US3925678A - Absorption layer for use during x-ray fluorescence analysis which prevents hard x-rays - Google Patents

Absorption layer for use during x-ray fluorescence analysis which prevents hard x-rays Download PDF

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Publication number
US3925678A
US3925678A US488076A US48807674A US3925678A US 3925678 A US3925678 A US 3925678A US 488076 A US488076 A US 488076A US 48807674 A US48807674 A US 48807674A US 3925678 A US3925678 A US 3925678A
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Prior art keywords
layer
aluminum
radiation
purity
ray fluorescence
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US488076A
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English (en)
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Otto Eberspaecher
Herman Pfisterer
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Siemens AG
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Siemens AG
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    • 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
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F1/00—Shielding characterised by the composition of the materials
    • G21F1/02—Selection of uniform shielding materials
    • G21F1/08—Metals; Alloys; Cermets, i.e. sintered mixtures of ceramics and metals
    • 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

  • FLUORESCENCE ANALYSIS WHICH PREVENTS HARD X-RAYS BACKGROUND OF THE INVENTION 1.
  • Field of the Invention The present invention relates to layers of material for 2.
  • Description of the Prior Art In x-ray fluorescence analysis, interfering radiation often is encountered due to the radiation from the specimen holder and the results obtained are ambiguous since it is impossible to determine which radiation originated from the specimen and which radiation originated from the specimen holder.
  • the present invention provides coding specimen holders with layers so as to prevent undesired radiation during x-ray fluorescence analysis.
  • X-ray fluorescence analysis is very versatile and can be used in the analysis of substances which consist of chemical elements with order numbers of z 8. Because of the high sensitivity of this method, in addition, this method is used in quantitative determinations of low concentrations, small specimen quantities, and for. determination of mass populations in thin layers and in many other applications. Thus, highly accurate measurements must be made of the low intensities of the characteristic line radiation in these applications.
  • parasitic signals these may originate from inherent, scatter, or fluorescent radiation from components which are either located inside the x-ray tube or fall within the path of the primary beam.
  • the specimen holder which holds the specimen being examined, is particularly critical. In order to limit the contour of the primary beam between the x-ray tube and the specimen under examination, a
  • the gold-plated diaphragm is inserted and is designed to operate with the specimen holder.
  • the specimen holder will be struck by at least a part of the primary beam. This excites fluorescent radiation from the elements in the specimen holder.
  • the specimen holder is by way of example made of AlMgSi 5O may also be roughened by repeated cleaning operations and can become damaged and contaminated.
  • the relatively soft, very high-purity gold and silver layers which have Vickers hardnesses of VH 1000 N/mm are not optimum materials for the absorption of the parasitic radiation emanating from the specimen holder.
  • radiation of wide line spectrum excited from the gold and silver in this layer material will contribute to the parasitic radiation problem.
  • the invention is based upon the realization that highpreventing undesirable effects in x-ray applications. 16 pumy layers of aluminum absorb hlgh-energy x rays and electrons and the aluminum simply produces low-energy Al x-ray fluorescent radiation which is not a source of serious interference and is not dangerous.
  • the aluminum will be applied galvanically from oxygen-free aprotic media over the specimen holder or other device and the aluminum layer will then be anodically oxidized in a GX bath and for reasons of purity, an oxalic bath can be used.
  • This method of anodizing is described relative to semiconductor components in the publication entitled Chemic-Ingenieur-Technik 36, (1964), pages 616-637.
  • the thicknessof the aluminum layer should be around 200 um and that of the Eloxal or anodically oxidized layer should be around 13 pm.
  • the thickness of the layer is sufficient to fully absorb the spectrum lines of the disturbing fluorescent radiation from all elements having an order number less than 31.
  • the radiation of all elements up to gallium will be abosrbed.
  • the spectrum lines of the L spectra of all elements up to iridium will be absorbed.
  • the very long wave AlK radiation usually does not interfere with most kinds of investigations and is not a problem. It is only where investigations involving the element aluminum are being conducted that the specimen holder must be made of an aluminum-free material asfor example from sintered carbon.
  • the surface of the layers of the present invention has very low adhesive power and attracts virtually no impurities.
  • the thickness of. the layers can be very accurately controlled; and thus precision components can be constructed.
  • FIG. 1 is a sectional view illustrating a first embodiment of the invention.
  • FIG. 2 is a sectional view illustrating a second embodiment of the invention.
  • FIG. 1 is a cross-sectional view according to the invention.
  • the material 1 which might, for example, be AlMgSi 1 is utilized as a specimen holder and the x-ray fluorescence radiation from this material is to be absorbed so as to prevent contamination and spurious radiation.
  • a layer 2 of high-purity aluminum which, for example, might have a purity of better than 99.999 percent, may be applied galvanically from an oxygen-free aprotic media to a thickness of around 200 um. Then the outer surface of the aluminum layer 2 is subjected to a high-purity anodic oxidation referred to as the Eloxal process so as to produce an Eloxal layer 21.
  • the Eloxal or anodically oxidized layer may have a thickness of around 13 pm.
  • the arrows 30 represent the primary x-ray beam and the arrows 31 represent a reflected x-ray beam.
  • FIG. 2 illustrates a modification of the invention wherein before depositing the aluminum layer 2 on the material 1 there is deposited a layer 4 of nickel or iron or copper.
  • X-ray fluorescence spectrograms were recorded, first using a specimen holder of uncoated material, and second, with a specimen holder having the layer system according to the invention. In both specimen holders, high-purity aluminum was used as a dummy specimen. The net intensity was measured, in other words, the gross intensity minus the background intensity for Ka lines of Mg, Si, Cr, Mn, Fe, and Ga. In this manner the intensity I, of the parasitic signals emanating from the specimen holder were measured. Thereafter, the intensity 1,, of these lines in solid specimens of pure samples of the above elements were measured. Then the quotient 1,/I was calculated and this ratio indicates the ratio between the intensity of the parasitic radiation and the intensity of the radiation to be measured.
  • This quotient is defined in this application as A in the case of the uncoated specimen holder and is designated as B in the case of the specimen holder coated with the layer system of the invention. Then the quotient (A B) /A was calculated which is a measure of the proportion of the parasitic radiation intesity absorbed by the layer system of the invention. The following table lists these quotients for the different kinds of radiation.
  • the additional layer 4 consisting of iron, nickel, or copper are provided. These layers can be electro-deposited on the material 1 before the layer 2.
  • the layer systems of the present invention are advantageous not only for the specimen holder used for x-ray fluorescence analysis, but they can also be used for diaphragms and other components subject to the effect of a primary beam as well as in x-ray apparatus of all kinds and for electron beam equipment.
  • a layered structure for x-ray absorption formed on and covering a base member comprising a first layer of high-purity aluminum formed on said base member, and a second layer of high-purity anodic oxidized aluminum formed on said first layer.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Metallurgy (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
US488076A 1973-07-18 1974-07-12 Absorption layer for use during x-ray fluorescence analysis which prevents hard x-rays Expired - Lifetime US3925678A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19732336652 DE2336652A1 (de) 1973-07-18 1973-07-18 Schichtsystem zur absorption von roentgenstrahlen

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US3925678A true US3925678A (en) 1975-12-09

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US (1) US3925678A (fr)
JP (1) JPS5044882A (fr)
BE (1) BE817811A (fr)
DE (1) DE2336652A1 (fr)
DK (1) DK385174A (fr)
FR (1) FR2238218B3 (fr)
IT (1) IT1017127B (fr)
LU (1) LU70538A1 (fr)
NL (1) NL7409479A (fr)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4764945A (en) * 1984-10-05 1988-08-16 Kawasaki Steel Corp. Method of measuring layer thickness and composition of alloy plating
US4821301A (en) * 1986-02-28 1989-04-11 Duke University X-ray reflection method and apparatus for chemical analysis of thin surface layers
WO2002006792A2 (fr) * 2000-07-18 2002-01-24 Uop Llc Procede de preparation d'echantillons en parallele
USRE37536E1 (en) 1982-11-26 2002-02-05 Uab Research Foundation Split energy level radiation detection
US20020016006A1 (en) * 2000-07-18 2002-02-07 Rune Wendelbo Process of parallel sample preparation
US6677162B1 (en) 2000-07-18 2004-01-13 Uop Llc Process of parallel sample preparation
US7341414B2 (en) * 2005-05-02 2008-03-11 Cummins Inc. Fastener and method for reducing stress failure in an engine component
US20130037717A1 (en) * 2011-08-09 2013-02-14 Ketek Gmbh Device for a Radiation Detector and Radiation Detector with the Device
EP4184153A4 (fr) * 2020-07-14 2024-04-17 Shimadzu Corporation Analyseur par fluorescence x

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3644736A (en) * 1968-11-05 1972-02-22 Giken Kogyo Kk Back-scattering absorber materials for gamma-rays

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3644736A (en) * 1968-11-05 1972-02-22 Giken Kogyo Kk Back-scattering absorber materials for gamma-rays

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
USRE37536E1 (en) 1982-11-26 2002-02-05 Uab Research Foundation Split energy level radiation detection
US4764945A (en) * 1984-10-05 1988-08-16 Kawasaki Steel Corp. Method of measuring layer thickness and composition of alloy plating
US4821301A (en) * 1986-02-28 1989-04-11 Duke University X-ray reflection method and apparatus for chemical analysis of thin surface layers
WO2002006792A2 (fr) * 2000-07-18 2002-01-24 Uop Llc Procede de preparation d'echantillons en parallele
US20020016006A1 (en) * 2000-07-18 2002-02-07 Rune Wendelbo Process of parallel sample preparation
WO2002006792A3 (fr) * 2000-07-18 2003-03-27 Uop Llc Procede de preparation d'echantillons en parallele
US6677162B1 (en) 2000-07-18 2004-01-13 Uop Llc Process of parallel sample preparation
US6806093B2 (en) 2000-07-18 2004-10-19 Uop Llc Process of parallel sample preparation
US7341414B2 (en) * 2005-05-02 2008-03-11 Cummins Inc. Fastener and method for reducing stress failure in an engine component
US20130037717A1 (en) * 2011-08-09 2013-02-14 Ketek Gmbh Device for a Radiation Detector and Radiation Detector with the Device
US8835857B2 (en) * 2011-08-09 2014-09-16 Ketek Gmbh Device for a radiation detector and radiation detector with the device
EP4184153A4 (fr) * 2020-07-14 2024-04-17 Shimadzu Corporation Analyseur par fluorescence x

Also Published As

Publication number Publication date
FR2238218B3 (fr) 1977-05-06
DE2336652A1 (de) 1975-01-30
IT1017127B (it) 1977-07-20
NL7409479A (nl) 1975-01-21
LU70538A1 (fr) 1974-11-28
BE817811A (fr) 1974-11-18
DK385174A (fr) 1975-03-10
FR2238218A1 (fr) 1975-02-14
JPS5044882A (fr) 1975-04-22

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