US3400265A - X-ray spectrometry apparatus having both interchangeable specimens and radiation sources - Google Patents

X-ray spectrometry apparatus having both interchangeable specimens and radiation sources Download PDF

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Publication number
US3400265A
US3400265A US443822A US44382265A US3400265A US 3400265 A US3400265 A US 3400265A US 443822 A US443822 A US 443822A US 44382265 A US44382265 A US 44382265A US 3400265 A US3400265 A US 3400265A
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US
United States
Prior art keywords
specimen
aperture
specimens
turret
interchangeable
Prior art date
Legal status (The legal status 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 status listed.)
Expired - Lifetime
Application number
US443822A
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English (en)
Inventor
Houbart Yvan
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Centre de Recherches Metallurgiques CRM ASBL
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Centre de Recherches Metallurgiques CRM ASBL
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/22Investigating 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
    • G01N23/225Investigating 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 using electron or ion
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/22Investigating 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
    • G01N23/223Investigating 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J35/00X-ray tubes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/07Investigating materials by wave or particle radiation secondary emission
    • G01N2223/076X-ray fluorescence

Definitions

  • the present invention relates to X-ray spectrometry and more particularly to an apparatus for X-ray spectrometry having a rotatable turret in which at least two specimens can be placed.
  • One particular object of the invention is the provision of a spectrometer which is universal in the sense that it can either be used for bombarding a specimen with electrons so that X-rays are produced or for projecting X- rays on to the specimen so that a fluorescence technique can be used.
  • a further object of the invention is to provide an improved apparatus in which the specimen under examination is maintained in the same evacuated space as a source of electrons or X-rays for the examination of the specimen, so that X-rays are projected through an aperture onto a detecting device comprising a crystal and a counter.
  • the detecting device is in a prolongation of the evacuated space of the electrons or X-rays source.
  • the entire X-ray path is under vacuum and the only absorbing matter is the window of the counter.
  • Yet a further object of the invention is the provision of a device for examination by X-ray techniques in which the space to be evacuated is as small as possible, and in which the volume put under atmospheric pressure when a specimen is introduced or removed is reduced to a minimum and does not include the space surrounding the electron or X-ray generating means.
  • FIGURES 1 and 2 are respectively a sid view and partial section of the device described in the Belgian patent specification, and is a view of the turret from below. 65
  • FIGURE 3 is a view on the line III-III of FIGURE 1.
  • FIGURES 4 and 5 are views of part of the novel spectrometer forming the subject matter of the present invention in accordance with two vertical sections at right angles to each other.
  • FIGURES 6 and 7 correspond to FIGURE 5 but ShOW the apparatus equipped for projecting a beam of electrons Patented Sept. 3, 1968 Fr I onto a specimen, and for projecting X-rays onto it, respectively.
  • the spectrometer represented comprises a non-rotatable base portion B and a rotatable turret T.
  • the base portion B has a vertically extending aperture 2 reaching as far as an oblique upper face 11 of the base portion.
  • This aperture 2 contains an electron gun 6 with a vertical axis 1.
  • the lower part of the electron gun is put in communication with a vacuum pump indicated diagrammatically while it is connected with a power pack indicated diagrammatically also.
  • the turret T is carried by a ball bearing 31 mounted in a recess 32 in the upper part of the base portion and is held down by a stud 14 on which a nut 30 is screwed.
  • a rim 13 projects above the oblique face 11 and surrounds partly the turret T.
  • the turret T has three circular apertures 16 in which specimens such as 8 can be carried by specimen holders 17 at such a distance from the axis 3 of rotation of the turret that as the turret is rotated they can be brought into position over the electron gun 6.
  • Each specimen is covered by a cap such as 18 with sealing means 19.
  • air can only be exhausted from under the specimen which is over the opening 20 of the base B.
  • This opening is connected to a vacuum rotary pump and air can be exhausted by means of an electromagnetic valve.
  • apertures 20 and 21 in the base B are connected to two high vacuum devices, independent from each other, each device comprising a vacuum rotary pump and a diffusion pump in the purpose to obtain a 1O mm. Hg vacuum.
  • the power pack creates a potential dilference between the filament 5 of the electron gun and the specimen 8 of about 10 kilovolts so that the electron bombardment of the specimen produces X-rays which emerge through an aperture 9 in the side of the base. I remind that this aperture 9 is in direct communication with the detecting device, which is of no interest for this present invention.
  • the turret is turned through in a clockwise direction. In this way, the specimen just examined comes over the aperture 21 where it can be removed by acting the electro magnetic valve connecting the aperture 21 only to the atmospheric pressure.
  • the unit becomes a semi-automatic device.
  • Powders and insulators may be examined using this high vacuum device with the condition of replacing the electron bombardment by photon bombardment (X-ray fluorescence technique).
  • the aperture 2 (see FIGURES 4 and 5) is in fact a blind hole open at its top end.
  • I provide two conical holes 41 and 42 (see FIGURE 5) in the part of the base surrounding the aperture 2, whose axes 43 and 44 are radial with respect to the vertical axis 45 of the aperture 2 and meet the axis 45 at vertically spaced positions.
  • the angle of the axis of rotation of the turret is 45 to the vertical.
  • I when I wish to examine a specimen by an X-ray fluorescence technique, I replace the electron gun 48 by an electron gun 54, as shown in FIGURE 7, which has an emitter 55 and a concentrating head 56 and sends out electrons towards the axis 45 of the aperture 2.
  • I place an anti-cathode 52 with a pyramidal end piece whose faces make an angle of about 45 to the vertical and have inserts of tungsten or chromium or alternatively electrolytic deposits of these metals.
  • a beam of electrons from the gun 54 impinges on the anti-cathode and the resulting beam of X-rays passes upwards and impinges against the bottom face of the specimen 8.
  • Electron gun 54 is insulated from the base B.
  • the emitter of the gun can be a heated filament connected with the power pack through a flexible cable.
  • an apparatus for examining a specimen by bombardment with radiation comprising a non-rotary base with a horizontal lower face and an upper face inclined at an acute angle to said lower face, an aperture opening upwardly through the upper face, a rotatable turret mounted over the upper inclined face, at least two specimen holders in the turret, at such distances from the axis of rotation of the turret that the specimens can be aligned with the aperture in the base and means for evacuating the aperture and preventing air from coming into contact with the lower face of the specimen, the improvement in which the aperture in the base plate is formed as a hole open at its upper end and closed at its lower end and having provision therein to enable at least one source of radiation to be introduced into the said aperture through the side walls thereof.
  • one source of radiation comprises an electron gun.
  • An apparatus as claimed in claim 1 in which an electron gun and an anti-cathode are introduced through the side walls of the aperture, in diametrically opposed relationship so as to bombard the sample with X-rays.
  • An apparatus as claimed in claim 1 in which an electron gun and an electron gun/anticathode combination are used together to bombard the sample simultaneously with electrons and X-rays.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
US443822A 1964-04-01 1965-03-30 X-ray spectrometry apparatus having both interchangeable specimens and radiation sources Expired - Lifetime US3400265A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
BE646014A BE646014A (de) 1964-04-01 1964-04-01

