commercial FEM software of MSC /Autoforge, hot die forging process of TC11 alloy turbine disc is then simulated. The results show that the Kumar-type constitutive relationship meets the practical need to a great extent.
2006, 35(2):257-260.
Abstract:
研究了Ti-45Al-9（Nb，W,B，Y）两相合金分别在760℃和815℃时，应力值在80MPa-300MPa区间的蠕变行为。蠕变前合金的显微组织为均匀细小的双态组织。将研究结果与高铌TiAl合金全片层组织的蠕变性能进行了对比，发现所研究的双态组织合金具有相对较弱的蠕变抗力，其最小蠕变速率较全片层组织Ti46A18．5Nb0．1C0．2B合金的要高1个数量级。蠕变应力指数表明，该合金在760℃～815℃2，80MPa-300 MPa的蠕变条件下，合金的蠕变受位错攀移控制。
研究了Ti-45Al-9（Nb，W,B，Y）两相合金分别在760℃和815℃时，应力值在80MPa-300MPa区间的蠕变行为。蠕变前合金的显微组织为均匀细小的双态组织。将研究结果与高铌TiAl合金全片层组织的蠕变性能进行了对比，发现所研究的双态组织合金具有相对较弱的蠕变抗力，其最小蠕变速率较全片层组织Ti46A18．5Nb0．1C0．2B合金的要高1个数量级。蠕变应力指数表明，该合金在760℃～815℃2，80MPa-300 MPa的蠕变条件下，合金的蠕变受位错攀移控制。
2006, 35(2):261-264.
Abstract:
测定了氘化对Zr3V3ODx物相的影响，发现Zr3V30Dx氘化物只有x≥2．0才能稳定存在，由于氘在晶格中的占位不同，随氘含量增加分别出现两种η-碳化物相的氘化物——β相和γ相。对Zr3V3ODx氘化物的热解析行为研究表明：Zr3V30Dx氘化物的稳定性随氘含量的增加而降低，β声相和γ相表现出不同的解析行为，其变化规律与Zr3V3ODx氘化物中的氘占位原则相一致。
测定了氘化对Zr3V3ODx物相的影响，发现Zr3V30Dx氘化物只有x≥2．0才能稳定存在，由于氘在晶格中的占位不同，随氘含量增加分别出现两种η-碳化物相的氘化物——β相和γ相。对Zr3V3ODx氘化物的热解析行为研究表明：Zr3V30Dx氘化物的稳定性随氘含量的增加而降低，β声相和γ相表现出不同的解析行为，其变化规律与Zr3V3ODx氘化物中的氘占位原则相一致。
2006, 35(2):265-269.
Abstract:
采用加工图理论分析了TC17（Ti-5Al-4Mo-4Cr-2Sn-2Zr）钛合金在高温变形过程中的片状α球化规律。结果表明：用加工图理论分析材料的高温变形行为能准确直观地反映出材料在不同变形条件下的组织演变规律。分析加工图发现：TC17合金在840℃～870℃，应变速率0．5s^-1～3s^-1之间变形是片状α组织球化的理想区域，此时对应的能量耗散效率值为45％左右；在850℃～910℃，较高应变速率（〉5s^-1）下对TC17合金加工易发生流变不稳定现象，形成绝热剪切带。
采用加工图理论分析了TC17（Ti-5Al-4Mo-4Cr-2Sn-2Zr）钛合金在高温变形过程中的片状α球化规律。结果表明：用加工图理论分析材料的高温变形行为能准确直观地反映出材料在不同变形条件下的组织演变规律。分析加工图发现：TC17合金在840℃～870℃，应变速率0．5s^-1～3s^-1之间变形是片状α组织球化的理想区域，此时对应的能量耗散效率值为45％左右；在850℃～910℃，较高应变速率（〉5s^-1）下对TC17合金加工易发生流变不稳定现象，形成绝热剪切带。
2006, 35(2):270-272.
