CN107238620B - X-ray fluorescence diffraction integrated analyzer of rotatable sample - Google Patents

X-ray fluorescence diffraction integrated analyzer of rotatable sample Download PDF

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CN107238620B
CN107238620B CN201710620594.XA CN201710620594A CN107238620B CN 107238620 B CN107238620 B CN 107238620B CN 201710620594 A CN201710620594 A CN 201710620594A CN 107238620 B CN107238620 B CN 107238620B
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fluorescence
diffraction
sample
ray
mounting plate
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CN107238620A (en
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杨勇奇
王典洪
倪效勇
徐朝玉
程卓
龚芳
熊德云
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China University of Geosciences
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China University of Geosciences
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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
    • G01N23/20Investigating 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
    • G01N23/20008Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G01N23/20025Sample holders or supports therefor
    • 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
    • G01N23/20Investigating 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
    • G01N23/205Investigating 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 using diffraction cameras
    • 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
    • G01N23/2204Specimen supports therefor; Sample conveying means therefore
    • 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
    • G01N23/2206Combination of two or more measurements, at least one measurement being that of secondary emission, e.g. combination of secondary electron [SE] measurement and back-scattered electron [BSE] measurement
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/05Investigating materials by wave or particle radiation by diffraction, scatter or reflection
    • G01N2223/056Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
    • G01N2223/0561Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction diffraction cameras
    • 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/10Different kinds of radiation or particles
    • G01N2223/101Different kinds of radiation or particles electromagnetic radiation
    • G01N2223/1016X-ray

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Abstract

The invention provides an X-ray fluorescence diffraction integrated analyzer of a rotatable sample, which comprises an X-ray generator, an X-ray diffraction analysis component, a fluorescence detector and a double-layer rotating platform, wherein the upper layer and the lower layer of the double-layer rotating platform are respectively a fluorescence sample tray and a diffraction sample tray; the X-ray diffraction analysis assembly comprises a collimation adjusting module and a diffraction detection module, the diffraction sample tray is positioned between the collimation adjusting module and the diffraction detection module, the fluorescence detector is positioned between the X-ray generator and the fluorescence sample tray, and the fluorescence analysis sample groove is arranged towards the fluorescence detector. The invention has the beneficial effects that: the X-ray fluorescence analysis and the X-ray diffraction analysis are integrated, and various samples can be contained at one time.

Description

X-ray fluorescence diffraction integrated analyzer of rotatable sample
Technical Field
The invention relates to the technical field of X-ray analysis, in particular to an X-ray fluorescence diffraction integrated analyzer of a rotatable sample.
Background
X-ray is an electromagnetic wave with extremely short wavelength and large energy, and when it is irradiated on the surface of an object, various effects occur simultaneously, and it can be used for various purposes. For example, the X-ray has a relatively strong penetrating effect, and the effect can be used for shooting X-ray pictures or industrial flaw detection and the like.
The fluorescence analysis is a technology for exciting a sample to emit fluorescence by utilizing X-rays, and analyzing the energy and the intensity of the fluorescence after the fluorescence is received by a detector.
The diffraction analysis is to utilize the fact that X-rays are scattered by atoms, photons with enhanced diffraction can be obtained in certain specific directions, the number of diffraction photons corresponding to the X-rays with different incident angles is received by a detector, the diffraction photons with the specific angles reflect the space structure information of substance atoms, and the method can be used for a technology mainly based on phase analysis and can also be used for qualitative and semi-quantitative analysis.
Although the fluorescence and diffraction analysis are similar in functional application, they cannot be completely replaced with each other, the fluorescence analysis focuses on the type and content of elements, and the diffraction analysis focuses on the spatial arrangement of atoms, so that if the two are combined, a more comprehensive and complete analysis can be completed, and the method has wider application.
At present, commercial instruments independently developed for X-ray fluorescence and diffraction analysis are mature, but few instruments with fluorescence and diffraction analysis functions are available. Generally, when two different functions are needed to be analyzed, a user needs to operate different devices respectively, and the working efficiency is low; and a plurality of devices are high in purchase cost, and particularly, X-ray diffraction analysis equipment occupies a large area and is not beneficial to use in a field environment. Therefore, the equipment integrating the fluorescence and diffraction analysis functions has good application prospect and value. Meanwhile, a conventional fluorescence and diffraction analysis instrument can only analyze one sample at a time, the sample needs to be manually replaced after one sample is analyzed, and when a plurality of samples are to be analyzed, the samples are frequently replaced, so that time and labor are spent, the damage of a protective door of the instrument is easily caused, and the sealing performance of the instrument is influenced. Therefore, a carrier device capable of accommodating a plurality of samples is needed to achieve the goal of loading a plurality of samples at a time for multiple analyses.
Aiming at the problems that a plurality of instruments for analyzing the X-ray fluorescence and diffraction combined function in the market at present are available, and a conventional instrument can only be used for loading and analyzing samples once, so that the working efficiency is low, the invention provides a rotatable multi-sample loading device, and combines the fluorescence and diffraction analysis functions to form the X-ray fluorescence and diffraction integrated analyzer of the rotatable sample.
Disclosure of Invention
In view of the above, embodiments of the present invention provide an integrated X-ray fluorescence and diffraction analyzer capable of accommodating multiple samples at a time and integrating X-ray fluorescence and X-ray diffraction analysis into a single rotatable sample.
The embodiment of the invention provides an X-ray fluorescence diffraction integrated analyzer of a rotatable sample, which comprises an X-ray generator, an X-ray diffraction analysis component, a fluorescence detector and a double-layer rotating platform, wherein the upper layer and the lower layer of the double-layer rotating platform are respectively a fluorescence sample tray and a diffraction sample tray; the X-ray diffraction analysis assembly is vertically installed in parallel with an X-ray light path and comprises an alignment adjusting module and a diffraction detection module which are arranged up and down, the diffraction sample tray is located between the alignment adjusting module and the diffraction detection module, the fluorescence detector is horizontally installed perpendicular to the X-ray light path and is located between the X-ray generator and the fluorescence sample tray, the surface of the fluorescence analysis sample groove, where a fluorescence sample is placed, is an inclined surface, and the inclined surface faces the fluorescence detector.
Furthermore, the number of the fluorescence analysis sample groove and the number of the light through holes are respectively three, and the included angle between the fluorescence analysis sample groove and the adjacent light through hole is 60 degrees.
Further, still include the fourth mounting panel that the level set up, step motor install in the fourth mounting panel, a vertical umbrella wheel with step motor connects in order to be in step motor's driving down vertical rotation, the rotary rod passes the center of a horizontal umbrella wheel and through a step bearing install in the fourth mounting panel, horizontal umbrella wheel with rotary rod fixed contact, just vertical umbrella wheel with the rodent intermeshing of horizontal umbrella wheel.
Furthermore, the fluorescent sample tray further comprises a second mounting plate which is horizontally arranged and is arranged above the fourth mounting plate, a bearing mounting seat is fixedly hung on the second mounting plate through four screw rods, and the upper end of the rotary rod penetrates through the fluorescent sample tray and then is mounted on the bearing mounting seat through an upper bearing seat.
The collimation adjusting module comprises a micrometer displacement table and a pinhole collimator arranged on the movable surface of the micrometer displacement table, the upper end surface of the micrometer displacement table is fixed on the lower surface of the third mounting plate, the pinhole collimator is arranged on the lower end surface of the micrometer displacement table, the micrometer displacement table is provided with an X-direction adjusting handle and a Y-direction adjusting handle perpendicular to the X-direction adjusting handle, the X-direction adjusting handle and the Y-direction adjusting handle are both connected with the movable surface to adjust the coordinate of the movable surface in the X-direction or in the Y-direction perpendicular to the X-direction, and the X-direction and the Y-direction are both perpendicular to the vertical direction.
Further, still including the level setting be located the first mounting panel of second mounting panel top, the X ray generator is fixed in through the angle sign indicating number the lower surface of first mounting panel.
Further, the fluorescence detector is fixed on the lower surface of the second mounting plate and is positioned between the second mounting plate and the bearing mounting seat.
Further, the fluorescence sample tray and the diffraction sample tray are fixed to the rotating rod through locking nuts located on the upper surface and the lower surface of each of the fluorescence sample tray and the diffraction sample tray.
The diffraction detection module comprises a vacuum cavity and a CCD detector, the vacuum cavity is clamped in the through hole and is downwards fixed on the fifth mounting plate, the CCD detector is located in the vacuum cavity, a beryllium window through which X rays can penetrate is arranged on the upper end face of the vacuum cavity, the CCD detector is located under the beryllium window, an aviation socket is arranged on the bottom wall of the vacuum cavity, and the CCD detector is connected with a system control unit through the aviation socket arranged on the bottom wall of the vacuum cavity.
Furthermore, the back of the CCD detector is connected with the bottom wall of the vacuum cavity through a red copper block, and a cooling fan is arranged on the outer side of the bottom wall of the vacuum cavity.
The technical scheme provided by the embodiment of the invention has the following beneficial effects: the X-ray fluorescence diffraction integrated analyzer of the rotatable sample integrates X-ray diffraction analysis and X-ray fluorescence into a whole due to the fact that the X-ray diffraction analysis component is vertically arranged in parallel to an X-ray light path and the fluorescence detector is horizontally arranged in perpendicular to the X-ray light path, so that the analyzer is convenient for analyzing samples with different analysis requirements and is beneficial to reducing analysis cost. The upper and lower two-layer of double-deck revolving stage is equipped with a plurality of fluorescence analysis sample groove and a plurality of diffraction analysis sample groove respectively, through rotatory double-deck revolving stage can carry out the analysis to the sample that is in the sample groove of difference, has avoided the waste of time and manpower because of frequently changing the sample and causing, can reduce the loss of equipment moreover.
Drawings
FIG. 1 is a perspective view of the exterior of an integrated X-ray fluorescence diffraction analyzer for a rotatable sample according to the present invention;
FIG. 2 is a perspective view of the interior of the integrated X-ray fluorescence diffraction analyzer of the rotatable sample of the present invention;
FIG. 3 is an external front view of the interior of the integrated X-ray fluorescence diffraction analyzer for rotatable samples of the present invention;
FIG. 4 is a perspective view of a double layer rotary stage of the integrated X-ray fluorescence diffraction analyzer for rotatable samples according to the present invention;
FIG. 5 is a bottom view of the micrometer displacement stage of the integrated X-ray fluorescence diffraction analyzer for rotatable samples according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
Referring to fig. 2 and 3, an embodiment of the present invention provides an X-ray fluorescence diffraction integrated analyzer for a rotatable sample, which is used for performing X-ray fluorescence analysis and X-ray diffraction analysis on a fluorescence sample and a diffraction sample, respectively, and includes an X-ray generator 3, an X-ray diffraction analysis assembly, and a fluorescence detector 4, and further includes a double-layer rotating platform, of which the upper layer and the lower layer are a fluorescence sample tray 51 and a diffraction sample tray 52, respectively.
Referring to fig. 1, the integrated X-ray fluorescence diffraction analyzer of a rotatable sample according to the present invention has a protective housing, handles for facilitating handling are symmetrically disposed on two opposite sides of the housing, the housing is a hollow structure, a cavity is a sample chamber, a sample chamber door 1 is disposed on the front side of the housing, and a boss handle 11 for facilitating opening and closing of the sample chamber door is disposed on the sample chamber door 1.
Referring to fig. 1 and 2, the top wall and the bottom wall of the housing are respectively a first mounting plate 21 and a fifth mounting plate 25, a second mounting plate 22, a third mounting plate 23 and a fourth mounting plate 24 are further sequentially arranged in the sample chamber from top to bottom, and the first mounting plate 21 to the fifth mounting plate 25 are all parallel and horizontally arranged.
Referring to fig. 2 and 3, the X-ray generator 3 is located between the first mounting plate 21 and the second mounting plate 22, and is fixed on the lower surface of the first mounting plate 21 through an angle code, a through hole is opened on the second mounting plate 22 to penetrate through the upper and lower surfaces of the second mounting plate 22, and the X-ray emitted by the X-ray generator 3 passes through the through hole.
Referring to fig. 2 and 3, a bearing mounting seat 26 is located between the second mounting plate 22 and the third mounting plate 23, and the bearing mounting seat 26 is fixed to the second mounting plate 22 by four screws.
Referring to fig. 2, 3 and 4, a rotating rod 53 penetrates through the central regions of the fluorescence sample tray 51 and the diffraction sample tray 52, and the fluorescence sample tray 51 and the diffraction sample tray 52 are fixed to the rotating rod 53 by locking nuts 533 on the respective upper and lower surfaces, so that the rotating rod 53 rotates, and the fluorescence sample tray 51 and the diffraction sample tray 52 rotate accordingly.
Referring to fig. 2, 3 and 4, a stepping motor 54 is horizontally mounted on the fourth mounting plate 24, an upright umbrella wheel 541 is connected to the stepping motor 54 to rotate in an upright direction under the driving of the stepping motor 54, the lower end of the rotating rod 53 passes through the center of a horizontal umbrella wheel 534 and is mounted on the fourth mounting plate 24 through a lower bearing seat 532, the horizontal umbrella wheel 534 is in fixed contact with the rotating rod 53, so that the horizontal umbrella wheel 534 rotates, and the rotating rod 53 rotates accordingly. And the teeth of the vertical umbrella wheel 541 and the horizontal umbrella wheel 534 are engaged with each other, and the horizontal umbrella wheel 534 rotates with the rotation of the vertical umbrella wheel 541. The upper end of the rotary rod 53 passes through the fluorescent sample tray 51 and is mounted to the bearing mount 26 via an upper bearing housing 531.
Referring to fig. 2, 3 and 4, the upper surface of the fluorescence sample tray 51 is provided with three fluorescence analysis sample grooves 511 and three light holes 512 spaced apart from the three fluorescence analysis sample grooves 511, and an included angle between each fluorescence analysis sample groove 511 and the adjacent light hole 512 is 60 °. The diffraction sample tray 52 is provided with three diffraction analysis sample grooves 521, the three diffraction analysis sample grooves 521 are in one-to-one correspondence with the three light-passing holes 512 in space, and X-rays can pass through the light-passing holes 512 and irradiate the diffraction analysis sample grooves 521 corresponding to the light-passing holes 512. The fluorescence analysis sample groove 511 is used for placing a fluorescence sample, and the diffraction analysis sample groove 521 is used for placing a diffraction sample, wherein the fluorescence analysis sample groove 512 is a right-angled trapezoid structure, an inclined surface thereof is provided with a containing groove for placing a sample, and the inclined surface faces the fluorescence detector 4.
Referring to fig. 2 and 3, the fluorescence sample tray 51 is located between the bearing mounting seat 26 and the third mounting plate 23, the fluorescence detector 4 is horizontally mounted perpendicular to the X-ray optical path, and the fluorescence detector 4 is located between the second mounting plate 22 and the bearing mounting seat 26, fixed to the lower surface of the second mounting plate 22 by an angle code, and surrounded by three fluorescence analysis sample grooves 512.
The X-ray diffraction analysis component is vertically installed in parallel with an X-ray light path and comprises a collimation adjusting module and a diffraction detection module which are arranged up and down, and the diffraction sample tray 52 is positioned between the collimation adjusting module and the diffraction detection module.
Referring to fig. 5, the collimation adjustment module includes a micrometer displacement stage 61 and a pinhole collimator 612 disposed on a movable surface 611 of the micrometer displacement stage 61, the micrometer displacement stage 6 has a through cavity penetrating up and down, an upper end surface of the micrometer displacement stage 61 is fixed on a lower surface of the third mounting plate 23, the movable surface 611 is located on a lower end surface of the micrometer displacement stage 61, the pinhole collimator 612 is located below a lower opening end of the through cavity, the micrometer displacement stage 61 has an X-direction adjustment handle 614 and a Y-direction adjustment handle 613 perpendicular to the X-direction adjustment handle 614, the X-direction adjustment handle 614 and the Y-direction adjustment handle 613 are both connected to the movable surface 611 to adjust a coordinate of the movable surface in an X direction or in a Y direction perpendicular to the X direction, and both the X direction and the Y direction are perpendicular to a vertical direction. The X-direction adjusting handle and the Y-direction adjusting handle are of micrometer structures. And a mechanical shutter is arranged at an opening at the upper end of the through cavity, the mechanical shutter is connected with the system control unit 7, and the opening or closing of the mechanical shutter is controlled by the system control unit 7, so that the exposure time and the exposure period of the diffraction sample are controlled.
Referring to fig. 2 and 4, a through hole is formed in the fourth mounting plate 24, the diffraction detection module includes a vacuum cavity 62 clamped in the through hole and fixed downward to the fifth mounting plate 25, and a CCD detector located in the vacuum cavity 62, a beryllium window 621 through which X-rays can pass is disposed on an upper end surface of the vacuum cavity 62, the CCD detector is located right below the beryllium window 621, an aviation socket is disposed on a bottom wall of the vacuum cavity 62, and the CCD detector is connected to the system control unit 7 through the aviation socket disposed on the bottom wall of the vacuum cavity 62. The system control unit 7 is connected to the stepping motor 54 to control the stepping motor 54 to rotate. In order to improve the heat dissipation performance, the back of the CCD detector is connected to the bottom wall of the vacuum chamber 62 through a red copper block, and a heat dissipation fan is provided outside the bottom wall of the vacuum chamber. The heat generated by the CCD detector during operation is transferred to the bottom wall of the vacuum cavity through the red copper block, and the heat dissipation fan can accelerate the heat dissipation of the bottom wall of the vacuum cavity 62.
In use, the sample chamber door 1 is opened first, three identical or different (according to actual requirements) fluorescent samples are placed in the three fluorescence analysis sample grooves 511 of the fluorescence sample tray 51, and three identical or different (according to actual requirements) diffraction samples are placed in the three diffraction analysis sample grooves 521 of the diffraction sample tray 52; then, the sample chamber door 1 is closed, the X-ray generator 3 and the system control unit 7 are opened, the vertical umbrella wheel 541 is driven to rotate by the system control unit 7, the horizontal umbrella wheel 534 is driven to rotate, and finally the rotating rod 53 is driven to rotate, so as to adjust the positions of the fluorescence analysis sample groove 511 and the diffraction analysis sample groove 521 on the fluorescence sample tray 51 and the diffraction sample tray 52.
If the X-ray fluorescence analysis is to be performed, one of the fluorescence analysis sample slots 511 is rotated into the X-ray optical path, so that the fluorescence sample in the fluorescence analysis sample slot 511 is irradiated by the X-ray, at this time, the detection port of the fluorescence detector 4 faces the sample storage slot of the fluorescence analysis sample slot 511, the fluorescence sample in the sample storage slot is secondarily excited under the irradiation of the X-ray to generate fluorescence photons, the fluorescence photons are detected by the fluorescence detector 4, the fluorescence detector 4 converts the detected optical signal into an electrical signal, and the electrical signal is transmitted to the system control unit 7 to be performed with the X-ray fluorescence analysis by the system control unit 7.
If the X-ray diffraction analysis is to be performed, the double-layer rotating table is rotated by 60 ° (both clockwise and counterclockwise), one of the diffraction analysis sample slots 521 and the corresponding light-passing hole 512 are rotated into the X-ray optical path, so that the diffraction sample in the diffraction analysis sample slot 521 is irradiated by the X-ray, at this time, the micrometer displacement table 61 is located right below the diffraction analysis sample slot 521, the system control unit 7 controls the coordinates of the movable surface 611 in the micrometer displacement table 7 through the connection with the micrometer displacement table 61 as required, so as to adjust the light flux entering the CCD detector after the X-ray irradiates the diffraction sample, and the CCD detector converts the detected light signal into an electrical signal and transmits the electrical signal to the system control unit 7 so as to perform the X-ray diffraction analysis by the system control unit 7.
If the X-ray fluorescence analysis of the next fluorescence sample is to be performed, the double-layer rotating platform is rotated by 60 degrees, and so on, and the relative analysis of the next sample (fluorescence sample or diffraction sample) is performed by rotating the double-layer rotating platform, without frequently opening the sample chamber door 1 to replace the sample.
The technical scheme provided by the embodiment of the invention has the following beneficial effects: the X-ray fluorescence diffraction integrated analyzer of the rotatable sample integrates X-ray diffraction analysis and X-ray fluorescence, is provided with the X-ray diffraction analysis component which is vertically arranged in parallel with an X-ray light path and the fluorescence detector 4 which is horizontally arranged in perpendicular to the X-ray light path, and is convenient for analyzing samples with different analysis requirements and beneficial to reducing the analysis cost. The upper and lower two-layer of double-deck revolving stage is equipped with a plurality of fluorescence analysis sample groove 511 and a plurality of diffraction analysis sample groove 521 respectively, through rotatory double-deck revolving stage can carry out the analysis to the sample that is in the sample groove of difference, has avoided the waste of time and manpower because of frequently changing the sample and causing, can reduce the loss of equipment moreover.
In this document, the terms front, back, upper and lower are used to define the components in the drawings and the positions of the components relative to each other, and are used for clarity and convenience of the technical solution. It is to be understood that the use of the directional terms should not be taken to limit the scope of the claims.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1. An X-ray fluorescence diffraction integrated analyzer of a rotatable sample, which comprises an X-ray generator, an X-ray diffraction analysis component and a fluorescence detector, and is characterized in that: the diffraction sample tray is provided with a plurality of diffraction analysis sample grooves which are in one-to-one correspondence with the plurality of light through holes, a stepping motor is connected with the double-layer rotating table through a rotating rod to drive the double-layer rotating table to rotate, the stepping motor is arranged on a fourth mounting plate, a vertical umbrella wheel is connected with the stepping motor to vertically rotate under the driving of the stepping motor, the rotating rod passes through the center of a horizontal umbrella wheel and is arranged on the fourth mounting plate through a lower bearing seat, the horizontal umbrella wheel is fixedly contacted with the rotating rod, and the engaging teeth of the vertical umbrella wheel and the horizontal umbrella wheel are mutually engaged; the X-ray diffraction analysis assembly is vertically installed in parallel with an X-ray light path and comprises a collimation adjusting module and a diffraction detection module which are vertically arranged, the collimation adjusting module comprises a micrometer displacement table and a pinhole collimator arranged on a movable surface of the micrometer displacement table, the upper end surface of the micrometer displacement table is fixed on the lower surface of a third mounting plate, the pinhole collimator is arranged on the lower end surface of the micrometer displacement table, the micrometer displacement table is provided with an X-direction adjusting handle and a Y-direction adjusting handle perpendicular to the X-direction adjusting handle, the X-direction adjusting handle and the Y-direction adjusting handle are both connected with the movable surface to adjust the coordinate of the movable surface in the X direction or the Y direction perpendicular to the X direction, the X direction and the Y direction are both perpendicular to the vertical direction, a through hole is formed in the fourth mounting plate, the diffraction detection module comprises a vacuum cavity clamped in the through hole and fixed on the fifth mounting plate downwards and a CCD detector positioned in the vacuum cavity, a beryllium window capable of allowing X-rays to penetrate through is arranged on the upper end surface of the vacuum cavity, the beryllium window is positioned below the sample diffraction detection module, the sample is positioned between the sample detection module and the fluorescence detection module, the fluorescence detection module is positioned between the second mounting plate, the fluorescence detection module is positioned between the sample mounting plate, and the fluorescence detection module, and the fluorescence detection module are positioned between the fluorescence detection module, and the fluorescence detection module are positioned between the fluorescence detection module, and the fluorescence detection module.
2. The integrated X-ray fluorescence diffraction analyzer for rotatable samples according to claim 1, wherein: the number of the fluorescence analysis sample grooves and the number of the light through holes are respectively three, and the included angle between the fluorescence analysis sample grooves and the adjacent light through holes is 60 degrees.
3. The integrated X-ray fluorescence diffraction analyzer for rotatable samples according to claim 1, wherein: the fourth mounting plate is horizontally arranged.
4. The integrated X-ray fluorescence diffraction analyzer for rotatable samples according to claim 3, wherein: the second mounting panel level sets up to be located fourth mounting panel top, a bearing mount pad through four fixed strings of lead screw locate the second mounting panel, the upper end of rotary rod passes behind the fluorescence sample tray through an bolster bearing housing install in the bearing mount pad.
5. The integrated X-ray fluorescence diffraction analyzer for rotatable samples according to claim 4, wherein: the third mounting plate is horizontally arranged and is positioned between the second mounting plate and the fourth mounting plate.
6. The integrated X-ray fluorescence diffraction analyzer for rotatable samples according to claim 4, wherein: still including the level setting be located the first mounting panel of second mounting panel top, the X ray generator is fixed in through the angle sign indicating number the lower surface of first mounting panel.
7. The integrated X-ray fluorescence diffraction analyzer for rotatable samples according to claim 4, wherein: the fluorescence detector is located between the second mounting plate and the bearing mount.
8. The integrated X-ray fluorescence diffraction analyzer for rotatable samples according to claim 3, wherein: the fluorescence sample tray and the diffraction sample tray are fixed on the rotating rod through locking nuts positioned on the upper surface and the lower surface of each fluorescence sample tray and the diffraction sample tray.
9. The integrated X-ray fluorescence diffraction analyzer for rotatable samples according to claim 3, wherein: the fifth mounting plate is horizontally arranged and located below the fourth mounting plate, an aviation socket is arranged on the bottom wall of the vacuum cavity, and the CCD detector is connected with the system control unit through the aviation socket arranged on the bottom wall of the vacuum cavity.
10. The integrated X-ray fluorescence diffraction analyzer for rotatable samples according to claim 9, wherein: the back of the CCD detector is connected with the bottom wall of the vacuum cavity through a red copper block, and a cooling fan is arranged on the outer side of the bottom wall of the vacuum cavity.
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