A study of cutting tool wear by neutron activation technique

A study of cutting tool wear with neutron activated cutting tools is described. The effect of cutting speed and cutting feed on the total tool wear is investigated for the tool and workpiece combination under consideration. A relation between relative tool life and cutting speed obtained from experimental data is given     

Complexometric determination of magnesium in nodular cast iron and alloyed cast iron roll samples

A complexometric method for the determination of magnesium in nodular cast iron, alloyed cast iron and roll samples has been developed. The bulk of the iron is removed by ether extraction and the phosphate as zirconium phosphate. The other elements are removed by extraction with dithiocarbamate into chloroform. Magnesium is then titrated with EDTA at pH 10, with Eriochrome Black T as indicator. Calcium interferes, but is very rarely present in such cast iron samples.     

High Precision Diamond Machining of Hybrid Sol-Gel Coatings

Flexible and economic production of complex reflective optical elements is achieved by high-precision machining of aluminum and copper with diamond tools. There is also an increasing demand for complex refractive optical elements like micro lens arrays, Fresnel lenses or prismatic surfaces on silicon wafers or metallic surfaces. For the production of these optical elements, hybrid sol-gel coatings based on methacryloxypropyltrimethoxysilane (MATMS) and zirconium (IV) tetra n-propoxide (ZTP) were deposited on aluminum substrates by spin-coating. The influence of the rotational velocity and the chemical sol composition on the coating thickness was determined. The hardness and elastic modulus of these coatings was measured as a function of the chemical composition. The machining characteristics of these coatings were investigated by high precision turning and fly cutting with diamond tools of different geometry. The resulting surface finish obtained was determined as a function of the machining parameters.     

微量稀土元素添加剂对YT14硬质合金粒度的影响

利用能谱仪的图像处理程序研究和微量混合稀土元素添加剂对ＹＴ１４硬质合金粒度的影响。结果表明：添加不影响硬质相ＷＣ和粘结相Ｃｏ的粒度，但可以抑制ＹＴ类硬质合金Ｃ固溶体晶粒长大，细化晶粒，使晶粒大小均匀。     

稀土变质及热处理对耐磨铸铁冲击疲劳性能的影响

采用金相显微镜、扫描电镜观察了经冲击疲劳试验后耐磨铸铁中碳化物的形貌、疲劳裂纹的萌生与扩展,测定了稀土含量及加热温度与裂纹的长度和裂纹扩展之间的关系曲线,在此基础上探讨了稀土变质及热处理对耐磨铸铁冲击疲劳性能的影响.结果表明: 稀土能推迟裂纹萌生的时间,降低裂纹扩展速率,提高其冲击疲劳抗力.当稀土与热处理共同作用时,效果更显著.其原因主要归于网状共晶碳化物形态与分布的改变.     

Investigation of the synthesis and internal structure of protective oxide layers on high-purity chromium with SIMS scanning techniques

The major problem affecting the application of chromium in high temperature processes is the ongoing spallation of the protective oxide layer formed during hot-gas oxidation. This results in a continuous material erosion. To gain a deeper insight in the spallation and oxidation process, a high-purity powder-metallurgically produced chromium sample was submitted to a two-stage hot gas oxidation process. The formed oxide layers were investigated by 3D SIMS and scanning SIMS. The formation of the protective oxide layer is carried by the diffusion of chromium from the bulk through the already existing oxide layer and the reaction of the diffused chromium with the oxygen from the gaseous phase. In parallel to the growing of the oxide layer, an accumulation of impurities at the interface oxide layer – bulk can be observed. The enrichment of trace elements at the interface level (for the investigated sample Cl and N) can be explained by the low solubility of these elements in chromium oxide and therefore their inability to diffuse through the already formed protective layer. Received: 24 June 1996 / Revised: 22 January 1997 / Accepted: 26 January 1997     

Surface characterization of functional iron–gallium alloys annealed under different conditions

Fe–Ga alloys are functional magnetostrictive materials, which are promising for application in actuators and sensors. Because surface properties of these alloys such as corrosion resistance are important in technological applications, it is required to characterize the chemical composition and state of the surface of these alloys, which depend on annealing conditions. In this study, X-ray absorption spectroscopy (XAS) and secondary ion mass spectrometry (SIMS) were used to characterize surface layers formed on the Fe–Ga alloys annealed under different atmospheric conditions. The XAS spectra of the annealed sample showed that the amount of gallium in the surface layers increased due to annealing, whereas the XAS spectra of the as-polished alloys revealed that the amounts of iron and gallium arise from the bulk composition. The XAS spectra of the alloys annealed in argon–hydrogen with residual oxygen showed that gallium is increased for its preferential oxidation. SIMS depth profile also showed the enrichment of gallium on the surface and the inhomogeneous distribution of iron on the surface layers.     

An effect of residual gas component on detected secondary ions during TOF‐SIMS depth profiling and a method to estimate contained component

With regard to Secondary Ion Mass Spectroscopy (SIMS) measurement of atmospheric gas elements, a problem occurs that the detected signal includes background components caused by residual gas along with contained components. Relating to this issue, an available method to quantify the contained components by separating the background ones had been established for Dynamic SIMS. Time‐of‐Flight SIMS with sputtering ion gun has also applied for depth profiling as well as Dynamic SIMS. However, few studies have attempted to investigate the secondary ion behavior of the atmospheric gas elements for depth profiling by Time‐of‐flight SIMS, especially for low concentration levels. In this study, experimental examinations of the secondary ions of the atmospheric gas elements, such as oxygen, hydrogen, and carbon in the silicon substrate, has been conducted in various analytical conditions of TOF‐SIMS depth profiling mode. Under the analytical conditions of our study, it has been proved that the background intensity of these elements was correlated to the sputtering rate. For the analysis of Floating Zone Silicon substrate, the oxygen intensity of the background component was proportional to the inverse number of the sputtering rate. Based on these facts, the total detected intensity of the atmospheric gas elements was able to be separated into the contained components and background ones by changing the sputtering rate during TOF‐SIMS measurement. An experimental result has shown that the contained oxygen concentration in the Czochralsk Silicon substrate estimated by the “TOF‐SIMS Raster Change Method” has successfully agreed with the result by the Dynamic SIMS.     

Structure of the metastable modification of iron(III) oxide

A new metastable modification of iron(III) oxide — protohematite — has_been studied. According to the X-ray diffractogram, protohematite (R3c) is identified as hematite (R3c) but characterized by other selection rules for IR and Raman active vibrations. Protohematite does not possess mechanical stability. The protohematite-hematite phase transition is initiated by heating above 900°C, or by pressure application, or by mechanochemical activation. The higher catalytic activity of protohematite compared to hematite may be explained by its structural features, namely, by lowered symmetry of the oxygen sublattice and by the effective tetrahedral environment of some iron cations. Translated fromZhurnal Strukturnoi Khimii, Vol. 41, No. 3, pp. 489-497, May—June, 2000.     

渗硼层磨损表面的XPS研究

用XPS研究了渗硼磨损表面的成分、元素价态及其随深度的变化。结果表明，磨损表面形成B2O3和铁的氧化物；随着深度的增加、B2O3和铁的氧化物含量减少。磨损表面主要表现为氧化磨损的特征。     

稀土对高铬铸铁碳化物形态及相变动力学的影响

研究了稀土元素对高铬铸铁中碳化物的影响，并对加稀土、不加稀土的高铬铸铁试样的连续冷却转变（ＣＣＴ）曲线进行了测定。结果表明，稀土元素能破碎高铬铸铁中的碳化物，使碳化物由网状、长条状向岛状、块状过渡。同时，稀土元素提高了高铬铸铁的固态相变温度并缩短了贝氏体的孕育期。     

Quantitative analysis of the Ge concentration in a SiGe quantum well: comparison of low-energy RBS and SIMS measurements

The germanium concentration and the position and thickness of the quantum well in molecular beam epitaxy (MBE)-grown SiGe were quantitatively analyzed via low-energy Rutherford backscattering (RBS) and secondary ion mass spectrometry (SIMS). In these samples, the concentrations of Si and Ge were assumed to be constant, except for the quantum well, where the germanium concentration was lower. The thickness of the analyzed quantum well was about 12 nm and it was situated at a depth of about 60 nm below the surface. A dip showed up in the RBS spectra due to the lower germanium concentration in the quantum well, and this was evaluated. Good depth resolution was required in order to obtain quantitative results, and this was obtained by choosing a primary energy of 500 keV and a tilt angle of 51° with respect to the surface normal. Quantitative information was deduced from the raw data by comparing it with SIMNRA simulated spectra. The SIMS measurements were performed with oxygen primary ions. Given the response function of the SIMS instrument (the SIMS depth profile of the germanium delta (δ) layer), and using the forward convolution (point-to-point convolution) model, it is possible to determine the germanium concentration and the thickness of the analyzed quantum well from the raw SIMS data. The aim of this work was to compare the results obtained via RBS and SIMS and to show their potential for use in the semiconductor and microelectronics industry. The detection of trace elements (here the doping element antimony) that could not be evaluated with RBS in low-energy mode is also demonstrated using SIMS instead.     

XRF and SIMS/SNMS analyses of Ba<Subscript>x</Subscript>Sr<Subscript>1−x</Subscript>TiO<Subscript>3</Subscript> dielectrics

The development of analytical tools and procedures for process control is a prerequisite for the integration of high permittivity and/or ferroelectric materials in CMOS devices. The thickness and composition of perovskite oxide films were determined by wavelength dispersive X-ray fluorescence analysis (XRF) with special emphasis on the ratio of the group-II elements to the Ti content, and a precision of 0.5% was achieved for a typical film thickness of 20-30 nm. Secondary ion mass spectrometry (SIMS) and sputtered neutrals mass spectrometry (SNMS) was used for depth profiling to determine film homogeneity and elemental interdiffusion at hetero-interfaces. Examples are given for Ba(x)Sr(1-x)TiO(3) and SrTiO(x) thin films which were grown in a prototype MOCVD production tool. No interdiffusion was observed for films grown at 600 degrees C on Pt electrodes in contrast to films grown directly on Si.     

Analysis of cast iron by x-ray fluorescence spectrometry

It is shown that a wide range of cast irons can be analysed on one calibration if the sample surfaces are prepared to a mirror finish with diamond paste. Polishing the samples with any abrasive material results in preferential removal of the softer constituents from the sample matrix. If coarser abrasives than diamond paste are used, the increased depth of the introduced sample inhomogeneity leads to unacceptable error limits for the determination of light elements.     

Dating of hydrated obsidian surfaces by SIMS-SS

A new approach to dating ancient obsidian artifacts based on the modeling of water diffusion profiles is evaluated using multiple archaeological test cases of known age. Hydrogen profiles from hydrated obsidian surfaces have been collected by secondary ion mass spectrometry (SIMS). The H₂O concentration versus depth profiles are modeled and diffusion ages have been produced. SIMS based dates for fourteen obsidian specimens of well-known age, ranging from 300-7000 years old, have been compared with radiocarbon ages. The convergence between the two dating methods is excellent and validates the new dating approach. This revised version was published online in July 2006 with corrections to the Cover Date.     

Essais en autoclave de flacons de verre a usage pharmaceutique

The behaviour in autoclave testing (French Pharmacopoeia) of bottles made from borosilicate glass (class I), surface-treated soda-lime glass (class II) and untreated sodalime glass (class III) is compared. Several (6–10) elements were determined by wet-chemical methods in the autoclave solutions. The results are compared with surface data obtained by secondary-ion mass spectrometry (SIMS) before and after the autoclaving. The SIMS profiles show that autoclaving of class I and II glasses scarcely modifies the surfaces of these glasses whereas class III glass is attacked to a depth of ca. 40 nm. The surface treatment with ammonium sulphate is shown to be efficient in reducing the diffusion of ions from the glass surface to the leaching solution. The validity of the hydrolytic resistance test given in the French Pharmacopoeia is confirmed.     

Surface/interface phenomena in nano‐multilayer coating under severing tribological conditions

An extensive study of surface/interface phenomena during wear of an adaptive TiAlCrSiYN/TiAlCrN nano‐multilayer coating deposited using physical vapor deposition was undertaken under increasingly severe tribological conditions associated with dry end milling of H13 hardened tool steel. The results of FEM modeling on the temperature/stress distribution at different cutting speeds outline actual cutting conditions on the both rake and flank frictional surfaces of the coated tool. Studies of the surface/interface phenomena were made by means of SEM/high‐resolution transmission electron microscopy/XPS analyses. Results demonstrate that intensifying tribological conditions facilitates improved wear performance of the adaptive coating layer. In extreme tribological conditions of ultra‐performance machining (cutting speed of 500 m/min), the self‐organization process establishes entirely through the formation of a nano‐scale layer of dynamically re‐generating tribo‐ceramic films. The formation of these surface nano‐films results in exceptionally efficient protection of the underlying coating layers. In response to the extreme external environment, the coating layer remained almost undamaged during a long run, demonstrating the capacity to efficiently replenish necessary tribo‐ceramic films. In this way, interconnection of various surface and undersurface processes is established in the hierarchically structured tribo‐films/coating layer. This integral performance is responsible for exceptional wear resistance under intensifying and extreme tribological conditions. Copyright © 2016 John Wiley & Sons, Ltd.     

Imaging surface spectroscopy for two- and three-dimensional characterization of materials

Secondary ion mass spectrometry (SIMS) exhibits a unique potential for the measurement of two-and three-dimensional distributions of trace elements in advanced materials, which is demonstrated on relevant technological problems. One example is the characterization of high purity iron. With this material segregation experiments have been performed and the initial and final distribution of the trace elements have been measured. Another example is the investigation of the corrosion behaviour of high purity chromium. Samples oxidized with ¹⁶O and ¹⁸O have been measured to explain the growing and adhesion of the oxide layer. All imaging techniques generate a vast quantitiy of data. In order to extract the important information the assistance of chemometric tools is essential. Detection of chemical phases by classification using neural networks or de-noising of scanning-SIMS images by wavelet-filtering demonstrates the increase of the performance of analytical imaging techniques.     

Treatment of products made of polymeric materials

The properties of polymeric materials are considered from the point of view of processability. The differences of the chip formation process during the treatment of products made of polymeric materials compared to the treatment of metal products are shown. The types of chips formed in the process of cutting plastics are studied, which, as during the treatment of metals, yield information on the phenomena occurring in the zone of cutting (deformations and temperatures) and the quality of the treated surfaces. The empirical dependences of the forces of cutting on the treated material, the material of the cutting edge of a tool, and its geometrical parameters are given. The problems of the wear of tools during the treatment of polymeric materials and the features typical for the treatment of polymeric materials by cutting are considered.     

SIMS/XPS characterization of surface layers formed in 3 mass% Si‐steel by annealing in oxygen at low partial pressure

Selective oxidation in silicon steel shows several interesting phenomena, such as the formation of an internal oxidation zone that depends on the oxidation conditions and the steel composition. In this work, SIMS and XPS were used for characterizing the formation processes of surface layers formed during selective oxidation of a typical silicon steel. The starting material is a secondary‐recrystallized 3 mass% Si‐steel sheet with a surface orientation of (011). Sample sheets were annealed at a temperature of 948–1023 K under an atmosphere with a low partial pressure of oxygen. The SIMS depth profiles show that the internal oxidation zone thickens and an iron‐rich layer that formed on the internal oxidation zone expands as the annealing temperature increases. Manganese and chromium levels increase outside the internal oxidation zone, whereas tin exists in the internal oxidation zone. The XPS results of the sample surface show that silicon and manganese levels increase on the sample surface to form oxides, and the chemical composition and state of these elements depend on the annealing temperature. In addition, tin increases on the surface of a relatively thick iron‐rich layer that formed on the internal oxidation layer. These experimental results are discussed on the basis of the thermodynamic characteristics of the elements. Copyright © 2003 John Wiley & Sons, Ltd.