US3394255A - Diffraction mechanism in which a monochromator diffracts the X-ray beam in planes transverse to an axis of specimen rotation - Google Patents

Diffraction mechanism in which a monochromator diffracts the X-ray beam in planes transverse to an axis of specimen rotation Download PDF

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Publication number
US3394255A
US3394255A US467214A US46721465A US3394255A US 3394255 A US3394255 A US 3394255A US 467214 A US467214 A US 467214A US 46721465 A US46721465 A US 46721465A US 3394255 A US3394255 A US 3394255A
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United States
Prior art keywords
specimen
axis
monochromator
theta
ray
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US467214A
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Jr Thomas C Furnas
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Philips Nuclear Medicine Inc
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Picker Corp
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Priority to US467214A priority Critical patent/US3394255A/en
Priority to NL6604700A priority patent/NL6604700A/xx
Priority to DE19661598924 priority patent/DE1598924B2/de
Priority to GB29010/66A priority patent/GB1139434A/en
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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
    • G01N23/20—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
    • G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
    • G01N23/2076—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions for spectrometry, i.e. using an analysing crystal, e.g. for measuring X-ray fluorescence spectrum of a sample with wavelength-dispersion, i.e. WDXFS
    • 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
    • G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions

Definitions

  • Each characteristic X-ray wavelength is diffracted a different and characteristic amount than other wavelengths such that the beam is separated into planes of radiation each of one characteristic wavelength.
  • the planes are transverse to an axis of specimen rotation.
  • the disclosure also includes a method of conducting X-ray diffraction studies with the X-ray planes so diffracted.
  • This invention relates to X-ray diffraction and more particularly to a novel and improved process and apparatus utilizing monochromator crystals for conducting X- ray diffraction studies.
  • X-ray diffraction In X-ray diffraction, it is customary to position a specimen for rotation about an axis known as the theta or the omega axis, and to rotate the specimen through an angle known alternately as theta or omega. As the specimen is rotated, it is irradiated with a beam of X-rays which is diffracted by the specimen. Customarily as the specimen is rotated through an angle theta the rays diffracted by the specimen are detected and then suitably recorded.
  • the clilfracting planes of the monochromator are parallel to the ditfracting planes of the specimen. (Actually 6 0 where O is the diffraction angle at the monochromator and a the diffraction angle at the specimen.) Strict parallelism is achieved when the diffraction angles of the crystal and monochromator are equal. When this is true then all the wave lengths diffracted from the monochromator are simultaneously diffracted from the specimen. Thus, the spectrum dispersed by the monochromator is recombined by reflection from specimen planes in the parallel (1, position.
  • the angular Width of the reflection measured by rotation of the specimen about two-theta or omega axis generally is called the instrument width as it somewhat characterizes (a) the sizes of apertures; (b) the mosaicity of the monochromator and of the specimen; (c) the net angular convergence of X-rays upon the specimen; and, (d) the ability of the specimen to diffract X-rays.
  • the Lorentz, polarization and dispersion correction for a particular reflection whether it is observed in the positive or negative twotheta region are the same.
  • this invention is also beneficial. This is true because the specimen will diffract in a manner which permits many stationary studies to be 4 conducted where in the past specimen rotation has been required.
  • the spectral dispersion of the monochromator is parallel to the omega, theta axis and, therefore, perpendicular to the plane of rotation about the coincident omega, theta axis.