Abstract:
在Fe-Cu-Nb-Si-B材料中适当增加Cu的含量，可以使淬态薄带纳米化。随薄带中Cu含量的增加，在淬态薄带Fe74.5-xCuxNb3Si13.5B9中可观察到巨磁阻抗效应的增强现象。高Cu含量（x≥2）试样的磁导率的变化率要远大于低Cu含量（x≤1．5）试样的相应数值。磁导率变化的大小与磁阻抗效应相关。高Cu含量有效增加了软磁α-Fe（Si）立方相的成核，提高了淬态薄带材料的软磁性。
在Fe-Cu-Nb-Si-B材料中适当增加Cu的含量，可以使淬态薄带纳米化。随薄带中Cu含量的增加，在淬态薄带Fe74.5-xCuxNb3Si13.5B9中可观察到巨磁阻抗效应的增强现象。高Cu含量（x≥2）试样的磁导率的变化率要远大于低Cu含量（x≤1．5）试样的相应数值。磁导率变化的大小与磁阻抗效应相关。高Cu含量有效增加了软磁α-Fe（Si）立方相的成核，提高了淬态薄带材料的软磁性。
23 Piezoelectric and Dielectric Properties of Sb2O3 Doped (Na0.84K0.16)0.5Bi0.5TiO3 Lead-Free Ceramics
2006, 35(2):273-276.
Abstract:
采用传统陶瓷的制备方法，制备出Sb2O3掺杂的（Na0．84K0．16）0．5Bi0．5TiO3的无铅压电陶瓷。XRD分析表明，Sb2O3的掺杂量在0．1％～0．6％（质量分数）范围内都能够形成纯钙钛矿（ABO3）型固溶体。陶瓷材料的介电常数-温度曲线显示陶瓷在升温过程中存在两个介电常数温度峰，结合不同温度下的电滞回线观测，认为两个介电峰分别是材料的铁电-反铁电和反铁电-顺电相变，宽化的介电峰同时也表明所研究陶瓷具有驰豫铁电体特征。测试了不同组成陶瓷的压电性能，在Sb2O3掺杂量为0．1％时陶瓷的压电常数d33=124pC／N，为所研究组成中的最大值，平面机电耦合系数kp=24．87％，略有下降，材料的介电常数ε33^T／ε0和介质损耗tanδ则随掺杂量的增加而增加。
采用传统陶瓷的制备方法，制备出Sb2O3掺杂的（Na0．84K0．16）0．5Bi0．5TiO3的无铅压电陶瓷。XRD分析表明，Sb2O3的掺杂量在0．1％～0．6％（质量分数）范围内都能够形成纯钙钛矿（ABO3）型固溶体。陶瓷材料的介电常数-温度曲线显示陶瓷在升温过程中存在两个介电常数温度峰，结合不同温度下的电滞回线观测，认为两个介电峰分别是材料的铁电-反铁电和反铁电-顺电相变，宽化的介电峰同时也表明所研究陶瓷具有驰豫铁电体特征。测试了不同组成陶瓷的压电性能，在Sb2O3掺杂量为0．1％时陶瓷的压电常数d33=124pC／N，为所研究组成中的最大值，平面机电耦合系数kp=24．87％，略有下降，材料的介电常数ε33^T／ε0和介质损耗tanδ则随掺杂量的增加而增加。
2006, 35(2):277-282.
Abstract:
The rare-earth-based AB5-type Mm(NiMnSiAl)4.3Co0.6-xFex (x = 0, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6) hydrogen storage alloys were prepared by casting and rapid quenching. The microstructures of the as-cast and quenched alloys were analyzed by XRD, SEM and TEM, and electrochemical cycle stability of the as-cast and quenched alloys were measured. The effects of substitution Fe for Co on microstructures and electrochemical cycle stability of the as-cast and quenched alloys were investigated in detail. The obtained results show that the effects of substitution Fe for Co on the phase structures of the as-cast and quenched alloys are imperceptible, but its effects on electrochemical cycle stability of the alloys are notable. The substitution Fe for Co can improve the cycle stability of the as-cast and quenched alloys. Especially, substitution Fe for Co can significantly enhance the cycle lives of the as-quenched alloys, which is mainly attributed to the grain refinement caused by substitution Fe for Co.
The rare-earth-based AB5-type Mm(NiMnSiAl)4.3Co0.6-xFex (x = 0, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6) hydrogen storage alloys were prepared by casting and rapid quenching. The microstructures of the as-cast and quenched alloys were analyzed by XRD, SEM and TEM, and electrochemical cycle stability of the as-cast and quenched alloys were measured. The effects of substitution Fe for Co on microstructures and electrochemical cycle stability of the as-cast and quenched alloys were investigated in detail. The obtained results show that the effects of substitution Fe for Co on the phase structures of the as-cast and quenched alloys are imperceptible, but its effects on electrochemical cycle stability of the alloys are notable. The substitution Fe for Co can improve the cycle stability of the as-cast and quenched alloys. Especially, substitution Fe for Co can significantly enhance the cycle lives of the as-quenched alloys, which is mainly attributed to the grain refinement caused by substitution Fe for Co.
2006, 35(2):283-286.
Abstract:
采用相转移法制备富锂掺锌的锰酸锂前驱体，然后在空气中进行焙烧反应合成了尖晶石型的Li1＋yZnxMn2-xO4粉体材料，并测试其结构形态特征。考察了该法合成的工艺条件对合成试样粉体产物电化学性能的影响。结果表明：当nLi：nZn：nMn=1．1：0．1：1．9时，反应时间为2h，在750℃空气环境下焙烧10h合成试样粉体过程较为简单，电极试样以10mA／g的恒电流密度充电至4．5V，并以相同的10mA／g恒电流密度放电至3．0V，其放电平台稳定在3．9V，比容量达到120mAh／g，性能稳定。
采用相转移法制备富锂掺锌的锰酸锂前驱体，然后在空气中进行焙烧反应合成了尖晶石型的Li1＋yZnxMn2-xO4粉体材料，并测试其结构形态特征。考察了该法合成的工艺条件对合成试样粉体产物电化学性能的影响。结果表明：当nLi：nZn：nMn=1．1：0．1：1．9时，反应时间为2h，在750℃空气环境下焙烧10h合成试样粉体过程较为简单，电极试样以10mA／g的恒电流密度充电至4．5V，并以相同的10mA／g恒电流密度放电至3．0V，其放电平台稳定在3．9V，比容量达到120mAh／g，性能稳定。
Liu Chunfang
,
Feng Yong
,
Xi Wei
,
Yang Zhijun
,
Liu Jingyan
,
Ji Ping
,
Lu Yafeng
,
Zhang Pingxiang
,
Wu Xiaozu
,
Zhou Lian
2006, 35(2):287-290.
Abstract:
The Ni5W alloy substrates with higher strength, lower magnetism and cubic texture were prepared by a powder metallurgy method for YBCO second-generation coated conductor. The results show that the cube texture fraction in the substrate increases obviously with increasing reduction and heat-treatment temperature. X-ray results show that raising total reduction increases actually quantities of cubic grains and nuclei in cold deformed samples. It can be seen that the time corresponding peak of the curve decreases according to relationship between heat-treatment time and (200) preferential orientation, which illustrates that temperature raises the grow rate of cube nuclei. As the results, the better process and excellent Ni5W substrate with 99%~100% cube textured fraction have been obtained by the study.
The Ni5W alloy substrates with higher strength, lower magnetism and cubic texture were prepared by a powder metallurgy method for YBCO second-generation coated conductor. The results show that the cube texture fraction in the substrate increases obviously with increasing reduction and heat-treatment temperature. X-ray results show that raising total reduction increases actually quantities of cubic grains and nuclei in cold deformed samples. It can be seen that the time corresponding peak of the curve decreases according to relationship between heat-treatment time and (200) preferential orientation, which illustrates that temperature raises the grow rate of cube nuclei. As the results, the better process and excellent Ni5W substrate with 99%~100% cube textured fraction have been obtained by the study.
2006, 35(2):291-294.
Abstract:
In the paper, the microstructure of PS45 coatings prepared by high velocity electric wire arc spraying was investigated by scanning electron microscope. Bonding strength was tested by electron tensile testing machine. The interface morphology of PS45 coatings was acquired by means of picture analysis and processing technology, the computing programs of fractal dimensions and multifractal spectrum were designed in Matlab language. The relations of the bonding strength to spray voltage and fractal dimension and multifractal spectrum were discussed. The results of analysis and calculation show that the better the bonding strength of PS45 coatings is, the more complicated the interface morphology and bigger fractal dimensions are. With spray voltage gone up, the better the interface uniformity is, the smaller the spectrum width is.
In the paper, the microstructure of PS45 coatings prepared by high velocity electric wire arc spraying was investigated by scanning electron microscope. Bonding strength was tested by electron tensile testing machine. The interface morphology of PS45 coatings was acquired by means of picture analysis and processing technology, the computing programs of fractal dimensions and multifractal spectrum were designed in Matlab language. The relations of the bonding strength to spray voltage and fractal dimension and multifractal spectrum were discussed. The results of analysis and calculation show that the better the bonding strength of PS45 coatings is, the more complicated the interface morphology and bigger fractal dimensions are. With spray voltage gone up, the better the interface uniformity is, the smaller the spectrum width is.
28 Nano Ruthenium Oxide/Carbon Nanotubes Composite Electrode Material for Electrochemical Capacitors
2006, 35(2):295-298.
Abstract:
利用氯化钌和碳酸氢钠为反应前驱体,采用溶胶凝胶方法制备了粒径小于70nm的超细氧化钌电极材料。将材料在210℃下加热烧结处理后,材料具有良好的表面特性和最大电化学比容量541F·g-1。当烧结温度在250℃以上时,氧化钌材料明显晶化,同时材料比容量迅速降低。伏安特性测试表明以碳纳米管作为基体制备复合电极可以显著改善氧化钌的容量特性,其中碳纳米管质量分数为20%的复合电极其比容量可以达到860F·g-1。恒流充放电测试证明氧化钌/碳纳米管复合电极组成的超电容器具有良好的大电流放电特性。还综合采用扫描电子显微镜、X射线衍射、热失重分析等手段探讨了烧结温度对氧化钌材料的表面特性、材料结构以及电化学特性的影响。
利用氯化钌和碳酸氢钠为反应前驱体,采用溶胶凝胶方法制备了粒径小于70nm的超细氧化钌电极材料。将材料在210℃下加热烧结处理后,材料具有良好的表面特性和最大电化学比容量541F·g-1。当烧结温度在250℃以上时,氧化钌材料明显晶化,同时材料比容量迅速降低。伏安特性测试表明以碳纳米管作为基体制备复合电极可以显著改善氧化钌的容量特性,其中碳纳米管质量分数为20%的复合电极其比容量可以达到860F·g-1。恒流充放电测试证明氧化钌/碳纳米管复合电极组成的超电容器具有良好的大电流放电特性。还综合采用扫描电子显微镜、X射线衍射、热失重分析等手段探讨了烧结温度对氧化钌材料的表面特性、材料结构以及电化学特性的影响。
2006, 35(2):299-302.
Abstract:
Solid-state method and wet method were employed to synthesize spinel compounds LiNixMn2-xO4.The experimental results indicate that the capacity of high voltage at 4.7 V increase with the increase of amount of Ni. There are impurities in LiNixMn2-xO4 which were made by solid-state method. The sample LiNi0.5Mn1.5O4 had a capacity of 121 mAh/g at first cycle, in which 100 mAh/g was at high voltage range. Its cycle retention rate after 50 cycles was over 92%. The LiNi0.5Mn1.5O4 synthesized by wet method show a single spinel phase without impurity phase. It deliver a discharge capacity of 140 mAh/g in the first cycle, in which 125 mAh/g was at high voltage range. Its cycle retention rate after 50 cycles was over 96%. The XPS experiment results indicate that the oxidation states of Ni and Mn in LiNi0.5Mn1.5O4 made by wet method are +2 and +4 respectively.
