火焰原子吸收光谱法测定铂铱合金中铱

样品经王水在烘箱中于180℃消解12h后,加入10mL100g/L氯化镧溶液和10mL100g/L硫酸铜溶液为释放剂,采用火焰原子吸收光谱法(FAAS)测定铂铱合金样品中铱。研究表明,铱浓度在15~100μg/mL范围内与其吸光度呈良好的线性关系,线性回归方程为A=0.00083ρ+0.0015,相关系数为0.9995,方法的检出限为0.0028μg/mL。采用方法对Pt25Ir和Pt10Ir样品中铱进行测定,并加入铱标准溶液进行加标回收试验,测得结果的相对标准偏差(n=11)为1.6%和2.3%,加标回收率为95%~101%。     

TiAl合金钎焊研究进展

TiAl合金钎焊因具有无气体杂质、对母材力学性能影响小、钎料成分易控制等突出优点而被广泛应用。概述了TiAl合金的发展历程及其组织特点,重点介绍了TiAl合金钎料种类以及钎焊工艺对焊接接头组织与性能的影响,最后指出TiAl合金钎焊技术的发展方向：加强焊接接头的动态试验研究,如疲劳性能、冲击韧性及蠕变试验;从扩散机理出发,首先进行热力学和动力学分析,再根据母材成分变化设计专用钎料;进一步扩展TiAl合金钎焊技术的应用领域。     

微波消解技术在分析难处理贵金属及其物质中铑、铱、铂、钯的研究与应用

提出了微波密闭消解难处理贵金属Rh,Ir粉及其冶金物料和矿石的新方法,对比了它们的微波密闭消解法与传统分(消)解法的条件,分析了贵金属Rh,Ir,Pt和Pd的含量。结果表明:上述各类物质对应消解时间分别为传统法的1/96~1/67,1/16~1/8和1/2,总分析流程均大大缩短;两种消(分)解法测得贵金属含量吻合;提出方法新颖、快速、实用。     

锍试金富集-电感耦合等离子体质谱法测定地质样品中铂钯铑铱

建立了锍试金富集电感耦合等离子体质谱法(ICP-MS)测定地质样品中铂、钯、铑、铱的新方法。样品用硫化镍富集,酸处理除去碱金属硫化物,过滤,残渣用盐酸和过氧化氢溶解,ICP-MS法测定。研究了富集时各种因素的影响。方法检出限:Pt为0.11ng/g,Pd为0.038ng/g,Rh为0.016ng/g,Ir为0.040ng/g;相对标准偏差(n=12):Pt为4.09%,Pd为4.75%,Rh为4.53%,Ir为4.78%。测定了国家一级地球化学标准物质中痕量Pt,Pd,Rh,Ir,结果与认定值相吻合。     

各种热电偶及其性能

表1(a)贵金属热电偶(单元和二元铂合金)序号 类Au与PtPt一IOIr与Pt,Ir与Pt型Pt一z5lr与Pt,Pt一201:与Pt-Ir与Pt一Zolr,Ir与Pt一3olrPt与PdPt一10Rh与PtPt一13Rh与PtP卜i3Rh与P卜O·SRh,Pt一z3Rh与Pt一iRhPt一20Rh与Pt一SRh,Pt一30Rh与Pt一6RhPt一40Rh与Pt一20RhRh与PtRh与Pt-10RhRh与P t--20Rh,Rh与Pt一30RhPt一6Ru与PtP卜10Ir与Au一40PdPt一ioRh与Au一遵OPdPt一i0lr与Pd,Pt一i5lr与PdQ甘n︸11,‘升口d‘自匕n匕 弓上,人,工‘上,上,1 1.人Pt一20Rh与PdIr与Pt一i0Rh 性能非常稳定,在。~600OC范围内温度电…     

多元光谱拟合校正-电感耦合等离子体原子发射光谱法测定铱化合物中19种杂质元素

铱化合物产品中杂质元素的准确测定,是判定产品级别的重要指标,以往常采用摄谱法进行测定,但Ca、Si、Mg、Fe、Na测定结果准确性差,周期较长。根据铱化合物易溶于水及酸的性质,采用盐酸溶解样品,电感耦合等离子体原子发射光谱法(ICP-AES)测定了三氯化铱、四氯化铱、氯铱酸、氯铱酸铵等铱化合物中Pt、Pd、Ru、Rh、Ag、Au、Cu、Fe、Zn、Ni、Mn、Mg、Al、Ca、Sn、Na、Si、Pb、K等19种杂质元素。基体Ir对Pt、Sn产生的光谱干扰采用多元光谱拟合(MSF)方法校正,杂质元素间没有干扰。方法的检出限(μg/mL)为0.078(Pt)、0.0080(Pd)、0.014(Ru)、0.031(Rh)、0.0029(Ag)、0.016(Au)、0.0035(Cu)、0.012(Fe)、0.014(Zn)、0.0098(Ni)、0.0010(Mn)、0.0022(Mg)、0.0016(Al)、0.021(Ca)、0.057(Sn)、0.020(Na)、0.11(Si)、0.014(Pb)和0.0083(K)。按照实验方法测定三氯化铱中Pt、Pd、Ru、Rh、Ag、Au、Cu、Fe、Zn、Ni、Mn、Mg、Al、Ca、Sn、Na、Si、Pb、K等19种元素,结果的相对标准偏差(RSD,n=9)为1.2%~7.4%;加标回收率在89%~114%之间。     

