CN103411986A - Thin-film diffraction instrument - Google Patents

Thin-film diffraction instrument Download PDF

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CN103411986A
CN103411986A CN2013103181080A CN201310318108A CN103411986A CN 103411986 A CN103411986 A CN 103411986A CN 2013103181080 A CN2013103181080 A CN 2013103181080A CN 201310318108 A CN201310318108 A CN 201310318108A CN 103411986 A CN103411986 A CN 103411986A
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film
ray
annex
thin
ray tube
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CN2013103181080A
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李玉德
王丽丽
刘世岗
郭非
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Beijing Normal University
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Beijing Normal University
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Abstract

The invention discloses a thin-film diffraction instrument which is used for analyzing and testing a thin-film material. The thin-film diffraction instrument comprises an X-ray tube used for supplying a line source, a thin-film accessory used for receiving and irradiating X-ray emitted by the X-ray tube, and a detector used for receiving and testing X-rays diffracted by tested thin-film material, wherein the thin-film accessory is formed by overlapping a plurality of cylindrical capillary tubes in a row, and in the cross section of the thin-film accessory, the centers of all the capillary tubes are on the same straight line. According to the invention, the light intensity of X-rays irradiated on the thin-film material is enhanced, so that the detector can analyze and test the thin-film material advantageously.