Solid-state method and wet method were employed to synthesize spinel compounds LiNixMn2-xO4.The experimental results indicate that the capacity of high voltage at 4.7 V increase with the increase of amount of Ni. There are impurities in LiNixMn2-xO4 which were made by solid-state method. The sample LiNi0.5Mn1.5O4 had a capacity of 121 mAh/g at first cycle, in which 100 mAh/g was at high voltage range. Its cycle retention rate after 50 cycles was over 92%. The LiNi0.5Mn1.5O4 synthesized by wet method show a single spinel phase without impurity phase. It deliver a discharge capacity of 140 mAh/g in the first cycle, in which 125 mAh/g was at high voltage range. Its cycle retention rate after 50 cycles was over 96%. The XPS experiment results indicate that the oxidation states of Ni and Mn in LiNi0.5Mn1.5O4 made by wet method are +2 and +4 respectively.
2006, 35(2):303-307.
Abstract:
The Mg-Ni alloys with different Ni content were prepared by high-energy ball milling. Their structures were determined with X-ray diffraction and their discharge capacities as an electrode were tested. The results show that, as the Ni content increase from Mg2Ni, Mg1.5Ni to MgNi (the ratio of the atom), the structure of Mg-Ni alloy changed from nano-Mg2Ni, amorphous-MgNi to nano-MgNi. The Mg-Ni alloys with different structure exhibit different discharge capacities. As the increase of Ni content, the number of nano-MgNi increase and the discharge capacity could reached 500 mAh/g. As the milling time prolonged, the nano-MgNi with scarcely nano-Ni could be attained. As there was almost no nano-Ni, its discharge capacity is decreased.
The Mg-Ni alloys with different Ni content were prepared by high-energy ball milling. Their structures were determined with X-ray diffraction and their discharge capacities as an electrode were tested. The results show that, as the Ni content increase from Mg2Ni, Mg1.5Ni to MgNi (the ratio of the atom), the structure of Mg-Ni alloy changed from nano-Mg2Ni, amorphous-MgNi to nano-MgNi. The Mg-Ni alloys with different structure exhibit different discharge capacities. As the increase of Ni content, the number of nano-MgNi increase and the discharge capacity could reached 500 mAh/g. As the milling time prolonged, the nano-MgNi with scarcely nano-Ni could be attained. As there was almost no nano-Ni, its discharge capacity is decreased.
2006, 35(2):308-311.
Abstract:
采用粉末冶金法制备了20％Ti-6Al-4V颗粒增强MB15镁基复合材料的试样。按照阿基米得法检测了不同状态试样的密度，借助光镜和扫描电镜探索了挤压棒变形和组织的特点，并结合室温拉伸试验研究了热挤压变形对试样组织及力学性能的影响规律。结果表明：烧结态的密度较低，而热挤后的密度已接近理论值：挤压棒的变形和组织都不均匀：二次挤压可以进一步细化晶粒、提高复合材料的力学性能；Ti-6Al-4V颗粒可以用来强化镁合金，且其增强效果明显好于SiC陶瓷颗粒。
采用粉末冶金法制备了20％Ti-6Al-4V颗粒增强MB15镁基复合材料的试样。按照阿基米得法检测了不同状态试样的密度，借助光镜和扫描电镜探索了挤压棒变形和组织的特点，并结合室温拉伸试验研究了热挤压变形对试样组织及力学性能的影响规律。结果表明：烧结态的密度较低，而热挤后的密度已接近理论值：挤压棒的变形和组织都不均匀：二次挤压可以进一步细化晶粒、提高复合材料的力学性能；Ti-6Al-4V颗粒可以用来强化镁合金，且其增强效果明显好于SiC陶瓷颗粒。
2006, 35(2):312-315.
