CN107228871B - Portable X-ray analysis device - Google Patents
Portable X-ray analysis device Download PDFInfo
- Publication number
- CN107228871B CN107228871B CN201710598573.2A CN201710598573A CN107228871B CN 107228871 B CN107228871 B CN 107228871B CN 201710598573 A CN201710598573 A CN 201710598573A CN 107228871 B CN107228871 B CN 107228871B
- Authority
- CN
- China
- Prior art keywords
- ray
- fluorescence
- sample
- diffraction
- analysis
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
- G01N23/2076—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions for spectrometry, i.e. using an analysing crystal, e.g. for measuring X-ray fluorescence spectrum of a sample with wavelength-dispersion, i.e. WDXFS
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—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 measuring secondary emission from the material
- G01N23/223—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 measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/10—Nuclear fusion reactors
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention provides a portable X-ray analysis device, which comprises an X-ray generator, an X-ray fluorescence analysis unit, an X-ray diffraction analysis unit and a spectrum analysis module, wherein the X-ray fluorescence analysis unit comprises a fluorescence sample stage for placing a fluorescence sample, the fluorescence sample stage comprises a first base which is horizontally arranged and provided with a notch and a sample loading inclined stage which is slidably arranged at the notch and provided with an inclined plane, the inclined plane is concavely provided with a placement groove, a first carrier for carrying the fluorescence sample is arranged at the placement groove, and a first through hole is positioned at the placement groove and penetrates through the sample loading inclined stage; the X-ray diffraction analysis unit comprises an X-ray collimation adjustment module, a diffraction sample table and a CCD detection module, wherein the X-ray collimation adjustment module is positioned under the first through hole, the diffraction sample table is connected with the lower end of the X-ray collimation adjustment module, and the CCD detection module is positioned under the diffraction sample table and is connected with the spectrum analysis module. The invention has the beneficial effects that: the analysis time is effectively shortened, the volume is small, the weight is light, the cost is low, and the operation in the field environment is convenient.
Description
Technical Field
The invention relates to the technical field of X-ray analysis, in particular to a portable X-ray analysis device.
Background
X-Ray Fluorescence (XRF) and X-Ray Diffraction (XRD) are two methods for mass composition analysis using different characteristics of X-rays. When a beam of X-rays is irradiated on the surface of a substance, scattering and absorption phenomena of the X-rays occur. Under certain conditions, the coherent scattering of X-rays forms diffraction fringes, and different diffraction fringes represent different material structures, so that the XRD detector is mainly used for analyzing the phase and crystal parameters of materials and is widely applied to the fields of materials, metallurgy, cement, mineral products and the like. The energy carried by the X-rays is absorbed by electrons in the material, and electron transition is generated to release fluorescent X-rays. The energy and quantity of the fluorescent X-rays are related to the element composition and content of substances, so that the X-ray fluorescent detector is mainly used for obtaining the element composition and quantitative analysis of a sample to be detected and is widely applied to mineral exploration, well logging, marine environment geological investigation and the like.
At present, in one analysis instrument, two analysis functions of XRF and XRD are realized. The adopted structure is mainly divided into two types:
(1) The combined structure mode is to assemble the main functional modules of XRF and XRD, and most of the ray source, the light path and the detector are independent, so that the analysis effect can be ensured to the greatest extent. Chinese patent CN200880007232 proposes a combined mode of common X-ray tubes, and XRD analysis adopts a goniometer-based method. Chinese patent CN201010569788 shows a combined structure of a common X-ray tube, in which XRD adopts an energy dispersion measurement method and a detector adopts a one-dimensional energy type; both of the above patents use a single sample, i.e., a sample common to XRD and XRF.
(2) Single structure mode, due to the miniaturization and portability of XRF, has become very mature, and portable research of XRD has been limited to only a few analytical instrument manufacturers. The single structure mode is adopted, and the XRF analysis function is mainly realized in the XRD analysis process. However, due to the different requirements of the two on the incident X-rays, and the fact that the fluorescence effect of the X-rays is an interference signal in the XRD analysis process, the XRD analysis effect can be reduced, and therefore, the XRF and XRD integrated instrument with a single structure mode is adopted, and the analysis function of XRD is mainly outstanding.
In recent years, miniaturization and portability of XRD analysis instruments have become important concerns for the industry. Some large XRD analysis instrument manufacturers have introduced desktop, miniaturized XRD, but are relatively few to use directly on site. The main impediments limiting portable XRD development are the inherent constraints of instrument weight, volume, and instrument performance metrics. For example, although the goniometer has high analysis accuracy and wide measurement angle range of XRD, the goniometer belongs to a precision mechanical rotating device and is inconvenient to work in a field environment.
Disclosure of Invention
In view of the above, embodiments of the present invention provide a portable X-ray analysis apparatus that can shorten analysis time, is small in size, light in weight, low in cost, and convenient to operate in a field environment.
The embodiment of the invention provides a portable X-ray analysis device, which comprises an X-ray generator, an X-ray fluorescence analysis unit, an X-ray diffraction analysis unit and a spectrum analysis module connected with the X-ray fluorescence analysis unit and the X-ray diffraction analysis unit, wherein the X-ray fluorescence analysis unit comprises a fluorescence sample stage for placing a fluorescence sample for fluorescence spectrum collection, the fluorescence sample stage comprises a first base which is horizontally arranged and provided with a notch and a sample loading inclined stage which is slidably arranged at the notch and provided with an inclined surface, the inclined surface of the sample loading inclined stage is concavely provided with a mounting groove, a first carrier for carrying the fluorescence sample is detachably arranged at the mounting groove, and a first through hole is positioned at the mounting groove and penetrates through the upper surface and the lower surface of the sample loading inclined stage; the X-ray diffraction analysis unit comprises an X-ray collimation adjustment module, a diffraction sample table and a CCD detection module, wherein the X-ray collimation adjustment module is positioned under the first through hole, the diffraction sample table is connected with the lower end of the X-ray collimation adjustment module, and the CCD detection module is positioned under the diffraction sample table and is connected with the spectrum analysis module.
Further, the X-ray fluorescence analysis unit further comprises a fluorescence detector for collecting fluorescence photons generated by secondary excitation of the fluorescent sample under the irradiation of X-rays and converting the collected fluorescence photons into fluorescence spectrum information, and a fluorescence control board connected with the fluorescence detector and used for reading the fluorescence spectrum information, and the spectrum analysis module is connected with the fluorescence control board to conduct fluorescence analysis.
Further, the inclined plane of dress appearance inclined plane with contained angle between the first base is 45, be equipped with on the side that is on the back of the side surface of dress appearance inclined plane with fluorescence detector is convenient to stimulate dress appearance inclined plane is relative the gliding handle of first base, the centre of first slide is circular sunken, fluorescence sample place in circular sunken.
Further, the portable X-ray analysis apparatus further includes a support structure including a mounting top plate at an upper end for mounting the fluorescence detector and the fluorescence sample stage, a mounting bottom plate at a lower end for mounting the CCD detection module, and a housing connecting the mounting top plate and the mounting bottom plate.
Further, the spectrum analysis module is located in the PC, a memory card is further arranged in the PC, the CCD detection module is connected with the spectrum analysis module through a diffraction control board, the diffraction control board comprises a CCD driving module used for driving the CCD detection module to operate and a diffraction preprocessing module used for receiving and processing each frame of spectrum image sent by the CCD detection module, the diffraction preprocessing module is connected with the memory card to transmit the processed spectrum image to the memory card for storage, and the diffraction preprocessing module is connected with the spectrum analysis module to transmit the processed spectrum image to the spectrum analysis module for sample crystal structure analysis.
Further, the CCD detection module comprises a beryllium window flange, a base flange and a hollow adapter flange which is connected with the beryllium window flange and the base flange, an X-ray permeable beryllium window is arranged at the center of the beryllium window flange, a vacuum cavity is formed by the side wall of the adapter flange, the base flange and the beryllium window in a surrounding mode, the CCD detection module further comprises a CCD detector, the CCD detector is located in the vacuum cavity and connected with a heat dissipation structure, and pins of the CCD detector are connected with the diffraction control board through aviation sockets arranged on the base flange.
Further, the heat radiation structure is including locating in the vacuum chamber and with the copper base plate that the inner wall of adapter flange is connected, and be located red copper frame and the indium piece in vacuum chamber, the back of CCD detector loops through the indium piece with red copper frame with base flange joint, the base flange outside is equipped with radiator fan, the copper base plate with the pin connection of CCD detector is used for with heat transfer on the CCD detector arrives the cavity in vacuum chamber and pass through the cavity gives off heat to the external world.
Further, the diffraction sample stage comprises a second base and a dovetail groove type flat plate, the second base is arranged horizontally, the dovetail groove type flat plate is slidably arranged on the second base, the second base is connected with the X-ray collimation adjustment module, a groove is formed in the upper surface of the second base in a downward concave mode, a second through hole is formed in the groove and penetrates through the upper surface and the lower surface of the second base, a second carrier sheet is mounted in the groove, a metal sheet layer is respectively coated on the upper surface and the lower surface of the second carrier sheet, through holes for placing diffraction samples used for collecting diffraction spectrums are formed in positions, corresponding to the second through holes, of the second carrier sheet, and organic films capable of preventing the diffraction samples from splashing and allowing X-rays to pass through are adhered in the through holes.
Further, the X-ray generator comprises an X-ray tube, a high-voltage power supply connected with the X-ray tube so as to enable a target material inside the X-ray tube to excite X-rays with a continuous spectrum, and an output regulator for reducing the spectrum width and the irradiation angle of the X-ray energy.
