CN212301375U - High-pressure X-ray diffractometer - Google Patents
High-pressure X-ray diffractometer Download PDFInfo
- Publication number
- CN212301375U CN212301375U CN202021924917.8U CN202021924917U CN212301375U CN 212301375 U CN212301375 U CN 212301375U CN 202021924917 U CN202021924917 U CN 202021924917U CN 212301375 U CN212301375 U CN 212301375U
- Authority
- CN
- China
- Prior art keywords
- ray
- sample
- detector
- needle tube
- electric
- 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
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The utility model discloses a high pressure X ray diffractometer, including X ray generator, X ray focusing lens, needle tubing, microscope, X ray detector, face detector and sample adjustment table, the X ray focusing lens sets up on X ray generator, needle tubing one end sets up on the X ray focusing lens, the other end of needle tubing is the taper type structure, the face detector is located needle tubing one side, and is located the transmission direction of the X ray of X ray generator transmission, the taper type end of needle tubing is towards the face detector, the sample adjustment table is located between needle tubing and the face detector, the microscope is located one side of sample adjustment table. The utility model can be used for high-pressure powder or single crystal X-ray diffraction; the distance from the sample to the surface detector can be ensured to be unchanged, and the obtained diffraction data is more credible; the X-ray irradiated on the sample can be ensured to be minimum in size, and the phenomenon that the light spot is overlarge and is irradiated on the sealing pad is avoided; the adjustment is accomplished by electrical control, and the experimenter is away from the X-ray irradiation.
Description
Technical Field
The utility model relates to an X-ray diffraction technical field specifically is X-ray diffraction device that small sample is in high pressure device.
Background
The X-ray diffraction method is one of the important means for studying the crystal structure. The X-ray diffraction under high pressure has high requirements on an X-ray light source due to the limitation of sample tiny, high-pressure devices and the like, namely, the X-ray light spot is small, the luminous flux is high and the like. The synchrotron radiation light source is the main light source used in the high-voltage experiment at present, but the service time of the synchrotron radiation light source is limited, along with the development of science and technology, the traditional X-ray machine is developed greatly, and the requirements of the high-voltage experiment are met by the intensity of the light source and the size of light spots. The X-ray diffractometer used in the laboratory is not limited in use time, and is a good diagnosis device for high-pressure samples.
At present, the angular dispersion diffraction method is widely used in the experiment of high-pressure X-ray diffraction, i.e. monochromatic X-rays are used to irradiate on the crystal, and the emergent diffracted light is received by the surface detector. If the sample is powdered, the diffracted light forms a ring on the detector; whereas if the sample is monocrystalline, the diffracted light forms a spot on the detector. Therefore, two diffraction techniques, a powder angular dispersion X-ray diffraction technique and a single crystal angular dispersion X-ray diffraction technique, are formed depending on the sample. The diffraction is generated under the condition that the incident light angle and wavelength must meet the bragg equation, and 2dsin θ is n λ, where λ is the incident X-ray wavelength, d interplanar spacing, and θ is the angle between the incident X-ray and the interplanar.
Due to the different grain directions in the powder, the diffraction signal can be obtained with the sample stationary. And the single crystal diffraction can obtain a diffraction signal which accords with a Bragg equation only by rotating a sample.
Due to the particularity of the high-pressure X-ray diffraction experiment, special requirements are imposed on an X-ray diffractometer used in a laboratory. The method mainly comprises the following aspects:
1) brightness of light source: since the experiment requires high pressure, the sample size is small and the diffraction is weak. In order to obtain a better diffraction signal, a high brightness light source is required, which is one of the key conditions for high voltage diffraction experiments.