Abstract:
采用Ni-51Cr（含质量分数为51％Cr）焊料高温钎焊再结晶SiC陶瓷，研究了连接温度、保温时间以及焊料量等对接头三点抗弯强度的影响，并对连接界面区域的微观结构及焊料反应产物进行了SEM，EDS及XRD分析。在本试验中，当连接温度为1360℃，保温时间为5min，焊料量为350mg时得到的接头三点抗弯强度最高，为74．2MPa。微观结构结果表明：SiC，Ni和Cr均发生了扩散；在母材SiC与焊料中间层之间，生成了一反应层，反应层的主要成分为Ni2Si和C：而Cr主要分布于焊料中间层中，以Cr23C6，Cr7C3等形式存在。
采用Ni-51Cr（含质量分数为51％Cr）焊料高温钎焊再结晶SiC陶瓷，研究了连接温度、保温时间以及焊料量等对接头三点抗弯强度的影响，并对连接界面区域的微观结构及焊料反应产物进行了SEM，EDS及XRD分析。在本试验中，当连接温度为1360℃，保温时间为5min，焊料量为350mg时得到的接头三点抗弯强度最高，为74．2MPa。微观结构结果表明：SiC，Ni和Cr均发生了扩散；在母材SiC与焊料中间层之间，生成了一反应层，反应层的主要成分为Ni2Si和C：而Cr主要分布于焊料中间层中，以Cr23C6，Cr7C3等形式存在。
33 Effect of Rhenium on Crystal Structure and Curie Temperatures of (Gd1-xREx)5Si4(RE=Dy, Ho) alloys
2006, 35(2):316-319.
Abstract:
用真空电弧熔炼制备（Gd1-xREx）5Si4（x=0．1，0．2，0．3，0．35）和（Gd1-xHox）5Si4（x=0．05，0．15，0．25）系列合金，在950℃下168h的真空热处理后，对其晶体结构、居里温度进行了研究。室温XRD分析发现该系列合金仍保持Gd5Si4的Sm5Ge4正交型结构，采用Rietveld法分析计算发现合金晶格常数随着X量的增加而逐渐减小。试样M-T磁化曲线测量结果表明：居里温度瓦在336K～260K连续可调，改变RE的含量可以得到不同的居里温度Tc;Tc近似呈线性变化，由此得出估计（Gd1-xREx）5Si4（RE=Dy，Ho）的Tc的计算公式。
用真空电弧熔炼制备（Gd1-xREx）5Si4（x=0．1，0．2，0．3，0．35）和（Gd1-xHox）5Si4（x=0．05，0．15，0．25）系列合金，在950℃下168h的真空热处理后，对其晶体结构、居里温度进行了研究。室温XRD分析发现该系列合金仍保持Gd5Si4的Sm5Ge4正交型结构，采用Rietveld法分析计算发现合金晶格常数随着X量的增加而逐渐减小。试样M-T磁化曲线测量结果表明：居里温度瓦在336K～260K连续可调，改变RE的含量可以得到不同的居里温度Tc;Tc近似呈线性变化，由此得出估计（Gd1-xREx）5Si4（RE=Dy，Ho）的Tc的计算公式。
34 Preparation and Electrochemical Characteristics of Mg-Based Composite Materials for Hydrogen Storage
2006, 35(2):320-323.
Abstract:
NiB powder was prepared by mechanically alloying in this paper and was composited mechanically with MgNi amorphous alloy. The effect of NiB on structure and electrochemical performance of MgNi-electrode was studied. The XRD analysis show that MgNi-NiB composite is amorphous phase. The electrochemical characteristics of this composite were also studied. The cycle life of the MgNi-NiB electrode is improved.
NiB powder was prepared by mechanically alloying in this paper and was composited mechanically with MgNi amorphous alloy. The effect of NiB on structure and electrochemical performance of MgNi-electrode was studied. The XRD analysis show that MgNi-NiB composite is amorphous phase. The electrochemical characteristics of this composite were also studied. The cycle life of the MgNi-NiB electrode is improved.
2006, 35(2):324-328.
Abstract:
Plating Cu on TiNi/Ti/SiO2/Si substrate in the HF+CuSO4 solution by separated electrodes chemical method was discussed in this essay. Si and TiNi/Ti/SiO2/Si are used as the anode and cathode. The best condition for the plating is as followings: distance for the electrodes is 0.5 mm, [HF] and [CuSO4] more than 8 wt% and 0.045 mol/L. Finally uniform deposited Cu film with complete coverage, few voids and preference of <111> is obtained. Also deposited Cu film does not contain Cu2O, which reduces the resistivity.
