US3852594A - X-ray diffraction apparatus - Google Patents

X-ray diffraction apparatus Download PDF

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Publication number
US3852594A
US3852594A US00382481A US38248173A US3852594A US 3852594 A US3852594 A US 3852594A US 00382481 A US00382481 A US 00382481A US 38248173 A US38248173 A US 38248173A US 3852594 A US3852594 A US 3852594A
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United States
Prior art keywords
specimen
slit
ray
ray diffraction
diffraction
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Expired - Lifetime
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US00382481A
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English (en)
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F Paolini
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Pepi Inc
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Pepi Inc
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Priority to US00382481A priority Critical patent/US3852594A/en
Priority to JP8404774A priority patent/JPS5328222B2/ja
Priority to CA205,335A priority patent/CA1016669A/en
Priority to GB3235674A priority patent/GB1473414A/en
Priority to AU71543/74A priority patent/AU493198B2/en
Application granted granted Critical
Publication of US3852594A publication Critical patent/US3852594A/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

Definitions

  • the specimen being investigated is rotated about an axis lying in its upper flat surface, to cause the X-raybeam to impinge upon the specimen at various angles, the rotation being so that the angle (0) between the specimen surface and a line drawn from the X-ray source to the center of the irradiated portion thereof ranges between 0 and 90.
  • the divergence slit remains stationary, so that, because of the rotation of the specimen with respect to the divergence slit and as a result of geometric considerations, the area of the specimen irradiated by the X-ray beam varies between a relatively small amount when the value of 6 is high (e .g 80) and arelatively large amount when the value of 6 is low (e.g., l0).
  • Such variation of the irradiate area is highly undesirable because of numerous adverse effects on the accuracy and reliability of the analysis.
  • the prior art has resorted to using, during each diffraction analysis, stationary divergence slits of various fixed sizes, with larger slit openings being employed for large 0 values and smaller slit openings being employed for smaller 6 values, thereby tending toequalize the irradiated area of the specimen as it is rotated over the range of 6 values.
  • the present invention overcomes, the above shortcomings by providing an apparatus permitting the rotation of the divergence slit in conjuction with the rotation of the X-ray irradiated specimen, whereby the dimensions of the X-ray irradiated portion of the specimen remain substantially constant during the rotation of the specimen.
  • the divergence slit is connected to a structural'element linked with a second structural element connected to the specimen such that the divergence slit rotates at a lower angular speed than the specimen such that the X-radiation is cut off from the specimen when the 0 value reaches zero.
  • FIG. 1 is a schematic representation of a prior art X-ray diffraction apparatus. 7
  • FIG. 2 is an isometric view of the X-ray diffraction apparatus of thepresent invention.
  • FIG. 3 is a schematic representation depicting a feature of the present invention.
  • FIG. 4 is a fragmentary sectional elevation view of a diffraction slit of the type employed in the present invention.
  • FIG. 5 is a number of curves depicting results obtained with the present invention.
  • FIG. 1 depicts the situation in the prior art where the X-ray diffraction specimen 10 is rotated with respect to a stationary divergencejslit 11 through which there passes X-radiation 12 from a source 13.
  • the specimen 10 is acutely disposed (i.e., 0,, is less than to an imaginary line 14 extending between the X-ray source and the center of the irradiated portion of the specimen, the portion of the specimen impinged by the X-radiation has a dimension S whereas the impinged portion dimension S .when when 0,, equals 90 (shown in broken lines) is substantially less than S
  • Such deviations in the dimensions of the X-radiation impinged portion of the specimen are unsatisfactory, as mentioned above.
  • FIG. 2 depicts a portion of the X-ray diffraction apparatus 20 in accordance with the present invention, containing and X-ray line source 22, as so-called Soller slit assembly 24, a rotatable divergence slit 25 mounted via a shaft to a cog wheel 26, a specimen holder 27 connected to a second cog wheel 28, the X-ray diffraction analysis specimen 29 which is mounted on the holder 27, the second cog wheel 28 being driven by'a drive shaft 30 whose rotatio'ii speed is co-ordinated with the rotation speed of the goiiiometer'(not shown) used with the diffraction apparatus, a mechanical linking means 31 (i.e., cog belt) linking the 'cog wheels 26 and 28, and a receiving slit 32, a Soller slit 33 and an anti-scatter slit 34 all (i.e., 32, 33, and 34) located between the specimen and the detector 35.