Description

A kind of film diffractometer
Technical field
The present invention relates to X ray determination techniques field, relate in particular to a kind of film diffractometer.
Background technology
Membraneous material has a wide range of applications in the modern science and technology field, and the X-ray diffraction technology is a kind of analytical test means of important membraneous material, and the development of membraneous material has been played to huge impetus.
At present, the widely used X-ray diffraction technology of analytical test membraneous material mainly comprises for the X ray lens diffractive technology of pointolite with for the parallel X-ray diffractive technology of line source.X ray lens diffractive technology is the X-ray of dispersing that utilizes X ray lens bleeding point light source to send, and the X-ray beam that will disperse becomes parallel X-ray beam, then shines on tested membraneous material.In research and production, what range of application was the widest is the parallel X-ray diffractive technology for line source, as shown in Figure 1, the X ray that line source 101 is launched is after rope draws slit 102 and divergent slit 103, shine tested membraneous material 104, after tested membraneous material 104 diffraction, then pass through anti-scatter slit 105 and film annex 106, finally be detected device 107 and receive and carry out analytical test.Wherein, divergent slit 103 and anti-scatter slit 105 are be used to keeping off parasitic light; Film annex 106 consists of a plurality of sheet metals, spacing between sheet metal peso draws slit 102 little, be used for X ray restriction in the horizontal direction, X ray becomes the X-ray beam that horizontal direction divergence is 0.1 to 0.2 degree after film annex 106, finally by detector 107, is received.
Yet the X-ray beam divergence in the horizontal direction that requires detector 107 to receive due to the parallel X-ray diffractive technology for line source is 0.1 to 0.2 degree.Therefore, as shown in Figure 2, the interplanar distance d that forms the sheet metal of film annex 106 draws the spacing of slit little a lot of than the rope on conventional powder diffractometer, to guarantee that divergence θ on the X-ray beam horizontal direction is between 0.1 to 0.2 degree.X-ray beam is in being issued to the process that is detected device 107 receptions by X-ray tube 101, rope draws slit 102 the part X ray can be kept off, in addition, divergent slit 103 and anti-scatter slit 105 also can block a part of X ray, X-ray beam also will pass through film annex 106, cause again light intensity further to weaken, the scope of divergence is 0.1 to 0.2 degree when X-ray beam arrives detector 107, most of X ray is kept off in this process, not only cause the waste of the energy, also produced the environmental radiation pollution.
Summary of the invention
The embodiment of the present invention provides a kind of film diffractometer, for realizing the analytical test better to membraneous material.
A kind of film diffractometer comprises: be used to the X-ray tube of line source is provided, receive the also film annex of outgoing for the X ray that X-ray tube is sent, and for receiving the X ray after tested membraneous material diffraction the detector of testing; Wherein, described film annex is by overlapping in a row the forming of columniform kapillary, and in the xsect of film annex, all centers of circle capillaceous are in a straight line.
The present invention has strengthened the light intensity intensity of the unit area X ray shone on membraneous material, is conducive to detector to membraneous material analysis and test.
Preferably, X-ray tube equals the distance that exports to tested membraneous material of film annex to the distance of the entrance of film annex.In test process, the distance that X-ray tube exports to tested membraneous material to the distance of film annex entrance and film annex is while equating, and the light intensity gain can reach maximum, is conducive to collection and the test of detector to the X ray of process membraneous material diffraction.
Preferably, the kapillary of composition film annex is identical.The kapillary that forms the film annex in the present embodiment is identical, has simplified operation, has also simplified production technology capillaceous.
Preferably, the size of the line source that provides along with X-ray tube of described quantity capillaceous and changing.The size of the line source that the quantity capillaceous that forms the film annex in the present embodiment provides along with X-ray tube and changing, be applicable to the needs of different measuring.
Preferably, the ratio of described interior diameter capillaceous and overall diameter is between 0.8 to 0.95.In the present embodiment, the interior diameter capillaceous of composition film annex and the ratio of overall diameter meet the certain numerical value scope, are applicable to the needs of different measuring.
Preferably, described kapillary is made by transparent material.The kapillary of being made by transparent material collimates and focuses on the X ray light intensity intensity obtained to X ray higher.
Preferably, described transparent material is glass.
Other features and advantages of the present invention will be set forth in the following description, and, partly from instructions, becoming apparent, or understand by implementing the present invention.Purpose of the present invention and other advantages can realize and obtain by specifically noted structure in the instructions writing, claims and accompanying drawing.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
The accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms the part of instructions, be used to explaining the present invention, is not construed as limiting the invention together with embodiments of the present invention.In the accompanying drawings:
Fig. 1 is the schematic diagram of X-ray diffraction Method And Principle in background technology;
Fig. 2 is the schematic diagram of X ray process film annex in background technology;
Fig. 3 is the structural representation of X ray film diffractometer in the embodiment of the present invention;
Fig. 4 is the structural representation of film annex in the embodiment of the present invention;
Fig. 5 is the sectional view along the A-A line of film annex in the embodiment of the present invention;
Fig. 6 is the cross-sectional view along the B-B line of film annex in the embodiment of the present invention;
Fig. 7 is that in the embodiment of the present invention, X ray shines the light distribution schematic diagram of tested thin-film material surface by the film annex.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein, only for description and interpretation the present invention, is not intended to limit the present invention.
The embodiment of the present invention is placed novel film annex, the optical device that this film annex is comprised of many columniform kapillaries between the X-ray tube that line source is provided and tested membraneous material.The one or many total reflection occurs in X ray in kapillary, realized effective deflection, and the divergence of the X-ray beam after this film annex outgoing is in 0.2 degree left and right; In addition, because many capillaries are overlapping in a row, therefore realized the restriction on horizontal and vertical directions to X-ray beam, so, no longer need film annex 106 again X ray to be carried out the restriction of horizontal direction.This X ray intensity that not only makes to shine unit area on tested membraneous material is larger, and can make the X ray loss of strength in the process that arrives detector after the membraneous material diffraction still less, be conducive to reception and the test of detector.
Referring to Fig. 3, the film diffractometer in the present embodiment comprises X-ray tube 301, film annex 302 and the detector 304 that line source is provided.
X-ray tube 301 is be used to providing the wire X ray.
Film annex 302 receives and outgoing for the X ray that X-ray tube 301 is sent.
As shown in Figure 4, film annex 302 is by many overlapping in a row the forming of columniform kapillary 401; As shown in Figure 5, film annex 302 is identical and the combination of a plurality of rectangles of alignment along the cross section of A-A; As shown in Figure 6, film annex 302 is the combination of a plurality of circles along the cross section of B-B, and in this cross section, all centers of circle are in a straight line; The light inlet of described film annex 302 is comprised of the mouth of pipe of many capillaries, and the light-emitting window of film annex 302 is comprised of the other end mouth of pipe of many capillaries.
Detector 304 is for receiving the X ray after tested membraneous material 303 diffraction and carrying out analytical test.
Tested membraneous material 303 is between film annex 302 and detector 304, and the x-ray bombardment after 302 outgoing of film annex, to tested membraneous material 303, occurs by detector 304, to be received after diffraction.
When testing, film annex 302 is arranged on the X-ray beam and the light path between tested membraneous material 303 that X-ray tube 301 sends, can allow X ray as much as possible be injected in the kapillary that forms film annex 302, after film annex 302 collimates and focuses on, shine on tested membraneous material 303.
Preferably, the kapillary of composition film annex 302 is all identical.The kapillary that forms the film annex in the present embodiment is identical, has simplified operation, has also simplified production technology capillaceous.
Preferably, X-ray tube 301 equals the distance of the tested membraneous material 303 of exporting to of film annex 302 to the distance of the entrance of film annex 302.For example, in test process, when X-ray tube all is 100mm to the distance that exports to tested membraneous material of the distance of the entrance of film annex 302 and film annex 302, the X ray shone on tested membraneous material 303 is the center of circle take spot center, diameter is that the interior light intensity gain of the scope of 300 μ m can reach 5.6 times, has strengthened collection and the test of detector to the X ray after the membraneous material diffraction.
In the scheme that the embodiment of the present invention provides, by by 302 pairs of X ray of the overlapping film annex formed in a row of many capillaries, being collimated and focused on: X ray is by capillary exit incident, total reflection occurs in kapillary, realized effective deflection, made the divergence of the X-ray beam after 302 outgoing of film annex in 0.2 degree left and right.That is to say, the rope in background technology draws slit, and this film annex 302 can increase the light intensity intensity of X ray on unit area shone on tested membraneous material 303, in addition, because many capillaries are overlapping in a row, X ray passes in kapillary, reduced loose veiling glare, can realize the restriction on horizontal and vertical directions to X-ray beam, therefore, at X ray, no longer need 106 pairs of X-ray beams of film annex to carry out the restriction of horizontal direction after membraneous material 303 diffraction, so, by using this film annex 302, the light intensity of X ray on unit area that not only makes to shine on tested membraneous material 303 is stronger, and loss of strength is still less in arriving the process of detector 304 to make X ray after membraneous material 303 diffraction, be conducive to reception and the test of detector.
Preferably, form the size of the line source that the quantity of the kapillary 401 of film annex 302 can provide along with X-ray tube and change.
Preferably, kapillary 401 is made by transparent material.
Preferably, the material of kapillary 401 is transparent glass material.Especially, this glass material is the foam glass that density is lower, and glass material comprises one or more elements in lithium Li, beryllium Be and boron at least.For example, the composition of glass comprises:
Figure BSA0000093077220000051
Preferably, the ratio of described interior diameter capillaceous and overall diameter is between 0.8 to 0.95.In the present embodiment, the interior diameter capillaceous of composition film annex and the ratio of overall diameter meet the certain numerical value scope, are applicable to the needs of different measuring.
For example, the diffractive technology of the parallel X-ray for line source provided in background technology, distance between the X ray exit portal of X-ray tube 101 and membraneous material 104 is 225mm, it is 50mm that the X ray exit portal of X-ray tube 101 and rope draw the distance between slit 102 entrances, it is 0.05mm that the formation rope draws the thickness of the tantalum piece of slit, spacing between tantalum piece is 0.5mm, and rope draws slit 102 length 70mm.In the film diffractometer that is provided with film annex 302 that the embodiment of the present invention provides, it is 100mm that the X-ray tube 301 of line source and the distance between film annex 302 entrances are provided, distance between 302 outlets of film annex and tested film 303 is 100mm, distance between X-ray tube 301 and membraneous material 303 is 225mm, the single capillary internal diameter is 0.77mm, the single capillary boss ratio is 0.8, and number of capillary is 11.When the light source size is 0.1*10mm, when the energy of the X ray of X-ray tube emission is 8.0keV, X ray through film annex 302 shine on tested membraneous material 303 light distribution as shown in Figure 7, the z axle means light intensity, the x axial coordinate of incidence point when the x axle means after X ray is by kapillary to incide on membraneous material; The y axle means that x-ray bombardment arrives the y axial coordinate of membraneous material.Use this film annex 302, be radiated at the long 16.39mm of being of hot spot on tested film, wide is 1.46mm, and the light intensity gain in the spot center diameter is 300 μ m scopes is 5.6 times.Wherein, light intensity gain is to compare and obtain with the light intensity of X ray after rope draws slit 102 in scheme that background technology shown in Figure 1 is introduced with the present invention, and the X ray in Fig. 1 is after rope draws slit 102 to shine membraneous material 104, also will limit in the horizontal direction through 106 pairs of X-ray beams of film annex, light intensity can further weaken in this process; In addition, divergent slit 103 and anti-scatter slit 105 also can block a part of X ray, visible, and the scheme that the present embodiment provides obviously is better than the scheme that background technology is introduced.
Obviously, those skilled in the art can carry out various changes and modification and not break away from the spirit and scope of the present invention the present invention.Like this, if within of the present invention these are revised and modification belongs to the scope of the claims in the present invention and equivalent technologies thereof, the present invention also is intended to comprise these changes and modification interior.

Claims (7)

1. film diffractometer, it is characterized in that, comprise: be used to the X-ray tube of line source is provided, receive the also film annex of outgoing for the X ray that X-ray tube is sent, and for receiving the X ray after tested membraneous material diffraction the detector of testing;
Wherein, described film annex is by overlapping in a row the forming of columniform kapillary, and in the xsect of film annex, all centers of circle capillaceous are in a straight line.
2. film diffractometer as claimed in claim 1, is characterized in that, X-ray tube equals the distance that exports to tested membraneous material of film annex to the distance of the entrance of film annex.
3. film diffractometer as claimed in claim 1, is characterized in that, the kapillary that forms the film annex is all identical.
4. film diffractometer as claimed in claim 1, is characterized in that, the size of the line source that described quantity capillaceous provides along with X-ray tube and changing.
5. film diffractometer as claimed in claim 1, is characterized in that, the ratio of described interior diameter capillaceous and overall diameter is between 0.8 to 0.95.
6. film diffractometer as claimed in claim 1, is characterized in that, described kapillary is made by transparent material.
7. film diffractometer as claimed in claim 6, is characterized in that, described transparent material is glass.
CN2013103181080A 2013-07-26 2013-07-26 Thin-film diffraction instrument Pending CN103411986A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09178676A (en) * 1995-12-22 1997-07-11 Toyota Motor Corp X-ray collimator and x-ray radiation apparatus
CN1504744A (en) * 2002-12-02 2004-06-16 中国科学技术大学 Method and apparatus for measuring and analyzing structure and component of combined sample
US20080084967A1 (en) * 2006-10-10 2008-04-10 Rigaku Corporation X-ray optical system
CN201368856Y (en) * 2008-10-20 2009-12-23 北京师范大学 Microbeam X-ray diffractometer based on capillary X-ray optical device
US20120248345A1 (en) * 2008-04-11 2012-10-04 Rigaku Innovative Technologies, Inc. Nanotube based device for guiding x-ray photons and neutrons
JP3183328U (en) * 2013-02-22 2013-05-16 株式会社島津製作所 Polycapillary optical element and X-ray diffraction apparatus
CN203337574U (en) * 2013-07-26 2013-12-11 北京师范大学 Thin-film diffractometer

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09178676A (en) * 1995-12-22 1997-07-11 Toyota Motor Corp X-ray collimator and x-ray radiation apparatus
CN1504744A (en) * 2002-12-02 2004-06-16 中国科学技术大学 Method and apparatus for measuring and analyzing structure and component of combined sample
US20080084967A1 (en) * 2006-10-10 2008-04-10 Rigaku Corporation X-ray optical system
US20120248345A1 (en) * 2008-04-11 2012-10-04 Rigaku Innovative Technologies, Inc. Nanotube based device for guiding x-ray photons and neutrons
CN201368856Y (en) * 2008-10-20 2009-12-23 北京师范大学 Microbeam X-ray diffractometer based on capillary X-ray optical device
JP3183328U (en) * 2013-02-22 2013-05-16 株式会社島津製作所 Polycapillary optical element and X-ray diffraction apparatus
CN203337574U (en) * 2013-07-26 2013-12-11 北京师范大学 Thin-film diffractometer

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Title
KARDIAWARMAN ET AL.: "Application of A Multifiber Collimating lens to Thin Film Structure Analysis", 《SPIE》 *
安国玉: "多毛细管平行束及其应用", 《物理》 *
杨帆等: "X射线衍射技术在薄膜残余应力测量中的应用", 《功能材料》 *

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Application publication date: 20131127