CN110320220A - The device and method of analysis of material shot-range ordered structure and long range ordered structure - Google Patents
The device and method of analysis of material shot-range ordered structure and long range ordered structure Download PDFInfo
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- CN110320220A CN110320220A CN201910666887.0A CN201910666887A CN110320220A CN 110320220 A CN110320220 A CN 110320220A CN 201910666887 A CN201910666887 A CN 201910666887A CN 110320220 A CN110320220 A CN 110320220A
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- 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
- G01N23/02—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 transmitting the radiation through the material
- G01N23/06—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 transmitting the radiation through the material and measuring the absorption
- G01N23/083—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 transmitting the radiation through the material and measuring the absorption the radiation being X-rays
- G01N23/085—X-ray absorption fine structure [XAFS], e.g. extended XAFS [EXAFS]
-
- 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
- G01N23/20083—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 by using a combination of at least two measurements at least one being a transmission measurement and one a scatter measurement
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- 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
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- 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
Abstract
Technical solution of the present invention discloses the device and method of a kind of analysis of material shot-range ordered structure and long range ordered structure, the detected materials sample being located on bearing assembly by the light beam irradiation that synchrotron radiation light source is emitted continuous spectrum, the first optical information can be obtained by multiple energy dispersive detectors, the X-ray diffraction test of the sample to be tested can be carried out based on first optical information, the second optical information can be obtained by position sensitive detector, the X-ray absorption fine structure test of the sample to be tested can be carried out based on second optical information.As it can be seen that technical solution of the present invention can quickly analysis of material shot-range ordered structure and long range ordered structure simultaneously.
Description
Technical field
This hair is related to material analysis characterization technique field, more specifically, being related to a kind of analysis of material shot-range ordered structure
With the device and method of long range ordered structure.
Background technique
In many materials scientific research, such as structure evolution of the electrode material of lithium battery under service condition, it requires
Real-time analysis under reaction condition in situ is carried out to the shot-range ordered structure (Local Structure) and long range ordered structure of material, this
Very high requirement is proposed to the time resolution of analytical technology.
X-ray absorption fine structure (XAFS) and X-ray diffraction (XRD) are two kinds of important technologies for studying the structure of matter,
XAFS can provide the structural information of shortrange order, and XRD gives the structural information of long-range order, and the two complements one another, big
It is used in the investigation of materials of amount.If the combination of both technologies got up, so that it may while carrying out local and long-range order knot
The analysis of structure.
Summary of the invention
In view of this, technical solution of the present invention provides a kind of analysis of material shot-range ordered structure and long range ordered structure
Device and method, can quickly analysis of material shot-range ordered structure and long range ordered structure simultaneously.
In view of this, the invention provides the following technical scheme:
A kind of device of analysis of material shot-range ordered structure and long range ordered structure characterized by comprising carrying group
Part, the bearing assembly is for loading detected materials sample；
Synchrotron radiation light source, for being emitted the light beam of continuous spectrum, to irradiate the detected materials sample；
Multiple energy dispersive detectors, the detection axis of the energy dispersive detector and the direction of illumination of the light beam have
There is different angles, the energy dispersive detector is used to detect the first optical information of position；First optical information is extremely
Few energy dispersion X-ray diffraction test for carrying out about the detected materials sample；
Light splitting convergence component, the light splitting convergence component are located in the range of exposures of the light beam, and being used for will be described to be measured
After the light beam light splitting that material sample penetrates, it is irradiated to position sensitive detector, the position sensitive detector is located at light splitting convergence component
Later, for detecting the second optical information of position；Second optical information is for carrying out about the detected materials sample
Energy dispersion X-ray Absorption Fine Structure test.
Preferably, in above-mentioned apparatus, the light splitting convergence component includes: bending analyzing crystal.
Preferably, in above-mentioned apparatus, further includes: the between the light splitting convergence component and the bearing assembly
One slit, first slit is for removing scattering light.
Preferably, in above-mentioned apparatus, further includes: between the synchrotron radiation light source and the bearing assembly
Two slits, second slit are used for card light, obtain the incident beam for needing size.
Preferably, in above-mentioned apparatus, described device has 11 energy dispersive detectors, and the angular range is
16.98 ° -68.27 °, X-ray diffraction test interplanar spacing range be
Preferably, in above-mentioned apparatus, further includes: host, the host and the energy dispersive detector and described
Position sensitive detector is separately connected, for carrying out the energy dispersion X about the detected materials sample based on first optical information
X ray diffraction test is used to carry out to inhale about the energy dispersion X-ray of the detected materials sample based on second optical information
Receive fine structure test.
Preferably, in above-mentioned apparatus, the host is also used to carry out based on first optical information about described to be measured
The x-ray fluorescence of material sample is tested.
Preferably, in above-mentioned apparatus, the host carries out the x-ray fluorescence test side about the detected materials sample
Method includes:
Draw the x-ray photon energy of at least two energy dispersive detector detections and the curve graph of intensity；
Based on x-ray fluorescence with the indeclinable characteristic of detection angle and the detection result of the energy dispersive detector,
Obtain fluorescence pattern and diffracting spectrum.
Preferably, in above-mentioned apparatus, the synchrotron radiation light source are as follows: undulator light source or Torsional pendulum apparatus light source or bending iron
Light source.
The present invention also provides the methods of a kind of analysis of material shot-range ordered structure and long range ordered structure, using above-mentioned
Device analysis material shot-range ordered structure and long range ordered structure described in one.
As can be seen from the above description, analysis of material shot-range ordered structure and long-range order knot that technical solution of the present invention provides
In the device and method of structure, by synchrotron radiation light source be emitted continuous spectrum light beam irradiation be located at bearing assembly on wait measure and monitor the growth of standing timber
Expect sample, the first optical information can be obtained by multiple energy dispersive detectors, institute can be carried out based on first optical information
The X-ray diffraction test of sample to be tested is stated, the second optical information can be obtained by position sensitive detector, be based on second optical information
It can carry out the X-ray absorption fine structure test of the sample to be tested.As it can be seen that technical solution of the present invention can quickly divide simultaneously
Analyse material shot-range ordered structure and long range ordered structure.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is a kind of schematic diagram of the device of conventional analysis material shot-range ordered structure and long range ordered structure；
Fig. 2 is the schematic diagram of the device of another conventional analysis material shot-range ordered structure and long range ordered structure；
Fig. 3 is a kind of device of analysis of material shot-range ordered structure and long range ordered structure provided in an embodiment of the present invention；
Fig. 4 is the dress of another analysis of material shot-range ordered structure and long range ordered structure provided in an embodiment of the present invention
It sets；
Fig. 5 is by a kind of probe angle provided in an embodiment of the present invention and survey interplanar distance curve graph；
Fig. 6 is a kind of curve graph for detecting x-ray photon energy and intensity provided in an embodiment of the present invention；
Fig. 7 is by another probe angle provided in an embodiment of the present invention and surveys interplanar distance curve graph.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The characterization of conventional XAFS needs to carry out energy scan by continuously changing the angle of monochromator, this mechanical movement
Process is usually relatively slower.Currently, there are two types of the quick XAFS characterization techniques of comparative maturity: the X-ray of quick scanning monochromator
Absorption spectroscopy techniques (QXAFS) and energy dispersion X-ray absorption spectroscopy techniques (EDXAFS).QXAFS characterizes the time can be down to number
Ten milliseconds of magnitudes, and EDXAFS is faster, the characterization time can be down to musec order.
Major embodiment using X-ray diffraction characterization material crystal structure is Prague (Bragg) diffraction formula, it may be assumed that
2dhklSin θ=λ (1)
Here dhklFor interplanar distance, the angle of angle of 2 θ between incident beam and outgoing beam, λ is incident X-rays
Wavelength.When incident light, emergent light and crystal face meet reflective relation and Bragg diffraction formula (1) simultaneously, diffraction is generated.
Obviously, there are two types of the schemes of diffraction here, and one is the wavelength X of fixed incident light, different interplanar distance dhklCorrespondence is different
Angle of diffraction θ, here it is conventional angular dispersion X-ray diffractions (ADXRD)；Another is fixed diffraction angle, θ, and use is white
Light x-ray bombardment sample, different interplanar distance dhklDiffraction is generated to the X-ray of different wave length λ in incident beam, here it is
Energy dispersion X-ray diffraction (EDXRD).Both diffraction modes may be used to quickly characterize, and time resolution can be down to
Microsecond is even lower, depends primarily on detector；Certainly, for the resolution capability Δ d/d of interplanar distance, ADXRD ratio EDXRD
It is much better.