  • Soller slit assembly 24 a rot
  • the divergence slit'cog wheel 26 include a number of teeth greater than that of the specimen cog wheel 28 (i.e., a slit cog to specimen cog tooth ratio greater than 1) so that the former rotates at a lower angular speed (i.e., provides a smaller corresponding angular displacement) than the former, it being especially preferred that the tooth ratios of these cog wheels be adjusted such that the beam be cut off from the specimen upon the 6 value reaching zero degrees and that the slit plane and the irradiated specimen surface be substantially parallel when 6 is 90.
  • the divergence slit cog where is the angular displacement of the specimen cog wheel 28 and 6,, is the initial angular displacement of the slit cog wheel 26 with respect to specimen cog wheel 28 (i.e., the initial angular disposition of the slit with respect to the specimen irradiated surface).
  • the diffraction slits having a finite thickness, the beam is cut off from the specimen before 6 reaches zero, so that the geometry ofthe diffraction slit should be considered in order that X-ray beam extinction occur (i.e., the beam is cut off from the specimen), under optimal conditions, when 6 equals exactly 0.
  • the length (S) of the X-ray irradiated portion of the specimen increases rapidly as 6 approaches zero. whereas a value of 6 less than 6 results in a decrease of the irradiated portion lengths as 6 approaches zero.
  • the latter situation i.e., 9 e results in premature extinction. in that the irradiated portion length is zero at some 0 value greater than zero.
  • Y it is further optimal that 0' 90 when 0 90, so that there is achieved an irradiated specimen portion of. maximum length for values of 6 approaching 90.
  • Equation 6 establishes the condition that must be met by numbers N and N of cog wheel teeth. N and N must also, of course, be integers. In practice, one picks values that most'closely satisfy Equation 6.
  • EXAMPLE 1 Using a diffraction slit having a cylindrical slitdefining body with a radius r of 0.60 mm, a body thickness t of 1.20 mm, and a slit opening width w of 5.00 mm, the value k of the diffraction slit is 3.10 mm and the extinctionan gle, e, is determined from Equation 3 to be 11 l0.-Therefore, when 6 0, 0,, should optimally be 11 l0 and, as a second optimal condition, when 6 90, 6 should also be 90. From Equation 6, the cog tooth number ratio, N/N' for the specimen and slit cog wheels should be about 79:90 for maintaining an irradiated specimen portion of substantially constant dimensions, this being done automatically during the specimen rotation. i I
  • the length, S, of the irradiated portion of the specimen was calculated for 0 valves over the range of 0 to the resulting S values being shown as Curve l in FIG. 5. In this situation 0 equals 90 when 6 is 90.
  • the length S of the irradiated portion of the specimen was calculated for 0 values over the range of 0 to 90, the resulting S values being shown by Curve ll in FIG. 5.
  • the significant improvement provided by setting 0,, at exactly the value of e is seen from the comparison of these curves, the length, S, of the irradiated portion in Curve ll not exhibiting the relatively sharp drop for the S value for very low 6 values i.e., about 6 5.
  • the S value was calculated over the range of 6 0 to- 0 90, the results being depicted as Curve ill in FIG. 5.
  • the present invention permits achieving an irradiated specimen portion of substantially constant dimensions over the rotation range for analyzed specimen. While setting 0,, at exactly eleads to a deviation of 0 from 90 when 6 equals 90, it is felt to be more preferable to set 6., at exactly the value of the extinction angle,,e, notwithstanding the fact that 6' will not equal 6 at 6 90, in order to avoid the drop in S values about 0 equals 5 and less.
  • An X-ray diffraction apparatus comprising:
  • c. means for rotating said specimen at a first angular velocity from a first position to a second position
  • a diffraction slit disposed between said specimen and said source such that said X-rays pass throug the opening of said slit;
  • An'X-ray diffraction apparatus as defined in claim 1, wherein at said first position said position is substantially perpendicular to an imaginary line extending from said X-ray source to the center of said portion and said second position said portion is substantially parallel to said imaginary lines and said diffraction slit is rotated between third and fourth positions, said diffraction on slit at said third position being substantially parallel to said specimen at said third position being substantially parallel to said specimen at said first position and at said fourth position being obliquely disposed to said specimen at said second position.
  • N and N are the teeth numbers for said first and second gear wheels, respectively;
  • 0 is the angular displacement of said first gear wheel
  • 1 e is the angular orientation of said second gear wheel when said beam iscut off from said specimen located at said second position.
  • a method of operating an X-ray diffraction apparatus comprising the steps of: r

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth 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)
US00382481A 1973-07-25 1973-07-25 X-ray diffraction apparatus Expired - Lifetime US3852594A (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
US00382481A US3852594A (en) 1973-07-25 1973-07-25 X-ray diffraction apparatus
JP8404774A JPS5328222B2 (enrdf_load_stackoverflow) 1973-07-25 1974-07-22
CA205,335A CA1016669A (en) 1973-07-25 1974-07-22 X-ray diffraction apparatus
GB3235674A GB1473414A (en) 1973-07-25 1974-07-22 X-ray diffraction apparatus
AU71543/74A AU493198B2 (en) 1973-07-25 1974-07-23 Xray diffraction apparatus

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Application Number Priority Date Filing Date Title
US00382481A US3852594A (en) 1973-07-25 1973-07-25 X-ray diffraction apparatus

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US3852594A true US3852594A (en) 1974-12-03

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JP (1) JPS5328222B2 (enrdf_load_stackoverflow)
CA (1) CA1016669A (enrdf_load_stackoverflow)
GB (1) GB1473414A (enrdf_load_stackoverflow)

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3000122A1 (de) * 1979-01-05 1980-07-24 Philips Corp Beugungsstrahlmonochromator
DE2907160A1 (de) * 1979-02-23 1980-09-04 Siemens Ag Roentgen-pulverdiffraktometer
US4223219A (en) * 1977-10-28 1980-09-16 Eberhard Born Method of and apparatus for producing texture topograms
US4278883A (en) * 1979-12-27 1981-07-14 The United States Of America As Represented By The Secretary Of The Interior Sample mount for X-ray diffraction
US4322618A (en) * 1979-01-05 1982-03-30 North American Philips Corporation Diffracted beam monochromator
EP0091150A1 (en) * 1982-03-31 1983-10-12 Koninklijke Philips Electronics N.V. X-ray analysis apparatus having an adjustable stray radiation slit
EP0115891A1 (en) * 1983-02-04 1984-08-15 Koninklijke Philips Electronics N.V. X-ray analysis apparatus
EP0143495A3 (en) * 1983-11-22 1985-07-03 N.V. Philips' Gloeilampenfabrieken X-ray analysis apparatus comprising a deflection system
US4691334A (en) * 1983-10-12 1987-09-01 U.S. Philips Corporation X-ray examination apparatus
US4696024A (en) * 1984-10-27 1987-09-22 Mtu Motoren- Und Turbinen-Union Muenchen Gmbh Method and apparatus for detecting flaws in single crystal test samples
US5008909A (en) * 1990-02-07 1991-04-16 The United States Of America As Represented By The Department Of Energy Diffractometer data collecting method and apparatus
US5115460A (en) * 1989-12-12 1992-05-19 U.S. Philips Corp. X-ray analysis apparatus comprising an adjustable slit diaphragm
WO1997025614A1 (en) * 1996-01-12 1997-07-17 Philips Electronics N.V. X-ray analysis apparatus including a rotatable primary collimator
US20040170250A1 (en) * 2003-02-28 2004-09-02 Osmic, Inc. X-ray optical system with adjustable convergence
US20040228440A1 (en) * 2003-05-14 2004-11-18 Bruker Axs Gmbh X-ray diffractometer for high flux grazing incidence diffraction
US20060023842A1 (en) * 2004-07-28 2006-02-02 General Electric Company Single-leaf X-ray collimator
US20080031416A1 (en) * 2006-08-01 2008-02-07 Rigaku Corporation X-ray diffraction apparatus
US20080084964A1 (en) * 2006-10-06 2008-04-10 Rigaku Corporation X-Ray Diffraction Measurement Method and X-Ray Diffraction Apparatus
USRE44870E1 (en) 1994-01-14 2014-04-29 Sandvik Intellectual Property Ab Aluminum oxide coated cutting tool and method of manufacturing thereof
EP3719484A1 (en) * 2019-04-04 2020-10-07 Malvern Panalytical B.V. X-ray beam shaping apparatus and method
US11808721B2 (en) 2021-01-29 2023-11-07 Rigaku Corporation X-ray analysis apparatus

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6163370U (enrdf_load_stackoverflow) * 1984-09-28 1986-04-30

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2870337A (en) * 1954-04-09 1959-01-20 Siemens Reiniger Werke Ag X-ray diffraction system
US2993993A (en) * 1958-06-19 1961-07-25 Tesla Np Diaphragm for limiting the field of view of three-stage electron microscopes
US3124681A (en) * 1964-03-10 Zingaro
US3361909A (en) * 1964-05-23 1968-01-02 Chirana Praha X-ray diffraction goniometer with specific drive mechanism for the specimen holder and detector
US3411000A (en) * 1965-04-14 1968-11-12 Siemens Ag X-ray diffractometer diaphragm which is synchronously rotated with the specimen
US3566111A (en) * 1967-06-19 1971-02-23 Siemens Ag Apparatus for varying the detector slit width in fully focusing x-ray spectrometers

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1497531A1 (de) * 1965-07-22 1969-03-27 Jeol Ltd Goniometer

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3124681A (en) * 1964-03-10 Zingaro
US2870337A (en) * 1954-04-09 1959-01-20 Siemens Reiniger Werke Ag X-ray diffraction system
US2993993A (en) * 1958-06-19 1961-07-25 Tesla Np Diaphragm for limiting the field of view of three-stage electron microscopes
US3361909A (en) * 1964-05-23 1968-01-02 Chirana Praha X-ray diffraction goniometer with specific drive mechanism for the specimen holder and detector
US3411000A (en) * 1965-04-14 1968-11-12 Siemens Ag X-ray diffractometer diaphragm which is synchronously rotated with the specimen
US3566111A (en) * 1967-06-19 1971-02-23 Siemens Ag Apparatus for varying the detector slit width in fully focusing x-ray spectrometers

Cited By (31)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4223219A (en) * 1977-10-28 1980-09-16 Eberhard Born Method of and apparatus for producing texture topograms
US4322618A (en) * 1979-01-05 1982-03-30 North American Philips Corporation Diffracted beam monochromator
DE3000122A1 (de) * 1979-01-05 1980-07-24 Philips Corp Beugungsstrahlmonochromator
DE2907160A1 (de) * 1979-02-23 1980-09-04 Siemens Ag Roentgen-pulverdiffraktometer
US4278883A (en) * 1979-12-27 1981-07-14 The United States Of America As Represented By The Secretary Of The Interior Sample mount for X-ray diffraction
US4535469A (en) * 1982-03-31 1985-08-13 U.S. Philips Corporation X-Ray analysis apparatus having an adjustable stray radiation slit
EP0091150A1 (en) * 1982-03-31 1983-10-12 Koninklijke Philips Electronics N.V. X-ray analysis apparatus having an adjustable stray radiation slit
EP0115891A1 (en) * 1983-02-04 1984-08-15 Koninklijke Philips Electronics N.V. X-ray analysis apparatus
US4800580A (en) * 1983-02-04 1989-01-24 U.S. Philips Corporation X-ray analysis apparatus
US4691334A (en) * 1983-10-12 1987-09-01 U.S. Philips Corporation X-ray examination apparatus
EP0143495A3 (en) * 1983-11-22 1985-07-03 N.V. Philips' Gloeilampenfabrieken X-ray analysis apparatus comprising a deflection system
AU572917B2 (en) * 1983-11-22 1988-05-19 N.V. Philips Gloeilampenfabrieken Charged particle deflection system for x-ray analysis
US4696024A (en) * 1984-10-27 1987-09-22 Mtu Motoren- Und Turbinen-Union Muenchen Gmbh Method and apparatus for detecting flaws in single crystal test samples
US5115460A (en) * 1989-12-12 1992-05-19 U.S. Philips Corp. X-ray analysis apparatus comprising an adjustable slit diaphragm
US5008909A (en) * 1990-02-07 1991-04-16 The United States Of America As Represented By The Department Of Energy Diffractometer data collecting method and apparatus
USRE44870E1 (en) 1994-01-14 2014-04-29 Sandvik Intellectual Property Ab Aluminum oxide coated cutting tool and method of manufacturing thereof
WO1997025614A1 (en) * 1996-01-12 1997-07-17 Philips Electronics N.V. X-ray analysis apparatus including a rotatable primary collimator
US20040170250A1 (en) * 2003-02-28 2004-09-02 Osmic, Inc. X-ray optical system with adjustable convergence
US7245699B2 (en) 2003-02-28 2007-07-17 Osmic, Inc. X-ray optical system with adjustable convergence
US20040228440A1 (en) * 2003-05-14 2004-11-18 Bruker Axs Gmbh X-ray diffractometer for high flux grazing incidence diffraction
US7085349B2 (en) * 2003-05-14 2006-08-01 Bruker Axs Gmbh X-ray diffractometer for high flux grazing incidence diffraction
US20060023842A1 (en) * 2004-07-28 2006-02-02 General Electric Company Single-leaf X-ray collimator
US7310410B2 (en) * 2004-07-28 2007-12-18 General Electric Co. Single-leaf X-ray collimator
US20080031416A1 (en) * 2006-08-01 2008-02-07 Rigaku Corporation X-ray diffraction apparatus
US7471766B2 (en) 2006-08-01 2008-12-30 Rigaku Corporation X-ray diffraction apparatus
US20080084964A1 (en) * 2006-10-06 2008-04-10 Rigaku Corporation X-Ray Diffraction Measurement Method and X-Ray Diffraction Apparatus
US7443952B2 (en) 2006-10-06 2008-10-28 Rigaku Corporation X-ray diffraction measurement method and X-ray diffraction apparatus
EP3719484A1 (en) * 2019-04-04 2020-10-07 Malvern Panalytical B.V. X-ray beam shaping apparatus and method
WO2020201565A1 (en) * 2019-04-04 2020-10-08 Malvern Panalytical B.V. X-ray beam shaping apparatus and method
US12007343B2 (en) 2019-04-04 2024-06-11 Malvern Panalytical B.V. X-ray beam shaping apparatus and method
US11808721B2 (en) 2021-01-29 2023-11-07 Rigaku Corporation X-ray analysis apparatus

Also Published As

Publication number Publication date
JPS5063982A (enrdf_load_stackoverflow) 1975-05-30
JPS5328222B2 (enrdf_load_stackoverflow) 1978-08-12
CA1016669A (en) 1977-08-30
AU7154374A (en) 1976-01-29
GB1473414A (en) 1977-05-11

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