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By Arne Westgren

ONLY in exceptional cases can the ordinary methods of chemistry be used for determining the constitution of compound metallic substances. Recourse has therefore been taken to special methods, the main expedients of which are, as we know, thermal analysis and metal microscopy. To these may be added-though more accessory-the determination of electric conductivity, specific volume, hardness or other properties. The information obtained by these methods has been compiled in equilibrium diagrams. Naturally, the technically most important alloys, such as steel, bronze and some others, have been subjected to very close study, and many investigators have devoted themselves to the solving of their problems of constitution. The equilibrium diagrams of these systems are therefore known today with a comparatively high degree of accuracy, even though it must be admitted that many details regarding their transformation reactions still remain to be completely explained. The equilibrium diagrams of the other alloys as a rule have not been determined so accurately. Most of them are based only on approximate determinations of the homogeneity ranges of the various phases. Thus extensive, detailed studies remain before these diagrams may be considered as established. Unfortunately, it must also be admitted that many of the alloy diagrams given in the present handbooks are as a whole very dubious. As a matter of fact, many of them may really only be viewed as the results of rather superficial, orientating investigations. In fact, there also seems to be a general opinion prevailing in our day that much work still remains to be done before the equilibrium conditions of the alloys may be considered as fully explained. At present, in almost all institutes for research on metals, as well as in many university laboratories, investigations to this effect are being carried out. As a rule, the classical methods of metallography, the thermal analysis and metal microscopy are applied.

Jan 1, 1931

By E. Spicer

X-Ray diffraction (XRD) provides useful information about the composition of an ore sample in terms of quantification of crystalline phases and amorphous content. The use of new, fast detection systems in XRD creates the opportunity to use this technique in modern process control. In the analysis of heavy mineral sands, XRD can identify the main mineral phases, such as ilmenite FeTiO3, rutile TiO2, Zircon ZrSiO4and quartz SiO2, and any other minor components present, such as anatase TiO2, magnetite Fe3O4, haematite Fe2O3or monazite (Ce, REE)PO4. Quantitative analysis is possible by various classical methods such as straight line or polynomial calibration with standards, but modern quantification analysis techniques such as Rietveld analysis (Bish and Howard, 1988) are attractive alternatives, as they do not require any standards or monitors. These methods offer impressive accuracy and speed of analysis. The Rietveld method compares calculated versus experimentally derived X-ray powder diffraction patterns for the sum of all crystalline phases. Another analysis technique offering great benefit to mining industries is cluster analysis. Enormous amounts of XRD measurement data are generated during the process control and material evaluation. New ways of handling such vast amounts of data are required to produce meaningful information for the end users. Cluster analysis greatly simplifies the analysis of a large amount of data from different processes or different raw materials, and automatically sorts closely related scans of an experiment into clusters and marks the most representative scan of each cluster as well as outlying patterns. The use of cluster analysis to evaluate the XRD data allows fast and reliable tracking of the process. It is the most economical procedure to have automatic data evaluation without involving any dedicated personnel in the process. Details of the techniques used, sample optimization methodologies, results, data precision and limitations will be discussed. The approach has potential as a relatively inexpensive, reliable tool, useful in the characterization of heavy minerals sand materials.

Jan 1, 2007

The problems of using comparatively simple x-ray diffraction equipment for quantitative analysis are examined. Internal standard and direct calibration procedures based upon the measurement of integrated diffraction energy (diffractometer peak area) have been developed for the determination of quartz in Broken Hill dusts. By these methods an accuracy of ± 10 per cent of the true value can be obtained and this can be improved to ±2 1/2 per cent by statistical methods if necessary.Rapid analysis for the components quartz, muscovite, rhodonite, galena, fluorite, sphalerite, calcite, and garnet has been developed by adaptation of direct calibration procedures and use of maximum diffraction energies (diffractometer peak height). Until more is know!) about the pathological effects of multi-component dusts of the Broken Hill type it seems undesirable to fix theIr allowable concentrations in terms of the quartz content.

Jan 1, 1968

By M. S. Seehra, V. Suresh Babu, R. S. Pandurangi

Different mixtures of the three polymorphs of silica viz. quartz, cristobalite and tridymite are analyzed by x-ray diffraction (XRD) and their IR spectra are investigated by photoacoustic spectroscopy. It is observed that XRD provides a higher resolution to distinguish between the three polymorphs in a sample than IR spectroscopy. In the latter, a sharp band near 617 cm-1 is characteristic of both cristobalite and tridymite. A mine dust sample is quantitatively analyzed by XRD and it is shown to contain illite, quartz, kaolinite and calcite.