Publications (1)

Publication Number Publication Date
US3400265A true US3400265A (en) 1968-09-03

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Application Number Title Priority Date Filing Date
US443822A Expired - Lifetime US3400265A (en) 1964-04-01 1965-03-30 X-ray spectrometry apparatus having both interchangeable specimens and radiation sources

Country Status (6)

Country Link
US (1) US3400265A (de)
BE (1) BE646014A (de)
DE (1) DE1960083U (de)
LU (1) LU48050A1 (de)
NL (1) NL6504158A (de)
SE (1) SE306436B (de)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4008683A (en) * 1973-07-16 1977-02-22 Varian Associates Machine for treating wafer-form items
US4033904A (en) * 1974-03-22 1977-07-05 Varian Associates, Inc. Interchangeable specimen trays and apparatus for a vacuum type testing system
US4044266A (en) * 1975-07-09 1977-08-23 Danfysik A/S Apparatus for ion-implantation in elements, especially discs of semi-conducting material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3073951A (en) * 1960-07-28 1963-01-15 Combustion Eng Vacuum lock
US3099743A (en) * 1961-07-07 1963-07-30 Ichinokawa Takeo Combined electron probe microanalyzer and x-ray diffraction instrument

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3073951A (en) * 1960-07-28 1963-01-15 Combustion Eng Vacuum lock
US3099743A (en) * 1961-07-07 1963-07-30 Ichinokawa Takeo Combined electron probe microanalyzer and x-ray diffraction instrument

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4008683A (en) * 1973-07-16 1977-02-22 Varian Associates Machine for treating wafer-form items
US4033904A (en) * 1974-03-22 1977-07-05 Varian Associates, Inc. Interchangeable specimen trays and apparatus for a vacuum type testing system
US4044266A (en) * 1975-07-09 1977-08-23 Danfysik A/S Apparatus for ion-implantation in elements, especially discs of semi-conducting material

Also Published As

Publication number Publication date
SE306436B (de) 1968-11-25
DE1960083U (de) 1967-05-11
BE646014A (de) 1964-10-01
NL6504158A (de) 1965-10-04
LU48050A1 (de) 1965-04-23

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