WO1999060388A1 - Procede et appareil d'analyse granulometrique par rayons x (xaps) - Google Patents

Procede et appareil d'analyse granulometrique par rayons x (xaps) Download PDF

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Publication number
WO1999060388A1
WO1999060388A1 PCT/US1999/010723 US9910723W WO9960388A1 WO 1999060388 A1 WO1999060388 A1 WO 1999060388A1 US 9910723 W US9910723 W US 9910723W WO 9960388 A1 WO9960388 A1 WO 9960388A1
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Prior art keywords
ray
diffracted
particle size
particles
determining
Prior art date
Application number
PCT/US1999/010723
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English (en)
Inventor
Rahmi Yazici
Dilhan M. Kalyon
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The Trustees Of The Stevens Institute Of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by The Trustees Of The Stevens Institute Of Technology filed Critical The Trustees Of The Stevens Institute Of Technology
Priority to US09/700,350 priority Critical patent/US6751287B1/en
Priority to AU37932/99A priority patent/AU3793299A/en
Publication of WO1999060388A1 publication Critical patent/WO1999060388A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/10—Investigating individual particles
    • G01N15/14—Optical investigation techniques, e.g. flow cytometry
    • G01N15/1456—Optical investigation techniques, e.g. flow cytometry without spatial resolution of the texture or inner structure of the particle, e.g. processing of pulse signals
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/10—Investigating individual particles
    • G01N15/14—Optical investigation techniques, e.g. flow cytometry
    • G01N2015/1486—Counting the particles
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/10—Investigating individual particles
    • G01N15/14—Optical investigation techniques, e.g. flow cytometry
    • G01N2015/1493—Particle size

Definitions

  • the present invention generally relates to a method and apparatus for x- ray analysis of particle size, XAPS for short, and more specifically to a method and apparatus for determining particle size and particle size distribution of crystalline particles comprising powders, suspensions or solids non-intrusively without the need to extractor separate the particles from the other ingredients of the materials.
  • the highlights of this era include holography for characterization of particles in mist and suspension systems; laser Doppler velocimetry (laser-photon correlation spectroscopy) for characterization of particles in aerosols and Brownian motion; eriometry (light/laser diffraction) for evaluating fine particle populations based upon group diffraction patterns; signature-waveform characterization of scattered light for fine particle analysis; fractal description of fine particle profiles; and a new generation of image analyzers with powerful digitization and computer routines for fine particle size and shape analysis.
  • SEM scanning electron microscope
  • SEM scanning electron microscopy
  • EDX energy dispersive x-ray fluorescence analysis
  • SEM with EDX is applicable in general only if the components contain different and contrasting elements that are heavier than oxygen and are not affected by the vacuum.
  • the EDX technique is also limited to submicron thick surface layers and prone to errors due to surface films. Use of SEM with EDX is time consuming and is not amenable for on-line applications.
  • X-ray diffraction methods can be applied to determine the size of particles in some special cases. Early work has been done with Debye and back- reflection cameras. In these x-ray diffraction techniques particles or grains of a polycrystalline material are irradiated with a collimated beam and diffraction takes place in the coherently reflecting planes of the particles. When large numbers of particles are irradiated under the incident beam, their diffraction spots overlap and form continuous diffraction lines on appropriate Debye rings. Continuity of the rings breakdown and individual diffraction spots are resolved if the number of diffraction particles is reduced. However, the number of diffracting particles is reduced and diffraction spots from individual particles are resolved only if the particle size is very large.
  • U.S. Patent No. 3,148,275 discloses a x-ray technique that is not for particle size analysis. Rather, it relates to a special sample holder to hold a curved specimen to improve wide-angle x-ray diffractometer (WAXRD).
  • WAXRD wide-angle x-ray diffractometer
  • U.S. Patent No. 4,649,556 discloses an indirect method to get information on the "average" particle size by making use of the variation of diffracted intensity with WAXRD 2 ⁇ angle using a point detector. It does not obtain direct information on the particle size and cannot do measurements on individual particles to get particle size distribution.
  • U.S. Patent No. 4,821,301 discloses a technique for glancing-angle x-ray-absorbance chemical analyses of thin (1000 A) films. It does not relate to particle size analysis.
  • U.S. Patent No. 5,128,976 does not disclose a particle size analyzer. Rather, it relates to an oscillation radiographer with a point detector. It is based on absorption contrast and uses a x-ray film to record it. It does not use any of the beam path on the detector system nor the type of data analysis that the present invention (XAPS) uses.