  • plane perpendicular (l, P) is proposed to describe the use of a plane grating, plane reflection crystal or a plane transmission crystal as the monochromator oriented with its dispersion perpendicular to the specimen rotation axis or specimen dispersion.
  • the primary source of X-radiation is positioned to one side of the monochromator away from the specimen.
  • the primary source is above or below the monochromator when the omega, theta axis is vertical.
  • the rays are directed at the monochromator at an angle such that a diffracted beam of a selected wave length is directed to the specimen.
  • FIGURE 1 is a perspective view of a diffractometcr made in accordance with this invention.
  • FIGURE 2 is an elevational view, on an enlarged scale with respect to FIGURE 1, of the novel tube and monochromator crystal support mechanism of this invention with parts broken away and removed;
  • FIGURE 4 is a top plan view of the structure and scale of FIGURE 2;
  • FIGURE 5 is an end elevational view of the structure and scale of FIGURE 2 as seen from the plane indicated by the line 5-5 of FIGURE 2;
  • FIGURE 6 is a sectional view, on an enlarged scale With respect to FIGURE 2, of the crystal support, as seen from the plane indicated by the line 66 of FIG- URE 2.
  • a diffractometer is shown generally at 10.
  • the diffractometer It is preferably of the type described and claimed in copending application Ser. No. 236,468, filed Nov. 2, 1962, which is now United States Patent 3,218,458 issued Nov. 16, 196 5, T. C. Furnas, Jr. and entitled Diffractometer.
  • the diffractometer includes a housing 11.
  • a two-theta member 12 is journaled in the housing 11 for rotation about a theta axis. Assuming the housing 11 is horizontal, the theta axis is a vertical axis which intersects the specimen, as will become more apparent from the subsequent description.
  • a two-theta arm 13 is secured to the two theta member 12.
  • the two-theta arm 13 supports the usual detector 15 and slit structure 16.
  • a cone-like collimator structure 17 is also secured to the two-theta arm 13 for collimating rays diffracted by a specimen before they pass through the slit 16 into a detector 15.
  • a goniometer is shown generally at 20.
  • the goniometer pictured is one of the type described and claimed in detail in US. Patent 3,189,741 issued June 15, 1965 to George V. Patser under the title Goniostat.
  • the goniostat 20 is mounted on a theta member 21 for rotation about the omega, theta axes.
  • the goniostat 20 includes a phi head 22 which supports a'specimen S at a position along the omega, theta axes.
  • the specimen S is also located on a chi axis which is the horizontal axis of the goniostat 20 when the housingll is horizontal.
  • the phi head 22 is orbital about the chi axis and equipped to selectively rotate the specimen S about a phi axis.
  • the chi axis is perpendicular to and intersects the omega, theta axes at the point where the specimen is rotated.
  • the phi axis intersects these axes at the same point and is also perpendicular to the chi axis.
  • a phi axis may'be any radius of the goniostat perpendicular to the chi axis.
  • An eye piece 23 is secured to the goniostat 20 and positioned for use in locating the specimen S precisely at the intersection of these axes.
  • a pair of X-ray tube support pedestals 25, 26 are fixed to the housing 11.
  • An X-ray tube and monochromator assembly is shown generally at 30.
  • the assembly 30 is secured to the pedestals 25, 26 as by bolts 31.
  • the assembly 30 will be best understood by reference to FIGURES 2-6.
  • the assembly 30 includes a base 32 which is the element of the assembly that is fixed to the pedestals 25, 26 by the bolts 31.
  • the base 32 includes an upstanding arm 33 which is at the right hand end of the base as viewed in FIGURE 2.
  • the upstanding arm 33 extends longitudinally of the base 32 and provides a support for monochromator and X-ray tube pivots as will become apparent presently.
  • the base includes a second upstanding arm 34 which is at the left hand end of the base as viewed in FIGURE 2.
  • the second upstanding arm 34 is transverse with respect to the base 32 and supports the mechanism for causing adjustment pivoting the X-ray tube about a crystal axis as will also become more apparent presently.
  • a rigid pivot support arm 35 is secured to the base arm 33 extending upward from the base and outward toward the goniostat 20.
  • a stepped crystal and tube Support shaft is provided at 37.
  • the crystal and tube support shaft 37 is rotatably supported in the pivot arm 35 by small and large bearings 38, 40.
  • a Washer 41 is clamped against one race of the small bearing 38 by a nut 42 Which threads on one end of the shaft 37.
  • the support shaft,37 includes an enlarged part 43 which engages a race of the large bearing so that the bearings 3840 serve not only to journal the support shaft 37 but also as thrust bearings to locate it axially.
  • An X-ray tube support member 45 is provided.
  • the support member 45 extends longitudinally with respect to the base 32.
  • the support member 45 includes an upstanding pivot arm 46 at its right hand end as seen in FIGURE 2.
  • the pivot arm 46 is journaled by a bearing 47 on an end portion 48 of the support shaft 37.
  • the end portion 48 is at the right hand end as seen in FIG- URE 2.
  • An examination of FIGURE 2 will show that the tube support base 45 is pivotal about the axis of the support shaft 37.
  • the mechanism for adjusting the tube support base 45 about the axis of the support shaft 37 will be described below.
  • An X-ray tube housing 50 is shown in solid lines in FIGURES 1 and 3 and indicated in phantom in FIG- URES 2, 4, and 5.
  • the X-ray tube housing 50 includes a focal spot end portion 51 of reduced size.
  • the end portion 21 is square in cross section and houses the X-ray tube target.
  • the target is indicated in dotted lines at 53 in FIGURE 2.
  • a spherical bearing support assembly is shown gen erally at 54.
  • This sup-port assembly 54 secures the focal spot end portion 51 of the X-ray tube housing 50 to the X-ray tube base 45.
  • the spherical bearing support assembly 54 is of the type described in detail in the above-referenced copending application for a diffractometer. As an examination of FIGURE 3 Will show, the spherical bearing shown in dotted lines at 55 is immediately below the focal spot of the target 53.
  • FIGURES 1 and 2 A knurled head 57 of a take-off angle adjustment screw is visible in FIGURES 1 and 2. A portion of the adjustment screw is visible at 58 in FIGURE 1.
  • the take-off angle adjustment is of the type described in the abovereferenced patent application.
  • the adjustment screw 58 threadably engages the X-ray tube housing 50 to shift it transversely with respect to the base 45 and adjust the take-off angle about the axis of the spherical bearing 55.
  • a pivot adjustment arm 60 extends upwardly from and forms one end of the X-ray tube support bracket '45.
  • the pivot adjustment arm 60 is at the left hand end of the bracket 45 as viewed in FIGURES 2 and 4.
  • An arcuately curved pivot control shoe 61 is secured to the upstanding arm 60 as by bolts 63.
  • An arcuately curved lower surface 64 of the shoe 61 rides on a pair of rollers 65 secured to the base arm 34.
  • a hold-down roller 66, FIG- URES 2 and 4 rides on an upper arcuate surface 67 of the shoe 61.
  • the hold-down roller 66 is also secured to the arm 34. Coaction of the rollers 65, 66 with the shoe 31 causes any relative movement to be along an arcuate path.
  • a worm gear 70 is secured to the arm 60 and the shoe 61 by the bolts 63.
  • a worm 71 engages the worm gear 70 such that rotation of the worm 71 will cause arcuate movement of the worm gear 70 and the connected mechanism.
  • rotation of the worm 70' will cause rotation of the X-ray tube about the axis of the support shaft 37.
  • An odometer 72 is secured to the base 32 and connected to the worm 71 by a worm shaft 73. Rotation of odometer handles 74 will cause rotation of the shaft 73 and thus pivotal adjustment movement of the X-ray tube about the axis of the support shaft 37.
  • the odometer is provided so that one can determine the amount of adjustment movement of the X-ray tube about the axis of the support shaft 37.
  • a semi-cylindrical segment 75 is cut out of the section 43 of the support shaft 37.
  • a monochromator crystal 76 is positioned in a recess 77 in the section 43 so that the monochromator crystal is disposed with its reflecting surface along the axis of the support shaft 37, and immediately below the segment 75.
  • the X-ray tube is preferably equipped with shutters of the type described and claimed in detail in US. Patent No. 3,113,214, issued to T. C. Furnas, In, on Dec. 3, 1963, under the title of Ditfractometer Shutter.
  • This shutter engages an insert 84 which defines the aperture 32 of the clip 81.
  • the clip 84 and the shutter together define an X-ray pervious passage which collimates and conducts the primary X-ray beam from the target 53 of X-ray tube to the monochromator crystal 76.
  • Rays diffracted by the monochromator crystal 76 pass through the aperture 83 0f the clip 8t) and into a collimating structure 85. These diffracted rays pass through the collimating structure 85 and are thence directed against the specimen S.
  • a disc 90 is secured to the end of the support shaft 37 opposite the washer 41.
  • An adjustment lever 91 is secured to the disc 9!
  • a spring 92 acts against the lever 9'1 forcing it into engagement with an adjustment set screw 93.
  • a specimen S is first mounted on the phi member 22.
  • the position of the specimen is adjusted until it is located on the cross hairs provided to the eye piece 23.
  • Manual adjustment of the phi, chi, omega, theta, and two-theta angles about their respective axes can be accomplished in the manner taught in the above-referenced patent and application until the specimen is precisely positioned for a desired study.
  • the X-ray tube is energized and the shutter opened.
  • the specimen S will be struck by substantially a single wave length of X-rays throughout its study and the specimen will be rotated appropriate amounts about the several axes.
  • the detector While the specimen is being rotated, the detector will be selectively rotated about the two-theta axis and, as noted in the introduction, always in the plane of a given and selected wave length of X-rays, due to the novel positioning of the monochromator crystal. It will be apparent that all but substantially Onewave length of X-rays pass either above or below both the specimen and the detector so that the specimen and detector are acted on by substantially a single wave length.
  • a detector for measuring rays diffracted by a specimen and mounted for positioning in a plurality of positions in a plane transverse to said axis.
  • the diffraction means is a monochromator crystal adjustable about an axis which is transverse and spaced from the previously mentioned axis and transverse to said beam.
  • specimen supporting means mounted on said omega member and including means to support a specimen at a location along said axis;
  • an X-ray tube assembly including a focal spot mounted on said housing and positioned with said crystal between the focal spot and said location;
  • said X-ray tube assembly including collimating means for delineating a beam of X-rays directed against said crystal whereby said crystal will diffract portions of said beam to said location.
  • the method of claim 10 including the step of adjusting a selected one of the X-ray source and crystal about an axis intersecting the crystal and transverse and spaced from the omega axis.
  • an X-ray tube and crystal assembly mounted on the pedestals and positioned to irradiate a specimen on the goniostat, said assembly comprising:
  • said pivot support shaft including a cutaway segmental portion defining a crystal opening
  • (b) means to collimate X-rays diffracted by said monochromator crystal and direct the collimated beam against the specimen.
  • said pivot shaft including a cutaway portion defining an opening
  • an X-ray diffraction means mounted in said opening in the path of a beam emanated by said X-ray tube and positioned to diffract X-rays toward said specimen.
  • first and second arcuately curved clips overlie one another and are mounted on said shaft support to close the perimeter of said opening, said clips respectively including a primary beam aperture in communication with an opening in the X-ray tube housing and a diffracted beam aperture positioned to conduct X-rays diffracted by said diffraction means toward said specimen.
  • said X-ray tube adjustment means includes a worm gear and a worm.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
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  • Spectroscopy & Molecular Physics (AREA)
  • Dispersion Chemistry (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
US467214A 1965-06-28 1965-06-28 Diffraction mechanism in which a monochromator diffracts the X-ray beam in planes transverse to an axis of specimen rotation Expired - Lifetime US3394255A (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US467214A US3394255A (en) 1965-06-28 1965-06-28 Diffraction mechanism in which a monochromator diffracts the X-ray beam in planes transverse to an axis of specimen rotation
NL6604700A NL6604700A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1965-06-28 1966-04-07
DE19661598924 DE1598924B2 (de) 1965-06-28 1966-06-24 Roentgenspektrometer
GB29010/66A GB1139434A (en) 1965-06-28 1966-06-28 Improvements relating to x-ray diffraction equipment

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US467214A US3394255A (en) 1965-06-28 1965-06-28 Diffraction mechanism in which a monochromator diffracts the X-ray beam in planes transverse to an axis of specimen rotation

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DE (1) DE1598924B2 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
GB (1) GB1139434A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
NL (1) NL6604700A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3631240A (en) * 1968-06-27 1971-12-28 Walter Hoppe Apparatus for holding and orienting a crystal in x-ray instruments measuring the microstructure thereof
US3714426A (en) * 1970-08-18 1973-01-30 Stoe & Cie Gmbh Method of x-ray analysis of crystal structure an x-ray goniometer for carrying out said method
US6285736B1 (en) * 1998-11-13 2001-09-04 Rigaku Corporation Method for X-ray micro-diffraction measurement and X-ray micro-diffraction apparatus
US6411676B1 (en) * 1998-04-28 2002-06-25 Nonius B.V. Method for determining parameters of a unit cell of a crystal structure using diffraction
US20140270090A1 (en) * 2013-03-15 2014-09-18 Proto Manufacturing Ltd. X-Ray Diffraction Apparatus And Method
CN111508633A (zh) * 2020-06-02 2020-08-07 中国计量科学研究院 单能x射线辐射装置

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2748501C3 (de) * 1977-10-28 1985-05-30 Born, Eberhard, Dr. Verfahren und Vorrichtung zur Erstellung von Texturtopogrammen

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3105901A (en) * 1959-03-30 1963-10-01 Philips Corp X-ray diffraction device with 360 rotatable specimen holder
US3213278A (en) * 1962-04-13 1965-10-19 Philips Corp X-ray spectrograph having plural detectors
US3322948A (en) * 1964-12-21 1967-05-30 Owens Illinois Inc X-ray diffraction goniometer wherein the specimen is stationary and the source and detector are movable

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3105901A (en) * 1959-03-30 1963-10-01 Philips Corp X-ray diffraction device with 360 rotatable specimen holder
US3213278A (en) * 1962-04-13 1965-10-19 Philips Corp X-ray spectrograph having plural detectors
US3322948A (en) * 1964-12-21 1967-05-30 Owens Illinois Inc X-ray diffraction goniometer wherein the specimen is stationary and the source and detector are movable

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3631240A (en) * 1968-06-27 1971-12-28 Walter Hoppe Apparatus for holding and orienting a crystal in x-ray instruments measuring the microstructure thereof
US3714426A (en) * 1970-08-18 1973-01-30 Stoe & Cie Gmbh Method of x-ray analysis of crystal structure an x-ray goniometer for carrying out said method
US6411676B1 (en) * 1998-04-28 2002-06-25 Nonius B.V. Method for determining parameters of a unit cell of a crystal structure using diffraction
US6285736B1 (en) * 1998-11-13 2001-09-04 Rigaku Corporation Method for X-ray micro-diffraction measurement and X-ray micro-diffraction apparatus
US20140270090A1 (en) * 2013-03-15 2014-09-18 Proto Manufacturing Ltd. X-Ray Diffraction Apparatus And Method
US9613728B2 (en) * 2013-03-15 2017-04-04 Proto Manufacturing Ltd. X-ray diffraction apparatus and method
CN111508633A (zh) * 2020-06-02 2020-08-07 中国计量科学研究院 单能x射线辐射装置
CN111508633B (zh) * 2020-06-02 2022-04-22 中国计量科学研究院 单能x射线辐射装置

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Publication number Publication date
DE1598924A1 (de) 1970-09-03
NL6604700A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1966-12-29
DE1598924B2 (de) 1971-11-25
GB1139434A (en) 1969-01-08

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