US3617738A - An electronic energy sample analysis device - Google Patents

An electronic energy sample analysis device Download PDF

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Publication number
US3617738A
US3617738A US760149A US3617738DA US3617738A US 3617738 A US3617738 A US 3617738A US 760149 A US760149 A US 760149A US 3617738D A US3617738D A US 3617738DA US 3617738 A US3617738 A US 3617738A
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US
United States
Prior art keywords
enclosure
turret
vacuum
aperture
sample
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
US760149A
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English (en)
Inventor
Yvan Louis Houbart
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US Philips Corp
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US Philips Corp
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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
    • 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
    • G01N23/2204—Specimen supports therefor; Sample conveying means therefore
    • 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 turret is then rotated to interchange the position of the through bores.
  • the through bore with the fresh sample is briefly opened into a further aperture leading by a conduit into the evacuated enclosure at a point remote from the bombardment zone so that the through bore is evacuated without significantly affecting the vacuum near the bombardment zone.
  • the present invention relates to improvements in devices used for sample analysis in processes in which the samples are placed under vacuum before being subjected to analysis, and particularly when analysis is to-be effected by fluorescence and/or direct X-ray emission techniques, the said samples being placed, at least at the actual moment at which analysis is effected, in an enclosure in which there is a particularly high vacuum, i.e., ofthe order of mm. Hg.
  • an electron emission device for emitting electrons into the enclosure and ensuring that their energy is sufficient to cause the appearance of a secondary X-ray on a sample struck by the electrons
  • a rotary support on which are mounted one or more assemblies, each composed of a cover, a sample and a sample support, each cover being secured in a sealed manner to the support which is able to slide, also in a sealed manner, on the outer wall of the enclosure, owing to the provision of a suitable packing which is preferably integral with the support, the latter being able to assume positions relative to the aperture such that each sample support may be located in turn in a sealed manner opposite the aperture and the sample is subjected in this position to electronic bombardment,
  • the assemblies were three in number and were located in recesses in the rotary support at an angle of 120 relative to one another about the axis of rotation of the support. Each sample is moved into three successive positions:
  • a working position in which the recess is located in front of the aperture provided in the enclosure and analysis may be carried out, radiation reaching the sample through the aperture.
  • This device operates satisfactorily, particularly because of the design of the seal which is an important feature thereof.
  • the present invention relates to improvements in the device described above which make it possible on the one hand to simplify the apparatus by reducing the number of diffusion pumps to one while on the other hand substantially reducing the minimum time required to obtain the results of a sample analysis.
  • the invention accordingly consist in a device for sample analysis, wherein the device comprises:
  • a device for emitting X-rays and both X-rays and/or electrons are herein defined as electronic energy into the enclosure and ensuring that the energy is sufficient to cause the appearance of secondary X-rays to be emitted from a sample struck by the electronic energy
  • a first aperture provided in the enclosure to allow passage of the X-rays and electrons directed on to the sample
  • a second aperture provided in the enclosure and connected, at the inside of the enclosure, to one end of a conduit, the other end of which is open and is located in the enclosure at a point sufficiently distant from the X-ray and electron emitter and sufficiently near the vacuum-producing device for any fluctuation in vacuum occurring at the other end to be practically eliminated by the vacuum-producing device before it can spread to the vicinity of the X-ray and electron emitter,
  • a support on which are mounted two assemblies each composed of a cover and a sample support, each assembly being integral with the support, while the cover is secured in a sealed manner to the support, the sample holder and any sample thereon being then located at the enclosure side of a hole which extends right through the support which is able to slide in a sealed manner on the outer wall of the enclosure, the support being able to assume fixed positions relatively to the two apertures provided in the wall such that each hole is located in front of the second and then in front of the first aperture, the support and its seal being large enough to close the two apertures in a sealed manner when no hole is located in front of the apertures,
  • a third aperture provided in the wall. of the enclosure or in the extension thereof, to which, on the enclosure side, there is connected in a sealed manner a passage connected to a vacuum-producing device able to produce at least a 10" mm. Hg. vacuum, and to a device for producing atmospheric pressure, the support also being able to slide in a sealed manner on the wall or extension thereof, so that each hole may be brought opposite the third aperture.
  • thewall on which the support slides is flat, the support rotates and the two holes are located diametrically opposite each other in the support and equidistant from the axis of rotation, the first and third apertures being located so that each of the two holes may be located successively opposite the first one and then the other aperture when the support moves l about its axis of rotation, while the second aperture is arranged so as to be opposite either of the holes for a brief period during the time when the hole moves from its position opposite the third aperture to that opposite the first aperture.
  • FIG. 1 is a diagrammatic sectional view of the device
  • F108, 2 and 3 show details of the device of HO. 1.
  • the device illustrated comprises an enclosure 1 in which a vacuum of 10 Torr (mm. Hg) is maintained by means of a high output diffusion pump 2.
  • This enclosure is closed near the top by a wall 3 which forms the base of a circular tray having three apertures 4, 5 and 6, the first two, 4 and 5, of which are located diametrically opposite one another while the third, 6 which is smaller, is located at to the first two relatively to the center of the wall 3 (see FIG. 3).