Plating Cu on TiNi/Ti/SiO2/Si substrate in the HF+CuSO4 solution by separated electrodes chemical method was discussed in this essay. Si and TiNi/Ti/SiO2/Si are used as the anode and cathode. The best condition for the plating is as followings: distance for the electrodes is 0.5 mm, [HF] and [CuSO4] more than 8 wt% and 0.045 mol/L. Finally uniform deposited Cu film with complete coverage, few voids and preference of <111> is obtained. Also deposited Cu film does not contain Cu2O, which reduces the resistivity.
36 Solid Phase Spectrophotometric Determination of Trace Amount of Lanthanum with DBC-Chlorophosphonazo
2006, 35(2):329-332.
Abstract:
在0.5 mo1·L-1盐酸介质中,La(Ⅲ)-(DBC-偶氮氯膦)所形成的络合物可吸附到201×7型苯乙烯阴离子树脂上.该固相显色体系最大吸收波长位于650 nm,镧的表观摩尔吸光系数为ε650nm=2.08×l05L·mol-1·cm-1.该固相分光光度法测定镧灵敏度为La(Ⅲ)-(DBC-偶氮氯膦)液相分光光度法灵敏度的2.31倍.镧在0～0.44 μg.ml-1范围内遵守比尔定律.考察了26种共存离子对测定镧的影响.本研究所建立的方法已成功地用于分子筛中镧的测定,结果满意.
在0.5 mo1·L-1盐酸介质中,La(Ⅲ)-(DBC-偶氮氯膦)所形成的络合物可吸附到201×7型苯乙烯阴离子树脂上.该固相显色体系最大吸收波长位于650 nm,镧的表观摩尔吸光系数为ε650nm=2.08×l05L·mol-1·cm-1.该固相分光光度法测定镧灵敏度为La(Ⅲ)-(DBC-偶氮氯膦)液相分光光度法灵敏度的2.31倍.镧在0～0.44 μg.ml-1范围内遵守比尔定律.考察了26种共存离子对测定镧的影响.本研究所建立的方法已成功地用于分子筛中镧的测定,结果满意.
2006, 35(2):333-336.
Abstract:
The determination of impurity elements of Sn, P, Ca, Nb, Ta, Mo, Cu, Pb, Zn, As, Mn, Bi and Fe in tungsten concentrates have been studied using ICP-MS. After the samples were completely liquated by Na202-NaOH, tungsten was precipitated in the form of H2WO4 and separated from the solution on the addition of water and nitric acid. Adding internal standard elements of ^45Sc, ^115In, ^205T1 to the sample solution, the effect of matrix, interface and fluctuation of instrument has been overcome effectively by use of matrix match and internal standard calibration method. By choosing the optional operation parameters and appropriate isotopes of element to be detected, the influence of mass spectrometry interference has been conquered effectively. The effect of acidity on the separation of tungsten and detected elements has been tested. The recovery for spiking sample was 90.5%-101.5%, and the relative standard deviation was 1.2%-7.8%. This method is a simple, rapid and accurate method, and it could be used in the testing of tungsten concentrates and tungsten products.
The determination of impurity elements of Sn, P, Ca, Nb, Ta, Mo, Cu, Pb, Zn, As, Mn, Bi and Fe in tungsten concentrates have been studied using ICP-MS. After the samples were completely liquated by Na202-NaOH, tungsten was precipitated in the form of H2WO4 and separated from the solution on the addition of water and nitric acid. Adding internal standard elements of ^45Sc, ^115In, ^205T1 to the sample solution, the effect of matrix, interface and fluctuation of instrument has been overcome effectively by use of matrix match and internal standard calibration method. By choosing the optional operation parameters and appropriate isotopes of element to be detected, the influence of mass spectrometry interference has been conquered effectively. The effect of acidity on the separation of tungsten and detected elements has been tested. The recovery for spiking sample was 90.5%-101.5%, and the relative standard deviation was 1.2%-7.8%. This method is a simple, rapid and accurate method, and it could be used in the testing of tungsten concentrates and tungsten products.
