Tetsu-to-Hagané
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ONLINE ISSN: 1883-2954
PRINT ISSN: 0021-1575

Tetsu-to-Hagané Vol. 77 (1991), No. 11

  • Recent and Future Trends of Analytical Techniques in Iron and Steel Industry in Japan

    pp. 1734-1740

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  • Separation and Determination of Trace Elements in Metals

    pp. 1741-1748

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  • 時空の流れの中に-鉄鋼分析の回顧と夢-/鉄鋼分析の流れ/分析化学研究が目指すもの-「分析化学の将来を問う」若手研究者懇談会より-

    pp. 1749-1755

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  • 日本鉄鋼協会共同研究会鉄鋼分析部会/日本鉄鋼協会鉄鋼標準試料委員会/日本鉄鋼協会ISO鉄鋼部会SC1(分析)分科会/日本鉄鋼連盟ISO/TC102(鉄鉱石)/SC2(分析)専門委員会/日本学術振興会製鋼第19委員会化学計測技術協議会/日本学術振興会マイクロビームアナリシス第141委員会

    pp. 1756-1801

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  • Certified Reference Materials for Analysis

    pp. 1802-1808

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  • Emission Spectrochemical Analysis of Iron and Steel

    pp. 1809-1816

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  • Rapid Determination of Small Amount of Carbon on Steel Making Process by Emission Spectrometric Analysis

    pp. 1817-1822

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    A rapid determination method of small amounts of carbon on steel making process by emission spectrometric analysis was studied. In this study, the influence of sample surface and measurment conditions on an analytical value were made clear. The followings results were obtained.
    (1)ZrO2 abrasive paper was better than Al2O3 one for the surface preparation of sample concerning analytical precision, while the grit size of polisher had no influence on analytical results.
    (2)A sample surface of small amount carbon had a thin and smooth layer by electrical spark remelting compared with an high carbon steel sample, therefore it results in necessity of less time for pre-spark-burn.
    (3)Regarding the carbon spectral line for analysis, C( I ) 165.8 nm was appropriate for the range below 0.01% content and C( I ) 193.1 nm was better for the range over 0.01%.
    (4)Interference for the carbon spectral by coexisting elements were not observed, however the presence of Al2O3 inclusion had influence on the carbon intensity. The interference might not be reduced without the classification technique of calibration curves.
  • Development of the Dual-cathode Glow Discharge Lamp and the Analytical Application to Steel Materials

    pp. 1823-1829

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    A modulated hollow cathode lamp with three electrodes can provide a spectrum pattern of sputtered atoms (sample) separated from the overall emission signals. The optimum conditions for operating the lamp are investigated. An argon pressure and a frequency of the pulsed discharges are examined to obtain the intense and reliable emission intensities. A negative voltage loaded between the intermediate electrode and the cathode sample is an important parameter in order to eliminate the undesired argon emission lines. Emission intensities of the sample strongly depend on a variation in this voltage, while those from argon atoms and ions hardly change. Selective detection of the sample emission lines can be achieved by modulating the voltage at frequencies of 100-300Hz.
  • Analysis of Trace Elements in High Alloy Steel by X-ray Fluorescence Spectrometry

    pp. 1830-1836

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    The X-ray fluorescence method was examined for determination of trace elements in high-alloy steels. Background intensities of XRF were varied with chemical composition of steel. This variance was caused by the absorption and enhancement effects of coexistent elements to background X-ray. In elements which have rather large atomic number, the background X-ray was found to be mainly composed of the compton scattered X-ray of the primary X-ray. In these elements the factor of interelement effect on background intensity was considered same as that in true fluorescent X-ray intensity from the sample. Thus the correction equation of interelement effect was shown below
    Wi= Xi (1 + ∑dijWj)-∑ (lij b·dij) Wj
    where Wi and Xi are corrected and uncorrected values of element i, b is the constant in calibration equation (Xi = aI+b), lij is the correction factor for spectral overlap, dij is the correction factor for interelement absorption effect and Wj is the content of coexistent element j. The validity of this equation was confirmed by experiments.
    The application of this correction equation improved accuracies in determination of Sn, Sb, Zr and Pb. The value of accuracy (σd=√(∑d2)/n-1) was decreased to 1/21/7 in comparison with the conventional method.
  • Development of Determination Method for Permeating Hydrogen Gas into High-strength Bolts

    pp. 1837-1842

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    It is well known that the delayed fracture of high-strength bolts is caused by trace amount of hydrogen absorbed in the operating environment of bolts. In order to establish the method for determination of this hydrogen, the hollow bolt collecting the permeating hydrogen gas has been developed. The detection system of hydrogen gas has been also developed by using SnO2 semiconductor gas sensor. The lower limit of determination for hydrogen is 1 vol ppm in this system. The developed hollow bolts were dipped in HCl solution, or were exposed in the environment of high temperature and high humidity. The hydrogen content was found to change with the condition of the environment. The hydrogen content was increased with the stress loaded on the bolts. The developed system can be used for the determination of hydrogen absorbed into the bolts in the practical environment.
  • Determination of Trace Amounts of Carbon, Nitrogen and Oxygen in Steel by Glow Discharge Mass Spectrometry

    pp. 1843-1850

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    A glow discharge mass spectrometry (GD/MS) was applied to a quantitative analysis of trace amounts of carbon, nitrogen and oxygen in high purity steel samples. Contaminants on sample surface were main interference for carbon determination. The contaminants can be eliminated succesively by glow discharge in advance of ion intensity measurement. The background can be improved by cooling the glow discharge cell. It was indispensable for nitrogen determination to evacuate the ion chamber for about 20 minutes after a sample was introduced to the system. A background for oxygen determination was improved effectively by purification of Ar gas with zirconium oxide catalyzer. Trace amounts of carbon, nitrogen and oxygen less than 20 ppm in steel were determined quantitatively.
  • Direct Analysis of Steels by Inductively Coupled Plasma Mass Spectrometry with a cw Q-switched Nd : YAG Laser

    pp. 1851-1858

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    A cw Q-switched Nd : YAG laser has been applied to a laser ablation system for the direct analysis of steels by inductively coupled plasma mass spectrometry (ICP-MS). The YAG laser used produced fine particles (particles size, about 0.02μm) at relatively high ablation rate (maximum 22μg s-1) ; and that was important feature to improve sensitivity and precision.
    Selective vaporization of volatile elements was occurred in the ablation process, but the magnitude was low. The use of iron as an internal standard was effective to improve accuracy and precision. Good accuracy was obtained for trace elements such as B, As, Nb, Sn and so on. On the other hand, precision ranged from 5 to 10(RSD, %) for the most of elements (isotope contents, 10200 μg g-1). Detection of Si, Al and P were problematic due to molecular interferences and some contaminations in ICP-MS measurement. But the limits of other 14 elements were excellent (0.01 μg g-1 for Nd5.6 μg g-1 for Ni at the effective integrating time of 0.18 s). It was found that the laser ablation analysis without standards has enough accuracy to apply semiquantitative analysis.
  • On-line Analysis and Automatic Analysis in Steel Making Processes

    pp. 1859-1867

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  • On-line Determination of Manganese in Molten Steel by Atomic Absorption Spectrometric Measurement of Evaporated Fine Dust at Converter

    pp. 1868-1873

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    For on-line determination of Mn in molten steel at converter, analysis of fine dust generated from the molten steel by atomic absorption spectrometry was examined. According to the characterization of the dust in dust collecting water, Mn was selectively evaporated from the molten steel to yield Mn enriched dust, but the amount of Mn in the fine dust (<10 μm) reflected on Mn content in molten steel. Atomic absorption analytical system with flame atomizer was developed for direct analysis of the fine dust and this was coupled with 0 G dust of the converter. Only fine particles extracted from the dust with cyclone were directly and continuously introduced into the atomizer of the system. The good linear correlation was obtained between the Mn contents of fine particles and the molten steel at the blowing end. But, the data obtained at the 8595% completion of blowing end showed poorer correlation between the Mn contents of the particles and molten steel. The reason was considered for that the relative evaporation rate of Mn to Fe varied at the 8595% completion of blowing end.
  • The Mechanism of Atomic Emission at a Hotspot and Its Application to the On-line Analysis of Molten Iron

    pp. 1874-1880

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    The mechanism of atomic emission at the hotspot was investigated, and the measurement of the atomic emission was applied to the on-line analysis of molten iron. The atom-radiating zone is found to be formed on the surface of molten iron by abserving the atomic emission and absorption of phenomena of Cu. The measured atomic emission is affected by the self-absorption effect, but fortunately it can be eliminated by the self-absorption factor. The emission of atoms is essentially governed by their vapor pressure and excitation efficiency. It is found that the elements such as Ni, Cr, Cu, and Pb, which have higher vapor pressure than that of iron and almost the same excitation efficiency as that of iron, radiate at the hotspot. On the contrary, the elements such as Mo and V, which have lower vapor pressure and almost the same excitation efficiency, are not found to radiate at the hotspot. The atomic emission intensity at the hotspot is linearly proportational to its concentration in molten iron. The direct measurement of the atomic emission at the hotspot is able to be applied to an on-line and real-time analysis of the former kind of elements in molten iron.
  • Development of Direct Analysis Method for Molten Steel with Ultra Fine Particle Generation-ICP Emission Spectrometry

    pp. 1881-1888

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    Direct determination of elements in molten steel without sampling has been developed with ultra fine particles (UFP) generation-inductively coupled plasma (ICP) atomic emission spectrometry. At first, (1) analytical conditions for UFP generation with spark discharge method and (2) the effect of plasma observation height and UFP contents on analytical precision were investigated with block steel samples. It was found that, (1) stability of carrier gas was the most important for analytical precision, and (2) suitable plasma obsevation height for the determination of C, P and S was 10 mm.
    Secondary, analytical conditions for UFP generation with Ar gas injection method were investigated with molten steel samples (Ar gas flow rate; 1525 Nl/min, nozzle immersed depth ; 10 mm).
    The analytical results of Mn, Cu, Ni, Cr, Nb, V, P, S in molten steel agreed with those obtained by the conventional method after sampling. It is important to keep at constant pressure in the probe for the generation of UFP.
    The time required for analysis of one cycle is approximately 90 s. The present method is more suitable for direct determination of elements in molten steel.
  • Ultratrace Chemical Analysis-State of the Art

    pp. 1889-1896

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  • A Modified Wet Chemical Oxidation-Nonaqueous Coulometric Titration for the Determination of Traces of Carbon in Metals

    pp. 1897-1901

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    When metal samples are decomposed with mixture solution of potassium dichromate and sulfuric acid, there are a lot of chances to have serious explosions because of the reaction between the hydrogen gas generated and the oxygen gas used as carrier gas. The assembly was developed for evacuating to remove the hydrogen with a vacuum pump through a palladium membrane heated at 400°C in order to avoid such a dangerous phenomenon. The wet chemical apparatus installed the newly developed assembly was used for the determination of traces of carbon in two kinds of high-purity iron, steels, aluminum and high-purity indium samples. Since the evolved hydrogen could be thoroughly removed from the train, the detonation was never encountered in the determination. The formed carbon dioxide was titrated coulometrically in nonaqueous medium, with a photometric end-point detection. Trace amounts of carbon [0.4252ppm(m/m)] in the metal samples could be determined in safety and with good precision and accuracy. The fluctuation of the blank value was little all through the experiment. The time taken to a single determination was 25 to 155 min.
  • Determination of Trace Amounts of Silicon and Phosphorous in Iron and Steel by Gel Phase Colorimetry

    pp. 1902-1907

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    The blue species of molybdosilicic acid and molybdophosphoric acid are strongly adsorbed on Sephadex gels, i. e., over 70% of blue species in a 100 ml colored solution is concentrated in 0.2 g of Sephadex G-25 within a half hour. Gel-phase colorimetry, based on the direct measurement of a gel-phase, which has adsorbed the blue species, has been applied to the microdetermination of silicon and phosphorous in iron and steel. The optimum condition for color development in the gel-phase has been examined on the basis of the procedure in JIS G 1212 for silicon and in JIS G 1214 for phosphorous. The colored gels were packed into a 2-mm cell. The absorbances at 810 and 500 nm for silicon and at 810 and 450 nm for phosphorous were measured using a reference of water-swollen gel. And the difference of absorbances was used for the determination of trace of silicon and phosphorous. Silicon and phosphorous at ppm-level in iron and steel could be determined by the present method.
  • Electrochemical and Chemical Dissolution Behavior of Zn-Fe Alloy Coatings and Its Application to the Analysis of Zn-Fe Alloy Layer

    pp. 1908-1915

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    Electrochemical and chemical dissolution behavior of Zn-Fe alloy coatings and steel sheets was investigated, and following two methods for selective dissolution of Zn-Fe alloy coatings from steel sheets were developed.
    (1) Alkali-dissolution method : In a strong alkaline solution (NaOH-triethanolamine (TEA)-H2O), Zn-Fe coatings are dissolved taking the form of ZnO22- and [Fe(OH)4·TEA]-, while steel sheets and Fe-Zn (Fe-P) coatings are insolble because passive films are formed on the surface.
    (2) Cathodic polarization electrolysis method : Under cathodic polarization (-1.2 Vvs. SCE) in a NH4NO3 electrolyte (NH4NO3-1, 10-phenanthroline (ο-phen)-MeOH-H2O (pH=10 adjusted by NH4OH)), Zn-Fe and Fe-Zn (Fe-P) coatings are dissolved taking the form of [Zn(NH3)4]2+ and [Fe-(ο-phen)3]2+. At this potential, dissolution of steel sheet is prevented by the ο-phen films adsorbed on the steel surface.
    Alkali-dissolution method is applicable to quantitative analysis of Zn-rich Zn-Fe layer (Fe<40%) coatings and upper/down layer of Fe-Zn (Fe-P)/Zn-Fe double layer coatings.
    Cathodic polarization electrolysis method is applicable to quantitative analysis of Fe-rich Zn-Fe layer (Fe<70%) coatings.
  • Determination of Trace Elemements in Iron and Steels by Graphite Furnace Atomic Absorption Spectrometry

    pp. 1916-1921

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    An analytical method has been established for the determination of trace amounts of bismuth, cadmium, cobalt, copper, indium, manganese, nickel, lead and thallium in iron and steels by graphite furnace AAS. The iron and steels were dissolved in nitric acid. After the solution (20μl) was pipetted into a L'vov platform furnace, it was ashed and then atomized by using argon as a purge gas, and atomic absorption of each analyte was measured. The effect of diverse elements was suppressed by the use of peak area measurement. Synthetic calibration solutions were prepared by adding each analyte standard solution to iron matrix solutions. For bismuth, cadmium, cobalt, copper, indium, manganese, nickel, lead and thallium, limit of detection (3σ of blank values) were 0.15 ppm, 0.004 ppm, 0.05 ppm, 0.07 ppm, 0.1 ppm, 0.04 ppm, 0.08 ppm, 0.1 ppm and 0.12 ppm, respectively, when one gram of the specimen was used.
  • Determination of Trace Amounts of Iron and Chromium in Alminium Nitride by Graphite-Furnace Atomic Absorption Spectrometry

    pp. 1922-1928

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    Determination of trace amounts of iron and chromium in aluminium nitride was investigated using acid pressure decomposition method with a teflon pressure vessel and graphite-furnace atomic absorption spectrometry. The sample (0.5g) was decomposed with 6 ml of sulfuric acid (1+1) and 2 ml of nitric acid (1+1) in the vessel at 160°C for 5 h. The sample solution was diluted to 50 ml with water, and determined directly with graphite-furnace atomic absorption spectrometry. Background of molecular absorption of aluminium oxide (AlO) interfered in determination of iron with wavelength 248.3 nm. But iron was determined by selecting wavelength of 372.0 nm. The limits (10 σ) of determination of in the present method were 0.8 and 0.1 ppm for Fe and Cr, respectively.
  • Determination of Th, U, Na and K in High-purity Tantalum

    pp. 1929-1935

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    Trace impurities in high-purity tantalum for ULSI were regulated severely, because they have effect on reliability of element performance. Radioactive elements and alkali metal elements which cause to trouble particularly, have been investigated by ICP-AES, fluorescence spectrometric method, and flameless-AAS after ion-exchange separation method.
    We examined conditions of ion-exchange separation of the object elements from matrix tantalum, influences of residual tantalum and acids for sample dissolution on measurement and the countermeasure for them, analytical conditions of ICP-AES, and correction method for fluorescence intensity of U, chiefly. The detection limits of the present methods were 2 ppb for Th, 0.5 ppb for U, and 0.01 ppb for Na and K, respectively.
  • Application of Electrothermal Vaporization for Inductively Coupled Plasma Atomic Emission Spectrometry and Inductively Coupled Plasma Mass Spectrometry

    pp. 1936-1943

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    The use of electrothermal vaporization(ETV) as a means of sample introduction provided a lot of advantages over conventional pneumatic nebulization for inductively coupled plasma atomic emission spectrometry (ICP-AES) and mass spectrometry (ICP-MS). Compared with the nebulization method, the ETV system needs smaller sample volume and higher sample transport efficiency can be attained.
    Application of the ETV system for ICP-AES made it possible to improve the detection limits of Al, Cr, Cu with sufficient precisions. Vaporization behavior of Cu in the presence of a large excess of Fe considerably depended on the heating program and the amount of Fe. Copper in pure iron reference materials were successfully determined by controlling the heating program and matrix matching of calibration standards.
    For ICP-MS, spectral interferences arising from water and/or acids in sample solution were removed with the ETV system. Rapid scan monitoring capability of ICP-MS made it possible to do multielemental analysis. Sufficient sensitivity equivalent to the nebulization method was attained for the simultaneous measurement of twenty five elements, but precisions were poor because the signals obtained with the ETV were transient and optimum heating programs were different for each element.
  • Determination of Trace Amount of Bismuth in Iron and Steel by Inductively Coupled Plasma Mass Spectrometry with Sample Introduction by Electrothermal Vaporization

    pp. 1944-1950

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    The performance of an inductively coupled plasma-mass spectrometer with an electrothermal vaporizer(ETV-ICP·MS)has been investigated as a function of several parameters associated with ETV operation.Signal profiles of bismuth in some acid solutions were measured using a pyro-coated graphite tube as the ETV device. Signal appearance time of bismuth in nitric acid was later than that in hydrochloric acid and the signal intensity of bismuth in nitric acid was lower than that in hydrochloric acid. The use of nickel as a modifier for bismuth in nitric acid improved the intensity to those of bismuth in hydrochloric acid and in aqua regia. The detection limit at the sub-picogram level which was 50-fold better than that obtained by nebulization with ICP·MS was obtained.
    This method was applied to the determination of bismuth in iron. The detection limit of 0.01 ppm which was 20-fold better than that obtained by nebulization with ICP·MS was obtained. However the signal intensity of bismuth in iron solution was depressed to the half of those obtained without iron and there was no effect of nickel as a modifier on the improvement of the sensitivity. Bismuth in some certified reference materials of iron which were dissolved in aqua regia was determined, and the results agreed with reference values.
  • Analysis of High-purity Iron with Inductively Coupled Plasma Source Mass Spectrometry

    pp. 1951-1958

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    The basic characteristics of inductively coupled plasma source mass spectrometry (ICP-MS) were investigated and operating parameters were optimized.
    For the determination of trace elements in high-purity iron, a rapid and precise method was developed. After dissolution of a small amount of sample in a PFA test tube, 4-methyl-2-pentanone extraction technique was applied for the separation of the analytes from Fe matrix. Consumption of reagent was supressed and all procedure from dissolution to extraction was carried out in the same test tube to give a low blank value.
    The use of the relationship between intensity and ionization potential enables a semiquantitative analysis without a calibration curve.
  • Determination of Trace Elements in High-purity Quartz by Inductively Coupled Plasma Mass Spectrometry

    pp. 1959-1964

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    Determination of Li, B, Mg, Cr, Mn, Ni, Co, Cu and Zr in high-purity quartz by inductively coupled plasma mass spectrometry (ICP-MS) was studied. Effect of mannitol, dulcitol or solbitol on suppression of boron volatillization from hydrofluoric acid solutions was examined. Boron volatillization was found to be completely suppressed by addition of 500-fold molar excess of dulcitol to boron or 1 000-fold molar excess of mannitol. Even 1 000-fold molar excess of solbitol was not sufficient for complete suppression. These organic compounds introduced to ICP-MS caused mass interference due to 40Ar12C with 52Cr and reduction of intensity by carbon deposition on the sampling cone orifice. Therefore the following analytical conditions were employed.
    (1) 2 mg of dulcitol was added.
    (2) Measurements were performed by deviding into 2 groups ; one group with dulcitol for Li, B and Mg determination, and the another without dulcitol for Cr, Mn, Ni, Co, Cu and Zr determination.
    (3) Be and V were added as the internal standards.
    The limits of detection (3σ) with present method were 0.0005 0.01 ppm. The proposed method was applied to the detemination of Li, B, Mg, Cr, Mn, Ni, Co, Cu and Zr in the practical quartz with satisfactory results.
  • Surface Analysis for Iron and Steel

    pp. 1965-1971

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  • Determination of Sputtering Yields for Quantitative In-depth Analysis of Surface Layer of Steels

    pp. 1972-1979

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    Experiments were conducted to determine sputtering yields for various materials under a practical sputtering condition of Scanning Auger Microscopy (SAM) and Secondary Ion Mass Spectrometry (SIMS).
    (1)Sputtering yields for Al, Ti, Cr, Mn, Fe, Ni, Cu, Zn, W and Ta are obtained for Ar+ ions with bulk specimens. The experimental value of each element is larger than that calculated with semi-empirical formula for normal incidence of Ar+ ions.
    (2)Sputtering yields for Al, Cr, Mn, Fe and Ni are obtained for irradiation with O2+ ions and N2+ ions with bulk specimens.
    (3)Sputtering yields for Al, Cr, Mn, Fe, Ni and Cu are obtained for irradiation with Ar+ ions, O2+ ions and N2+ ions with film specimens evaporated on stainless steel. These values nearly agree to those obtained with polycrystalline bulk specimens for each element.
    (4)Spuuttering yield of Fe-Ni alloy for Ar+ ions increases with Ni concentration up to 25.6 mass%.
    (5)Sputtering yield for Cr2O3 is obtained for Ar+ ions and O2+ ions with the specimen prepared by thermal oxidation of Cr-evaporated glass with known coating weight.
    Some of the results are applied to conversion of sputtering time to the sputtered amount in the depth-profiles. These results agree with those obtained with other techniques.
  • Determination of Trace Impurities in Steel Samples by Nonresonant Laser Post-ionization

    pp. 1980-1984

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    Sputtered Neutral Mass Spectrometry (SNMS) employing nonresonant laser post-ionization has been studied for quantitative analysis of steel standard sample. SNMS technique can overcome weakpoint of the conventional SIMS, that is, low quantitativeness, by means of detecting sputtered neutrals.
    Because the numbers of sputtered neutrals are proportional to the concentration of the surface of the sample. In this report, impurity elements in the steel sample were evaluated quantitatively down to ppm level. And metallic contaminant elements on the silicon surface were confirmed to be quantitatively determined down to 1011 atoms/cm2. And post-ionization efficiency was also estimated, resulting nearly 16%.
  • Quantitative In-depth Analysis of Iron Oxide Films by Glow Discharge Spectrometry

    pp. 1985-1991

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    A method for the quantitative analysis for oxide films on steels with glow discharge emission spectrometry (GDS) was examined. The sputtering rate and the light intensities were measured with standard samples with oxide films of known composition or known composition and thickness, and apparent emission yields (Rn) for elements were determined. By converting the light intensities to the sputtered amount with the Rn's for an interval in a sputtering profile in an unknown sample, the composition can be obtained from the amount ratio of sputtered elements. The sputtering depth can be calculated from the sputtered amount divided by the density of each element for the sputtering time. The apparent density of oxygen for the depth conversion was estimated to be 1.82 from measurements of standard samples with oxide films of known composition and thickness. The results analyzed by the present method were in consistency with those obtained with another method. The present analysis involves little matrix effect, and facilitates the quantification of the sputtering depth which is difficult to obtain in AES, XPS and SIMS.
  • Surface Segregation of Trace Elements in Fe-42Ni Alloy

    pp. 1992-1999

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    The surface compositions of Fe-42 wt%Ni alloy at high temperatures have been observed in ultra high vacuum by using AES ( Auger Electron Spectroscopy).
    Phosphorus, manganese, chromium, boron, nitrogen and sulfur segregate to the surface at various temperatures. Phosphorus, is dominant at temperatures from 550°C to 600°C. Boron nitride is substituted the element from 600°C to 850°C. Moreover, sulfur substitute boron nitride above 850°C. B KLL AES spectrum and Bls EELS (Electron Energy Loss Spectroscopy) spectrum have revealed that boron and nitrogen precipitate as boron nitride after the annealing. Moreover, boron segregates as a boron at the first stage. At the second stage, boron nitride is formed as a result of the surface reaction between the segregated boron and nitrogen which segregates after the boron segregation. Auger images have revealed that the coverage of the elements is almost uniform at the surface.
    The calculation of the intensity of the AES peak revealed that the thickness of the layer for the surface segregated elements is about one or three monolayers.
  • Chemical State Analysis of Hydrated Chromium Oxide Film on Tin Free Steel Using Fourier Transform Infra-red Spectrometry

    pp. 2000-2006

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    The chemical state of the water in the hydrated chromium oxide film on Tin Free Steel (TFS) was studied under atmospheric pressure using Fourier Transform Infra-red Spectrometer (FTIR).
    Following results were obtained;
    (1)Emission spectra can be measured at as low as 50°C where a dehydration commences. The characteristic bands in emission spectra agree well with those in reflection-absorption spectra.
    (2)A broad and weak absorption is observed at 950 cm-1. It is attributed to the water in the film, because it disappears when TFS is heated at 200°C. On the contrary, the absorption caused by bending vibration in HOH at 1 590 cm-1 remains even after heating at 300°C. It is therefore presumed that there are two chemical states of the water in the film, and the absorption at 950 cm-1 to the water which is free from the chemical structure of the film.
    (3)A clear correlation is found between the lacquer adhesivity of TFS and the ratio of the absorption intensitys at 1 590 cm-1 and 950 cm-1. This relation can be utilized for evaluation of the lacquer adhesivity.
  • Analysis of Surface Cleanliness on Silicon Wafers Using Total Reflection XRF Excited by Synchrotron Radiation

    pp. 2007-2013

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    The monitoring of surface cleanliness of silicon waters is very important. Total Reflection X-ray Fluorescence is expected to be highly sensitive for the ultra trace contaminants on the top surface. Synchorotron radiation is an appropriate X-ray source. This method was applied to relatively heavy elements such as Cr, Fe, Ni, Zn, which were suffused on silicon wafer surfaces by spin coating technique. This method has been found to have high quantitativeness and its minimum detection limits for those elements was found to be the order of 1011 atoms/cm2. And this method was also found to be applicable to the real samples in the course of cleaning.
  • Quantitative Analysis of Gamma Prime Phase in Nickel Base Superalloys

    pp. 2014-2020

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    A rapid and precise method for quantitative analysis of γ' phase in nickel base superalloys has been developed by improving of extraction method of the precipitates.
    The results obtained are summarized as follows:
    (1)The precipitates including γ' phase are quantitatively and precisely extracted by potentiostatic electrolysis in 1% ammonium sulfate-1% tartaric acid-water or 1% ammonium sulfate-1% citric acid-water electrolyte.
    (2)Only the γ' phase adhered to the sample surface after potentiostatic electrolysis can be dissolved by dipping samples into (1+4)HCl solution at 60°C for 10 minutes.
    (3)The amount and chemical composition of γ' phase and other precipitates can be determined respectively by analyzing solution and residues obtained from the above mentioned (2).
    (4)The rapidity and precision of this method is excellent compared with the conventional methods which use filtration or centrifugation for collection of residues.
    (5)This method gave instructive informations about precipitation behavior of γ' phase.
  • Investigation on Determination of Titanium Precipitates in Steel by Secondary Ion Mass Spectroscopy

    pp. 2021-2026

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    Analytical conditions were examined for the determination of titanium precipitates in steel as titanium carbide and titanium nitride by secondary ion mass spectroscopy. Characteristic polyatomic ions related to the compounds were sought by comparison of the intensity of polyatomic ions for various samples. The intensity of polyatomic ions were calculated by fitting the SIMS spectra to the relative isotopic abundance of each ion using non linear least square method. The polyatomic ions TiC+ and Ti2C+ were selected for the characteristic ions of titanium carbide and TiN+ and Ti2N+ for titanium nitride because of higher intensity and good reproducibility. The compressed disks of mixed powder of iron, titanium carbide and titanium nitride, with a few μm diameter, enble the determination of titanium carbide and nitride to less than 1 wt%.
  • The Simple Determination Method of Precipitates in Steels by X-ray Diffraction Technique with Y2O3 as Internal Standard Materials

    pp. 2027-2032

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    The simply quantitative state analysis method of precipitates in steels has been established by X-ray diffraction technique with adding constant amount of Y2O3 as internal standard material.
    The procedure is as follows :
    (1)The residues extracted from steels by potentiostatic electrolysis are dispersed in methanol with 100 ml beaker.
    (2)5.0 ml of Y2O3 dispersing solution (50 mg/250 ml methanol) is added in above mentioned solution and after that this solution is dispersed by ultrasonic vibration.
    (3)This solution is filtrated and the residues are collected on filter.
    (4)The X-ray diffraction pattern of residues is measured and its peak intensity ratios of precipitates to Y2O3 are calculated. The amount of precipitates are determined from these peak intensity ratios by calibration curves, which are preliminaly made from relation between peak intensity ratio and the amount of precipitates.
    This method can simply estimate state of precipitates quantitatively compared with conventional extracted residues decomposition method.
  • Micro Analysis in Materials Development

    pp. 2033-2037

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  • Materials Characterization by Synchrotron Radiations

    pp. 2038-2043

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  • Development and Application of Synchrotron Radiation Dynamic Topography for Observation of Secondary Recrystallization Process

    pp. 2044-2051

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    White X-ray topography by synchrotron radiation provides a powerful means for dynamic imaging and mapping of structural inhomogeneities in bulk materials. "Synchrotron radiation dynamic micro topography method" has been developed by a combination of a high performance furnace and a direct type X-ray TV camera to white synchrotron radiation for the best use of the highly bright and parallel beam of synchrotron radiation source at the Photon Factory in the National Laboratory for High Energy Physics. The method has been applied to dynamic observation of rapidly progressing phenomena at high-temperatures such as the migration of secondary recrystallization fronts in grain-oriented silicon steel.
    The migration of secondary recrystallization fronts is found not uniform in both time and location. Migrating fronts show a zigzag shape and move from protruding points preferentially. The migrating behavior shows the following three types : burst motion at a rate of 0.05 to 0.2 mm/s, gradual migration with 0.01 to 0.02 mm/s, and standstill state. The size of regions consumed by a front motion is constant and is as large as 0.2 to 1.0 mm in diameter. Dislocations are observed in the growing grains and subboundaries are formed by connection of migration fronts to surround retained areas.
  • Microbeam X-ray Diffraction from the Cross-section of Metallic Materials with Inhomogeneous Structure

    pp. 2052-2059

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    The accuracy in the determination of lattice parameters of diffraction patterns by means of microbeam X-ray diffraction method has been studied with a curved position sensitive proportional counter for the cross-sectional measurements of partially crystallized Fe-B-Si amorphous ribbons and sintered Ni-Cu-Mo alloyed steels after case-hardening.
    It was found that the accuracy of lattice parameters was 0.2% when the parallel X-ray beam with 50 μm width was used. The sizes of X-ray spots at the specimen surface were two or three times as large as those of the collimeters.
    The crystalline phases formed in a thick amorphous ribbon by rapid quenching of Fe78.5B13Si8.5 alloy liquid were α-Fe(Si) and Fe2B. The critical thickness of glass formation in the present quenching condition was about 40 μm.
    Standard diviation of the dimensional change in the sintered compacts of Ni-Cu-Mo alloyed steel powders became smaller when Ni content increased, because microstrain in the martensitic structure became smaller with Ni content after case-hardening.
  • AP-FIM Analysis of Partitioning of Alloying Elements between Spinodally-decomposed Phases in Fe-Cr-Co-Si Alloys

    pp. 2060-2067

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    Partition of alloying elements between spinodally-decomposed phases in Fe-Cr-Co-Si alloys was examined by Atom-Probe Field-Ion Microscope (AP-FIM). The results showed that the ferromagnetic particle (α1) is rich in Fe and Co, and the weak-ferromagnetic matrix (α2) rich in Cr and Si. The enrichment of Si in the α2 phase was explained through thermodynamical considerations. Si is more strongly bonded to Cr than to Fe. The improvement of hard magnetic properties by Si additions was found and discussed in terms of the changes in saturation magnetization of the α1 and α2 phases. The increase in coercive force may be mainly attributed to the reduction of saturation magnetization of the α2 phase by the addition of Si.

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