XAFS-XRD is combined, since XRD test speed is relatively fast, determine combination characterization speed is wherein
The part XAFS.A kind of prior art is that the mode of serial acquisition QXAFS and ADXRD data is taken to realize dynamic structure table
Sign, as shown in FIG. 1, FIG. 1 is the signals of a kind of conventional analysis material shot-range ordered structure and the device of long range ordered structure for principle
Figure, comprising: synchrotron radiation light source 11, slit 12, quick scanning monochromator 13, another slit 14, incident intensity monitor 15, to
Survey material sample 10, position sensitive detector 16 and transmission X-ray detector 17.
Mode shown in Fig. 1, if synchrotron radiation light beam is by the way that after slit 12, by quick scanning monochromator 13, generation connects
Continuous spectrum after incident intensity detector 15, is irradiated to detected materials sample 10, transmitted light beam after another slit 14
It beats in X-ray detector 17 below, corresponding detection information can be obtained, the detection information is for carrying out detected materials sample 10
XAFS test, obtain XAFS data.When alternately XRD is tested, quick scanning monochromator 13 is controlled in a fixed angle
So that emergent light is monochromatic light, the scattering light after the monochromatic light exposure to detected materials sample 10 uses curved position sensitive detector
16 detections, can obtain corresponding detection information, which is used to carry out the XRD test of detected materials sample 10, obtain XRD
Data.
Which carries out the XRD test and XAFS test of detected materials sample 10 using serial measurement method respectively, although
It can will be joined described in Fig. 1 by controlling the data acquisition for sweeping the gate signal of monochromator quickly come alternately QXAFS and ADXRD
With shortening to 60ms the normal period of mode, but for faster chemical kinetics and Kinematic process, time resolution energy
Power is unable to meet demand, needs the higher characterization technique of time resolution.
Compared to QXAFS, EDXAFS has higher time resolution, time resolution up to musec order, because
This, it is the effective ways for improving time resolution that EDXAFS and the combination of XRD technology, which are got up,.But existing EDXAFS-
In the combination scheme of ADXRD, as shown in Fig. 2, Fig. 2 is another conventional analysis material shot-range ordered structure and long range ordered structure
Device schematic diagram, comprising: synchrotron radiation light source 21, slit 22, bending analyzing crystal 23, mobile slit 24, wait measure and monitor the growth of standing timber
Expect sample 20, position sensitive detector 25 and another position sensitive detector 26.Which, the white light beam from synchrotron radiation light source are curved
Bent analyzing crystal 23 reflects and converges to detected materials sample 20, and it is quick to get to subsequent position by the light beam of detected materials sample 20
On detector 26, corresponding detection information is obtained, which is used to carry out the EDXAFS test of detected materials sample 10, obtains
Take EDXAFS data.When needing to acquire diffraction data, it is moved to behind bending analyzing crystal 23, is blocked out with mobile slit 24
The light beam of energy narrower bandwidth is irradiated to detected materials sample 20, quick using the another one for being located at 20 side of detected materials sample
Detector 25 acquires diffracted signal, can obtain corresponding detection information, and the detection information is for carrying out detected materials sample 20
ADXRD test, obtains ADXRD data.
Scheme shown in Fig. 2 needs the side of the detected materials sample 20 in EDXAFS device to increase a position sensitive detector 25
To detect ADXRD signal.The program can theoretically acquire EDXAFS data and ADXRD data simultaneously, still, due to incident light
Energy bandwidth it is too big (Δ E/E~10%), this causes collected diffracted signal peak width big, d (interplanar distance) value resolution ratio
It is low, while x-ray fluorescence also causes diffraction back end to increase, signal-to-noise ratio reduces.Therefore, in this scheme actual implementation, lead to
It is often using serial mode interleaved acquisition EDXAFS data and ADXRD data；When adopting ADXRD data, a slit 24 is moved
Enter the light beam (Fig. 2) that optical path card goes out energy narrower bandwidth.Clearly as mobile mechanical slot is employed herein, it is combined
Characterization speed is difficult to be reduced to a few tens of milliseconds or less.
So requiring the dynamic structure of higher material to study time resolution, it is also necessary to a kind of test side faster
Case does not need mobile mechanical part in view of this, EDXAFS and EDXRD are combined by technical solution of the embodiment of the present invention, can be with
The bottleneck for breaking through millisecond magnitude, reaches the time resolution of microsecond, and technical solution of the embodiment of the present invention belongs to material analysis characterization neck
Domain, Nuclear Science and Technology subject, synchrotron radiation and application direction, can be used for the research of material science, be related to chemistry, physics and
The subjects such as material.
Technical solution of the embodiment of the present invention studies a question for the dynamic structure of material, and providing one kind can measure simultaneously
The device and method of EDXAFS and EDXRD, improve time resolution, are of great significance for leading basic research.
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing and specific real
Applying mode, the present invention is described in further detail.
With reference to Fig. 3, Fig. 3 is a kind of analysis of material shot-range ordered structure and long range ordered structure provided in an embodiment of the present invention
Device, described device include: synchrotron radiation light source 31, bearing assembly 33, multiple energy dispersive detectors 37, light splitting convergence portion
Part 35 and position sensitive detector 36.
The bearing assembly 33 is for loading detected materials sample 30.The hardware construction of device can be set based on demand,
Setting bearing assembly 33 is sample loading stage, or is sample holder etc., to the tool of the bearing assembly 33 in the embodiment of the present invention
Body implementation is without limitation.
The synchrotron radiation light source 31 is used to be emitted the light beam of continuous spectrum, to irradiate the detected materials sample 30.This
In inventive embodiments, the light beam that the synchrotron radiation light source 31 is emitted is synchrotron radiation light, and wavelength coverage is big, is had from remote
Infrared, visible light, the ultraviolet continuous spectrum until within the scope of X-ray.
The detection axis of the energy dispersive detector 37 has different 2 θ of angle, institute from the direction of illumination of the light beam
Energy dispersive detector 37 is stated for detecting the first optical information of position；First optical information be at least used for carry out about
The energy dispersion X-ray diffraction (EDXRD) of the detected materials sample 30 is tested, and EDXRD data are obtained.
The light splitting convergence component 35 is located in the range of exposures of the light beam, for the detected materials sample 30 is saturating
After the light beam light splitting crossed, it is irradiated to position sensitive detector 36, the position sensitive detector 36 is located at after light splitting convergence component, uses
The second optical information in detection position；Second optical information is used to carry out the energy color about the detected materials sample
X-ray absorption fine structure (EDXAFS) test is dissipated, EDXAFS data are obtained.
Optionally, the light splitting convergence component 35 includes: bending analyzing crystal, different wave length light can be gone out by difference
Firing angle degree separates, and light is irradiated to position sensitive detector 36.Described device further include: be located at light splitting convergence component 35 and institute
The first slit 34 between bearing assembly 33 is stated, first slit 34 is for removing scattering light.Described device further include: be located at
The second slit 32 between the synchrotron radiation light source 31 and the bearing assembly 33, second slit 32 are used for card light, obtain
It must need the incident beam of size.
In described device of the embodiment of the present invention, described device, which can be set, has 11 energy dispersive detectors 27,
The angular range is 16.98 ° -68.27 °, and the interplanar spacing range of X-ray diffraction test is
With reference to Fig. 4, Fig. 4 is another analysis of material shot-range ordered structure and long-range order knot provided in an embodiment of the present invention
The device of structure, based on mode shown in Fig. 3, Fig. 4 shown device further include: host 38, the host 38 are visited with the energy dispersion
It surveys device 37 and the position sensitive detector 36 is separately connected, for being carried out based on first optical information about the detected materials
The energy dispersion X-ray diffraction of sample 30 is tested, based on second optical information for carrying out about the detected materials sample
30 energy dispersion X-ray Absorption Fine Structure test.
Optionally, the host 38 is also used to carry out based on first optical information about the detected materials sample 30
X-ray fluorescence test.Specifically, the host progress includes: about the x-ray fluorescence test method of the detected materials sample
Draw the x-ray photon energy of at least two energy dispersive detector detections and the curve graph of intensity；Based on x-ray fluorescence
With the indeclinable characteristic of detection angle and the detection result of the energy dispersive detector 37, fluorescence pattern and diffraction pattern are obtained
Spectrum.
In described device of the embodiment of the present invention, in order to guarantee incident 30 optic angle of detected materials sample in EDXRD test process
The consistency of degree, different from mode shown in Fig. 2, detected materials sample 30 is placed on incident light by described device of the embodiment of the present invention
The previous section on road after light beam penetrates detected materials sample 30, then is irradiated to light splitting convergence component 35, and then pass through the quick detection in position
Device 36 detects the second optical information, carries out EDXAFS test, and then obtain EDXAFS data.In order to avoid detected materials sample 30 dissipates
The influence that light tests EDXAFS is penetrated, is provided with the first slit 34 between detected materials sample 30 and light splitting convergence component 35,
Fall to scatter light for card.2 position θ of special angle of optical path side is provided with the X-ray energy dispersion detector 37 of series, uses
In the diffraction data of detection EDXRD.
31 outgoing beam of synchrotron radiation light source is continuous spectrum, has multiple wavelength λ values, is based on Bragg diffraction law,
Different wave length value corresponds to different angle of diffraction, therefore the multiple energy dispersive detectors 37 of series are arranged, and respectively corresponds different 2 θ of angle.
It is only to show an energy dispersive detector 37 with 2 θ of special angle in Fig. 3 and Fig. 4, can have demand setting energy
37 numbers of dispersion detector and its 2 θ of corresponding angle, technical solution of the present invention are not specifically limited in this embodiment.
EDXRD part of detecting is analyzed, according to Bragg diffraction law, the calculation formula of EDXRD can be such as following table
Show:
Wherein, E is incident x-ray photons energy, and h is Planck's constant, and c is light beam, and 2 θ are incident light and emergent light
Therefore angle places energy dispersive detector 37 in 2 position θ of fixed angle, acquires the ENERGY E of diffraction photon, it can obtain
Counter structure information.
According to formula (2) it is found that when 2 θ of angle of diffraction of light is fixed, the photon energy E and mirror surface spacing that detect
dhklIt corresponds.Conventional EDXRD is tested, since the energy bandwidth △ E of incident light is larger, usually at an angle
Sufficiently large d can be had by placing energy-probehklIt is worth range.Then, EDXAFS-EDXRD test is combined in synchrotron radiation
When, since EDXAFS tests the beam energy narrower bandwidth used, an angle places 37 intelligent detecting of energy dispersive detector
The interplanar distance value of part range.Therefore, consider that multi-angle places energy dispersive detector in described device of the embodiment of the present invention
37, it is based on this, carries out following simple calculating.
In the embodiment of the present invention, the synchrotron radiation light source 31 can be undulator light source or Torsional pendulum apparatus light source or bending iron
Light source.Specifically, the light beam of continuous spectrum is generated by undulator light source, or, generating continuous spectrum by Torsional pendulum apparatus light source
Light beam, or the light beam by bending iron light source generation continuous spectrum.
Current synchrotron radiation light sources multiple in the world have EDXAFS p-wire station, by taking the ID24 line station of RSRF as an example, the line
The about 1keV incident beam of energy bandwidth can be provided in taper-undulator (undulator) mode by standing.With energy battery
For material, wherein common member is known as iron, cobalt, nickel, manganese etc., if the K ABSORPTION EDGE of ferro element is 7.111keV.It is false based on this
If carry out EDXAFS-EDXRD combination experiment, incident photon energy is that 7~8keV is depicted according to formula (2) at different angles
The curve that 2 θ place the interplanar distance that energy dispersive detector 37 can cover is spent, as shown in Figure 5.
With reference to Fig. 5, Fig. 5 is by a kind of probe angle provided in an embodiment of the present invention and survey interplanar distance curve graph, base
In Fig. 5 it is found that this is the results show that if will coverInterplanar spacing range, need to put at 11 angles
Set detector D1-D11, that is to say, that total energy dispersive detector 37 for needing 11 2 θ of corresponding different angle, table 1 list
The angle value and detectable interplanar spacing range that these detectors are placed.
The position of 1 X-ray energy dispersion detector of table and measurement method
As can be seen from the above description, the temporal resolution of microsecond may be implemented in described device of the embodiment of the present invention；With tradition
Your EDXAFS test is compared, before 30 position of detected materials sample is moved to focus lamp by described device of the embodiment of the present invention, benefit
In the interference using the first slit 34 removal Scattering and diffracting signal to XAFS signal, and detected materials sample 30 is after focus lamp
When, it is difficult to remove these interference signals, and behind 30 position of detected materials sample that moves forward, practical irradiation detected materials sample 30
X-ray beam energy bandwidth is bigger, is conducive to EDXRD test.
Due to being exactly that can be believed by energy dispersive detector 37 in acquisition X-ray diffraction using another benefit of EDXRD
It while breath, acquires x-ray fluorescence (XRF), XRF is determined for element information in detected materials sample 30.Since XRF believes
Number when isotropic emission, it is and when EDXRD diffracted signal closely related with angle of diffraction, therefore it is different to pass through comparison
Position sensor collected data distinguish XRF signal and EDXRD, and realization principle is as shown in Figure 6.
With reference to Fig. 6, Fig. 6 is a kind of curve graph for detecting x-ray photon energy and intensity provided in an embodiment of the present invention, point
The detection result of two energy dispersive detectors 37 of other 2 θ=30 ° of placed angle and 2 θ=50 °, draws the X-ray detected
The curve graph of photon energy and intensity, based on x-ray fluorescence with the indeclinable characteristic of detection angle it is found that in Fig. 6, F1、F2And F3
These three wave crests correspond to fluorescence spectrum signal, remaining is diffraction peak-to-peak signal.Fluorescence spectrum peak position does not change with detection angle, is based on
This characteristic can obtain fluorescence pattern and diffracting spectrum according to the detection result of the energy dispersive detector 37.
As above-mentioned, since synchrotron radiation incident photon energy bandwidth is insufficient, need to be arranged multiple energy dispersive detectors 37.
In described device, the resolution capability of energy dispersive detector 37 is in 100eV or so.
In the embodiment of the present invention, light splitting convergence component 35 can be bending analyzing crystal.Analyzing crystal is bent by setting
Position and angle, can make in light beam be suitble to XAFS test part optical band pass through, pass through bending analyzing crystal light
Beam energy bandwidth narrows, in order to carry out XAFS test.
In other modes, the synchrotron radiation light source 31 can also be synchrotron radiation Torsional pendulum apparatus (wiggler) light source, such as super
Broader energy bandwidth can be provided by leading Torsional pendulum apparatus light source, energy range in 5-50keV, using the light source can it is more efficient into
Row diffraction test, at this point, as shown in fig. 7, Fig. 7 is by another probe angle provided in an embodiment of the present invention and surveys interplanar
Away from curve graph, when using 5-50keV light source, can only be covered in 20 ° of placement detectorsRange, can
To be placed around two or three detectors at 20 °, fluorescence signal and diffracted signal can be distinguished, different detectors are acquired
To Information revision after be overlapped signal-to-noise ratio can be improved.
Based on the above embodiment, another embodiment of the present invention additionally provides a kind of analysis of material shot-range ordered structure and long-range
The method of ordered structure, which is using device analysis material shot-range ordered structure and long-range order knot described in above-described embodiment
Structure.
The method of the embodiment of the present invention uses above-described embodiment described device, and EDXAFS-EDXRD combination may be implemented and survey
Examination.
The invention patent technology is related to the side of a kind of while quick analysis of material shortrange order and long range ordered structure information
Method.The present invention devises scheme associated with EDXAFS-EDXRD, using White-beam Synchrotron Radiation as light source, using EDXAFS technology table
The shot-range ordered structure information for levying material, using the long range ordered structure information of EDXRD characterization material.This method may be implemented micro-
The characterization speed and time resolution of second-time, have broken the bottleneck of original millisecond of magnitude, are material structure dynamic evolution
Characterization provide a kind of scheme.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment may refer to each other.For method disclosed in embodiment
For, since it is corresponding with device disclosed in embodiment, so being described relatively simple, related place corresponds to portion referring to device
It defends oneself bright.
It should also be noted that, herein, relational terms such as first and second and the like are used merely to one
Entity or operation are distinguished with another entity or operation, without necessarily requiring or implying between these entities or operation
There are any actual relationship or orders.Moreover, the terms "include", "comprise" or its any other variant are intended to contain
Lid non-exclusive inclusion, so that article or equipment including a series of elements not only include those elements, but also
It including other elements that are not explicitly listed, or further include for this article or the intrinsic element of equipment.Do not having
In the case where more limitations, the element that is limited by sentence "including a ...", it is not excluded that in the article including above-mentioned element
Or there is also other identical elements in equipment.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (10)
1. a kind of device of analysis of material shot-range ordered structure and long range ordered structure characterized by comprising
Bearing assembly, the bearing assembly is for loading detected materials sample；
Synchrotron radiation light source, for being emitted the light beam of continuous spectrum, to irradiate the detected materials sample；
Multiple energy dispersive detectors, the detection axis of the energy dispersive detector and the direction of illumination of the light beam have not
Same angle, the energy dispersive detector are used to detect the first optical information of position；First optical information is at least used
It is tested in carrying out the energy dispersion X-ray diffraction about the detected materials sample；
Light splitting convergence component, the light splitting convergence component are located in the range of exposures of the light beam, are used for the detected materials
After the light beam light splitting that sample penetrates, it is irradiated to position sensitive detector, the position sensitive detector is located at after light splitting convergence component,
For detecting the second optical information of position；Second optical information is used to carry out the energy about the detected materials sample
The test of dispersion X-ray Absorption Fine Structure.
2. the apparatus according to claim 1, which is characterized in that the light splitting convergence component includes: bending analyzing crystal.
3. the apparatus according to claim 1, which is characterized in that further include: it is held positioned at light splitting convergence component with described
The first slit between component is carried, first slit is for removing scattering light.
4. the apparatus according to claim 1, which is characterized in that further include: it is held positioned at the synchrotron radiation light source with described
The second slit between component is carried, second slit is used for card light, obtains the incident beam for needing size.
5. the apparatus according to claim 1, which is characterized in that described device has 11 energy dispersive detectors,
The angular range is 16.98 ° -68.27 °, and the interplanar spacing range of X-ray diffraction test is
6. device according to claim 1-5, which is characterized in that further include: host, the host and the energy
Chromatic dispersion quantity detector and the position sensitive detector are separately connected, for being carried out based on first optical information about described to be measured
The energy dispersion X-ray diffraction of material sample is tested, based on second optical information for carrying out about the detected materials sample
The energy dispersion X-ray Absorption Fine Structure of product is tested.
7. device according to claim 6, which is characterized in that the host is also used to carry out based on first optical information
X-ray fluorescence about the detected materials sample is tested.
8. device according to claim 7, which is characterized in that the host carries out the X about the detected materials sample
Ray fluorescence test method includes:
Draw the x-ray photon energy of at least two energy dispersive detector detections and the curve graph of intensity；
Based on x-ray fluorescence with the indeclinable characteristic of detection angle and the detection result of the energy dispersive detector, obtain
Fluorescence pattern and diffracting spectrum.
9. device according to claim 1-8, which is characterized in that the synchrotron radiation light source are as follows: undulator light
Source or Torsional pendulum apparatus light source or bending iron light source.
10. a kind of method of analysis of material shot-range ordered structure and long range ordered structure, which is characterized in that using such as claim
The described in any item device analysis material shot-range ordered structures of 1-9 and long range ordered structure.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002116151A (en) * | 2000-10-06 | 2002-04-19 | Rikogaku Shinkokai | Method for spectroscopically evaluating bismuth layered structural ferroelectric material and manufacturing method for ferroelectric product |
| CN1504744A (en) * | 2002-12-02 | 2004-06-16 | 中国科学技术大学 | Method and apparatus for measuring and analyzing structure and component of combined sample |
| CN1749741A (en) * | 2004-09-16 | 2006-03-22 | 中国科学院高能物理研究所 | The X ray absorption spectrum detector and the method thereof that are used for chemical valence state research |
| CN102133106A (en) * | 2011-01-30 | 2011-07-27 | 中国科学院合肥物质科学研究院 | Method for conducting fast and automatic nondestructive testing (NDT) to heroin hidden in human body |
| WO2016187623A1 (en) * | 2015-05-15 | 2016-11-24 | Sigray, Inc. | X-ray techniques using structured illumination |
-
2019
- 2019-07-23 CN CN201910666887.0A patent/CN110320220B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002116151A (en) * | 2000-10-06 | 2002-04-19 | Rikogaku Shinkokai | Method for spectroscopically evaluating bismuth layered structural ferroelectric material and manufacturing method for ferroelectric product |
| CN1504744A (en) * | 2002-12-02 | 2004-06-16 | 中国科学技术大学 | Method and apparatus for measuring and analyzing structure and component of combined sample |
| CN1749741A (en) * | 2004-09-16 | 2006-03-22 | 中国科学院高能物理研究所 | The X ray absorption spectrum detector and the method thereof that are used for chemical valence state research |
| CN102133106A (en) * | 2011-01-30 | 2011-07-27 | 中国科学院合肥物质科学研究院 | Method for conducting fast and automatic nondestructive testing (NDT) to heroin hidden in human body |
| WO2016187623A1 (en) * | 2015-05-15 | 2016-11-24 | Sigray, Inc. | X-ray techniques using structured illumination |
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