  • U.S. Patent No. 5,373,544 does not disclose a particle size analyzer.
  • XAPS linear position sensitive detector in horizontal configuration as opposed to a vertical configuration of the present invention
  • U.S. Patent No. 5,446,777 discloses WAXRD with a horizontal linear position-sensitive detector that is designed to carry out location - specific WAXRD measurements on a give sample. It does not relate to a particle size analyzer.
  • the apparatus of the present invention which comprises a x-ray source, a monochromator, a goniometer, a position sensitive detector and computer means for interpreting the data obtained at the position sensitive detector.
  • the method of the present invention includes the steps of generating an x-ray; narrowing the wavelength of the x-ray by means of a monochromator; placing a specimen in the path of the x-ray beam; allowing the particles to diffract the beam; detecting the diffracted beam with a position sensitive detector; collecting the diffraction data from individual particles; rocking or rotating the specimen or the x-ray source for successive times to cover the angular range of reflection of the particles; compilation of the diffraction data in the computer memory to construct the intensity profile for individual particles; and interpreting the data to determine particle size and distribution of crystalline particles.
  • particle size and particle size distribution of crystalline particles in powders, suspensions and solids can be determined upon collection of samples from a process and characterization off-line at another location with the apparatus and method of the present invention, or on-line with the process using the apparatus and the method of the present invention.
  • the present invention allows for these determinations to be made in situ, without the need for separating the particles, and sufficiently fast so that the generated data can be used in a process control algorithm for quality and process control.
  • FIG. 1 is a schematic view of the present invention, X-ray Analyzer for
  • XAPS Particle Size
  • FIG. 2 is a graph of intensity versus azimuthal position ⁇ on a Debye arc obtained by the X-ray Analyzer for Particle Size (XAPS) configuration in
  • FIG. 3 is a schematic view of the present invention, X-ray Analyzer for Particle Size (XAPS), equipped with a position-sensitive area detector for simultaneous analysis of multiple Debye arcs from different lattice planes and multiple components/phases/polymorphs in a mixed composite material.
  • XAPS X-ray Analyzer for Particle Size
  • FIG.4 is a graph of intensity versus azimuthal position ⁇ on two Debye arcs versus the angular position ⁇ obtained by the X-ray Analyzer for Particle Size (XAPS) configuration in Figure 3.
  • FIG. 5 is a graph of a typical X-ray Analyzer for Particle Size (XAPS) data for a single particle.
  • FIG. 6 (A) - 6(C) are flow charts showing the basic steps of the two computer programs used in connection with the invention, for data collection and analysis.
  • FIG.7 is a graph of absorption correction factors for spherical aluminum particles and Cu K- ⁇ radiation versus the particle size.
  • FIG. 8 is a block diagram of the apparatus used in this invention.
  • FIG. 9 is a block diagram of a modified apparatus for performing the present invention in real or near-real time, as part of the production process.
  • FIGS. 10a, 10b, and 10c are photomicrographs of the (a) “First,” (b) “Second” and (c) "Third” samples of the atomized aluminum powders obtained by scanning electron microscope (SEM) at 500x magnification.
  • FIGS. 11a and lib are graphs of the "First" sample of atomized aluminum powder.
  • FIG. 11a contains the results of scanning electron microscopy (SEM) measurements, Frequency (number percent) vs. Particle size (microns), and
  • FIG. lib reports the results of X-ray Analyzer for Particle Size (XAPS) measurements, Frequency (number percent) vs. Intensity (photons per second).
  • FIGS. 12a and 12b are graphs of the "Second" sample of atomized aluminum powder.
  • FIG. 12a contains the results of scanning electron microscopy (SEM) measurements, Frequency (number percent) vs. Particle size (microns), and
  • FIG. 12b reports the results of X-ray Analyzer for Particle Size
  • FIG. 13 is calibration curve for conversion of X-ray Analyzer for Particle Size (XAPS) intensity values obtained from aluminum particles to X-ray Analyzer for Particle Size (XAPS) particle size values.
  • FIGS. 14a and 14b are particle size distribution of the "Third" sample of atomized aluminum powder.
  • FIG. 14a contains the results of scanning electron microscopy (SEM) measurements, Frequency (number percent) vs. Particle size (microns), and
  • FIG. 14b reports the results of X-ray Analyzer for Particle Size (XAPS) measurements, Frequency (number percent) vs. Particle size (microns).
  • FIGS. 15a and 15b are SEM photomicrographs of HNIW powders.