2) X-ray wavelength: the limited number of diffraction peaks due to the limitation of the diffraction opening angle (typically 2 θ ═ 25 degrees) of the DAC device is disadvantageous for the structure of the solved substance. According to the bragg formula, the shorter the wavelength is at a certain diffraction angle, the more diffraction peaks are obtained, and the X-rays are absorbed by the diamond due to the passage of the X-rays through the diamond anvil (both incident and diffracted light pass), while the shorter the wavelength is, the less. From both aspects, it can be seen that the short wavelength is advantageous for high pressure X-ray diffraction.
3) Spot size: the pressure achieved by the sample is directly related to the anvil face diameter and sample chamber size, and to achieve very high pressures, the anvil face diameter and sample chamber size are sufficiently small. The sample pressure of 120GPa, the sample cavity is generally less than 100 microns, so that the light spot of an X-ray diffractometer is required to be not more than 70X 70 microns2。
4) Diffraction resolution: the diffraction resolution is dependent on factors such as the emittance of the light source, the X-ray wavelength and the sample-to-detector distance. The smaller the emittance of the light source, the better; the longer the wavelength of the X-ray is, the diffraction peak moves to a high angle, which is beneficial to separating adjacent diffraction peaks and increasing the diffraction resolution; the distance between the sample and the detector is increased, so that adjacent diffraction peaks can be separated, and diffraction resolution is increased. The first two are related to the X-ray source, and the last term is to calculate the sample-to-detector distance based on the diffraction field angle of the DAC and the detector size, in principle, the diffraction resolution is increased as much as possible, i.e. the distance is increased, thus requiring a large-size detector.
5) Sample positioning: since the sample is in a high pressure apparatus, special methods are required to determine the distance of the sample from the X-ray alignment and detector.
According to the characteristics of the high-voltage X-ray diffraction experiment, an X-ray generator is selected to meet the following requirements: because X-rays need to pass through the diamond anvil to irradiate a sample and diffraction signals also need to pass through the diamond anvil to irradiate a detector, the wavelength of the X-rays needs to be short, and the X-rays have strong penetrating power and are absorbed by the diamond anvil otherwise; the high pressure experiments require a small sample size, which requires a high X-ray intensity, otherwise no diffraction signal can be observed.
In order to generate extremely high pressure, the diameter of an anvil surface of the diamond anvil is very small, generally about 300 micrometers, the diameter of a sample cavity is generally smaller than 200 micrometers, and the diameter of a sample is smaller than 100 micrometers, so that a light spot irradiated on the sample is required to be smaller than 100 micrometers, and the X-ray generated by the conventional X-ray generator is larger and larger along with the increase of the transmission distance, so that the requirement of a high-pressure experiment cannot be met.
The X-ray diffractometer on the current market is not suitable for high-pressure diffraction experiments.
SUMMERY OF THE UTILITY MODEL
In view of the technical deficiencies of the prior art, it is an object of the present invention to provide a high pressure X-ray diffractometer which is specifically adapted for high pressure powder or single crystal X-ray diffraction.
In order to solve the technical problem, the utility model adopts the following technical scheme:
the high-voltage X-ray diffractometer is characterized by comprising an X-ray generator, an X-ray focusing mirror, a needle tube, a microscope, an X-ray detector, a surface detector and a sample adjusting platform, wherein the X-ray focusing mirror is arranged on the X-ray generator, one end of the needle tube is arranged on the X-ray focusing mirror, the other end of the needle tube is of a conical structure, the surface detector is positioned on one side of the needle tube and is positioned in the transmission direction of X-rays emitted by the X-ray generator, the conical end of the needle tube faces the surface detector, the sample adjusting platform is positioned between the needle tube and the surface detector, the microscope is positioned on one side of the sample adjusting platform, the X-ray detector is positioned between the sample adjusting platform and the surface detector, the sample adjusting platform is a 5-axis or 6-axis electric platform, and comprises an electric rotary platform and four or five electric displacement platforms, the needle tube, the X-ray focusing lens, the emission port of the X-ray generator, the X-ray detector and the center line of the surface detector are all on the same horizontal line, a guide rail is arranged below the surface detector, and a three-dimensional manual displacement table is arranged below the microscope;
preferably, the electric displacement table of the sample adjusting table comprises a vertical displacement table and four or five horizontal displacement tables, two of the horizontal displacement tables form a two-dimensional electric displacement table and are arranged on the electric turntable, the vertical displacement table is arranged on the electric turntable or below the electric turntable, and the remaining 1 or 2 horizontal displacement tables are arranged below the electric turntable.
The beneficial effects of the utility model reside in that: can be used for high pressure powder or single crystal X-ray diffraction; the distance from the sample to the surface detector can be ensured to be unchanged, and the obtained diffraction data is more credible; the X-ray irradiated on the sample can be ensured to be minimum in size, and the phenomenon that the light spot is overlarge and is irradiated on the sealing pad is avoided; the adjustment is accomplished by electrical control, and the experimenter is away from the X-ray irradiation.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a top view of the high-pressure X-ray diffractometer of the present invention;
FIG. 2 is a schematic structural view of a sample adjusting table of the high-pressure X-ray diffractometer of the present invention;
description of reference numerals:
the X-ray microscope comprises an X-ray generator 1, an X-ray focusing mirror 2, a needle tube 3, a microscope 4, an X-ray detector 5, a surface detector 6, a sample adjusting table 7, an X-ray 8, a high-voltage device 9, a horizontal displacement table 10, a vertical displacement table 11 and an electric rotary table 12.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
As shown in fig. 1-2, the high-voltage X-ray diffractometer comprises an X-ray generator 1, an X-ray focusing mirror 2, a needle tube 3, a microscope 4, an X-ray detector 5, a surface detector 6 and a sample adjusting platform 7, wherein the X-ray focusing mirror 2 is arranged on the X-ray generator 1, one end of the needle tube 3 is arranged on the X-ray focusing mirror 2, the other end of the needle tube 3 is in a cone-shaped structure, the surface detector 6 is positioned on one side of the needle tube 3 and is positioned in the transmission direction of X-rays 8 emitted by the X-ray generator 1, the cone-shaped end of the needle tube 3 faces the surface detector 6, the sample adjusting platform 7 is positioned between the needle tube 3 and the surface detector 6, the microscope 4 is positioned on one side of the sample adjusting platform 7, the X-ray detector 5 is positioned between the sample adjusting platform 7 and the surface detector 6, the sample adjusting platform 7 is a 5-axis or, the sample adjusting platform 7 comprises an electric turntable 12 and four or five electric displacement platforms, the needle tube 3, the X-ray focusing lens 2, the emission port of the X-ray generator 1, the X-ray detector 5 and the center line of the surface detector 6 are all on the same horizontal line, a guide rail is arranged below the surface detector 6, and a three-dimensional manual displacement platform is arranged below the microscope 4;
further, the electric displacement table of the sample adjusting table 7 comprises a vertical displacement table 11 and four or five horizontal displacement tables 10, two horizontal displacement tables 10 form a two-dimensional electric displacement table and are arranged on the electric rotary table 12, the vertical displacement table 11 is arranged on the electric rotary table 12 or below the electric rotary table 12, and the remaining 1 or 2 horizontal displacement tables 10 are arranged below the electric rotary table 12.
When in use, the high-voltage device 9 is placed on the sample adjusting table 7, and sample scanning is carried out, so that a sample in the high-voltage device 9 is positioned at the rotating center of the electric turntable 12, and the X-ray 8 also passes through the rotating center of the electric turntable 12; the rotation center of the electric turntable 12 is determined through the two-dimensional electric displacement table on the electric turntable 12 and the microscope 4, and then the rotation center is aligned with the X-ray 8 through the horizontal displacement table 10 below the electric turntable 12; the X-ray detector 5 is used for detecting X-rays 8 during sample scanning, detecting the intensity of the X-rays 8 after the X-rays pass through the sample, and confirming the position of the sample relative to the X-rays 8 through the intensity change of the X-rays 8 so as to enable the sample to be accurately aligned with the X-rays 8;
the height of the microscope 4 is adjusted through a three-dimensional manual displacement table under the microscope 4 to be consistent with a sample, and the microscope 4 is used for searching the rotating center of the electric turntable 12 and initially positioning the sample;
the initial positioning method comprises the following steps: (a) placing a cross filament at the position of a sample, wherein the cross filament consists of a transverse filament and a vertical filament, and the diameter of the filament is less than 20 microns; (b) adjusting the microscope 4 to see the cross hairs on the display and placing the cross point in the center of the display; (c) rotating the sample by an electric turntable 12180 degrees, with the cross filament offset; (d) measuring the offset distance, respectively moving the horizontal displacement table 10 on the electric turntable 12 in the sample adjusting table 7 and the displacement table of the microscope 4 by half distance, and placing the cross point of the cross wires in the center of the display; (f) the electric turntable 12 rotates to the zero point, the deviation of the cross wire is observed again, the calibration is carried out again, the operation is repeated for a plurality of times, and the fact that the cross wire is almost not deviated on the display when the electric turntable 12 rotates is observed. When the high-voltage device 9 is placed on the sample table for the first time, the microscope 4 is used for positioning, the horizontal displacement table 10 of the sample adjusting table 7 is adjusted, and the sample is adjusted to the center of the display;
during X-ray diffraction, the X-ray generator 1 emits X-rays 8, after the X-rays are focused by the focusing lens, the X-rays 8 are focused to meet the size of a high-voltage experiment, the shape of a light spot is further limited by the needle tube 3, the size of the X-rays 8 light spot irradiated on a sample is limited, the tail part of the light spot is clamped off, the X-rays 8 light spot meets the requirement of the high-voltage experiment, X-rays 8 light beams are irradiated on the sample in the high-voltage device 9, and a transmission diffraction spectrum is collected by the surface detector 6;
a guide rail is arranged below the surface detector 6, so that the detector can move along the direction of the X-ray 8, and the receiving diffraction angle of the surface detector 6 is adjusted.
The sample adjusting table 7, the X-ray detector 5 and the microscope 4 are matched, so that a sample in the high-voltage device can be positioned at the rotating center of the electric turntable 12 of the sample adjusting table 7, and the X-ray 8 also passes through the rotating center of the electric turntable 12.
The sample adjusting table 7 is matched with the microscope 4, the rotation center of the electric turntable 12 can be determined through the two-dimensional electric displacement table on the electric turntable 12 of the sample adjusting table 7 and the microscope 4, and then the rotation center is aligned with the X ray 8 through the horizontal displacement table 10 below the electric turntable 12.
The X-ray generator 1, the X-ray focusing lens 2 and the needle tube 3 are matched, the X-ray generator 1 emits X-rays, the X-ray focusing lens 2 focuses the X-rays, the shape of light spots is further limited by the needle tube 3, and X-ray beams required by a high-voltage experiment are obtained.
The design of the utility model can be used for high-pressure powder or single crystal X-ray diffraction; the distance from the sample to the surface detector 6 can be ensured to be unchanged, and the obtained diffraction data is more credible; the X-ray 8 irradiated on the sample can be ensured to be minimum in size, and the phenomenon that the X-ray is irradiated on the sealing pad due to overlarge light spots is avoided; the adjustment is accomplished by electrical control, and the experimenter is away from the X-ray irradiation.