  • the seal between the turret and the wall is achieved by means of a special seal comprising two O-rings 11 and 12 coaxial with the axis 8 and connected together by six spokes positioned at an angle of 60 relative to one another and also constituting part of the seal which is solid with the turret 7.
  • Each of the bores 9 and 10 is closed at the outside by a sealed cover 13, 14 respectively, each cover being provided with a sample holder 36 and a sample 37 located in the corresponding bore.
  • the aperture 4 is connected in a sealed manner to a conduit 15 leading to a vane pump 16 through a valve 17.
  • the aperture 5 is located exactly opposite an X-ray tube 18, the outlet window of which has been removed, the tube 18 being mounted in the sidewall 19 of the enclosure 1, while the aperture 6 is connected at the enclosure side to a tube 20, the lower end 21 of which is substantially lower than the X-ray tube 18.
  • the diffusion pump 2 is provided with a screen 22 which may be adjusted from outside the enclosure by means of a lever 23.
  • the screen 22 rests in a sealed manner on a circular support 24 solid with the body of the pump.
  • a line 25 containing a valve 26 connects the vane pump 16 either to the enclosure or to the diffusion pump through a reservoir 27,
  • an air intake device 28 is located in the conduit 15 while a cooling jacket 29 (using freon) is connected to the diffusion pump.
  • An X-ray measuring device 30 mounted in the wall 19 essentially comprises, located within an auxiliary enclosure 31 in which the pressure is 5X 1 Torr, a collimator 33, a crystal 34 and a counter 35 suitably arranged.
  • the collimator 33 obturates completely and in an almost sealed manner the wall 32 common to the enclosure 1 and the enclosure 31.
  • the pressure of l0 Torr reigning in the enclosure 31 is obtained by means of the diffusion pump 2 which acts through the collimator 33, the difference in pressure being due to the loss in charge through the collimator.
  • the pump is then reconnected to the tank 27, the screen 22 is moved upwards by means of the lever 23, which is made possible by the balance of pressure on either side of the screen, and the diffusion pump 2 is operated so as to produce a vacuum of 10" Torr in the enclosures 1, including the X-ray tube, and a vacuum of 5X10" Torr in the enclosure 31.
  • the X-ray tube is then switched on as is the measuring device.
  • the turret 7 is loaded with a single sample 37 which is located in the bore 9 opening into the aperture 4 and supported by the cover 13. Once the vacuum in each of the enclosures has reached the value desired, the turret 7 carrying the sample to be analyzed is rotated through 180. At the moment at which the sample-which is then under a vacuum of 10 Torrpasses in front of the aperture 6, the effect of the low pressure in the enclosure 1 evacuates the small quantity of air which is in the recess instantaneously through the tube 20, essentially without disturbing the level of vacuum in the enclosure 1. Moreover, the low position of the aperture 21 of the tube 20 prevents any fluctuation in vacuum reaching the X- ray tube and disturbing its functioning.
  • the sample is then bombarded with electrons as it reaches its position in front of the aperture 5, without there being any fluctuations in the pressure within the enclosure.
  • the valve 17 is closed and the bore 10 brought to atmospheric pressure by means of the device 28, the pump 16 and the tank 27 being protected from the atmospheric pressure by closure of the valve 17.
  • the bore 10 is loaded with a sample 37, the valve 26 is closed temporarily and the recess again connected to the pump 16 so that the cycle can recommence.
  • the time necessary for the completion of a cycle of operations does not exceed 2 min. sec. and is often less than this.
  • the device which only needs one diffusion pump, makes it possible to insert an urgent" sample in a series of samples for analysis with particular rapidity and to effect its analysis by the fluorescence process in a very short time, since in the worst possible case there cannot be more than one sample to be analyzed which is already loaded on the turret 7, thus reducing to a minimum the waiting time required before the urgent sample can be inserted in the device and analyzed.
  • the intermediate seal which ensures the tight connection between the support and the enclosure may take a number of forms, but particularly advantageous use may be made of the seal described in US. Pat. No. 3,356,844 which allows the vacuum of IO Torr to be maintained in the enclosure, even when the turret is in motion, and ensures that there is no connection between the two bores provided in the turret.
  • this seal also enables it permanently to se arate from each other the second and third apertures (locate at 90 from each other) due to the presence of spokes located at 60 to each other, since there is always at least one spoke located between the two apertures and insulating them from each other.
  • An electronic energy sample analysis device comprising:
  • a first aperture provided in the enclosure to allow passage of the electronic energy directed on to a sample
  • a second aperture provided in the enclosure and connected, at the inside of the enclosure, to one end ofa conduit, the other end of which conduit is open and is located in the enclosure at a point intermediate the electronic energy means and the vacuum producing means so that any fluctuation in vacuum which occurs at said other end is essentially eliminated by the vacuum producing means before the fluctuation can spread to the electronic energy means,
  • a turret mounted in sealing engagement with the enclosure over said apertures and having two bores in it, each bore being capped by a cover and containing a sample support adapted to support a sample, the cover being secured in a sealed manner to the turret and the sample holder being located at the enclosure end of each bore which extends through the turret and which turret slides in a sealed manner on the enclosure, the turret further being able to assume fixed positions relatively to the two apertures such that the bores may be selectively located adjacent and placed in communication with said first and second apertures; and
  • a third aperture provided in the enclosure, a conduit having one end connected in a sealed manner to the enclosure side of the aperture, the other end being selectively engageable with a second vacuum producing means able to produce at least a 10 mm. Hg. vacuum and to atmospheric pressure, the turret also being slidable in a sealed manner so that each bore may also be selectively brought adjacent and placed in communication with the third aperture.
  • a device as claimed in claim 1, wherein said means for emitting electronic energy is an X-ray tube and the physical juxtaposition of said other end of the conduit intermediate said X-ray tube and said vacuum-producing means permits said vacuum-producing means to correct any fluctuation in vacuum before it can effect the functioning of said X-ray tube.

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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)
US760149A 1967-09-18 1968-09-17 An electronic energy sample analysis device Expired - Lifetime US3617738A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
LU54494 1967-09-18

Publications (1)

Publication Number Publication Date
US3617738A true US3617738A (en) 1971-11-02

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US760149A Expired - Lifetime US3617738A (en) 1967-09-18 1968-09-17 An electronic energy sample analysis device

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US (1) US3617738A (xx)
BE (1) BE720090A (xx)
CH (1) CH507516A (xx)
DE (1) DE1798251A1 (xx)
FR (1) FR1579962A (xx)
GB (1) GB1236049A (xx)
LU (1) LU54494A1 (xx)
NL (1) NL6813325A (xx)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3795808A (en) * 1971-05-18 1974-03-05 P Knights Electron microscopes

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2175667B1 (xx) * 1972-03-17 1974-08-02 Aquitaine Petrole

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3356844A (en) * 1963-07-02 1967-12-05 Centre Nat Rech Metall Rotatable sample changer for an electron probe microanalyzer having means for maintaining a vacuum in the analysis chamber
US3415987A (en) * 1964-09-28 1968-12-10 Petrales D Aquitaine Soc Nat D Specimen changer for an x-ray fluorescence spectrometer
US3440417A (en) * 1964-06-03 1969-04-22 Ass Elect Ind Vacuum lock sample insertion probe for a mass spectrometer

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3356844A (en) * 1963-07-02 1967-12-05 Centre Nat Rech Metall Rotatable sample changer for an electron probe microanalyzer having means for maintaining a vacuum in the analysis chamber
US3440417A (en) * 1964-06-03 1969-04-22 Ass Elect Ind Vacuum lock sample insertion probe for a mass spectrometer
US3415987A (en) * 1964-09-28 1968-12-10 Petrales D Aquitaine Soc Nat D Specimen changer for an x-ray fluorescence spectrometer

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3795808A (en) * 1971-05-18 1974-03-05 P Knights Electron microscopes

Also Published As

Publication number Publication date
CH507516A (fr) 1971-05-15
DE1798251A1 (de) 1972-02-10
FR1579962A (xx) 1969-08-29
GB1236049A (en) 1971-06-16
NL6813325A (xx) 1969-03-20
LU54494A1 (xx) 1969-06-24
BE720090A (xx) 1969-02-03

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