Jan 1, 1991

By Henrique Kahn, Daniel Uliana, Juliana Antoniassi, Viviane Shimizu

"Mineral exploration and geometallurgy require a large number of samples for physical, chemical and mineralogical assays. The combination of all these data and their spatial distribution define the ore variability. This is important in exploration programs and crucial in feasibility studies as well as at the production operation level. Ore mineralogical composition and its associations, characterizing the geological formation and mineralization, are the main keys to define the ore domains and its variability, which can be quickly assessed by cluster analysis and by modern automated mineralogy tools. One hundred and ten copper ore samples from Sossego mine, in Brazil were compared and classified by X-ray diffraction cluster analysis based on the position and the intensity of the diffracted peaks. Initially four ore types were categorized based on content of major minerals: quartz, feldspar, amphibole, iron oxides, mica and chlorite. Results showed a strong correlation between the grouping and the samples location in Sequeirinho and Sossego orebodies, with a straight link to types/intensities of hydrothermal alteration prevailing in each body, which reflects the mineralogical composition and thus the X-ray patterns. Samples from four recognized ore types were submitted to detailed automated mineralogical studies by electron beam image analysis and differ strongly from each other regarding their chemical and mineralogical compositions and relevant parameters for mineral processing. Chalcopyrite is essentially the only valuable mineral, occurring both as submillimetric grains included in other minerals and as larger crystals. Except for pyrite, other sulfide minerals occur as traces. Chalcopyrite liberation curves indicate that samples from Sossego have higher liberation degree than those from Sequeirinho. The proposed method proved to be very efficient and accurate to classify a large number of samples within a short time frame, allowing the distinction of the ore types regarding their mineralogical composition as well as the mineral processing parameters."

Jan 1, 2014

By Sabri Ergun

NEW theoretical data are presented for the intensity of X-rays diffracted from randomly oriented aromatic and alicyclic molecules and diamondlike structures such as are found in coals, cokes, and carbonaceous materials. Data have been computed using the Debye interference function. Computations for the smaller molecules have been made with the Univac 1204 computer: those for large structures, with either the IBM 704 or Bendix G-20 computer. A brief theoretical introduction of the Dobye interference function is given, and an outline is made of the treatment of experimental data so that the experimental interference function can be obtained.

Jan 1, 1965

By G. Belardi, G. Marruzzo, P. Plescia

This paper presents the results of grinding tests performed on magnetite from Kiruna (Sweden) and on chromite from Skoumtza (Macedonia. Greece). Stresses were measured by XRD, which determined the variations in the characteristic structural spacings of the minerals both before and after, grinding in a HSM/250 Herzog laboratory ring mill. Anal Isis of the magnetite and c hromite crystallinstallin was performed hi measuring the broadening of the strongest diffraction peak (311). .Also, structural analysis on chromite was carried out using the Mikheev model. Ultrafine-grinding tests on the magnetite and chomite demonstrated that this type of treatment can induce profound variations m the surface-stress state. These included plastic variations of the cell followed by "chemical" stress with oxidation front the stricture to form hydroxide or carbonate, films. This can have a great influence on the mineral reactivity to flotation reagents

Jan 1, 1996

By G. Roy

Interest in metal-hydrogen systems can be manifold. Small amounts of hydrogen adsorbed by elemental metals and alloys usually result in strong changes in the physical and mechanical properties of engineering materials. Overwhelmingly, these changes, viz. hydrogen embrittlement, are considered deleterious with respect to structural performance of engineering materials. However, the changes, often studied by metallurgists and metal physicists, can present new possibilities and applications. A prominent example is the recent interest in safe, solid-state hydrogen storage in metallic lattices. In a new laboratory in MTL, Ottawa, a study has been initiated to investigate the effect of "micro- and macro- alloying" of Al and Mg powders with hydrogen (in high-energy mechanical alloying mills) on plastic deformation in metal and metal hydride structures. It is anticipated that high-rate impacting and subsequent grain refinement in the mill will have an effect on hydrogen storage capacity in lightweight magnesium and aluminum alloys. First examination of the state-of-stress by X-ray diffraction in high-rate milled, nanostructured pure aluminum, aluminum milled with a solid surfactant, and aluminum or magnesium alloy milled with hydride and/or gas hydrogen will be presented.