It will be apparent to those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (2)
1. The high-voltage X-ray diffractometer is characterized by comprising an X-ray generator, an X-ray focusing mirror, a needle tube, a microscope, an X-ray detector, a surface detector and a sample adjusting platform, wherein the X-ray focusing mirror is arranged on the X-ray generator, one end of the needle tube is arranged on the X-ray focusing mirror, the other end of the needle tube is of a conical structure, the surface detector is positioned on one side of the needle tube and is positioned in the transmission direction of X-rays emitted by the X-ray generator, the conical end of the needle tube faces the surface detector, the sample adjusting platform is positioned between the needle tube and the surface detector, the microscope is positioned on one side of the sample adjusting platform, the X-ray detector is positioned between the sample adjusting platform and the surface detector, the sample adjusting platform is a 5-axis or 6-axis electric platform, and comprises an electric rotary platform and four or five electric displacement platforms, the needle tube, the X-ray focusing lens, the emitting port of the X-ray generator, the X-ray detector and the center line of the surface detector are all on the same horizontal line, a guide rail is arranged below the surface detector, and a three-dimensional manual displacement table is arranged below the microscope.
2. The high-voltage X-ray diffractometer according to claim 1, wherein the electric displacement stages of the sample conditioning stage comprise a vertical displacement stage and four or five horizontal displacement stages, two of the horizontal displacement stages constitute a two-dimensional electric displacement stage and are disposed on the electric turntable, the vertical displacement stage is disposed on or under the electric turntable, and the remaining 1 or 2 horizontal displacement stages are disposed under the electric turntable.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021924917.8U CN212301375U (en) | 2020-09-04 | 2020-09-04 | High-pressure X-ray diffractometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021924917.8U CN212301375U (en) | 2020-09-04 | 2020-09-04 | High-pressure X-ray diffractometer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN212301375U true CN212301375U (en) | 2021-01-05 |
Family
ID=73934257
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202021924917.8U Active CN212301375U (en) | 2020-09-04 | 2020-09-04 | High-pressure X-ray diffractometer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN212301375U (en) |
-
2020
- 2020-09-04 CN CN202021924917.8U patent/CN212301375U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US6359964B1 (en) | X-ray analysis apparatus including a parabolic X-ray mirror and a crystal monochromator | |
| Fischetti et al. | Mini-beam collimator enables microcrystallography experiments on standard beamlines | |
| CN104090289B (en) | X-ray system | |
| JP2008268105A (en) | X-ray beam source, x-ray beam irradiator, x-ray beam radiographic device, x-ray beam computer tomography device, x-ray element mapping examination apparatus and x-ray beam forming method | |
| JP3996821B2 (en) | X-ray analyzer | |
| JP2004020397A (en) | System for evaluating crystal | |
| JP2004301862A (en) | Apparatus for analyzing surface of electrically insulated sample | |
| DE112015000433B4 (en) | Sample holder, viewing system, and imaging process | |
| CN212301375U (en) | High-pressure X-ray diffractometer | |
| CN111929336A (en) | High-pressure X-ray diffractometer | |
| CN203705371U (en) | X-ray spectrometer for measuring all elements | |
| TW201822242A (en) | Apparatus for combined STEM and EDS tomography | |
| US4280049A (en) | X-ray spectrometer | |
| Yiming et al. | An investigation of X-ray fluorescence analysis with an X-ray focusing system (X-ray lens) | |
| US3322950A (en) | Linear accelerator radiotherapy device and associated beam defining structure | |
| CN208125648U (en) | MICRO-BEAM XRF ANALYSIS system based on combination X-ray capillary | |
| CN109187589A (en) | A kind of burnt X-ray spectral analysis device of Large focal spot copolymerization | |
| CN108398450A (en) | Microbeam X-ray fluorescence analytical method based on combination X-ray capillary | |
| CN111458364A (en) | Multi-detector X-ray fluorescence micro-area scanning instrument and imaging method thereof | |
| JP3567185B2 (en) | Sample analyzer | |
| CN113218974A (en) | X-ray absorption spectrum measuring system | |
| CN108709898A (en) | MICRO-BEAM XRF ANALYSIS system based on combination X-ray capillary | |
| CN217425257U (en) | X-ray high-voltage diffractometer | |
| JP2602523B2 (en) | Cathodoluminescence measuring device | |
| Sánchez et al. | SRXRF analysis with spatial resolution of dental calculus |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |