Synthesis of Ti3SiC2 by spark plasma sintering(SPS)of elemental powders

Ti3SiC2 materials have been fabricated by spark plasma sintering of the elemental powders with the addition of Al.At the heating rate of 80℃/min and under the pressure of 30MPa,the ideal synthesis temperature of Ti3SiC2 is in the range of 1150-1250℃.The addition of Al is in favor of the formation of Ti3SiC2.The synthesized compound has the molecular of Ti3Si0.8Al0.2C2 and lattice parameters of α=0.3069nm,c=1.7670nm.Its grain is plane-shape with a size of about 50μm in the elongated dimension.The prepared material has Vickers hardness of 3.5-5.5GPa(at 1N and 15s) and is as readily machinable as graphite‘s.     

高温熔融-电感耦合等离子体原子发射光谱法测定含铁尘泥中5种有害元素

准确、快速地测定含铁尘泥中有害元素,对含铁尘泥节能降废项目研究及综合利用有着重要的指导意义。实验针对含铁尘泥试样因含碳量高,导致常规酸溶解方法如果不增加除碳步骤则很难完全分解试样的问题,采用高温熔融法将试样制成熔融液后倾倒于稀酸中溶解的方法,解决了碳含量高难溶解的问题。采用四硼酸锂-碳酸锂混合熔剂在高温下将试样熔融,熔融液高温倾倒于稀酸中制成澄清溶液,由于骤冷,试样炸裂成微小玻璃珠,无迸溅,操作简单,使得后续溶解过程快速完成,从而建立了电感耦合等离子体原子发射光谱(ICP-AES)测定P、Pb、K、Na、Zn共5种有害元素的方法。按照实验方法测定含铁尘泥中P、Pb、K、Na、Zn,测定值的相对标准偏差(RSD,n=9)在1.4%～5.7%之间,加标回收率在96%～110%之间。研究结果表明方法能够满足含铁尘泥样品中5种元素的定量分析要求。     

我国冶金分析定量检测仪器的发展趋势

为了了解我国分析仪器的发展,推动冶金分析领域定量检测技术的进步,文章以北京分析测试学术报告会暨展览会(BCEIA)在国内的展示成果为依托,选择电感耦合等离子体发射光谱(ICP-OES)、电感耦合等离子体质谱(ICP-MS)、X射线荧光光谱(XRF)、激光诱导击穿光谱(LIBS)等基础定量检测仪器为主要分析对象,归纳总结了这些仪器的发展过程、基本原理和主要结构。从分析检测人员的视角,讨论了该检测仪器的优势特点及应用效果;展望了定量分析检测技术的发展趋势;提出了以定量检测仪器为基础的新型高端科学仪器的发展前景。又以激光剥蚀电感耦合等离子体质谱(LA-ICP-MS)、辉光放电质谱(GD-MS)、电子探针X射线显微分析仪(EPMA)等拓展联用检测仪器为例,介绍了设备的主要特点及应用,最终总结出LA-ICP-MS为固体样品中微量元素分析的常用技术,GD-MS技术是痕量元素分析的重要手段,EPMA技术因具有与其他仪器结合包容性高的优点,虽然在使用过程中存在一定的缺陷,但已成为通用的分析手段。而我国定量分析检测技术正朝着现场化、专用化及标准化的方向发展。     

电感耦合等离子体原子发射光谱法测定云南某矿山锑矿选矿流程样品中锑

锑在现代工业体系中占有重要地位,快速准确测定锑矿中锑含量对锑矿的采选具有重要指导意义。云南某矿山锑矿以萤石为主要伴生矿,现有的盐酸、硝酸、氢氟酸和高氯酸混酸体系无法彻底分解样品,而采用碱熔处理流程长且引入大量基体,均无法满足准确快速测定的要求。选择硫酸-氢氟酸混酸体系分解样品,再用酒石酸-盐酸混合溶液加热浸取,锑完全溶解于溶液中,选择Sb 206.833{463}nm为分析谱线,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定锑。结果表明,锑的质量浓度在5.0～80 μg/mL范围内与其发射强度呈良好的线性关系,校准曲线线性相关系数r=0.999 8;方法的检出限为0.012 μg/mL。按照实验方法对锑矿石成分分析标准物质和锑矿选矿流程样品中锑进行测定,结果的相对标准偏差(RSD,n=5)为0.71%～5.7%;标准物质的认定值和测定值相一致;锑矿选矿流程样品中锑的加标回收率为97%～102%,满足国家地质矿产行业标准DZ/T 0130—2006的要求。     

Electric and mechanical performances of Bi0.5Sb1.5Te3 prepared by spark plasma sintering

Thermoelectric (TE) materials are a kind of functional materials which can be used to convert directly heat energy to electricity or reversely.The thermoelectric effects hold great potential for application in power generation and refrigeration.Bi2Te3 and its alloys are well known as best TE materials currently available near room temperature.This paper studies respectively the effects of spark plasma sintering (SPS) on electric performance of Bi0.5Sb1.5Te3 thermoelectric materials that are prepared through vacuum melting and ball milling.Through X-ray Diffraction and cold field emission scanning electric microscope s4800, the phase constituent and microstructure of the TE materials samples were analyzed.Electric conductivity and power factor can be improved with the rise of Spark Plasma Sintering temperature (from 300 to 500 ℃) and pressure(from 30 to 60 MPa), and the density and mechanical strength of Bi0.5Sb1.5Te3 thermoelectric material increase, too.     

Quantification of trace amounts of impurities in high purity cobalt by high resolution inductively coupled plasma mass spectrometry

An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of 24 elements (Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, Sb, Ba, Pt, Au, and Pb) in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCl. The matrix effects because of the presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the deter- mination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits were 0.016-1.50 μg?g?1, the recovery ratios were 92.2%-111.2%, and the RSD was less than 3.6%. The method was accurate, quick, and convenient. It was applied to the determination of trace impurities in high purity cobalt with satisfactory results.     

等离子原位合成Ni-Al金属间化合物涂层的组织与性能研究

利用等离子激发原位反应在碳钢表面合成了Ni-A1金属问化合物涂层。借助金相显微镜、扫描电镜、X射线衍射仪和显微硬度计对涂层的组织和性能进行了研究。结果表明：当Ni和Al的质量百分比为4：1时，涂层与基体呈冶金结合，无裂纹和气孔等缺陷；涂层的主要组成相为NiAl和NiAl；涂层组织为细密的树枝晶；涂层的硬度高于基体，硬度可达630HV；涂层耐蚀性能良好。     

ZrB2-SiC基超高温陶瓷（UHTCs）的反应烧结及SHS粉体制备

用普通反应热压方法（RHP）和反应放电等离子体方法（R-SPS）原位反应制备了ZrB2-SiC，ZrB2-SiC—ZrC，ZrB2-SiC-ZrN，以及ZrB2-SiC-AIN4种复合材料。从密度，物相以及显微结构等方面比较了两种烧结方式之间的差别，对于升温速度较慢的普通热压方法，反应分步进行，显微结构不均匀；对于升温速度快的放电等离子体烧结，原料间的自蔓延反应被点着，反应速度快，显微结构均匀。同时以红外灯的热量为点火源，引发了Zr，Si及B4C间在空气气氛下的自蔓延反应，制备了较纯及粒径约为1μm的活性粉体。     

Study On the Tribological Behavior of the Arc-added Glow Discharge Plasma Non-hydrogen Carburization On Titanium Alloy Surfaces

This paper introduces a new titanium alloys surface strengthening treatment by using the arc-added glow discharge plasmas non-hydrogen carburization technique. High purity and high strength graphite is selected as cooling cathode arc source for supplying carbon atoms and particle, which migrate to the titanium alloy(Ti6Al4V) surface and form modified layer. Thus, the hydrogen embrittlement is avoided while the tfibological behavior of the titanium alloy surface is improved in the respects of anti-friction and anti-wear ability.The tribological behavior of the modified layer under dry sliding against SAE52100 steel was evaluated on a ball-on-disc test rig. The results showed that the modified layer obtained a thickness of 30μm at 980℃, 30minutes. The microhardness of the Ti6Al4V alloy surface attained 936 HV, which was much larger than that of the Ti6AI4V alloy. The Ti6AI4V alloy was characterized by adhesion wear and scuffing under dry sliding against the steel, while the surface modified layer experienced much abated adhesion wear and scuffing under the same testing condition. This could be attributed to the carbon dement with different modalities exists in the modified layer.The modified layer showed good friction-reducing and fair anti-wear ability in dry sliding against the steel. Using the SEM,XRD and XPS, the phase structure and morphology of the carburization modified layer was analyzed.     

A machine vision approach to seam tracking in real-time in PAW of large-diameter stainless steel tube

Manual monitoring and seam tracking through watching weld pool images in real-time, by naked eyes or by industrial TV, are experience-depended, subjective, labor intensive, and sometimes biased. So it is necessary to realize the automation of computer-aided seam tracking. A PAW (plasma arc welding) seam tracking system was developed, which senses the molten pool and the seam in one frame by a vision sensor, and then detects the seam deviation to adjust the work piece motion adaptively to the seam position sensed by vision sensor. A novel molten pool area image-processing algorithm based on machine vision was proposed. The algorithm processes each image at the speed of 20 frames/second in real-time to extract three feature variables to get the seam deviation. It is proved experimentally that the algorithm is very fast and effective. Issues related to the algorithm are also discussed.