  • FIG. 15a is a SEM photomicrograph of "fine” HNIW powders at 2000x magnification and
  • FIG. 15b is a SEM photomicrograph of "coarse” HNIW powders at 300x magnification.
  • FIG. 16 is a graph of particle size distribution of the "fine” and “coarse” HNIW powders shown in FIGS. 15a and 15b, as measured by the X-Ray Analyzer for Particles (XAPS), frequency (number percent) verses particle size (microns).
  • XAPS X-Ray Analyzer for Particles
  • microns particle size
  • the present invention comprises a novel method and apparatus that can effectively measure the "true” size of individual crystalline particles, with the diffraction information that is directly proportional to particle mass, and determine the particle size distribution characteristics in loose powders, suspensions, and solids.
  • the technique can also differentiate the particles of the multiple ingredients in a given mixed state and quantitatively measure the particle size distribution and the relative volume fraction and phase or polymorph of each component.
  • the method and apparatus of the present invention can be used to determine the particle size of individual crystalline and semi-crystalline particles including powders, grains and whiskers, in loose powders, particle-filled viscous suspensions and multi-particle solid materials.
  • the present invention is a non-invasive technique that requires minimum sample preparation. Measurements can be carried out in ambient atmosphere without the need for the application of vacuum, carrier fluids or other medium. Each measurement may take only a few minutes of time or less depending on the sample material and may even be performed "on-line" at production facilities.
  • a monochromatic x-ray beam 20 is directed at a specimen 30 and impinges on particles comprising the specimen which causes a diffraction of the x-ray beam indicated at 40a, 40b, 40c, and 40d emanating from particles a, b, c, d on the specimen.
  • These diffracted beams 40a-40d are picked up by position sensitive detector 50a, through entry slit 52.
  • the azimuthal position ⁇ on the Debye arc which is made to coincide with the length of the PSD, is identified and the intensity I is measured as graphically shown in FIG. 2.
  • a computer means is utilized to interpret the data from the position sensitive detector 50a.
  • the XAPS unit utilizes a highly parallel crystal monochromatization where the monochromator can be symmetrically or asymmetrically cut, flat or curved, single, two-parallel or channel-cut crystals
  • other means of obtaining highly parallel monochromatic beam are also considered.
  • combined use of filters, curved mirrors, tapered capillaries or parallel and monochromatic sources such as accelerators, plasma- discharge units or a synchrotron source can all be used.
  • This setup for the present invention is carried out in a high precision ⁇ - ⁇ diffractometer and includes a x-ray source, a ⁇ - ⁇ goniometer for rotating the sample or the x-ray source, and a detector such as a position sensitive detector
  • a monochromator such as a crystal-monochromator and various slits, collimators and capillaries may be used to obtain a highly parallel monochromatic x-ray beam 20 having very narrow wavelength.
  • X-ray film, a position sensitive detector, or a CCD camera can be used to detect and differentiate the diffraction of the monochromatic x-ray beam from the individual particles of the specimen.
  • the present invention is based on double-crystal diffractometry method, where individual particles are regarded as the second or test crystal of the double crystal diffractometer.
  • the particulate sample or the x-ray source may be oscillated, rotated or rocked for a sum of several tens of minutes of arc about the Bragg angle, while being irradiated by a crystal or otherwise monochromated parallel x-ray beam.
  • Several particles (or grains) in the sample will be in Bragg reflecting positions which result in individual microscopic diffraction spots along the appropriate Debye arc. These spots are detected by a position-sensitive detector (PSD) either linear 50a and oriented parallel to the
  • These principles of operation of the XAPS method and the diffraction peaks obtained are schematically shown in FIGS. 1 and 2 for one dimensional detectors 50a, and in FIGS. 3 and 4 for two dimensional detectors 50b.
  • the intensity distribution of each diffraction spot of an individual particle and its location and distribution are then stored in a computer for subsequent numerical analysis (see FIG. 5).
  • the integrated intensity of an individual diffraction spot is directly proportional to the volume and mass of the particular diffracting particle in the sample.
  • the primary x-ray beam 20 can be monochromatized in a number of ways like diffraction from the planes of a flat or channel-cut crystal. Upon monochromatization the resultant monochromatic beam has a very small horizontal convergence and is nearly parallel, while the vertical divergence of the beam is controlled by a slit, collimator or capillary systems.
  • the sample under investigation is mounted on a two-dimensional microscope stage which enables precise selection of the region of interest. The axis of the sample holder is rotated by a stepping motor for orienting along an appropriate angle.
  • Various detectors including a one- dimensional position-sensitive detector, which is located parallel to the Debye arc, a two-dimensional position sensitive detectors a CCD camera or a fiberoptic detector or an image plate or film or any other two-dimensional position sensitive detection system can be used.
  • a typical source i.e., 0.5-3 kW diffraction tube with a Cu target may be used as the x-ray source, however, other sources including rotating anode sources using Cr, Mo or other targets that generate softer or harder x-rays are useable. Each measurement may take up to a few minutes. The speed and resolution can also be enhanced, if necessary.
  • the present invention can typically analyze particles ranging in size from 0.5 ⁇ m to 300 ⁇ m in diameter, without altering its x-ray optics. These limits however, can be expanded by making appropriate changes in the x-ray optics.
  • the lower limit of the particle size analysis can be further lowered from 0.5 ⁇ m.
  • the upper limit in the particle size analysis can be further increased from 300 ⁇ m to several millimeters.
  • the vertical and horizontal divergence of the monochromatic beam can be adjusted, for example, by adjustable slits, for vertical and by use of asymmetric crystals, for horizontal divergence, and through such alterations of the x-ray optics the width of the beam divergence can be tuned with that of the angular-range-of-reflection of the given particles, and this way the particle size can also be determined from a single exposure without rocking the sample or the beam.
  • FIGS. 6(A) - 6(C) Flow charts of programs used in the present invention are shown in FIGS. 6(A) - 6(C).
  • the programs are used to determine the particle size/intensity/distribution and utilize algorithms for data interpretation, background correction, peak and integrated intensity determination and statistical analysis and graphics for the deduction of particle size distribution parameters.
  • These include: 1) a program (XAPS DATA COLLECT), FIG. 6 A, that has been developed for automation of the moving parts in the XAPS apparatus and for data acquisition; and 2) a program (XAPS DAT ANALYST),
  • FIGS. 6(B) and 6(C) for data analysis to determine the particle size/intensity/distribution, including a set of algorithms for data interpolation, background correction, peak and integrated intensity determination and statistical analysis and graphics for the deduction of particle size and microstrain distribution parameters.
  • the x-ray intensity spectra of multiple particle reflections are collected and displayed, as shown schematically in FIGS. 2 and 4, by a multichannel analyzer (MCA) and a computer. Subsequently, the spectra from individual particles are stored in the computer as shown in FIG. 5 for further analysis.
  • MCA multichannel analyzer
  • a large particle population can readily be analyzed at each region of interest by taking multiple exposures at the Bragg angle. Also, the entire sample surface can be analyzed by moving the sample with a microstage relative to the incident beam.
  • the integrated intensity of the diffraction from an individual particle is directly proportional to the volume of the particle.
  • the intensity is given by:
  • I diffracted beam intensity
  • I 0 incident beam intensity
  • K constant
  • r distance from the diffraction site
  • F structure factor (material dependent)
  • p multiplicity factor (material dependent)
  • ⁇ Bragg angle (material and x-ray wavelength dependent)
  • A absorption factor (material, x-ray wavelength and (particle) size and shape dependent)
  • e ⁇ 2M temperature factor.
  • the absorption factor is given by:
  • the present invention is applicable to particles which are crystalline or highly amorphous particles and particles with excessive plastic deformations cannot be analyzed by this method and apparatus.
  • the x-ray source for the system could be a rotating anode or a sealed x-ray tube 112 with its high- voltage supply 110.
  • These x-ray generators are available from numerous manufacturers. The ones currently utilized are a Rotaflex rotating anode system by Rigaku, Danvers,
  • a monochromator 118 and a ⁇ - ⁇ - ⁇ goniometer 170 currently used is made by Picker model 3488L. Similar goniometer and monochromators are also available by Huber, Blake Industries, Scotch Plains, New Jersey. Currently a flat symmetric-cut Si (III) single crystal and an asymmetric-cut Si (III) crystal are used in the monochromator 118 to obtain a monochromatic parallel beam 120. This beam 120 is diffracted by particles in the sample 130 to create diffracted beam 140.
  • the Picker unit has been retrofitted with a stepping motor system for automation: model MO92-FC08 motor by Superior Electric, Bristol, Connecticut, and a stepper control model DPH37 by Anaheim Automation, Anaheim, California. Sample rotation/rocking step of 0.1 minutes of arc about angles ⁇ , ⁇ , is made possible with this system. For the off-line XAPS system shown in FIG. 8, only the sample 130 is rotated or rocked.
  • PSD position sensitive detector
  • PSD 150 there are two linear PSD 150 and related PSD electronics 152 systems that are used in the current invention.
  • PSD system is manufactured by TEC, Knoxville, Tennessee, Model 200-PD-01 detector and Model 200-DM-01 signal processing electronics.
  • the other PSD system is manufactured by M
  • the computer 160 used for automation of the goniometer 170, data acquisition from the PSD electronics 152 and for data analysis, is an IBM-PC type computer 486 or better, available from numerous manufacturers.
  • the signals from the PSD electronics module 152 are captured by a multi-channel analyzer (MCA) PC-board installed in the PC.
  • MCA multi-channel analyzer
  • FIG. 9 A block diagram of the XAPS system of the present invention for on-line applications is shown in FIG. 9.
  • the on-line version is designed and built for carrying out particle size distribution analysis in processing and manufacturing environments, on-site and on-line with the processing equipment 282 so that manufactured products such as powders, powder-binder suspensions or powder- binder solid articles are analyzed immediately for quality control.
  • conveyor system 280 in FIG. 9, Model 2100 by Dormer, Hugo, Minnesota is employed to bring the sample material to the correct position at the center of the x-ray unit 270b.
  • particle size distribution of particles found in the powder, suspension or solid forms may be analyzed sequentially.
  • the measurements are done intermittently where the conveyor is brought to a halt for each sampling during XAPS measurements.
  • the goniometer 270b employed for on-line analysis is a vertical theta-theta goniometer Model D8 manufactured by Bruker, AXS, Madison, Wisconsin.
  • the goniometer has a circular opening 272 in the middle to accommodate the conveyor to pass through, see 280 passing through 270b in FIG. 16.
  • the x-ray source 212b in this version comprises a sealed-tube x-ray generator.
  • the x-ray source 212b rotates/rocks with theta ( ⁇ ) motion instead of the sample.
  • the sample is not rotated, but held stationary, in this on-line version of XAPS, making it possible to deliver and analyze samples in as-processed condition.
  • the monochromator 218b includes a curved x-ray mirror for focusing and to obtain a higher x-ray intensity.
  • the beam 220 is diffracted by particles in the sample 230 to create a diffracted beam 240.
  • the PSD system 250 and 252 is made by M Braun as previously set forth.
  • the computer means 260b used in the on-line version of XAPS is designed to handle additional tasks compared to the off-line version.
  • the computer means of the on-line version is able to do near-real time analysis by multi-tasking and also the on-line version is capable of controlling the conveyor 280 motion and communicating with the processing equipment 282 for feedback and quality control tasks.
  • the x-ray unit can be made to move at the same linear speed as the conveyor to allow the determination of the particle size without interrupting the flow of the process streams.
  • the x-ray unit can be kept fixed but the data acquisition system can be programmed to "follow" the moving particles on the conveyor to allow the determination of the particle size without interrupting the flow of the process streams.
  • particle size measurements were carried out on three aluminum powders, which were processed by gas- atomization from melt, and all three constituted near-spherical particles.
  • the average particle size of two of the powder grades were specified by the manufacturer, Ampal, Inc., as 8 ⁇ m and 55 ⁇ m, respectively and were used as the calibration samples.
  • the "Third" aluminum powder lot with an unknown particle size distribution was used as test material.
  • a double-sided conductive carbon adhesive tape was used as the mounting medium to hold the loose powder during the x-ray diffraction and scanning electron microscopy (SEM) measurements. Particles were spread on the tape in a monolayer for stability and ease of SEM image analysis.
  • Control measurements of particle size distribution were carried out with a scanning electron microscope.
  • the typical SEM photomicrographs of the three atomized aluminum powders are shown in FIGS. 10a, 10b, and 10c.
  • all three powders exhibit nodular particles with rounded near- spherical features which are typical of gas-atomization-from-melt powder processing.
  • the secondary electron images of the particles were photographed at high magnification and images were analyzed for particle size determination.
  • An image analysis software was employed for these studies.
  • the results of the particle size distribution measurements of the "First" and "Second" aluminum powders are graphically shown in FIGS. 11 and 12, respectively. In FIGS.
  • FIG. 14b The average particle size by number values obtained with the present invention and SEM methods were seven microns and five microns, respectively. These results are in very good agreement considering that the particle size distribution of this "Third" sample extends from 0.5 ⁇ m to 40 ⁇ m. The technique has been also applied to other materials.
  • the results of XAPS particle size distribution analysis of HNIW (hexanitro-hexaazaiso- wurtzitane) powders are shown in FIGS. 15a and 15b and 16. In these analysis "Fine” and “Course” HNIW powders were analyzed and similar calibration techniques, as with the aluminum powders, were applied to determine the particle size distributions. As shown in FIGS.
  • This demonstration is indicative of the ability of the technique of the present invention to capture changes in particle size distribution which can occur during crystallization, processing or heat treatment and suggests its potential for use as an off-line or on-line quality control monitoring technique during manufacturing operations.
  • Every crystalline material generates characteristic diffraction peaks at different Bragg angles.
  • particles from each material generate diffraction spots at separate Debye arcs positioned at unique ⁇ angles.
  • Particles with different crystal structures can be analyzed by the present invention by: (1) either sequentially placing a position sensitive linear detector (PSD) at the appropriate Debye arcs as shown in FIG. 1, or (2) simultaneously, by employing multiple linear PSD's, or a 2-dimensional PSD or a CCD camera , or a fiberoptic detector or an image plate or a film, or any other two-dimensional position sensitive detection system 50b, as shown in FIG. 3.
  • PSD position sensitive linear detector
  • the particle size and relative particle volume fraction of multiple phases or polymorphs can be determined at a given location in the mixture, such as shown in FIG. 4, where 40a, 40b, 40c and 40d versus 40e, 40f, 40g, 40h and 40i could originate from two different phases or components.

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Abstract

L'invention concerne un appareil comportant une source (112) de rayons X, un monochromateur (118), un goniomètre (170), un détecteur (150) de position, un mécanisme permettant de faire basculer ou tourner l'échantillon ou la source de rayons X, et un dispositif (160) d'ordinateur servant à interpréter les données obtenues au détecteur de position. Le procédé de l'invention comporte les étapes consistant à produire un rayonnement X; réduire la longueur d'onde du faisceau de rayons X; permettre aux particules de diffracter le faisceau; détecter le faisceau diffracté à l'aide du détecteur de position; recueillir les données de diffraction provenant des particules individuelles; faire basculer ou tourner l'échantillon ou la source de rayons X plusieurs fois successivement de façon à couvrir la plage angulaire de réflexion des particules; compiler les données de diffraction dans la mémoire d'ordinateur de manière à construire le profil d'intensité des particules individuelles; et interpréter les données pour déterminer la granulométrie et la répartition granulométrique.
PCT/US1999/010723 1998-05-15 1999-05-14 Procede et appareil d'analyse granulometrique par rayons x (xaps) WO1999060388A1 (fr)

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US09/700,350 US6751287B1 (en) 1998-05-15 1999-05-14 Method and apparatus for x-ray analysis of particle size (XAPS)
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Cited By (6)

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WO2002025247A2 (fr) * 2000-09-20 2002-03-28 Menguc M Pinar Procede et appareil non intrusifs permettant de caracteriser des particules par diffusion d'elements matriciels au moyen d'une radiation polarisee elliptiquement
EP1540319A1 (fr) * 2002-07-26 2005-06-15 Hypernex, Inc. Analyse quantitative de phases de materiaux polycristallins textures
EP2634566A1 (fr) * 2012-02-28 2013-09-04 PANalytical B.V. Microdiffraction
EP2706344A1 (fr) * 2012-09-05 2014-03-12 Paul Scherrer Institut Système pour mesurer une distribution granulométrique des particules d'une matière particulaire
CN113049617A (zh) * 2021-03-09 2021-06-29 西湖大学 基于单晶衍射仪的广角散射测试方法及装置
CN113740212A (zh) * 2021-08-26 2021-12-03 西南交通大学 用于研究湿法制粒中颗粒成核生长的设备、系统和方法

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EP2706344A1 (fr) * 2012-09-05 2014-03-12 Paul Scherrer Institut Système pour mesurer une distribution granulométrique des particules d'une matière particulaire
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CN113049617A (zh) * 2021-03-09 2021-06-29 西湖大学 基于单晶衍射仪的广角散射测试方法及装置
CN113049617B (zh) * 2021-03-09 2024-04-02 西湖大学 基于单晶衍射仪的广角散射测试方法及装置
CN113740212A (zh) * 2021-08-26 2021-12-03 西南交通大学 用于研究湿法制粒中颗粒成核生长的设备、系统和方法

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