Jan 1, 2005

X-ray analysis of polycrystalline powder samples has grown beyond its roots in the world of laboratory research and is now regarded as one of the most powerful industrial process-control tools in the field of building materials. This is the key to characterise the element and crystalline phase composition of the material. This is due largely to the development of industrial X-ray analytical systems such as PANalyticalÆs twin solution, which has transformed the advanced analytical techniques born in the laboratory into a robust, workmanlike and easy-to-use tool for todayÆs heavy industries. The increasing use of alternative fuels makes the Bogue method less reliable. Therefore, the real phase quantification by the Rietveld method is the only choice. Additional fine-tuning of the Rietveld method by using alternative methods guarantees the most accurate quantitative results. Moreover, the recent development of ultra high-speed X-ray detectors allows for æon the flyÆ quantitative X-ray diffraction analysis and a truly interactive process and quality control.

Jan 1, 2008

By Robert Anderson

The diffraction of x-rays by cold-worked and heavily polished surfaces of metals gives, no evidence of an amorphous state and typically perfect crystallographic diffraction' patterns are obtained. Severely cold-worked metals, reduced as much as 98 per cent. in area, give true crystallographic diffraction patterns, and polished surfaces of large single crystals of metal give typical crystallographic patterns. The conclusion is drawn, on basis of x-ray evidence, that metals are fragmented on cold work and polishing and not amorphized. THE purpose of this paper is to report evidence, regarding, metal: structures, that is contradictory to the amorphous-metal, hypothesis of Beilby, and particularly evidence that is opposed to the proposition that a vitreous amorphous layer is produced by polishing a piece of metal. According to the theory of Beilby, which has been developed, by Rosenhain and others, polishing a piece of metal greatly affects the condition of the metal at or near the surface polished, making that surface entirely different in character from the metal beneath. A vitreous amorphous surface film is said to be formed. The polishing process, on the basis of Beilby's explanation, is well known-and does not' require discussion here, but it is advisable to seek the precise meaning of,., the term "amorphous." According to Beilby, "amorphous means. Non-crystalline in the most intimate sense of the word'; the molecules are not marshalled in crystalline order and orientation." According to Rosenhain, the amorphous condition is that assumed by a metal when, the .crystalline arrangement is completely broken up so that the atoms exist in a state of disorderly arrangement similar to that ;which exists in the liquid state. Thus, from the point of view of the phase rule, the "amorphous phase" is regarded as being identical with the liquid phase. Amorphous metal is often likened to an undercooled liquid. A crystalline substance is one in which the atoms are arranged in space according to some definite repeating geometrical pattern. The existence of amorphous metal has not been definitely proved.

Jan 1, 1925

The use of solid state detector and radioisotope x-ray source for x-ray fluorescence analysis is illustrated by analysis for iron, copper, zinc, tin, and lead in about 700 samples taken from Australian mineral process streams. Limits of detection based on counting statistics (3 standard deviations) range from 0·001 to 0·004 per cent by weight element. The analysis accuracy was usualIy between 2 to 10 per cent (rms) of the mean element concentration and was determined by comparison with assays supplied by mineral companies. In most cases the main cause of error appears to be due to this assay and not the x-ray fluorescence technique.Some potential fields of application of solid state detector and radioisotope x-ray source for analyses in the mineral industry are indicated.

Jan 1, 1974

By Doon Gibbs

In this talk, we review highlights of x-ray magnetic scattering studies performed during the last decade, concentrating at the beginning on experiments on the rare earth metal holmium.(1-4) Besides intrinsic interest in the x-ray scattering cross-section and its description, studies of this type are motivated by the possibility that new structural and magnetic properties of rare earth metals might be revealed, and that new techniques may thereby be developed. As a result, interest in x-ray magnetic scattering experiments. has grown rapidly during the last 10 years particularly, with the regular application of synchrotron radiation techniques- Magnetic scattering experiments have by now been performed at most of the x-ray synchrotrons around the world. In addition, insertion .device beamlines dedicated to x-ray magnetic scattering experiments are planned at each of the next-generation storage rings presently under construction in the United States (APS), Europe (ESRF), and Japan (SPRING-8). Generally, the results of x-ray magnetic scattering experiments may be analyzed within two regimes of the incident x-ray energy, namely, in the limit of high x-ray energies, when the incident x-ray energy lies above the excitation energy of any absorption edge, and at resonance, when the incident energy lies near an absorption edge. In the high energy limit, the amplitude for x-ray magnetic scattering has the simple form [L(Q)?A + S(Q)?B](5-7) Here, L(Q) and S(Q) refer to the Fourier 'transforms of the atomic orbital and spin magnetization densities, respectively, and the vectors A and B depend on the incident and scattered wavevectors and on the: incident and scattered polarization vectors. 7) Because the vectors A and B are not identical, the polarization dependence of the orbital contribution to the magnetic cross-section differs from that of the spin contribution. This leads to the possibility that the orbital and spin magnetization densities maybe distinguished, in x-ray scattering experiments. The same distinction is not directly possible by neutron diffraction techniques (in dipole approximation, where the polarization dependence of the orbital contribution is identical to that of the spin contribution), and is important to a fundamental understanding of the electronic structure of magnetic materials. A particular

Jan 1, 1992

By G. Sachs

According to Tammann,' the explanation of the effect of mechanical deformation in producing changes in the properties of metals is one of the most important problems of physical metallurgy, taking rank with the study of the constitution of alloy systems; and this problem has long attracted the attention of practitioner and scientist alike. Its solution was not advanced materially until Tammann2 set up his translation hypothesis with its crystallographic basis, while other hypotheses, such as the amorphous metal hypothesis of Beilby3 and Rosenhain,4 have been shown by more intensive studies to be less and less satisfactory. The principles of the Tammann translation hypothesis have proved to be useful even up to today and in spite of all of the recent accumulation of experimental data, while the differences of opinion which have arisen relate to the extent to which the hypothesis accounts for the observed changes Ïn properties and to what extent further assumptions are necessary. Stimulated by the proposals of Tammann, there soon developed a lively experimental activity which aimed at the elucidation of the structural or crystallographic changes produced by the mechanical deformation of metals. Parallel movements of crystal "blocks" along definite crystal slip planes had already been observed by Ewing and Rosenhain5 in 1900, in metals which had been moderately deformed but without shedding light on the crystallographic nature of the processes accompanying more severe deformation. The solution of this important problem was not advanced until a much later date, or until the methods of X-ray crystal analysis had become available. Shortly after the discovery of the diffraction of X-ray by crystals, symmetrical diffraction effects were

Jan 1, 1931

By Franz Wever

The importance of the Widmanstätten structure to structure theory in metallography has been recognized by many writers.l It is a structure produced by the precipitation of a, new phase from a solid solution upon cooling as a result of changing solid solubility, and displays a characteristic appearance indicating a crystallographic relationship between the new phase and the original solid solution (Fig. 1). First discovered in 1808 by Alois de Widmanstätten2, the structure has been traced by analogy through many alloy systems. Particularly is this true of the steels. Sorby's classic work3 on the microstructure of iron and steel was in essence an attempt to explain the origin of this characteristic structure in meteoric iron. He observed in a Ressemer steel and in a cast-steel ingot structures which we now recognize as typical Widmanstatten figures.4 Osmond Observed structures in a steel ingot analog-ous to those found in meteorites. Arnold and Mc William6 obtained (and recognized) a

Jan 1, 1931

By Arne F. Westgren

X-ray analysis and single-crystal study have been utilized in recent years as a new means of following constitutional changes in alloys. If such transformations can be suppressed by rapid cooling, they can be followed at room temperature in a particularly convenient manner. In the following we shall consider changes in solubility and polymorphic transformations with particular reference to phenomena of the age-hardening type. Finally a thermodynamic viewpoint is developed for examining such transformations. Changes in Solubility 1. Determinations of solubility limits in the solid state which show decreasing solubility with falling temperature are made as follows: A series of alloys extending into the heterogeneous region is prepared and quenched fromas high a temperature as possible, whereupon their lattice parameters are determined. Then one or more alloys are quenched from temperatures at which they are heterogeneous and their lattice parameters likwwise determined. For the purpose of determining the parameter the apparatus shown in Fig. 1 has been very useful for it produces sharp films in a short time which can be accurately read. High-order reflections (interferences) from the object are recorded on a film which is placed exactly perpendicular to the X-ray beam. The specimen usually has the shape of a small round bar.l Fig. 2 shows a selection of such exposures of silver-rich Cu-Ag alloys, and Fig. 3 gives the measurements made from these films. Fig. 4 gives the solubility curve which results.2 This curve is shifted to lower concentrations than the curve that is obtained from metallographic or physical methods. The X-ray method unquestionably gives more reliable data

Jan 1, 1931

By Martin Lebeuf

The phenomena occurring in the cathode and at the cathode surface of aluminum electrolysis cells are very important in regards to cathode voltage drop and cathode wear. In the current study, laboratory-scale aluminum electrolysis cell cathodes were analyzed by X-ray microtomography. This technique allows an excellent visualization of the distribution of different substances, if their respective X-ray attenuation coefficients are different enough. In the current case, the important difference in the mean atomic number between cryolitic bath and graphitic carbon results in good contrasts. The volumetric bath penetration profile, porosity and impurities distribution in the cathode were thus obtained. Furthermore, metallic impurities and bath heterogeneities were observed at the cathode surface. Observations were also made with Scanning Electron Microscopy - Energy Dispersive Spectroscopy (SEM-EDS).

Jan 1, 2011

By Ralph E. Wood

X-ray fluorescence analysis can be profitably applied in the mineral industry by improving evaluation and control analyses, while offering lower cost and greater speed than conventional methods. Chemical analyses are not only a major item of cost in exploration and mining, as well as in milling and chemical treatment, but often cause evaluation and control of processing steps to lag behind operations. In the fields of geology and mining, the X-ray technique can be employed without destroying samples and, if necessary, specimens can be analyzed and then used, unchanged, in other evaluation techniques. Results are quickly made available for decisions on progress of exploration or sorting of waste and ore.

Jan 6, 1959

By E. O. Chartkoff

IN 1926 one of the authors published researches on the determination and description of the iron-tungsten and iron-molybdenum systems,1 including the equilibrium diagrams. In 1929, further work was carried on, including the examination by X-rays, which is recorded here. Measurements were made of changes in lattice parameters in the solid solutions. Precipitation from the solid solution and the accompanying changes in hardness were studied as well as the formation of the intermetallic compound phases upon sintering a mixture of metal powders.

Jan 1, 1930

By R. V. Kononko, A. Yu. Chikin, R. N. Rakhmeev, Yu. O. Fedorov

"The focus of the study is finding a solution that can help to improve diamond recovery in diamond-bearing gravity concentrates upgrading flowsheets. The purpose of the study was to develop and prove scientifically a separation method of diamonds recovery from gravity concentrates regardless of their fluorescence ability induced by X-ray radiation. Two promising recovery methods applicable to diamonds of this type are proposed, i.e. an X-ray radiometric method based on an instantaneous analysis of a secondary X-ray spectrum of separated particles, and a triboelectric method that relies on noncontact measurements of particle charges obtained during its motion in a vibratory tray. As a part of the laboratory study, X-ray fluorescence spectra of the collection of diamond crystals and main associated minerals and rocks at a particle size of -6+3 mm were produced. The analysis of the produced secondary X-ray spectra showed a significant difference between crystals, minerals and rocks within the analytical area of Ca, Fe and Zr due to the absence of calcium, iron and zircon elements in diamonds. Additionally, the scattered X-radiation level of diamonds substantially increased under the influence of X-ray radiation. Such a difference is a physical base of a new method of diamonds recovery from mineral mixtures. The laboratory study on triboelectric characteristics showed that a significant portion of diamonds gained an electric charge of a magnitude that was much higher, compared to associated minerals and rocks. The laboratory and industrial tests and the separation indicators demonstrated a high efficiency. A proposed X-ray radiometric method provides recovery of all types of diamonds regardless of X-ray fluorescence levels, with high selectivity and recovery rate of at least 98%. This proposed separation method is protected by a patent of Russian Federation (No. 2551486, “A method of X-ray radiometric separation of diamond-bearing materials”). Triboelectric separation organized in two stages (main and control) ensures recovery of up to 98-100% of diamonds at a particle size -5+2 and -2+1 mm,. More than 10 triboelectric separators successfully operate in active diamond processing plants in the Russian Federation."

Jan 1, 2018

By Ancel St. John

DURING a session on coal and coke at the February, 1926, meeting of the American Institute of Mining and Metallurgical Engineers, the writer called attention to the important work on the X-ray analysis of coal1,2 being carried on in England by C. Norman Kemp and his associates. This aroused so much interest that a paper on the subject was requested for the October meeting. It has seemed advisable to make this paper a preliminary survey of the present status in the application of X-ray methods to coal problems and to follow it from time to time with further articles as the art develops. A survey of this sort naturally divides itself into two parts, radioscopic analysis of the distribution of constituents through the body of the coal, and diffraction analysis of the state of association of the elementary components. In this article the subject matter concerning radioscopic analysis has been drawn almost entirely from the writings of Kemp and his associates and the illustrations have been specially furnished by him. It is a pleasure to record here a great indebtedness for this courtesy and cooperation. The subject matter and illustrations concerning diffraction analysis are taken from the author's unpublished researches.

Jan 10, 1926