CN110987990A - High-energy monochromatic flash X-ray diffraction imaging method and system - Google Patents
High-energy monochromatic flash X-ray diffraction imaging method and system Download PDFInfo
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Abstract
The invention discloses a high-energy monochromatic flash X-ray diffraction imaging system, which comprises an emission collimation module, a monochromatic separation module and a diffraction imaging module, wherein the emission collimation module comprises a flash X-ray machine and a collimation unit, the flash X-ray machine emits X rays, and the collimation unit is connected with the flash X-ray machine and is positioned on the edge line of an X-ray emergent end; the monochromatic separation module is arranged along the X-ray and comprises a monochromatic unit and an emergent unit, the monochromatic unit is connected with the emergent unit, and the emergent unit is positioned on one side of an emergent end of the monochromatic unit; the diffraction imaging module is positioned on the line of the exit direction of the monochromatic separation module and comprises an imaging plate and a rotating seat, and the rotating seat is arranged at the bottom end of the imaging plate; the method solves the problem of difficult separation of flash X-ray monochromatic light, and the determined accurate diffraction angle can improve the signal-to-noise ratio of the diffraction image and greatly reduce the complexity of the system.
Description
Technical Field
The invention relates to the technical field of X-ray monochromatic separation, in particular to a high-energy monochromatic flash X-ray diffraction imaging method and system.
Background
Both X-ray and transmission electron microscopy can study defects within the crystal. Although transmission electron microscopes have very high resolution, the sample preparation process is complicated, the sample needs to be destroyed, and only a small portion of the sample can be observed at a time. Even if in-situ tensile testing is possible, the specimen thickness needs to be reduced to the micrometer level. However, the research of the in-situ plastic deformation by the X-ray method can be carried out without destroying crystals, the sample can be observed integrally, the sample preparation is easy, and the type of the dislocation can be determined and the dislocation density can be estimated.
X-ray diffraction experiments to study in-situ tension or compression mostly need to be performed on synchrotron radiation devices. Because the synchrotron radiation light source is huge in size, the whole system is high in technical complexity and very expensive in cost, and the place for holding the synchrotron radiation light source is few, the experiment has many limitations. Therefore, the development of related industries is limited, and therefore, a high-energy monochromatic flash X-ray diffraction imaging method and system are provided, so that the X-ray diffraction experiment is miniaturized and simplified.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The invention is provided in view of the problems of incomplete monochromaticity and low intensity of the existing flash X-ray.
Therefore, one technical problem to be solved by the present invention is to provide a high-energy monochromatic flash X-ray diffraction imaging method and system, which aims to generate a flash X-ray with short wavelength, high intensity and good monochromaticity, which can be used for analyzing the evolution of in-situ dislocation of a crystal.
In order to solve the technical problems, the invention provides the following technical scheme: a high-energy monochromatic flash X-ray diffraction imaging system comprises an emission collimation module, a monochromatic separation module and a diffraction imaging module, wherein the emission collimation module comprises a flash X-ray machine and a collimation unit, the flash X-ray machine emits X-rays, and the collimation unit is connected with the flash X-ray machine and is positioned on the edge line of an X-ray emitting end; the monochromatic separation module is arranged along the X-ray and comprises a monochromatic unit and an emergent unit, the monochromatic unit is connected with the emergent unit, and the emergent unit is positioned on one side of the emergent end of the monochromatic unit; the diffraction imaging module is positioned on the line along the emergent direction of the monochromatic separation module and comprises an imaging plate and a rotating seat, and the rotating seat is arranged at the bottom end of the imaging plate.
As a preferable scheme of the high-energy monochromatic flash X-ray diffraction imaging method and system, the flash X-ray machine comprises a high-voltage pulse generator and a flash X-ray tube, and X rays emitted by the flash X-ray tube comprise K α rays, K α rays and K β rays.
As a preferred scheme of the high-energy monochromatic flash X-ray diffraction imaging method and system, the method comprises the following steps: the collimating unit comprises a lead collimator, a brass tube collimator and a glass capillary tube, the brass tube collimator is connected with the outlet end of the lead collimator, and the glass capillary tube is arranged in the inner cavity of the lead collimator and communicated with the inlet end and the outlet end of the lead collimator.
As a preferred scheme of the high-energy monochromatic flash X-ray diffraction imaging method and system, the method comprises the following steps: the mono-color unit includes a brass cylinder, a single crystal positioned in the interior cavity of the brass cylinder and placed on top of the angular stage, and an angular stage having a bottom extending through the side wall of the brass cylinder on the outside thereof.
As a preferred scheme of the high-energy monochromatic flash X-ray diffraction imaging method and system, the method comprises the following steps: the angle station comprises a pitching table, a rotating table and a fine adjustment rod, wherein the pitching table is fixed to the top of the rotating table, and the fine adjustment rod is connected to the rotating axis of the rotating table.
As a preferred scheme of the high-energy monochromatic flash X-ray diffraction imaging method and system, the method comprises the following steps: the emergent unit comprises an emergent brass tube, a transverse moving plate and a longitudinal moving plate, the transverse moving plate and the longitudinal moving plate are respectively and movably matched with two ends of the emergent brass tube, and one end of the emergent brass tube, which is matched with the transverse moving plate, is connected with the emergent end of the brass cylinder.
As a preferred scheme of the high-energy monochromatic flash X-ray diffraction imaging method and system, the method comprises the following steps: a limiting rod and a connecting groove are arranged at one end of the outgoing brass pipe matched with the transverse moving plate, and a U-shaped sliding groove is arranged at one end of the outgoing brass pipe matched with the longitudinal moving plate; the middle part of the side wall of the transverse moving plate is provided with a longitudinal slit; and the middle part of the side wall of the longitudinal moving plate is provided with a transverse slit.
Another technical problem to be solved by the present invention is to provide a high-energy monochromatic flash X-ray diffraction imaging method, which aims to generate a flash X-ray with short wavelength, high intensity and good monochromaticity, which can be used for analyzing the evolution of in-situ dislocations of a crystal by operating the system.
In order to solve the technical problems, the invention provides the following technical scheme: a high-energy monochromatic flash X-ray diffraction imaging method adopts the diffraction imaging system and further comprises the following steps:
determining suitable experimental parameters including selection of said single crystal and flash X-ray tube anode materials;
calculating the length of the collimation unit according to the selected materials, and then respectively calculating diffraction angles of the K α ray and the K α ray and the difference value of the diffraction angles of the K α ray and the K α ray;
establishing a diffraction imaging model of monochromatic flash X-rays according to the calculated value; starting the model, and determining the optimal diffraction position of the single crystal through adjustment;
and adjusting the rotating seat to ensure that the X-ray obtains the optimal diffraction imaging effect on the imaging plate after monochromatic separation.
As a preferred scheme of the high-energy monochromatic flash X-ray diffraction imaging method and system, the method comprises the following steps: and respectively calculating the lengths of the lead collimator and the brass tube collimator according to the calculated length of the collimating unit, wherein the outer diameter of the brass tube collimator is far smaller than that of the lead collimator, and the inner diameters of the brass tube collimator and the brass tube collimator are the same.
As a preferred scheme of the high-energy monochromatic flash X-ray diffraction imaging method and system, the method comprises the following steps: in the adjusting process, the pitching table is roughly adjusted, so that the single crystal is vertical to the horizontal plane; and driving the rotating table by finely adjusting the fine adjusting rod, and determining that the single crystal is at the optimal diffraction position by matching with the imaging plate.
The invention has the beneficial effects that:
the invention utilizes the flash X-ray machine to generate X-rays, the intensity and the incident width of the X-rays are kept through the collimation unit, and the non-required X-rays are removed through the monochromatic unit, so that the flash X-rays with short wavelength, high intensity and good monochromaticity, which can be used for carrying out crystal in-situ dislocation evolution analysis, are obtained, and the flash X-rays have wide practicability and extremely high economy; the method solves the problem of difficult separation of flash X-ray monochromatic light, and the determined accurate diffraction angle can improve the signal-to-noise ratio of the diffraction image and greatly reduce the complexity of the system.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a schematic diagram of the overall structure of the high-energy monochromatic flash X-ray diffraction imaging method and system of the present invention.
FIG. 2 is a schematic diagram of the high-power monochromatic flash X-ray diffraction imaging system according to the present invention.
FIG. 3 is a schematic diagram of the position of a lead slit of the high-energy monochromatic flash X-ray diffraction imaging system of the present invention.
FIG. 4 is a schematic diagram of a single crystal diffraction optical path in a single color unit of the high-energy monochromatic flash X-ray diffraction imaging method and system of the present invention.
FIG. 5 is a schematic diagram of an exit unit structure of the high-energy monochromatic flash X-ray diffraction imaging method and system of the present invention.
FIG. 6 is a schematic diagram of a local explosion structure of an exit unit of the high-energy monochromatic flash X-ray diffraction imaging method and system of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Furthermore, the present invention is described in detail with reference to the drawings, and in the detailed description of the embodiments of the present invention, the cross-sectional view illustrating the structure of the device is not enlarged partially according to the general scale for convenience of illustration, and the drawings are only exemplary and should not be construed as limiting the scope of the present invention. In addition, the three-dimensional dimensions of length, width and depth should be included in the actual fabrication.
Example 1
Referring to fig. 1, for the first embodiment of the present invention, a high-energy monochromatic flash X-ray diffraction imaging method and system are provided, the system includes an emission collimation module 100, a monochromatic separation module 200 and a diffraction imaging module 300, wherein the emission collimation module 100 includes a flash X-ray machine 101 and a collimation unit 102, the flash X-ray machine 101 emits X-rays, and the collimation unit 102 is connected to the flash X-ray machine 101 and is located on an X-ray exit end edge line; the monochromatic separation module 200 is arranged on the line of the X-ray and comprises a monochromatic unit 201 and an emergent unit 202, the monochromatic unit 201 is connected with the emergent unit 202, and the emergent unit 202 is positioned on one side of the emergent end of the monochromatic unit 201; the diffraction imaging module 300 is located on the line of the emergent direction of the monochromatic separation module 200, and comprises an imaging plate 301 and a rotating seat 302, wherein the rotating seat 302 is arranged at the bottom end of the imaging plate 301.
Wherein, the flash X-ray machine 101 in the emission collimation module 100 has strong portability, and the generated X-ray has a certain intensity, the photon energy of the generated X-ray is between 10keV and 2MeV, the flash X-ray machine 101 is used for generating and emitting X-ray, the collimation unit 102 collimates the generated X-ray, the intensity and the emitting width of the X-ray are maintained, the X-ray emitted from the collimation unit 102 enters the monochromatic unit 201 in the monochromatic separation module 200, in the monochromatic unit 201, the X-ray which does not meet the bragg condition is removed, and the monochromatic X-ray which meets the condition is separated and emitted, the emitted monochromatic X-ray enters the emission unit 202, and the emission unit 202 can limit the divergence of the monochromatic X-ray emitted from the monochromatic unit 201 and control the emitting direction of the monochromatic X-ray, the monochromatic X-ray emitted from the emission unit 202 enters the sample to be measured at a specific angle, the diffracted beam is finally imaged on the imaging plate 301 in the diffractive imaging module 300. The evolution process of dislocation in the deformation process of the sample to be detected can be analyzed by observing the change of diffraction spots on the imaging plate.
Example 2
Referring to fig. 1 and 2, a second embodiment of the present invention, which is different from the first embodiment, is a flash X-ray machine 101 including a high voltage pulse generator and a flash X-ray tube emitting X-rays including K α 1 rays, K α 2 rays and K β rays.
Compared with the embodiment 1, further, the high-voltage pulse generator in the flash X-ray machine 101 is used in cooperation with the console to realize that the flash X-ray tube emits high-energy flash X-rays, and the exposure time reaches the nanosecond level; preferably, the anode material of the flash X-ray tube is a molybdenum (Mo) target for emitting short X-ray pulses of high energy and high brightness.
It should be noted that the X-rays emitted by the flash X-ray diode include continuous X-rays and characteristic X-rays, wherein the characteristic X-rays further include K α 1 ray, K α 2 ray and K β ray, while the incident flash X-rays required for the actual in-situ tensile diffraction test are strictly monochromatic K α 1 ray, so that the monochromatic unit 201 realizes that only the monochromatic K α 1 ray which remains collimated is emitted from the exit unit 202, whereas the K α 2 ray and the K β ray are absorbed by the single crystal 201b in the monochromatic unit 201 because they do not satisfy the bragg condition, and the continuous X-rays are absorbed when passing through the lead collimator 102 a.
The rest of the structure is the same as that of embodiment 1.
Example 3
Referring to fig. 1, 2 and 3, a third embodiment of the present invention, which differs from the second embodiment, is: the collimating unit 102 includes a lead collimator 102a, a brass tube collimator 102b and a glass capillary tube 102c, the brass tube collimator 102b is connected to the outlet end of the lead collimator 102a, and the glass capillary tube 102c is disposed in the inner cavity of the lead collimator 102a and is communicated with the inlet end and the outlet end thereof.
Compared with the embodiment 2, further, the collimating unit 102 selects the lead collimator 102a and the brass tube collimator 102b to perform double collimation, the lead collimator 102a is connected with the brass tube collimator 102b, and light channels for emitting X-rays are arranged inside the lead collimator 102a and the brass tube collimator 102b and are communicated with each other; it should be noted that the lead collimator 102a is also used for absorbing the continuous X-ray; meanwhile, in order to limit the incidence width of the X-ray incident into the single crystal 201b in the monochromating unit 201, a lead slit having a width of 0.3mm is attached to the junction of the flash X-ray diode and the lead collimator 102 a.
The glass capillary 102c is an optical device manufactured according to the total reflection principle, and the angle of the incident X-ray and the angle of the optical channel of the glass capillary 102c need to satisfy the total reflection condition. The glass capillary tube 102c is arranged in the lead collimator 102a, the glass capillary tube 102c is used as a waveguide tube of the X-ray by utilizing the total reflection principle that the incident angle is smaller than the critical angle, the propagation direction of the light beam is changed, the X-ray is adjusted to be parallel or converged, a high-brightness light beam with a certain shape and size is used as an X-ray source, the addition of the glass capillary tube 102c can ensure that the flash X-ray after certain attenuation has enough intensity after being emitted from the monochromatic unit 201, so that an imaging plate has obvious diffraction spots, the energy loss of the flash X-ray can be reduced, the collimation of the flash X-ray can be effectively improved, and the utilization rate of the X-ray can be effectively improved.
Further, since the X-ray is attenuated after being emitted, and the longer the length of the brass collimator 102b is, the better the monochromatic separation effect of the X-ray is, but the intensity of the X-ray is also weakened, it is necessary to calculate the most suitable length ratio of the lead collimator 102a to the brass collimator 102b to ensure that the X-ray emitted from the collimating unit 102 has sufficient intensity and collimation.
The rest of the structure is the same as that of embodiment 2.
Example 4
Referring to fig. 1 and 2, a fourth embodiment of the present invention, which is different from the third embodiment, is: the mono-color unit 201 includes a brass cylinder 201a, a single crystal 201b, and an angular stage 201c, the single crystal 201b being located in the inner cavity of the brass cylinder 201a and being placed on top of the angular stage 201c, the bottom of the angular stage 201c extending through the side wall of the brass cylinder 201a on the outside thereof.
The angular position stage 201c comprises a pitching stage 201c-1, a rotating stage 201c-2 and a fine adjustment rod 201c-3, wherein the pitching stage 201c-1 is fixed on the top of the rotating stage 201c-2, and the fine adjustment rod 201c-3 is connected to the rotating axis of the rotating stage 201 c-2.
Compared with the embodiment 3, further, the single-color unit 201 is installed at the outlet of the brass collimator 102b, wherein the brass cylinder 201a is provided with an upper cover plate and a lower cover plate of brass for integrally sealing the single crystal 201b, preferably, the single crystal 201b in the present X-ray single-color separation system is a germanium (Ge) single crystal, the single crystal 201b is placed on a single crystal fixing frame, the top of the pitching table 201c-1 is hinged with a pitching table connecting plate, the single crystal fixing frame is installed on the top of the pitching table connecting plate, the fine tuning rod 201c-3 is connected with the rotating table 201c-2, which includes a fine tuning bolt frame and a digital display, the pitching table 201c-1 is used for adjusting the vertical angle at which the single crystal 201b is placed, and the rotating table 201c-2 is used for adjusting the included angle between the X-ray and the single crystal 201b, preferably, since the difference between the angles of the K α 1 ray and the K α 2 ray is small, it is difficult to read out on the rotating table 201c-2 by naked eyes, therefore, the length of the fine tuning rod 201c-3 is lengthened, so that the fine tuning rod 201c-3 is obviously shifted, and the displacement can be obtained by directly reading.
The rest of the structure is the same as that of example 3.
Example 5
Referring to fig. 1, 2, 5 and 6, a fifth embodiment of the present invention, which is different from the fourth embodiment, is: the emitting unit 202 includes an emitting brass tube 202a, a lateral moving plate 202b and a longitudinal moving plate 202c, the lateral moving plate 202b and the longitudinal moving plate 202c are respectively movably fitted at two ends of the emitting brass tube 202a, and one end of the emitting brass tube 202a fitted with the lateral moving plate 202b is connected to an emitting end of the brass cylinder 201 a.
A limiting rod and a connecting groove are arranged at one end of the outgoing brass tube 202a matched with the transverse moving plate 202b, and a U-shaped sliding groove is arranged at one end matched with the longitudinal moving plate 202 c;
the middle part of the side wall of the transverse moving plate 202b is provided with a longitudinal slit 202 b-1;
the middle of the sidewall of the longitudinal moving plate 202c is opened with a transverse slit 202 c-1.
Compared with the embodiment 4, the exit unit 202 is further used for limiting the emittance of the X-ray emitted from the monochromatic unit 201 and controlling the exit direction of the monochromatic X-ray, wherein the exit brass tube 202a is fixed with the side wall of the brass cylinder 201a, the angle formed by the exit brass tube 202b and the Ge single crystal is kept to be just the diffraction angle of the K α 1 ray, an optical channel is arranged in the inner cavity of the exit brass tube 202b, the transverse moving plate 202b and the longitudinal moving plate 202c are movably matched at the two ends of the exit brass tube 202a, and the longitudinal slit 202b-1, the transverse slit 202c-1 and the optical channel in the exit brass tube 202b are matched and communicated, so as to limit the exit direction of the monochromatic X-ray.
The structure of the outgoing brass tube 202a, the structure of the horizontal moving plate 202b and the structure of the vertical moving plate 202c are shown in the drawing, the horizontal moving plate 202b is U-shaped and is clamped in a connecting groove at the end of the outgoing brass tube 202a, and the horizontal moving plate 202b is limited and slides through the matching of a limiting rod; the longitudinal moving plate 202c is in a shape of a Chinese character 'zhong', limiting screws are symmetrically arranged at two ends of the rectangular plate, and the longitudinal moving plate longitudinally slides in the U-shaped sliding groove and is limited and adjusted through fine adjustment screws at two ends of the longitudinal moving plate.
The rest of the structure is the same as that of example 4.
Example 6
With reference to fig. 1 to 6, a sixth embodiment of the present invention provides a high-energy monochromatic flash X-ray diffraction imaging method, where the imaging method employs the above-mentioned diffraction imaging system, and further includes the following steps:
determining suitable experimental parameters including selection of single crystal 201b and flash X-ray tube anode materials;
calculating the length of the collimating unit 102 according to the selected material, and then respectively calculating the diffraction angles of the K α 1 ray and the K α 2 ray and the difference value of the diffraction angles;
adjusting the imaging plate rotating base 302 so that the imaging plate 301 is always perpendicular to the horizontal plane and the direction thereof is perpendicular to the direction of the monochromatic X-rays emitted from the transverse slit 202 c-1;
establishing a diffraction imaging model of monochromatic flash X-rays according to the calculated value; starting the model, and recording the position with the maximum brightness of the imaging plate 301, namely the maximum number of received X-ray photons by adjusting the 201 angular position table, wherein the position is the diffraction position of the crystal 201 b;
the monochromatic X-rays emitted from the transverse slit 202c-1 and incident into the sample to be measured can cause a specific crystal plane of the sample to be measured to generate diffraction, the direction of a diffraction beam is calculated according to the known crystal plane direction of the sample to be measured, and the imaging plate rotating base 302 is adjusted, so that the imaging plate 301 is always perpendicular to the horizontal plane and perpendicular to the direction of the diffraction beam.
