WO1989012817A1 - Spectrometre a micro-faisceau de rayons x - Google Patents

Spectrometre a micro-faisceau de rayons x Download PDF

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Publication number
WO1989012817A1
WO1989012817A1 PCT/SE1989/000346 SE8900346W WO8912817A1 WO 1989012817 A1 WO1989012817 A1 WO 1989012817A1 SE 8900346 W SE8900346 W SE 8900346W WO 8912817 A1 WO8912817 A1 WO 8912817A1
Authority
WO
WIPO (PCT)
Prior art keywords
capillary
ray
rays
instrument according
collimator
Prior art date
Application number
PCT/SE1989/000346
Other languages
English (en)
Inventor
Anders Rindby
Per Engström
Sture Larsson
Bengt Stocklassa
Original Assignee
Anders Rindby
Engstroem Per
Sture Larsson
Bengt Stocklassa
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.)
Filing date
Publication date
Application filed by Anders Rindby, Engstroem Per, Sture Larsson, Bengt Stocklassa filed Critical Anders Rindby
Publication of WO1989012817A1 publication Critical patent/WO1989012817A1/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
    • G01N23/22—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 measuring secondary emission from the material
    • G01N23/223—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 measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/07—Investigating materials by wave or particle radiation secondary emission
    • G01N2223/076—X-ray fluorescence

Definitions

  • the innovation concerns an instrument for detecting trace amounts of different elements in sample volumes with a size of its linear dimension down to about one micrometer.
  • the innovation is based on a technique to achieve monochromatic microbeams of X-ray from a conventional X-ray tube by utilizing the selective absorption of X-rays in the anode and the reflecting properties of X-rays inside capillary tubes
  • X-ray induced X-ray fluorescence has been used for analysing elements since long time.
  • X-ray tubes or radioactive sources has normally been used as X-ray sources. Theses types of X-ray sources are isotropic and microbeams of X-rays can be achieved by collimating the beam with the use of absorbing materials. This means that only a small fraction of the source intensity can be utilized and for beamsizes down to about 100 ⁇ m in diameter, only X-ray tubes sources can provide the sufficient intensity for generating any detectable amount of fluorescent radiation.
  • the sample By using X-ray tubes as the source the sample will be exposed to the characteristic X-ray lines from the anode as well as a continuous distribution of X-rays (the bremsstralungspectra) which will reduce the sensitivity for detecting fluorescent radiation substantially due to the scattering of primary radiation into the detector, which always take place inside the sample.
  • the collimator Because of the penetrating power of X-rays and the construction of the X-ray tube, the collimator, used for generating a small beam, has to be relatively thick and placed a certain distance away from the source, which will reduce the intensity of X-rays out from the collimator.
  • Capillaries can be manufactured from many different types of glass materials but only a few of these materials will provide a surface quality sufficient for total reflexion of X-rays.
  • a thin layer of heavy metals Tianium or heavier
  • the reflectivety can be increased.
  • the critical angle can attain "extreme" values which can be utilized by combining the anode-material (rather the energy of the characteristic X-ray lines from the anode-material) with the surface-material (rather the energy of the absorption-edge in the surface- material).
  • the spectrometer as described in fig. 1, is based on a X-ray tube 1 with a with a line focus 2 on the anode.
  • the capillary which is attached to a vessel 8 filled with mercury in order to absorb any radiation outside the capillary, is put in close proximity to the beryllium window at the point focal output
  • the vessel 8 (with the mercury) together with the capillary constitutes the so called capillary collimator.
  • the vessel is put into a holder 4 which can be adjusted with high precision in a plane perpendicular to the X-ray beam (coming out from the capillary) as well as parallel to it by means of two micrometer screws 6.
  • the tilt-angles in the vertical and horizontal plane of the spectrometer are also adjustable with high precision by two other micrometer screws 7. with these screws the "take off" angle (the angle between the capillary and the anode plane) can be carefully adjusted which will determined the strength of the selective absorption within the " anode.
  • the X-ray will pass inside the capillary 3 and the sample 9 to be analysed will be applied precisely in front of the capillary output.
  • the fluorescent radiation of characteristic X-rays from the atoms in the sample will be detected by a semiconducting detector 10 , which, due to the fact that the beam is very small and parallel, can be placed very close to the sample. This will give a very efficient detection of the fluorescent radiation.
  • Semiconducting detectors for detecting X-rays are usually made of silicon or germanium crystals with a large intrinsic volume and a high voltage is applied over this crystal (see R. Woldseth, X-ray Energy spectrometry Kevex Corp. Burlinggame California U.S.A 1973 or G. Bertolini and G. Restelli, Spectrometry with solid state detectors. Atomic Inner-Shell Processes vol II ed. B. Crasemann Academic Press New York 1975).
  • an optimal position (corresponding to the largest intensity of X-rays) can easily be determined.
  • the largest intensity will normally be attained at very small "take off” angle. At these angles the projection of the focalspot at the plane perpendicular to the beam will be so small that almost every point at the focalspot can contribute to the intensity inside the capillary. At these small “take off” angles the selective absorption in the anode will be so strong that the "bremsstralung" radiation (the non-characteristic part of the
  • Fig. 3 a and 3 b represents spectra from a hair analysis with a chromium- resp. molybdenum- anode in the X-ray tube and with a capillary made of boronsilicate with a diameter of 200 ⁇ m.