金属Nb对Co基钎料焊接的影响

以WCo75钎料为研究基础,结合分析Co-Nb和Nb-W二元相图,设计了理论成分比例为Co∶W∶Nb=65∶25∶10(%,质量分数)的合金钎料,以期获得温度段合适,符合阴极钎焊标准的高温钎料。对WCo75和Co-W-Nb这两个体系钎料的熔化温度、润湿性以及其铺展后的焊缝形貌成分进行了测试、分析、对比,研究并讨论了Nb的影响。结果表明:加入金属Nb可以有效地将WCo75钎料的熔点由1480.0降至1238.5℃,润湿角也由小于20°减小至5°左右,效果显著。两种钎料都有良好的焊接效果,焊后没有裂纹或熔蚀、熔析等不良缺陷。能够在得到的焊接组织中发现富集相(富Co相靠近自由端而富W相靠近基材),钎料与母材之间有一定的相互扩散。加入Nb后,一方面不会改变钎料层的富集趋势,另一方面能够显著地促进W向Mo母材的扩散,同时,不会因为造成阴极的污染或是毒化而影响其发射效率。     

Ag-28Cu钎焊TiNiSMA接头的微观组织特征

为充分发挥SMA的高阻尼特性,制作高性能的新型阻尼器,本文开展了TiNiSMA的钎焊制备及其性能研究。研究结果表明:焊接接头的界面组织主要为a-Ti+Ti2Cu(TiCu2及Ti(Ni,Cu))+Ag一次固溶体+Ag-Cu共晶。随着钎焊温度的不断升高,焊缝尺寸不断减小。钎焊温度为870℃时,连接层与母材界面以小型锯齿状结合,而生成的Ti2Cu相对形状记忆效应有利,组织致密。     

焊接热输入对酒钢2205双相不锈钢相比例的影响

2205是一种新型的双相不锈钢,其中的组织为奥氏体和铁素体。当奥氏体与铁素体的比例接近1:1时焊接接头力学性能最好。通过对奥氏体含量与冷却速度的关系,得出冷却速度过慢容易在接头中形成脆性相(σ相)。无论是焊接接头的微观组织结构还是合金元素在铁素体和奥氏体两相中的分布都接近于母材;这样的焊接接头力学性能最好。通过控制热输入最终获得接近于母材的焊接接头。     

烧结钎焊粉末冶金零件研究

烧结钎焊是一种已确立的粉末冶金零件连接工艺,经常用于生产汽车零部件。成功的钎焊连接主要取决于钎焊合金、连接表面与烧结气氛间的相互作用。将广泛使用的钎焊合金,Ancorbraze 72(AB 72),设计成与焊接的母体材料形成合金和能局部密封钢粉末冶金零件的表面孔隙,从而可防止因熔渗造成钎料材料的大量损失。本文将检验在不同生产工艺条件下钎焊的性状,和研究与表征焊剂与铁使钎焊合金的改性对熔化与凝固性状的影响。     

Phase Transformation and Shape Memory Effect of Ti(Pt, Ir)

The martensitic transformation and shape memory effect of Ti₅₀(Pt, Ir)₅₀ with 5?C37.5 at. pct Ir were investigated using differential thermal analysis (DTA), high-temperature X-ray diffraction (HT-XRD), and compression tests. The austenite finish temperature, A _f, increased with increasing Ir content from 1331?K (1058?°C) in Ti-50 at. pct Pt to 1491?K (1218?°C) in Ti-12.5Pt-37.5Ir. The structure of the parent and martensite phases was identified as B2 and B19 in all tested alloys. A large strain recovery rate was obtained in Ti₅₀(Pt, Ir)₅₀ with 10 to 30 at. pct Ir. The highest shape recovery ratio was 57?pct in Ti-25Pt-25Ir after deformation at 1123?K (850?°C), followed by heating to above A _f. Using HT-XRD, the dependence of lattice parameter change on Ir content and temperature was investigated. The volume change during phase transformation from B2 to B19 was estimated using the lattice parameter of the B2 and B19 phases. Strain recovery is discussed along with volume change and lattice parameter change.     

Ir-Nb-Si ternary refractory superalloys with a three-phase Fcc/L12/silicide structure for high-temperature applications: Phase and microstructural evolution

To find a new phase with the potential to improve the high-temperature strength of Ir-based superalloys, the novel idea of introducing silicides into the Ir-Nb binary was implemented. Hypoeutectic Ir-10Nb, eutectic Ir-16Nb, and hypereutectic Ir-25Nb alloys were used as bases, and 5 mol pct Si was added through the removal of Ir. XRD (XRD), scanning electron microscopy (SEM), and electron-probe microanalysis (EPMA) revealed the formation of a three-phase fcc/L1₂/silicide microstructure in the Ir-Nb-Si ternary after Si addition. The type of silicide formed was dependent on heat-treated temperatures and Nb content. After heat treatment at 1750 °C and 1600 °C, a tie-triangle composed of fcc/L1₂/silicide (Ir₂Si) appeared in the Ir-10Nb-5Si and Ir-16Nb-5Si alloys; in the Ir-25Nb-5Si alloy, an L1₂ and silicide (Ir,Nb)₂Si tie-line was observed. In the as-cast and 1300 °C heat-treated samples, the Ir-10Nb-5Si microstructure changed to a two-phase fcc/silicide structure, while the Ir-16Nb-5Si alloy maintained a three-phase fcc/L1₂/silicide structure. The Ir-25Nb-5Si alloy, however, had the same phases as that at 1600 °C. Silicides typically continuously or discontinuously distribute along the interdendritic regions or grain boundaries of the fcc or the L1₂ phase. With the addition of Si, it was found that both the eutectic point and solid solubility of Nb in Ir would shift toward Ir.     

Effect of Coatings on the Heat Resistance of VT-41 and VIT1 Alloys during Isothermal Oxidation

The influence of aluminide coatings on high-temperature α + β VT-41 alloy and a VIT1 alloy based on the Ti₂NbAl orthophase on the isothermal heat resistance at 700°C is studied during oxidation in still air. NiCrAlY and Al(Si) coatings are found to substantially increase the heat resistance of the alloys at 700°C. The phase composition of the aluminosilicide layer (TiAl₃ + TiSi₂ + Ti₅Si₃) under the NiCrAlY coating significantly retards the titanium diffusion to the NiCrAlY layer and can be used as a diffusion barrier and a aluminum source for the NiCrAlY layer during high-temperature oxidation.     

Overview of Strategies for High-Temperature Creep and Oxidation Resistance of Alumina-Forming Austenitic Stainless Steels

A family of creep-resistant, alumina-forming austenitic (AFA) stainless steel alloys is under development for structural use in fossil energy conversion and combustion system applications. The AFA alloys developed to date exhibit comparable creep-rupture lives to state-of-the-art advanced austenitic alloys, and superior oxidation resistance in the ~923 K to 1173 K (650 °C to 900 °C) temperature range due to the formation of a protective Al₂O₃ scale rather than the Cr₂O₃ scales that form on conventional stainless steel alloys. This article overviews the alloy design approaches used to obtain high-temperature creep strength in AFA alloys via considerations of phase equilibrium from thermodynamic calculations as well as microstructure characterization. Strengthening precipitates under evaluation include MC-type carbides or intermetallic phases such as NiAl-B2, Fe₂(Mo,Nb)-Laves, Ni₃Al-L1₂, etc. in the austenitic single-phase matrix. Creep, tensile, and oxidation properties of the AFA alloys are discussed relative to compositional and microstructural factors.     

Features of high-temperature oxidation in air of silver and alloy Ag-Cu, and adsorption of oxygen on silver

Thermodynamic calculations are provided for equilibrium in the system Ag-O₂. Kinetics of high-temperature (up to 900 °C) oxidation in air of plates made from pure silver (99.99 mass% Ag) and jewellery alloy 84 at.% Ag-16 at.% Cu are studied by nonisothermal thermogravimetry, and differential and petrographic analyses of the reaction products. Mechanisms are established for the corresponding oxidation reactions confirming the absence of chemical reaction for pure silver with oxygen at T > 422 K. The Wagner theory for oxidation of alloys containing precious metals is confirmed by the results. The temperature ranges are determined for van de Waals adsorption and chemisorption of oxygen at the surface of very pure silver powder with a specific surface area S = 0.4 m²/g.     

High-Temperature Creep and Oxidation Behavior of Mo-Si-B Alloys with High Ti Contents

Multiphase alloys in the Mo-Si-B system are potential high-temperature structural materials due to their good oxidation and creep resistance. Since they suffer from relatively high densities, the current study focuses on the influence of density-reducing Ti additions on creep and oxidation behavior at temperatures above 1273 K (1000 °C). Two alloys with compositions of Mo-12.5Si-8.5B-27.5Ti and Mo-9Si-8B-29Ti (in at. pct) were synthesized by arc melting and then homogenized by annealing in vacuum for 150 hours at 1873 K (1600 °C). Both alloys show similar creep behavior at stresses of 100 to 300 MPa and temperatures of 1473 K and 1573 K (1200 °C and 1300 °C), although they possess different intermetallic volume fractions. They exhibit superior creep resistance and lower density than a state-of-the-art Ni-base superalloy (single-crystalline CMSX-4) as well as other Mo-Si-B alloys. Solid solution strengthening due to Ti was confirmed by Vickers hardness measurements and is believed to be the reason for the significant increase in creep resistance compared to Mo-Si-B alloys without Ti, but with comparable microstructural length scales. The addition of Ti degrades oxidation resistance relative to a Mo-9Si-8B reference alloy due to the formation of a relatively porous duplex layer with titania matrix enabling easy inward diffusion of oxygen.     

Oxide Scales Formed on NiTi and NiPtTi Shape Memory Alloys

Ni-49Ti and Ni-30Pt-50Ti (nominal at. pct) shape memory alloys (SMAs) were isothermally oxidized in air over the temperature range of 773?K to 1173?K (500?°C to 900?°C) for 100?hours. The oxidation kinetics, presented in detail in a companion study, show ~4 times reduction in oxidation rate due to Pt.[1] The microstructure, composition, and phase content of the scales and depletion zones were determined by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and X-ray diffraction (XRD). A relatively pure TiO₂ rutile structure was identified as the predominant scale surface feature, typified by a distinct highly striated and faceted crystal morphology, with crystal size proportional to oxidation temperature. The complex layered structure beneath these crystals was characterized by semiquantitative XRD of serial/taper polished sections and SEM/EDS of cross sections for samples oxidized at 973?K (700?°C). In general, graded mixtures of TiO₂, NiTiO₃, NiO, Ni(Ti), or Pt(Ni) metallic dispersoids, and continuous Ni₃Ti or Pt-rich metal depletion zones, were observed from the gas surface to the substrate interior. Overall, substantial depletion of Ti occurred due to the formation of predominantly TiO₂ scales. It is proposed that the Ni-30Pt-50Ti alloy oxidized more slowly than the binary Ni-49Ti alloy by decreasing oxygen and titanium diffusion through the thin Pt-rich layer.     

Correlation between Microstructures and Oxidation Resistance in Zr-Nb-Ti Alloys

Oxidation behavior of Zr-10Nb-10Ti and Zr-10Nb-20Ti (compositions are in atomic percent) alloys has been investigated in air between 300 °C and 700 °C. Higher Ti content in the alloy enhances the oxidation resistance. The calculated isotherms by PANDAT[1,2] show that 20Ti enters a three-phase (αZr-hcp, βNb-bcc, and βZr-bcc) region at 500 °C, while 10Ti alloy continues to be a two-phase (αZr and βNb) alloy until 550 °C and then enters the three-phase (αZr, βNb, and βZr) region. Both alloys have a single-phase βZr solid solution at 700 °C, which is detrimental for the oxidation resistance. The βNb phase greatly contributes to the oxidation resistance in these two alloys. The common oxidation products have been identified as TiO₂, ZrO₂, and Nb₂O₅. Both alloys suffer from pest oxidation at temperatures between 500 °C and 550 °C, respectively (20Ti and 10Ti), up to 700 °C. X-ray diffraction (XRD) indicates strong peaks for monoclinic structure of ZrO₂ at temperatures above 600 °C.     

Mechanical properties of Ir-Nb alloys containing Ni and Al

Two alloys made by adding 5 or 10 at. pct, respectively, of Ni-18.9 at. pct Al to an Ir-15 at. pct Nb alloy were investigated. The microstructure and compressive strength at temperatures between room temperature and 1800 °C were investigated to evaluate the potential of these alloys for ultra-high-temperature use. Their microstructural evolution indicated that the two alloys formed fcc and L1₂-Ir₃Nb two-phase structures. The fcc and L1₂ two-phase structures were examined by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The 0.2 pct flow stresses were above 1000 MPa at temperatures up to 1200 °C, about 150 MPa at 1500 °C, and over 100 MPa at 1800 °C. The strength of the quaternary Ir-base alloys at 1200 °C was even higher than that of Ir-base binary and ternary alloys. And the strength of quaternary Ir-Nb-Ni-Al was equivalent to that of the Ir-15 at. pct Nb binary alloy at 1800 °C. The compressive ductility of quaternary (around 20 pct) was improved drastically compared with that of the Ir-base binary alloy (lower than 10 pct) and the ternary Ir-base alloys (about 11 pct). An excellent balance of high-temperature strength and ductility was obtained in the alloy with 10 at. pct Ni-18.9 at. pct Al. The effect of Ni and Al on the strength of the Ir-Nb binary alloy is discussed.