According to the calculated length of the collimating unit 102, the lengths of the lead collimator 102a and the brass tube collimator 102b are calculated, and the outer diameter of the brass tube collimator 102b is much smaller than the outer diameter of the lead collimator 102a, and the inner diameters of the two are the same and are communicated.
In the adjusting process, the pitching table 201c-1 is roughly adjusted, so that the single crystal 201b is vertical to the horizontal plane; then, the rotating platform 201c-2 is driven by shifting the fine tuning rod 201c-3, and the optimal diffraction position of the single crystal 201b is determined by matching with the imaging plate 301.
The imaging system comprises a single crystal 201b, an X-ray diode, a lead collimator 102a, a brass tube collimator 102b, a lead tube collimator 102a, a brass tube collimator 102b, a K α 1 ray, a K α 2 ray, a K α ray, a K8932 ray, a K α ray and a Mo target, wherein the single crystal 201b is Ge single crystal, the X-ray diode anode material is Mo target, and the optimal length ratio of the lead collimator 102a to the brass tube collimator 102b is calculated according to.
Determination of appropriate experimental parameters
Determining the respective diffraction angles theta of the Mo-K α 1 ray and the Mo-K α 2 ray1、θ2The difference theta between the diffraction angles, the rotating diameter of the rotating table 201c-2 and the length of the fine adjustment rod 201c-3, and the angle of rotation of the rotating table 201c-2 during fine adjustment of the single crystal are converted into the length L of the brass tube collimator 102b2. Meanwhile, the voltage parameters, the delay emission time and the like of the flash X-ray machine 101 are further determined according to specific conditions.
The length X of the lead collimator 102a is calculatedpbIs recorded as L1
Experiments show that when the anode material of the X-ray diode is a W target, a 25mm steel plate can penetrate through the position of 2.5m, and when a Mo target is adopted, the strength change coefficient is as follows: zMo/ZW＝42/74
Attenuation according to X-ray equation:
wherein: k is a constant, Z is the atomic number of the metal absorbing the X-rays, X is the thickness of the steel sheet, and λ represents the wavelength of the X-rays. Furthermore, for point sources, the intensity of the X-rays is inversely proportional to the square of the source distance, i.e.:
the distance r from the anode target surface in the flash X-ray tube to the window of the X-ray tube in the systempb125mm, known as rFe12500mm for steel, IFe1Is when r isFe1Intensity of X-ray corresponding to 2500mm, IFe2To point light source r at X-ray distanceFe2The strength of the penetration steel plate is marked as F; for lead, IPb1Is when r ispb1Intensity of X-ray at 25mm, Ipb2Is an X-ray distance point light source rPb2Intensity of where r isFe2＝rPb2。
The change in wavelength λ from W to Mo target was not taken into account, but only the change in atomic number Z. According to formulae (1), (2), (3) and (4), the following formula is obtained:
I0exp[-kλ3ZFe 3ρFeF]/25002＝(42/74)I0exp[-kλ3ZPb 3ρPbxpb]/252(5)
the length X of the lead collimator required for completely absorbing the scattered flash X-rays can be calculatedpbIs recorded as L1。
The (220) plane is selected as the crystal plane of the Ge single crystal, the crystal plane parameters and the crystal plane spacing d are known, and the crystal lattice constant a of Ge is 0.5658nm according to the following formula:
it can be calculated that d is 0.3267nm, the flash X-ray machine 101 uses a Mo target, and the wavelength λ is obtained by searchingMo-Kα10.07093nm, wavelength λMo-Kα2K was calculated according to bragg's law (7) at 0.07135nmα1Ray, Kα2Bragg angle theta of ray1And theta2。
2dsinθ＝nλ (7)
Subtracting the two to obtain Kα1Ray sum Kα2The angular difference θ between the bragg angles of the rays, i.e., the difference between the diffraction angles thereof, was 0.06 °. Then according to the width d (0.3 mm) of the lead slit) The sum L of the lengths of the lead collimator 102a and the brass tube collimator 102b is calculated, that is:
L＝d/tanθ (8)
the length L of the lead collimator 102a is subtracted from the length L1The length L of the brass tube collimator 102b can be obtained2。
In the adjusting process, the specific operation steps are as follows:
1) firstly, the light path of flash X-ray diffraction is adjusted, firstly, Ge single crystal is rotated and coarsely adjusted to form K α 1 ray diffraction angle theta with the horizontal direction1The coarse tuning process is as follows:
firstly, finely adjusting a pitching table 201c-1 to ensure that the Ge single crystal installed in the monochromatic unit 201 is always in a vertical direction, then determining the optical path axis of incident light by using the collimation unit 102, adjusting the position of the crystal to enable the surface normal line to coincide with the optical path axis and determining the crystal as a reference position, and finally adjusting the position of the crystal to enable the included angle between the surface of the crystal and the optical path axis to be at a K α 1 ray diffraction angle theta1In the vicinity, the angle is determined as the initial diffraction angle.
2) The direction in which the Ge single crystal is rotated after rough adjustment is not very precise, and fine adjustment of the Ge single crystal is required.
The fine tuning process is as follows:
the method comprises the steps of enabling a flash X-ray machine to generate flash X-rays, enabling the flash X-rays to pass through a lead slit, a lead collimator 102a and a brass tube collimator 102b at the moment, and then enabling the flash X-rays to enter a Ge single crystal in a monochromatic unit 201, using a fine tuning rod 201c-3 to match with a digital display to adjust a rotating table 201c-2 according to the calculated difference theta (smaller than 0.1 degree) of diffraction angles of K α 1 rays and K α 2 rays, ensuring that the rotating angle of the rotating table 201c-2 does not exceed the angle theta every time, judging the optimal diffraction position of the Ge single crystal according to the brightness change of diffraction imaging on an imaging plate 301, namely when the number of diffracted photons received on the imaging plate is the maximum, recording the optimal diffraction position, and rotating the Ge single crystal in the monochromatic unit 201 to the optimal diffraction position every time when a flash X-ray diffraction experiment is carried out.
3) After the position of the Ge single crystal is adjusted, a flash X-ray diffraction experiment can be performed. The diffraction direction of the diffraction line is calculated according to the crystal plane direction of the crystal to be measured, and then the imaging plate 301 is adjusted to be in the direction which is optimal for receiving the diffraction line.
4) Then, an external controller and a high-voltage pulse generator are adjusted, so that the flash X-ray diode emits high-energy flash X-rays, and the exposure time reaches a nanosecond level.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. A high-energy monochromatic flash X-ray diffraction imaging system, characterized by: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
the emission collimation module (100) comprises a flash X-ray machine (101) and a collimation unit (102), wherein the flash X-ray machine (101) emits X rays, and the collimation unit (102) is connected with the flash X-ray machine (101) and is positioned on the edge line of the X-ray emitting end;
the monochromatic separation module (200) is arranged on the line of the X-ray and comprises a monochromatic unit (201) and an emergent unit (202), the monochromatic unit (201) is connected with the emergent unit (202), and the emergent unit (202) is positioned on one side of the emergent end of the monochromatic unit (201);
the diffraction imaging module (300) is positioned on the line of the emergent direction of the monochromatic separation module (200) and comprises an imaging plate (301) and a rotating seat (302), and the rotating seat (302) is arranged at the bottom end of the imaging plate (301).
2. The high-energy monochromatic flash X-ray diffraction imaging system according to claim 1, wherein the flash X-ray machine (101) comprises a high-voltage pulse generator and a flash X-ray tube, and the X-rays emitted by the flash X-ray tube comprise K α 1 rays, K α 2 rays and K β rays.
3. The high-energy monochromatic flash X-ray diffraction imaging system of claim 2, wherein: the collimating unit (102) comprises a lead collimator (102a), a brass tube collimator (102b) and a glass capillary tube (102c), the brass tube collimator (102b) is connected to the outlet end of the lead collimator (102a), and the glass capillary tube (102c) is arranged in the inner cavity of the lead collimator (102a) and communicated with the inlet end and the outlet end of the lead collimator.
4. The high-energy monochromatic flash X-ray diffraction imaging system of claim 3, wherein: the mono-color unit (201) comprises a brass cylinder (201a), a single crystal (201b) and an angular position table (201c), wherein the single crystal (201b) is positioned in the inner cavity of the brass cylinder (201a) and is placed at the top of the angular position table (201c), and the bottom of the angular position table (201c) extends through the side wall of the brass cylinder (201a) and is arranged at the outer side of the side wall.
5. The high-energy monochromatic flash X-ray diffraction imaging system of any one of claims 1 to 4, wherein: the angular position table (201c) comprises a pitching table (201c-1), a rotating table (201c-2) and a fine adjustment rod (201c-3), wherein the pitching table (201c-1) is fixed at the top of the rotating table (201c-2), and the fine adjustment rod (201c-3) is connected to the rotating axis of the rotating table (201 c-2).
6. The high-energy monochromatic flash X-ray diffraction imaging system of claim 5, wherein: the emergent unit (202) comprises an emergent brass tube (202a), a transverse moving plate (202b) and a longitudinal moving plate (202c), the transverse moving plate (202b) and the longitudinal moving plate (202c) are respectively and movably matched with two ends of the emergent brass tube (202a), and one end, matched with the transverse moving plate (202b), of the emergent brass tube (202a) is connected with the emergent end of the brass cylinder (201 a).
7. The high-energy monochromatic flash X-ray diffraction imaging system of claim 6, wherein: a limiting rod and a connecting groove are arranged at one end of the outgoing brass tube (202a) matched with the transverse moving plate (202b), and a U-shaped sliding groove is arranged at one end of the outgoing brass tube (202c) matched with the longitudinal moving plate (202 c);
the middle part of the side wall of the transverse moving plate (202b) is provided with a longitudinal slit (202 b-1);
the middle part of the side wall of the longitudinal moving plate (202c) is provided with a transverse slit (202 c-1).
8. A high-energy monochromatic flash X-ray diffraction imaging method is characterized in that: the diffractive imaging system employing claim 1, comprising:
determining suitable experimental parameters including selecting said single crystal (201b) and a flash X-ray tube anode material;
calculating the length of the collimating unit (102) according to the selected material, and then calculating the diffraction angles of the K α 1 ray and the K α 2 ray and the difference value of the diffraction angles of the two rays respectively;
establishing a diffraction imaging model of monochromatic flash X-rays according to the calculated value;
enabling the model, and determining the optimal diffraction position of the single crystal (201b) through adjustment;
the rotating base (302) is adjusted to obtain the best diffraction imaging effect on the imaging plate (301) after the monochromatic separation of the X-rays.
9. The high-energy monochromatic flash X-ray diffraction imaging method of claim 8, wherein: according to the calculated length of the collimation unit (102), the lengths of the lead collimator (102a) and the brass tube collimator (102b) are calculated respectively, the outer diameter of the brass tube collimator (102b) is far smaller than that of the lead collimator (102a), and the inner diameters of the lead collimator and the brass tube collimator are the same.
10. The high-energy monochromatic flash X-ray diffraction imaging method of claim 9, wherein: during adjustment, the pitching table (201c-1) is roughly adjusted, so that the single crystal (201b) is kept vertical to the horizontal plane;
and driving the rotating platform (201c-2) by finely adjusting the fine adjusting rod (201c-3) and matching with the imaging plate (301) to determine that the monocrystal (201b) is in the optimal diffraction position.
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