Abstract

L'innovation concerne la structure d'un instrument destiné à l'analyse d'oligo-éléments dans des échantillons présentant une dimension de l'ordre du millimètre, par fluorescence aux rayons X. L'appareil comporte un micro-faisceau de rayons X monochromatiques et un détecteur de rayons X (10) pour détecter le rayonnement fluorescent émanant de l'échantillon (9). On utilise comme source de rayons X un tube radiogène (1) avec une ligne focale (2), et le rayonnement est guidé à l'extérieur jusqu'à l'échantillon par un capillaire (3). La mise en oeuvre de la réflexion totale des rayons X qui peut se produire à l'intérieur du capillaire (3) permet d'obtenir une intensité élevée ainsi qu'une suppression efficace des rayons X de haute énergie par rapport aux rayons X de faible énergie. Parallèlement, la mise à profit de l'absorption sélective intervenant pour de faibles angles entre le capillaire et le plan anodique permet de supprimer efficacement le rayonnement à la fois inférieur (faible énergie) et supérieur (haute énergie) au rayonnement propre émanant de l'anode.
PCT/SE1989/000346 1988-06-23 1989-06-19 Spectrometre a micro-faisceau de rayons x WO1989012817A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
SE8802372A SE8802372L (sv) 1988-06-23 1988-06-23 Mikroroentgenstraale-spektrometer
SE8802372-6 1988-06-23

Publications (1)

Publication Number Publication Date
WO1989012817A1 true WO1989012817A1 (fr) 1989-12-28

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/SE1989/000346 WO1989012817A1 (fr) 1988-06-23 1989-06-19 Spectrometre a micro-faisceau de rayons x

Country Status (2)

Country Link
SE (1) SE8802372L (fr)
WO (1) WO1989012817A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101858874A (zh) * 2010-05-18 2010-10-13 北京师范大学 微束质子荧光谱仪

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4317036A (en) * 1980-03-11 1982-02-23 Wang Chia Gee Scanning X-ray microscope

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4317036A (en) * 1980-03-11 1982-02-23 Wang Chia Gee Scanning X-ray microscope

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
NUCLEAR INSTRUMENTS AND METHODS IN PHYSICS RESEARCH A249, (1986), 536-540, A. RINDBY, "Applications of Fiber Technique in the X-Ray Region", see page 537 "Apparatus" and "Discussion" page 539. *
NUCLEAR INSTRUMENTS AND METHODS IN PHYSICS RESEARCH B36, (1989), 222-226, P. ENGSTROM et al., "A 200 mu m X-Ray Microbeam Spectrometer". *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101858874A (zh) * 2010-05-18 2010-10-13 北京师范大学 微束质子荧光谱仪
CN101858874B (zh) * 2010-05-18 2012-07-25 北京师范大学 微束质子荧光谱仪

Also Published As

Publication number Publication date
SE8802372D0 (sv) 1988-06-23
SE8802372L (sv) 1989-12-24

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