Further, the X-ray collimation adjustment module comprises an upper lead sheet and a lower lead sheet which are provided with round holes and are arranged up and down, and the round holes of the upper lead sheet and the round holes of the lower lead sheet are mutually aligned.
The technical scheme provided by the embodiment of the invention has the beneficial effects that: the portable X-ray analysis device provided by the invention has the advantages that (1) the two-dimensional CCD detection module is adopted, the goniometer is omitted, diffraction information within a certain angle range can be obtained at the same time, the analysis time is shortened, the self weight of the device is reduced, and the portable X-ray analysis device has the characteristics of portability and is beneficial to field application. (2) The X-ray diffraction analysis (XRD analysis) and the X-ray diffraction analysis (XRF analysis) share one set of X-ray generator, so that the volume of the instrument is reduced, the cost is saved, the structural design of the instrument is facilitated, and the radiation of X-rays is reduced. (3) The optical paths of the X-ray diffraction analysis (XRD analysis) and the X-ray diffraction analysis (XRF analysis) are mutually independent, so that mutual interference does not exist, and the analysis effect of the device is ensured.
Drawings
FIG. 1 is a schematic view showing the overall structure of a portable X-ray analysis apparatus according to the present invention;
FIG. 2 is a front view of a fluorescent sample stage of the portable X-ray analysis apparatus of the present invention;
FIG. 3 is a top view of FIG. 2;
FIG. 4 is a bottom view of a diffraction sample stage of the portable X-ray analysis apparatus of the present invention;
fig. 5 is a schematic structural view of a CCD detection module of the portable X-ray analysis apparatus of the present invention.
Detailed Description
For the purpose of making 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. 1, an embodiment of the present invention provides a portable X-ray analysis device, which includes an X-ray generator 1, an X-ray fluorescence analysis unit, an X-ray diffraction analysis unit, and a spectrum analysis module connected to the X-ray fluorescence analysis unit and the X-ray diffraction analysis unit.
Referring to fig. 1, the portable X-ray analysis apparatus further includes a support structure including a mounting top plate 41 at an upper end, a mounting bottom plate 40 at a lower end, and a housing 8 connecting the mounting top plate 41 and the mounting bottom plate 40. The mounting top plate 41, the mounting bottom plate 40 and the housing 8 together form a closed space for isolating from the outside, and the closed space can prevent external light from being emitted into the interior to interfere with the internal X-rays and prevent the internal X-rays from being emitted to cause radiation pollution.
The X-ray generator 1 comprises an X-ray tube, a high-voltage power supply connected with the X-ray tube for exciting a target material inside the X-ray tube to emit X-rays with a continuous spectrum, and an output regulator for reducing the spectrum width and the irradiation angle of the X-ray energy. The input end of the high-voltage power supply is connected with an external low-voltage direct-current power supply, and the voltage output by the output end of the high-voltage power supply and the output current are continuous and adjustable. Under the excitation of the high-voltage power supply, the X-ray tube excites X-rays with continuous spectrums, but the photon energy spectrum of the X-rays is relatively wide, so that XRD analysis is not facilitated, a part of photons with higher energy in the X-rays are filtered out through the output regulator, and meanwhile, the irradiation angle of the X-rays is converged to a smaller range, so that the demand of XRD analysis can be met.
Referring to fig. 1, 2 and 3, the X-ray fluorescence analysis unit is used for XRF analysis, and includes a fluorescence sample stage 2 for placing a fluorescence sample for fluorescence spectrum collection, the fluorescence sample stage 2 includes a first base 11 horizontally arranged and a sample loading ramp 12 having an inclined plane, an included angle between the sample loading ramp 12 and the first base 11 is 45 °, the first base 11 has a notch, two opposite sides of the notch are provided with first sliding grooves, the sample loading ramp 12 is clamped in the first sliding grooves, a handle 14 for conveniently pulling the sample loading ramp 12 to slide relative to the first base 11 is provided on a side surface of the sample loading ramp 12, the sample loading ramp 12 can slide along the first sliding grooves under the action of external force, and can slide out of the first base 11 according to needs, so as to facilitate replacement of the fluorescence sample. The inclined surface of the sample loading inclined table 12 is concavely provided with a placement groove, a first sample carrying sheet 13 for carrying the fluorescent sample is detachably arranged in the placement groove, the middle of the first sample carrying sheet 13 is a circular recess 19, the fluorescent sample is arranged in the circular recess 19, the inclined surface of the sample loading inclined table 12 is provided with a plurality of fixing holes 17, the first sample carrying sheet 13 is fixed on the inclined surface of the sample loading inclined table 12 through the cooperation of a plurality of fixing screws and the plurality of fixing holes 17, and the fluorescent sample is a powdery sample. A first through hole 18 is located in the mounting groove and penetrates through the upper and lower surfaces of the sample loading ramp 12, and the upper surface of the sample loading ramp 12 is the inclined surface. The upper surface of the first base 11 is further provided with a plurality of first mounting holes 15 for mounting a housing for shielding the X-ray light path, and the fluorescent sample stage 2 is fixed to the mounting top plate 41 of the supporting structure through the housing.
The X-ray fluorescence analysis unit further comprises a fluorescence detector 7 for collecting fluorescence photons generated by secondary excitation of the fluorescent sample under the irradiation of X-rays and converting the collected fluorescence photons into fluorescence spectrum information, and a fluorescence control board 9 connected with the fluorescence detector 7 and used for reading the fluorescence spectrum information, wherein the spectrum analysis module is connected with the fluorescence control board 9 for fluorescence analysis. The fluorescence detector 7 is mounted on the mounting top plate 41 of the supporting structure, and the fluorescence control plate 9 is located outside the closed space.
Referring to fig. 1 and 4, the X-ray diffraction analysis unit is used for XRD analysis, and includes an X-ray collimation adjustment module 3 located right below the first through hole 18, a plurality of second mounting holes 16 are further formed on the first base 11 for mounting the X-ray collimation adjustment module 3, and the X-ray collimation adjustment module 3 includes an upper lead sheet and a lower lead sheet, which have circular holes and are disposed up and down, and the circular holes of the upper lead sheet and the circular holes of the lower lead sheet are aligned with each other. The superimposed round holes form a photon channel of X-rays, the aperture of the round holes is smaller, namely the aperture of the channel is smaller, X-ray photons with larger included angles between the movement track and the channel can strike the upper lead sheet or the lower lead sheet and cannot be emitted from the channel, so that the number of the X-ray photons irradiated on a diffraction sample is small, and a single photon counting mode required by XRD analysis is met. The effective aperture of the channel can be further reduced by staggering the round holes of the upper lead sheet and the lower lead sheet by a proper distance, so that the included angle between the X-ray photons emitted from the channel and the channel is smaller, and the collimation effect is achieved.
Referring to fig. 1 and 4, the X-ray diffraction analysis unit further includes a diffraction sample stage 4 located below the X-ray collimation adjustment module 3 and connected to the X-ray collimation adjustment module 3, and a CCD detection module 5 located below the diffraction sample stage 4 and connected to the spectrum analysis module. The diffraction sample table 4 comprises a second base and a dovetail groove type flat plate 38 which are horizontally arranged, a second sliding groove is formed in the second base, the dovetail groove type flat plate 38 is clamped in the second sliding groove, one end of the dovetail groove type flat plate 38 is connected with a baffle 36, a handle 37 is arranged on the outer side of the baffle 36, the dovetail groove type flat plate 38 can slide along the second sliding groove under the action of external force pulling the handle 37, and the dovetail groove type flat plate 38 can slide out of the second base under the condition that the requirement is met, so that a sample can be replaced conveniently. The second base is connected with the X-ray collimation adjustment module 3, a groove is concavely arranged in the central area of the lower surface of the dovetail groove type flat plate 38, a second carrying sheet 22 is installed in the groove through the cooperation of screws and screw holes 24 of the groove, a second through hole is positioned in the groove and extends upwards to penetrate through the upper surface and the lower surface of the second base, a layer of metal sheet layer is respectively covered on the upper surface and the lower surface of the second carrying sheet 22, a through hole 23 for placing diffraction samples used for collecting diffraction spectrums is arranged on the position, corresponding to the second through hole, of the second carrying sheet 22, and an organic film which prevents the diffraction samples from splashing and allows the X-rays to pass through is stuck in the through hole 23. The through hole 23 in the middle of the second slide 22 is aligned with the central axis of the second through hole, facilitating the passage of diffracted light. In loading, the metal sheet layer on the upper surface of the second slide 22 is removed, and the diffraction sample is put into the through hole 23, and then the metal sheet layer on the upper surface is mounted so as to be adhered to the upper surface of the second slide 22.
The spectrum analysis module is positioned in the PC, and a memory card is also arranged in the PC. The CCD detection module 5 is connected with the spectrum analysis module through the diffraction control board 6, the diffraction control board 6 comprises a CCD driving module used for driving the CCD detection module 5 to operate and a diffraction preprocessing module used for receiving and processing each frame of spectrum image sent by the CCD detection module 5, the diffraction preprocessing module is connected with the memory card to transmit the processed spectrum image to the memory card for storage, and meanwhile, the diffraction preprocessing module is connected with the spectrum analysis module to transmit the processed spectrum image to the spectrum analysis module for sample crystal structure analysis.
Referring to fig. 5, the CCD detection module 5 includes a beryllium window flange 25, a base flange 27, and an adapter flange 26 connecting the beryllium window flange 25 and the base flange 27 and hollow inside, wherein a beryllium window 28 through which X-rays can pass is disposed at a central position of the beryllium window flange 25, and the beryllium window 28 is made of metal beryllium and has good X-ray projectivity. The adapter flange 26, the base flange 27, the beryllium window 28 and/or the beryllium window flange 25 together enclose a vacuum cavity, the CCD detection module 5 further includes a CCD detector 29, and the CCD detector 29 is located in the vacuum cavity and connected with a heat dissipation structure. The heat radiation structure is including locating in the vacuum chamber and with the copper base plate 31 that the inner wall of adapter flange 26 is connected, and be located red copper frame 32 and the indium piece 30 in vacuum chamber, the back of CCD detector 29 loops through indium piece 30 with red copper frame 32 with base flange 27 is connected, the outside radiator fan that is equipped with of base flange 27, indium piece 30 with red copper frame 32 all has fine heat conductivity, indium piece 30 plays the thermal buffering effect. The copper substrate 31 is connected with pins of the CCD detector 29 to transfer heat on the CCD detector 29 to the cavity of the vacuum cavity, the heat is emitted to the outside through the cavity, the pins of the CCD detector 29 are connected with a plurality of wires 34 welded on the copper substrate 31 through the copper substrate 31, the wires 34 are connected with an aviation socket 33 arranged on the base flange 27, the aviation socket 33 on the base flange 27 is connected with the diffraction control board 6, and finally the connection between the CCD detector 29 and the diffraction control board 6 is realized.
When the X-ray fluorescence analysis is required, the first slide 13 is placed in the placement groove, so that the first slide 13 shields the first through hole 18, the X-rays are prevented from being emitted into the following X-ray collimation adjustment module 3 and the subsequent elements through the first through hole 18, a fluorescent sample on the first slide 13 generates a fluorescent effect under the irradiation of the X-rays, and fluorescent photons are generated by secondary excitation, the fluorescent photons are collected by the fluorescent detector 7 and converted into fluorescent spectrum information, the fluorescent spectrum information is read by the fluorescent control board 9, the fluorescent spectrum information read by the fluorescent control board is transmitted to the spectrum analysis module, and then the spectrum analysis module performs the X-ray fluorescence analysis according to the fluorescent spectrum information.
When the X-ray diffraction analysis is required, the first slide 13 on the fluorescent sample stage 2 is taken down, the first through hole 18 is exposed, the X-ray passes through the first through hole 18, irradiates the X-ray collimation adjustment module 3 and the subsequent elements thereof, irradiates the diffraction sample after being collimated by the X-ray collimation adjustment module 3, then detects the photon pixel unit of the X-ray transmitted through the diffraction sample by the CCD detection module 5, converts the photon pixel unit into electric charge, and the diffraction control board 6 reads the electric charge of each pixel after the exposure period of the CCD detection module 5 is finished, and transmits the electric charge to the spectrum analysis module for the X-ray diffraction analysis after processing.
The technical scheme provided by the embodiment of the invention has the beneficial effects that: the portable X-ray analysis device provided by the invention has the advantages that (1) the two-dimensional CCD detection module 5 is adopted, the goniometer is omitted, diffraction information within a certain angle range can be obtained at the same time, the analysis time is shortened, the self weight of the device is reduced, and the portable X-ray analysis device has the characteristics of portability and is beneficial to field application. (2) The X-ray diffraction analysis (XRD analysis) and the X-ray diffraction analysis (XRF analysis) share the same set of X-ray generator 1, so that the volume of the instrument is reduced, the cost is saved, the structural design of the instrument is facilitated, and the radiation of X-rays is reduced. (3) The optical paths of the X-ray diffraction analysis (XRD analysis) and the X-ray diffraction analysis (XRF analysis) are mutually independent, so that mutual interference does not exist, and the analysis effect of the device is ensured.
In this document, terms such as front, rear, upper, lower, etc. are defined with respect to the positions of the components in the drawings and with respect to each other, for clarity and convenience in expressing the technical solution. It should be understood that the use of such orientation terms should not limit the scope of the protection sought herein.
The embodiments described above and features of the embodiments herein may be combined with each other without conflict.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (7)
1. The utility model provides a portable X ray analysis device, includes X ray generator, X ray fluorescence analysis unit, X ray diffraction analysis unit and with X ray fluorescence analysis unit with the spectral analysis module that X ray diffraction analysis unit is connected, its characterized in that: the X-ray fluorescence analysis unit comprises a fluorescence sample stage for placing a fluorescence sample for fluorescence spectrum collection, wherein the fluorescence sample stage comprises a first base which is horizontally arranged and provided with a notch and a sample loading inclined stage which is slidably arranged on the notch and provided with an inclined surface, the inclined surface of the sample loading inclined stage is concavely provided with a placement groove, a first slide for bearing the fluorescence sample is detachably arranged in the placement groove, and a first through hole is positioned in the placement groove and penetrates through the upper surface and the lower surface of the sample loading inclined stage; the X-ray diffraction analysis unit comprises an X-ray collimation adjustment module, a diffraction sample table and a CCD detection module, wherein the X-ray collimation adjustment module is positioned under the first through hole, the diffraction sample table is connected with the lower end of the X-ray collimation adjustment module, and the CCD detection module is positioned under the diffraction sample table and is connected with the spectrum analysis module;
the X-ray fluorescence analysis unit further comprises a fluorescence detector for collecting fluorescence photons generated by secondary excitation of the fluorescent sample under the irradiation of X rays and converting the collected fluorescence photons into fluorescence spectrum information, and a fluorescence control board connected with the fluorescence detector and used for reading the fluorescence spectrum information, wherein the spectrum analysis module is connected with the fluorescence control board for fluorescence analysis;
the included angle between the inclined surface of the sample loading inclined table and the first base is 45 degrees, a handle which is convenient to pull the sample loading inclined table to slide relative to the first base is arranged on one side, opposite to the fluorescent detector, of the side surface of the sample loading inclined table, a circular recess is formed in the middle of the first slide, and the fluorescent sample is placed in the circular recess;
the diffraction sample stage comprises a second base and a dovetail groove type flat plate, wherein the second base is horizontally arranged, the dovetail groove type flat plate is slidably arranged on the second base, the second base is connected with the X-ray collimation adjustment module, a groove is concavely formed in the lower surface of the dovetail groove type flat plate upwards, a second through hole is formed in the groove and extends upwards to penetrate through the upper surface and the lower surface of the second base, a second carrier is mounted in the groove, a metal sheet layer is respectively coated on the upper surface and the lower surface of the second carrier, a through hole for placing a diffraction sample used for collecting diffraction spectrums is formed in the position, corresponding to the second through hole, of the second carrier, and an organic film which can prevent the diffraction sample from splashing and allow X-rays to pass through is adhered in the through hole;
placing a first slide in the placement slot, covering the first through hole; the fluorescent sample on the first slide is irradiated by the X-rays emitted by the X-ray generator to generate a fluorescent effect in the irradiation of the X-rays, so that X-ray fluorescence analysis is performed;
taking down the first slide, enabling an X-ray generator to emit X-rays to pass through the first through hole, and irradiating the X-rays to the diffraction sample after being collimated by the X-ray collimation adjusting module; thereby performing X-ray diffraction analysis.
2. The portable X-ray analysis apparatus of claim 1, wherein: the portable X-ray analysis device further comprises a supporting structure, wherein the supporting structure comprises a mounting top plate, a mounting bottom plate and a shell, the mounting top plate is arranged at the upper end and used for mounting the fluorescence detector and the fluorescence sample table, the mounting bottom plate is arranged at the lower end and used for mounting the CCD detection module, and the shell is connected with the mounting top plate and the mounting bottom plate.
3. The portable X-ray analysis apparatus of claim 1, wherein: the optical spectrum analysis module is located in the PC, a memory card is further arranged in the PC, the CCD detection module is connected with the optical spectrum analysis module through a diffraction control board, the diffraction control board comprises a CCD driving module used for driving the CCD detection module to operate and a diffraction preprocessing module used for receiving and processing each frame of optical spectrum image sent by the CCD detection module, the diffraction preprocessing module is connected with the memory card to transmit the processed optical spectrum image to the memory card for storage, and the diffraction preprocessing module is connected with the optical spectrum analysis module to transmit the processed optical spectrum image to the optical spectrum analysis module for sample crystal structure analysis.
4. A portable X-ray analysis apparatus according to claim 3, wherein: the CCD detection module comprises a beryllium window flange, a base flange and a hollow adapter flange, wherein the beryllium window flange is connected with the base flange, the beryllium window is arranged at the center of the beryllium window flange, the X-rays can penetrate through the beryllium window, the side wall of the adapter flange, the base flange and the beryllium window jointly enclose a vacuum cavity, the CCD detection module further comprises a CCD detector, the CCD detector is located in the vacuum cavity and connected with a heat dissipation structure, and pins of the CCD detector are connected with the diffraction control board through aviation sockets arranged on the base flange.
5. The portable X-ray analysis apparatus of claim 4, wherein: the heat radiation structure is including locating in the vacuum chamber and with adapter flange's the copper base plate of inner wall connection, and be located red copper frame and the indium piece in vacuum chamber, the back of CCD detector loops through the indium piece with red copper frame with base flange connects, the base flange outside is equipped with radiator fan, the copper base plate with CCD detector's pin connection is used for with heat transfer on the CCD detector arrives the cavity in vacuum chamber and pass through the cavity gives off heat to the external world.
6. The portable X-ray analysis apparatus of claim 1, wherein: the X-ray generator comprises an X-ray tube, a high-voltage power supply connected with the X-ray tube so as to enable a target material inside the X-ray tube to excite X-rays with a continuous spectrum, and an output regulator for reducing the spectrum width and the irradiation angle of the X-ray energy.
7. The portable X-ray analysis apparatus of claim 1, wherein: the X-ray collimation adjusting module comprises an upper lead sheet and a lower lead sheet which are provided with round holes and are arranged up and down, and the round holes of the upper lead sheet and the round holes of the lower lead sheet are mutually aligned.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710598573.2A CN107228871B (en) | 2017-07-21 | 2017-07-21 | Portable X-ray analysis device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710598573.2A CN107228871B (en) | 2017-07-21 | 2017-07-21 | Portable X-ray analysis device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107228871A CN107228871A (en) | 2017-10-03 |
| CN107228871B true CN107228871B (en) | 2023-07-04 |
Family
ID=59957614
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710598573.2A Active CN107228871B (en) | 2017-07-21 | 2017-07-21 | Portable X-ray analysis device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107228871B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108267467A (en) * | 2018-03-26 | 2018-07-10 | 中国地质大学（武汉） | A kind of portable multi-purpose X-ray analyzer |
| CN112432964A (en) * | 2020-12-16 | 2021-03-02 | 中国科学院广州能源研究所 | Sample holder for natural gas hydrate X-ray diffractometer test and application thereof |
| EP4019951A1 (en) | 2020-12-24 | 2022-06-29 | Inel S.A.S | Apparatuses and methods for combined simultaneous analyses of materials |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3919549A (en) * | 1972-03-17 | 1975-11-11 | Aquitaine Petrole | Portable X-ray spectrometer |
| JPH0572106A (en) * | 1991-09-17 | 1993-03-23 | Shimadzu Corp | Particle size distribution measuring device |
| CN1618258A (en) * | 2001-12-04 | 2005-05-18 | X射线光学系统公司 | X-ray source assembly having enhanced output stability, and fluid stream analysis applications thereof |
| GB0921965D0 (en) * | 2009-12-17 | 2010-02-03 | Thermo Fisher Scient Ecublens | Method and apparatus for performing x-ray analysis of a sample |
| CN102435625A (en) * | 2011-12-27 | 2012-05-02 | 东莞新能源科技有限公司 | Method and sample shelf for X-ray diffraction in-situ test |
| CN206020313U (en) * | 2016-09-09 | 2017-03-15 | 广州市怡文环境科技股份有限公司 | A kind of total reflection X-ray fluorescence analysis device |
Family Cites Families (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2930466B2 (en) * | 1992-02-14 | 1999-08-03 | 三菱重工業株式会社 | 2D image radiation detector |
| JP2999072B2 (en) * | 1992-08-25 | 2000-01-17 | 三菱重工業株式会社 | Surface analyzer |
| JP3593412B2 (en) * | 1996-03-26 | 2004-11-24 | 株式会社リガク | X-ray analyzer and attachment for X-ray fluorescence analysis |
| US6542578B2 (en) * | 1999-11-13 | 2003-04-01 | Heimann Systems Gmbh | Apparatus for determining the crystalline and polycrystalline materials of an item |
| JP2003139724A (en) * | 2001-11-01 | 2003-05-14 | Hitachi Ltd | Ct unit |
| CN1270176C (en) * | 2002-12-02 | 2006-08-16 | 中国科学技术大学 | Method and apparatus for measuring and analyzing structure and component of combined sample |
| DE102005039642B3 (en) * | 2005-08-22 | 2007-02-22 | Yxlon International Security Gmbh | Collimator system for x-ray diffractometery, e.g. for luggage inspection, has primary collimator with ring-shaped opening, and secondary collimator with cylindrical- and conical-surface apertures |
| GB2447252B (en) * | 2007-03-06 | 2012-03-14 | Thermo Fisher Scientific Inc | X-ray analysis instrument |
| WO2009043095A1 (en) * | 2007-10-03 | 2009-04-09 | Commonwealth Scientific And Industrial Research Organisation | An online energy dispersive x-ray diffraction analyser |
| CN102830004B (en) * | 2012-08-28 | 2014-11-12 | 浙江世纪康大医疗科技有限公司 | Low-resistance horizontal sample shelf mechanism |
| EP2722866A1 (en) * | 2012-10-22 | 2014-04-23 | Fei Company | Configurable charged-particle beam apparatus |
| CN105938113B (en) * | 2015-03-03 | 2020-03-27 | 马尔文帕纳科公司 | Quantitative X-ray analysis-multi-light path instrument |
| CN105651801B (en) * | 2015-12-30 | 2018-10-16 | 北京矿冶研究总院 | Online analysis method for ore pulp minerals |
| CN105806860A (en) * | 2016-03-08 | 2016-07-27 | 中国科学院上海应用物理研究所 | Full-field X-ray imaging system and full-field X-ray imaging method |
| CN106124540A (en) * | 2016-06-20 | 2016-11-16 | 同济大学 | A kind of X-ray diffraction back pressure method of preferred orientation that can reduce is through sample board |
| CN106595764A (en) * | 2016-12-15 | 2017-04-26 | 中国地质大学（武汉） | Distributive detecting and analyzing system in combination with XRD and XRF |
| CN207198068U (en) * | 2017-07-21 | 2018-04-06 | 中国地质大学（武汉） | A kind of Portable X-ray analysis device |
-
2017
- 2017-07-21 CN CN201710598573.2A patent/CN107228871B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3919549A (en) * | 1972-03-17 | 1975-11-11 | Aquitaine Petrole | Portable X-ray spectrometer |
| JPH0572106A (en) * | 1991-09-17 | 1993-03-23 | Shimadzu Corp | Particle size distribution measuring device |
| CN1618258A (en) * | 2001-12-04 | 2005-05-18 | X射线光学系统公司 | X-ray source assembly having enhanced output stability, and fluid stream analysis applications thereof |
| GB0921965D0 (en) * | 2009-12-17 | 2010-02-03 | Thermo Fisher Scient Ecublens | Method and apparatus for performing x-ray analysis of a sample |
| CN102435625A (en) * | 2011-12-27 | 2012-05-02 | 东莞新能源科技有限公司 | Method and sample shelf for X-ray diffraction in-situ test |
| CN206020313U (en) * | 2016-09-09 | 2017-03-15 | 广州市怡文环境科技股份有限公司 | A kind of total reflection X-ray fluorescence analysis device |
Non-Patent Citations (3)
| Title |
|---|
| An innovative combination of non-invasive UV–Visible-FORS, XRD and XRF techniques to study Roman wall paintings from Seville, Spain;Isabel Garofano et al.;Journal of Cultural Heritage;全文 * |
| X 射线荧光光谱仪的发展及应用;胡波 等;核电子学与探测技术;第35卷(第7期);全文 * |
| 波长色散型X射线荧光光谱仪与能量色散型X射线荧光光谱仪的比较;宋苏环,黄衍信,谢涛,张兰;现代仪器(第06期);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107228871A (en) | 2017-10-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Németh et al. | Laboratory von Hámos X-ray spectroscopy for routine sample characterization | |
| Rosasco et al. | The analysis of discrete fine particles by Raman spectroscopy | |
| CN107228871B (en) | Portable X-ray analysis device | |
| CN107238620B (en) | X-ray fluorescence diffraction integrated analyzer of rotatable sample | |
| Gianoncelli et al. | Simultaneous soft X-ray transmission and emission microscopy | |
| JP2843319B1 (en) | Microstrip gas chamber high-speed data acquisition system and sample measurement method using the same | |
| CN101144786B (en) | Portable soil heavy metal analyzer | |
| Cuevas et al. | Portable energy dispersive X-ray fluorescence and X-ray diffraction and radiography system for archaeometry | |
| Acquafredda | XRF technique | |
| CN102628950B (en) | Device for performing performance test on X-ray flat panel detector | |
| US9408583B2 (en) | Portable gamma camera | |
| Wobrauschek et al. | A novel vacuum spectrometer for total reflection x-ray fluorescence analysis with two exchangeable low power x-ray sources for the analysis of low, medium, and high Z elements in sequence | |
| CN114729907A (en) | System and method for computed tomography fluorescence imaging | |
| US3944822A (en) | Polarization excitation device for X-ray fluorescence analysis | |
| Szalóki et al. | Confocal macro X‐ray fluorescence spectrometer on commercial 3D printer | |
| US3433954A (en) | Semiconductor x-ray emission spectrometer | |
| US11796492B2 (en) | Apparatuses and methods for combined simultaneous analyses of materials | |
| Sahle et al. | Improving the spatial and statistical accuracy in X-ray Raman scattering based direct tomography | |
| Crittin et al. | The new prompt gamma-ray activation facility at the Paul Scherrer Institute, Switzerland | |
| CN207198068U (en) | A kind of Portable X-ray analysis device | |
| JP3982732B2 (en) | X-ray fluorescence measurement equipment | |
| Yiming et al. | An investigation of X-ray fluorescence analysis with an X-ray focusing system (X-ray lens) | |
| CN201126429Y (en) | Portable soil heavy metal analyzer | |
| Moss et al. | miniPixD: a compact sample analysis system which combines X-ray imaging and diffraction | |
| Bufon et al. | A novel multi-cell silicon drift detector for Low Energy X-Ray Fluorescence (LEXRF) spectroscopy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |