CN108627530A - A kind of Wavelength Dispersive X-Ray Fluorescence Analysis instrument - Google Patents

A kind of Wavelength Dispersive X-Ray Fluorescence Analysis instrument Download PDF

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Publication number
CN108627530A
CN108627530A CN201810509525.6A CN201810509525A CN108627530A CN 108627530 A CN108627530 A CN 108627530A CN 201810509525 A CN201810509525 A CN 201810509525A CN 108627530 A CN108627530 A CN 108627530A
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Prior art keywords
single channel
capillary
ray
sub
pipe
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李玉德
林晓燕
王兴艺
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Beijing Normal University
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Beijing Normal University
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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
    • G01N23/223Investigating 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
    • 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
    • G01N23/2209Investigating 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 wavelength dispersive spectroscopy [WDS]
    • 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

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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)
  • Spectroscopy & Molecular Physics (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

The present invention relates to a kind of Wavelength Dispersive X-Ray Fluorescence Analysis instrument, which is characterized in that the fluorescence analyser includes X-ray source, collimation multiple capillary lens, flat crystal and focuses multiple capillary lens;The X-ray source is used to emit the multi-wavelength X-ray with bremsstrahlung and characteristic radiation;The collimation multiple capillary lens are used to multi-wavelength X-ray collimation be quasi-parallel X-ray;The flat crystal is used to carry out monochromatization to the quasi-parallel X-ray for meeting Bragg diffraction condition;The quasi-parallel X-ray focusing illumination sample of monochrome for focusing multiple capillary lens and being used to the flat crystal being emitted.

Description

A kind of Wavelength Dispersive X-Ray Fluorescence Analysis instrument
Technical field
The present invention relates to a kind of fluorescence analysers, especially with regard to a kind of Wavelength Dispersive X-Ray Fluorescence Analysis instrument.
Background technology
X-ray fluorescence analysis technology can test the chemical element of substance, object phase, material evidence material, be material supply section A kind of quick, accurate and economic multielement analysis method that, life science, environmental science etc. generally use.X-ray is glimmering Light analyzer is the versatility scientific instrument in fluorescence analysis field, can be carried out non-destructive testing to product and quality of materials, to people Photoetching inspection etc. of the body into practise medicine inspection and microcircuit.Wavelength Dispersive X-Ray Fluorescence Analysis instrument is a kind of important fluorescence analyser, Have the characteristics that detect that detection limit is low, high sensitivity, detection speed are fast, include mainly X source system, light beam regulator control system, Detector system and computer four are most of.The X-ray that X source generates has bremsstrahlung and characteristic radiation, is not single wavelength. And scattering of the bremsstrahlung continuous spectrum on sample is the main source of X-ray fluorescence spectra back end, limits the detection of instrument Detection limit.
The X that current international Wavelength Dispersive X-Ray Fluorescence Analysis instrument sends out micro-focus X-ray source using the hyperboloid bent crystal Ray carries out Bragg diffraction monochromatization and is focused into the tens of hot spots to hundreds of microns of diameter, is carried out to the element in sample single Wavelength excites.Since there is no continuous spectrums to be incident on sample, tested elemental characteristic line scattering back end is low, thus with the peak back of the body Than low detection limits can carry out qualitative and quantitative detection to micro or even trace element.The hyperboloid bent crystal is to utilize mechanical press-bending method Ellipsoid type is made in flat crystal with piezoelectric ceramics method, the diverging X-ray that in this way can emit dotted focal spot X source converts Monochromatizing, the X-ray of focusing.But due to by pressing bend method, flat crystal being made to become the ellipsoid of standard necessarily It is very difficult.And tangent bend crystal has strict requirements to the focal spot size and shape of X source, and it is micro- to be only applicable to tens The smaller dotted focal spot light sources of meter Yi Zhi.
Invention content
In view of the above-mentioned problems, the object of the present invention is to provide one kind being suitable for large-sized face focal spot X source, and being capable of shape At the Wavelength Dispersive X-Ray Fluorescence Analysis instrument of ten micron dimension focal beam spots.
To achieve the above object, the present invention takes following technical scheme:A kind of Wavelength Dispersive X-Ray Fluorescence Analysis instrument, It is characterized in that, which includes that X-ray source, collimation multiple capillary lens, flat crystal and focusing multiple capillary are saturating Mirror;The X-ray source is used to emit the multi-wavelength X-ray with bremsstrahlung and characteristic radiation;The collimation multiple capillary is saturating Mirror is used to multi-wavelength X-ray collimation be quasi-parallel X-ray;The flat crystal is used for meeting the quasi-parallel of Bragg diffraction condition X-ray carries out monochromatization;The multiple capillary lens that focus are used to the quasi-parallel X-ray of monochrome that the flat crystal is emitted focusing photograph Penetrate sample.
Further, the collimation multiple capillary lens are formed by several single channel capillary group close-packed arrays, Mei Yisuo It states single channel capillary group to be formed by the sub- pipe close-packed arrays of several single channel capillarys, along each single channel of central axis The diameter of the sub- pipe of single channel capillary in capillary group constantly increases, and along the difference single channel capillary of a certain longitudinal section The diameter of the sub- pipe of single channel capillary of group is different.
Further, a diameter of 6.83mm of arrival end, a diameter of 9.11mm in outlet end of the collimation multiple capillary lens, Pipe range is 45mm, and the collimation multiple capillary lens include the six circle single channel capillary groups.
Further, for a certain longitudinal section of the collimation multiple capillary lens, it is located at the list at longitudinal section center The sub- pipe diameter of single channel capillary of Channel Capillary group is 0.03mm, the single channel capillary of the second circle single channel capillary group A diameter of 0.025mm of sub- pipe, and so on, single channel capillary of third circle to the single channel capillary group of the 6th circle Pipe diameter is followed successively by 0.0197mm, 0.0117mm, 0.0073mm and 0.0035mm.
Further, the longitudinal section of each single channel capillary group is hexagon.
Further, the focusing multiple capillary lens are formed by the sub- pipe close-packed arrays of a large amount of single channel capillarys, in The diameter of all sub- pipes of single channel capillary of mandrel line constantly reduces, and along all single channel hairs of a certain longitudinal section Thin sub- pipe diameter is identical.
Further, the sub- pipe of single channel capillary uses glass material.
Further, the flat crystal uses graphite crystal or carborundum crystals.
The invention adopts the above technical scheme, which has the following advantages:1, with existing tangent bend Crystallization Wavelength Dispersive X-Ray Fluorescence Analysis instrument is compared, and it is burnt that Wavelength Dispersive X-Ray Fluorescence Analysis instrument of the invention is suitable for large-sized face Spot X source focuses multiple capillary lens by control, can form the hot spot of ten micron dimensions.2, double curved with primary event Bent crystal phase ratio, single channel capillary sub- pipe of the present invention play waveguide, can be limited anti-by the X-ray of multiple total reflection Penetrate space realize wide-angle deflection, substantially reduce X source to sample to be tested operating distance.In this way, fluorescence point can be reduced The volume of analyzer, convenient for forming portable instrument.
Description of the drawings
Fig. 1 is Bragg's equation principle schematic;
Fig. 2 is the Wavelength Dispersive X-Ray Fluorescence Analysis instrument light path schematic diagram of the present invention;
Fig. 3 is the collimation multiple capillary lens enlarged diagram of the present invention.
Specific implementation mode
Come to carry out detailed description to the present invention below in conjunction with attached drawing.It should be appreciated, however, that attached drawing has been provided only more Understand the present invention well, they should not be interpreted as limitation of the present invention.
As shown in Figure 1, according to Bragg's equation, when the incident angle θ and wavelength X of the X-ray for being incident on crystal meet item Part:
2dsin θ=n λ, n=1,2,3...
In formula, d is the vertical distance of adjacent two crystal face, when the optical path difference for being irradiated to adjacent two crystal face is the n of X-ray wavelength Times when, the diffracted intensity of X-ray will mutually be reinforced.
As shown in Fig. 2, Wavelength Dispersive X-Ray Fluorescence Analysis instrument provided by the invention, including X-ray source 1, collimation crinosity Tubule lens 2, flat crystal 3 and focusing multiple capillary lens 4.
Multi-wavelength X-ray with bremsstrahlung and characteristic radiation is emitted to collimation multiple capillary lens 2 by X-ray source 1, Diverging X-ray collimation is that quasi-parallel X-ray is emitted to flat crystal 3 by collimation multiple capillary lens 2, and flat crystal 3 is used for meeting The quasi-parallel X-ray of Bragg diffraction condition carries out monochromatization, and the quasi-parallel X-ray of monochrome being emitted through flat crystal 3 is emitted to focusing Multiple capillary lens 4 focus multiple capillary lens 4 and are used for monochromatic quasi-parallel smooth focusing illumination sample.
In a preferred embodiment, as shown in figure 3, collimation multiple capillary lens 2 are by several single channel capillary groups Close-packed arrays form, all single channel capillary groups can according to identical curvature bending, to change the direction of propagation of X-ray, Ensure that outgoing X-ray is quasi-parallel.Each single channel capillary group is formed by the sub- pipe close-packed arrays of several single channel capillarys, along The diameter of the sub- pipe of single channel capillary in central axis (paths direction) all single channel capillary groups constantly increases, and accurate The single channel capillary of the different single channel capillary groups of the longitudinal section (from the section of central axis upright) of straight multiple capillary lens 2 The diameter of sub- pipe differs.Each sub- inside pipe wall of single channel capillary constitutes reflecting surface, and multi-wavelength X-ray is by single channel capillary sub- pipe One end enters to be totally reflected in inner wall, and is exported by the other end of the sub- pipe of single channel capillary.Positioned at collimation multiple capillary lens 2 The sub- pipe diameter of single channel capillary of the single channel capillary group of longitudinal section is gradually reduced by center to outside, overcomes collimation crinosity Tubule lens peripheral edge portion is emitted the larger disadvantage of divergence of X-ray beam, improves the entirely outgoing X of collimation multiple capillary lens 2 The depth of parallelism of light beam.The a diameter of 6.83mm of arrival end of multiple capillary lens 2, collimation capillary lens 2 are collimated in the present embodiment The a diameter of 9.11mm in outlet end, some longitudinal section of pipe range 45mm, the collimation multiple capillary lens 2 of the present embodiment include 6 Single channel capillary group is enclosed, the sub- pipe diameter of single channel capillary of centrally located single channel capillary group is 0.03mm, the second circle Single channel capillary group the sub- pipe diameter of single channel capillary be 0.025mm, and so on, third circle to the 6th circle single channel The sub- pipe diameter of single channel capillary of capillary group is followed successively by 0.0197mm, 0.0117mm, 0.0073mm and 0.0035mm, with this For, without being limited thereto, single channel capillary of each single channel capillary group of other longitudinal sections of collimation multiple capillary lens 2 The diameter of pipe can be configured as needed.
In a preferred embodiment, the longitudinal section of each single channel capillary group is hexagon.
In a preferred embodiment, multiple capillary lens 4 are focused by the sub- pipe close-packed arrays of a large amount of single channel capillarys and At the diameter along all sub- pipes of single channel capillary of central axis constantly reduces, and focuses the longitudinal section of multiple capillary lens 4 The diameter of all sub- pipes of single channel capillary in (section with central axis upright) is identical.In each single channel capillary sub- pipe Wall constitutes reflecting surface, and the quasi-parallel light of monochrome being emitted through flat crystal 3 is entered by the sub- pipe one end of single channel capillary to be occurred in inner wall Total reflection, and exported by the other end of the sub- pipe of single channel capillary.Wherein, focus arrival end, the outlet end of multiple capillary lens 4 with And pipe range can be configured according to actual needs, not limited herein.
In a preferred embodiment, glass material may be used in all sub- Guan Jun of single channel capillary, utilizes glass The smooth property of material ensure that the efficiency of transmission of X-ray, reduce light intensity loss of the X-ray in transmission process.
In a preferred embodiment, graphite crystal or carborundum crystals may be used in flat crystal 3.
The various embodiments described above are merely to illustrate the present invention, wherein the structure of each component, connection type and manufacture craft etc. are all It can be varied from, every equivalents carried out based on the technical solution of the present invention and improvement should not exclude Except protection scope of the present invention.

Claims (8)

1. a kind of Wavelength Dispersive X-Ray Fluorescence Analysis instrument, which is characterized in that the fluorescence analyser include X-ray source, collimation it is more Capillary lens, flat crystal and focusing multiple capillary lens;
The X-ray source is used to emit the multi-wavelength X-ray with bremsstrahlung and characteristic radiation;
The collimation multiple capillary lens are used to multi-wavelength X-ray collimation be quasi-parallel X-ray;
The flat crystal is used to carry out monochromatization to the quasi-parallel X-ray for meeting Bragg diffraction condition;
The quasi-parallel X-ray focusing illumination sample of monochrome for focusing multiple capillary lens and being used to the flat crystal being emitted.
2. Wavelength Dispersive X-Ray Fluorescence Analysis instrument according to claim 1, which is characterized in that the collimation multiple capillary Lens are formed by several single channel capillary group close-packed arrays, and each single channel capillary group is by several single channel capillarys Sub- pipe close-packed arrays form, along the sub- pipe of single channel capillary in each single channel capillary group of central axis diameter not It is disconnected to increase, and the diameter of the sub- pipe of single channel capillary along the difference single channel capillary group of a certain longitudinal section is different.
3. Wavelength Dispersive X-Ray Fluorescence Analysis instrument according to claim 2, which is characterized in that the collimation multiple capillary The a diameter of 6.83mm of arrival end of lens, a diameter of 9.11mm in outlet end, pipe range 45mm, the collimation multiple capillary lens packet Include the six circles single channel capillary group.
4. Wavelength Dispersive X-Ray Fluorescence Analysis instrument according to claim 2, which is characterized in that for the collimation crinosity The a certain longitudinal section of tubule lens, the sub- pipe diameter of single channel capillary positioned at the single channel capillary group at longitudinal section center are 0.03mm, a diameter of 0.025mm of the sub- pipe of single channel capillary of the second circle single channel capillary group, and so on, third Enclose to the 6th circle the single channel capillary group the sub- pipe diameter of single channel capillary be followed successively by 0.0197mm, 0.0117mm, 0.0073mm and 0.0035mm.
5. Wavelength Dispersive X-Ray Fluorescence Analysis instrument according to claim 2 or 3, which is characterized in that each single channel The longitudinal section of capillary group is hexagon.
6. Wavelength Dispersive X-Ray Fluorescence Analysis instrument according to claim 1, which is characterized in that the focusing multiple capillary Lens are formed by the sub- pipe close-packed arrays of a large amount of single channel capillarys, along the diameter of all sub- pipes of single channel capillary of central axis Constantly reduce, and identical along all sub- pipe diameters of single channel capillary of a certain longitudinal section.
7. the Wavelength Dispersive X-Ray Fluorescence Analysis instrument according to claim 2 or 6, which is characterized in that the single channel capillary Sub- pipe uses glass material.
8. Wavelength Dispersive X-Ray Fluorescence Analysis instrument according to claim 5, which is characterized in that the flat crystal uses Graphite crystal or carborundum crystals.
CN201810509525.6A 2018-05-24 2018-05-24 A kind of Wavelength Dispersive X-Ray Fluorescence Analysis instrument Pending CN108627530A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113203757A (en) * 2021-05-07 2021-08-03 北京市辐射中心 All-optical X-ray microscopic imaging system

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JPH11352079A (en) * 1998-06-10 1999-12-24 Rigaku Denki Kk Xafs measuring method and apparatus thereof
TW445488B (en) * 1998-04-22 2001-07-11 Smithsonian Astrophysical Obse X-ray diagnostic system
US20020148808A1 (en) * 2001-03-12 2002-10-17 Ifg Institut Fur Geratebau Gmbh Capillary optical element with a complex structure of capillaries and a method for its manufacture
JP2007093316A (en) * 2005-09-28 2007-04-12 Shimadzu Corp X-ray focusing arrangement
US20080084967A1 (en) * 2006-10-10 2008-04-10 Rigaku Corporation X-ray optical system
CN101499327A (en) * 2009-03-20 2009-08-05 北京师范大学 Plateau capillary X-ray converging lens
CN101498647A (en) * 2009-03-20 2009-08-05 北京师范大学 Micro-beam X-ray fluorescence equipment used for atmosphere particle single-particle analysis
US20150213912A1 (en) * 2012-09-14 2015-07-30 Hamamatsu Photonics K.K. Polycapillary lens
CN104833685A (en) * 2015-04-21 2015-08-12 北京师范大学 X ray grating imaging system
CN204758507U (en) * 2015-04-21 2015-11-11 北京师范大学 X ray grating imaging system
CN208255102U (en) * 2018-05-24 2018-12-18 北京师范大学 A kind of Wavelength Dispersive X-Ray Fluorescence Analysis instrument

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW445488B (en) * 1998-04-22 2001-07-11 Smithsonian Astrophysical Obse X-ray diagnostic system
JPH11352079A (en) * 1998-06-10 1999-12-24 Rigaku Denki Kk Xafs measuring method and apparatus thereof
US20020148808A1 (en) * 2001-03-12 2002-10-17 Ifg Institut Fur Geratebau Gmbh Capillary optical element with a complex structure of capillaries and a method for its manufacture
JP2007093316A (en) * 2005-09-28 2007-04-12 Shimadzu Corp X-ray focusing arrangement
US20080084967A1 (en) * 2006-10-10 2008-04-10 Rigaku Corporation X-ray optical system
CN101499327A (en) * 2009-03-20 2009-08-05 北京师范大学 Plateau capillary X-ray converging lens
CN101498647A (en) * 2009-03-20 2009-08-05 北京师范大学 Micro-beam X-ray fluorescence equipment used for atmosphere particle single-particle analysis
US20150213912A1 (en) * 2012-09-14 2015-07-30 Hamamatsu Photonics K.K. Polycapillary lens
CN104833685A (en) * 2015-04-21 2015-08-12 北京师范大学 X ray grating imaging system
CN204758507U (en) * 2015-04-21 2015-11-11 北京师范大学 X ray grating imaging system
CN208255102U (en) * 2018-05-24 2018-12-18 北京师范大学 A kind of Wavelength Dispersive X-Ray Fluorescence Analysis instrument

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113203757A (en) * 2021-05-07 2021-08-03 北京市辐射中心 All-optical X-ray microscopic imaging system
CN113203757B (en) * 2021-05-07 2024-03-22 北京市辐射中心 All-optical X-ray microscopic imaging system

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