CN115616011A - Ultrasonic suspension sample table for synchrotron radiation X-ray scattering test - Google Patents

Ultrasonic suspension sample table for synchrotron radiation X-ray scattering test Download PDF

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CN115616011A
CN115616011A CN202211346061.4A CN202211346061A CN115616011A CN 115616011 A CN115616011 A CN 115616011A CN 202211346061 A CN202211346061 A CN 202211346061A CN 115616011 A CN115616011 A CN 115616011A
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stage
axis
sample
optical axis
ultrasonic
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洪春霞
缪夏然
周平
边风刚
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Shanghai Advanced Research Institute of CAS
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Shanghai Advanced Research Institute of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G01N23/20025Sample holders or supports therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/10Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G01N23/20025Sample holders or supports therefor
    • G01N23/20033Sample holders or supports therefor provided with temperature control or heating means
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/201Investigating 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 measuring small-angle scattering
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/05Investigating materials by wave or particle radiation by diffraction, scatter or reflection
    • G01N2223/054Investigating materials by wave or particle radiation by diffraction, scatter or reflection small angle scatter
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/10Different kinds of radiation or particles
    • G01N2223/101Different kinds of radiation or particles electromagnetic radiation
    • G01N2223/1016X-ray
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/30Accessories, mechanical or electrical features
    • G01N2223/309Accessories, mechanical or electrical features support of sample holder
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/30Accessories, mechanical or electrical features
    • G01N2223/31Accessories, mechanical or electrical features temperature control
    • G01N2223/3106Accessories, mechanical or electrical features temperature control heating, furnaces
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/60Specific applications or type of materials
    • G01N2223/637Specific applications or type of materials liquid

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Abstract

The invention relates to an ultrasonic suspension sample stage for synchrotron radiation X-ray scattering test, which comprises a real-time detection light focusing device and an ultrasonic suspension device, wherein the real-time detection light focusing device and the ultrasonic suspension device are sequentially arranged on a first optical axis along the incident direction of X-rays; the real-time detection light focusing device comprises a CCD camera, an electric zoom lens barrel and a plane reflector which are sequentially arranged on a second optical axis vertical to the first optical axis, wherein the plane reflector is positioned at the intersection point of the first optical axis and the second optical axis; the plane reflector is provided with a through hole for X-ray to pass through. According to the ultrasonic suspension sample stage for the synchrotron radiation X-ray scattering test, disclosed by the invention, a sample can be suspended during the scattering test through the ultrasonic suspension device, so that the influence of other supporting materials on a scattering signal is avoided; the light path and the X-ray during testing are coaxial through the real-time detection light-focusing device, the field difference is eliminated, and meanwhile, the X-ray can be ensured to irradiate the preset position of the sample in real time.

Description

Ultrasonic suspension sample table for synchrotron radiation X-ray scattering test
Technical Field
The invention relates to the technical field of synchrotron radiation X-ray scattering tests, in particular to an ultrasonic suspension sample table for synchrotron radiation X-ray scattering tests.
Background
The synchrotron radiation X-ray technology is an important means for researching the microstructure evolution law of a liquid (melt) material under the action of an external field, such as the dynamic self-assembly behavior of a liquid nano material, the evaporation phase transformation behavior of colloid drops, the cooling crystallization behavior of a soft substance solution and the like.
Because of gravity, the liquid (melt) material needs to be encapsulated in a cavity made of a specific material when the synchrotron radiation X-ray scattering test is carried out at present, which brings great inconvenience to the collection of scattering signals and the analysis of data, such as: the difference of the electron cloud density of the liquid (melt) material is small, and the scattering signal of the liquid (melt) material can be further weakened by the absorption of the cavity material on the X-ray, even the scattering signal of the liquid (melt) material disappears; scattering signals (scattering rings, orientation, stray and the like) also exist in the cavity material, and the scattering signals may shield the scattering signals of the liquid (melt) material, so that the difficulty of data analysis is increased; the cavity material is contacted with the liquid (melt) material, and the microstructure evolution behavior of the liquid (melt) material under the action of an external force field and the like can be influenced.
If the liquid (solution) material can be suspended by the ultrasonic suspension device during the synchrotron radiation X-ray scattering test, and is not in contact with other supporting materials, no other window material is arranged on an X-ray light path, and the problems can be well solved. However, the experimental station for synchrotron radiation X-ray scattering test has a small space and many internal devices, so the spatial layout of the ultrasonic suspension device and other devices of the experimental station is a technical problem to be solved urgently; in addition, since the X-ray is invisible light, how to ensure that the X-ray enters a specific part of the suspended sample after the X-ray reaches the sample point of the experiment station is another technical problem to be solved.
Disclosure of Invention
The invention aims to provide an ultrasonic suspension sample stage for synchrotron radiation X-ray scattering test, which can suspend a sample during test, guide X-rays to enter a preset position of the sample and detect the light focusing state of the sample in real time.
In view of the above, the present invention provides an ultrasonic suspension sample stage for synchrotron radiation X-ray scattering test, comprising a real-time detection focusing device and an ultrasonic suspension device, which are sequentially arranged on a first optical axis along an incident direction of X-rays, wherein the ultrasonic suspension device is arranged to suspend a sample on the first optical axis.
The real-time detection light-focusing device comprises a CCD camera, an electric zoom lens barrel and a plane reflector which are sequentially arranged on a second optical axis vertical to the first optical axis, wherein the plane reflector is positioned at the intersection of the first optical axis and the second optical axis.
And the plane reflector is provided with a through hole for X-rays to pass through.
Furthermore, the real-time detection focusing device further comprises a first electric platform and a second electric platform, the first electric platform is arranged on the second electric platform, the CCD camera and the electric zoom lens barrel are arranged on the first electric platform, the second electric platform is arranged to adjust the position of the X axis and the position of the Z axis of the first electric platform, and the first electric platform is arranged to adjust the position of the CCD camera and the position of the electric zoom lens barrel on the lens focusing axis and the position of the Y axis.
Furthermore, the second electric platform comprises an X-axis sliding table and a Z-axis sliding table, the Z-axis sliding table is arranged on the X-axis sliding table or the X-axis sliding table is arranged on the Z-axis sliding table, the X-axis sliding table is arranged to be capable of moving on the X axis, and the Z-axis sliding table is arranged to be capable of moving on the Z axis.
Further, an adjusting platform is arranged on the second electric platform, the plane reflecting mirror is arranged on the adjusting platform, and the adjusting platform is arranged to adjust the inclination angle of the plane reflecting mirror and the X axis and the rotation angle around the Z axis, so that the X ray can completely pass through the through hole on the plane reflecting mirror.
Further, adjust the platform and include inclination platform and revolving stage, inclination platform locates on the support frame, the revolving stage is located inclination bench, the plane mirror is located on the revolving stage, inclination platform sets up to adjust the angle of pitch of plane mirror and X axle, the revolving stage sets up to adjust the plane mirror is around the rotation angle of Z axle.
Further, the real-time detection focusing device further comprises a shell, the CCD camera, the electric zoom lens barrel, the plane reflector, the first electric platform and the second electric platform are all arranged in the shell, and a through hole for X-rays to pass through is formed in the shell.
Further, the CCD camera control device further comprises a control device, and the control device is electrically connected or in communication connection with the CCD camera.
Further, the plane mirror is elliptical; and/or, the plane reflector is plated with a film; and/or the included angle between the plane reflector and the first optical axis and the included angle between the plane reflector and the second optical axis are both 45 degrees.
Further, the ultrasonic suspension device comprises an ultrasonic generator, an amplitude transformer, an emission end, a reflection end supporting platform and a C-shaped frame, wherein the ultrasonic generator is electrically connected with the amplitude transformer, the amplitude transformer and the emission end are fixed at the top end of the C-shaped frame, the reflection end supporting platform is arranged at the bottom end of the C-shaped frame, the reflection end is arranged on the reflection end supporting platform, and the reflection end supporting platform is arranged to adjust the position of the reflection end, so that the reflection end, the amplitude transformer and the emission end are concentrically arranged and are positioned under the amplitude transformer and the emission end.
Further, the device comprises a heating device and a temperature measuring device, wherein the heating device is used for heating the sample, and the temperature measuring device is used for monitoring the real-time temperature of the sample.
According to the ultrasonic suspension sample stage for the synchrotron radiation X-ray scattering test, disclosed by the invention, a sample can be suspended during the scattering test through the ultrasonic suspension device, so that the influence of other supporting materials on a scattering signal is avoided; the light path and the X-ray are coaxial during testing through the real-time detection light-focusing device, the field difference is eliminated, and meanwhile, the X-ray can be ensured to irradiate the preset position of the sample in real time; the sample is heated through the heating device, so that the microstructure evolution law of the sample under the action of the thermal external force can be conveniently researched.
Drawings
FIG. 1 is a schematic structural diagram of an ultrasonic suspension sample stage for synchrotron radiation X-ray scattering test according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of an adjustment platform according to an embodiment of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
As shown in fig. 1, an embodiment of the present invention provides an ultrasonic levitation sample stage for synchrotron radiation X-ray scattering test, including a real-time detection focusing device 100 and an ultrasonic levitation device 200 sequentially disposed on a first optical axis I along an incident direction of X-rays, where the ultrasonic levitation device 200 is configured to levitate a sample 700 on the first optical axis I, and the real-time detection focusing device 100 is configured to make the X-rays incident on a preset position of the sample 700 and detect a focusing state of the sample in real time. In some embodiments, the first optical axis I is a horizontal optical axis (i.e., Y-axis) and the X-rays are synchrotron radiation X-rays provided by the beam-line station.
The real-time detection focusing device 100 comprises a CCD camera 101, an electric zoom lens barrel 102 and a plane mirror 103 which are sequentially arranged on a second optical axis II, wherein the electric zoom lens barrel 102 is fixed on the CCD camera 101 to adjust the magnification to realize the magnification and the reduction of an image on the CCD camera 101, and the plane mirror 103 is positioned at the intersection point of the first optical axis I and the second optical axis II and is used for reflecting light irradiated on the plane mirror to the CCD camera 101. Specifically, during the test, the visible light irradiates on the sample 700 and is then reflected by the sample 700, the reflected light reaches the plane mirror 103 along the first optical axis I and is then reflected by the CCD camera 101, and the CCD camera 101 performs imaging by using the reflected light of the sample 700. The plane mirror 103 is provided with a through hole (for example, a through hole with a diameter of 2mm is drilled at the center, not shown in the figure) through which the X-ray passes, wherein the second optical axis II is an axis (i.e., X-axis) perpendicular to the first optical axis I in the horizontal plane. In some embodiments, the real-time light focusing detection apparatus 100 may further include a second motorized stage 105, the second motorized stage 105 is provided with a first motorized stage 104, the CCD camera 101 and the motorized zoom lens barrel 102 are provided on the first motorized stage 104, and the first motorized stage 104 is configured to adjust positions of the CCD camera 101 and the motorized zoom lens barrel 102 in the lens focusing axis and the Y axis, so as to adjust the focal length and center the lens field of view. In this embodiment, the lens focusing axis may coincide with the X axis. The second motorized stage 105 is configured to be movable in the same direction as the X-axis and the Z-axis (i.e., the third axis III, which is perpendicular to the horizontal plane) to adjust the X-axis and Z-axis positions of the device (e.g., the first motorized stage 104) positioned thereon.
The second motorized stage 105 may be a slide table of a ball screw structure. Specifically, the second electric platform 105 may include an X-axis sliding table 1051 and a Z-axis sliding table 1052, both the X-axis sliding table 1051 and the Z-axis sliding table 1052 adopt ball screw structures, and a motor drives the ball screw structures to move the X-axis of the X-axis sliding table 1051, and the Z-axis sliding table 1052 can move the Z-axis, and the Z-axis sliding table 1052 is installed on the X-axis sliding table 1051, so the X-axis sliding table 1051 can drive the Z-axis sliding table 1052 to move on the X-axis, and the Z-axis sliding table 1052 itself can move on the Z-axis, and therefore, the device located on the Z-axis sliding table 1052 can move on the X-axis and the Z-axis simultaneously. In other embodiments, the X-axis sliding table 1051 may be installed on the Z-axis sliding table 1052, so that the Z-axis sliding table 1052 may drive the X-axis sliding table 1051 to move along the Z-axis, and thus the device located on the X-axis sliding table 1051 may move along the X-axis and the Z-axis. Similarly, the first electric platform 104 may also adopt a similar structure, and only needs to adjust the direction of the ball screw structure to the lens focusing axis and the Y axis.
In some embodiments, the plane mirror 103 is elliptical with a thickness of 6mm. In other embodiments, the normal of the plane mirror 103 forms an angle of 45 ° with both the first optical axis I and the second optical axis II, and the mirror surface of the plane mirror 103 faces the CCD camera 101, so that the reflected light of the sample 700 can be observed in the CCD camera 101, and the occupied space of the CCD camera 101 can be minimized, thereby facilitating the scattering test. The surface of the plane mirror 103 may be coated to increase the reflectivity of light.
During testing, the center of the field of view of the CCD camera 101 and the X-ray need to be focused on the same point of the sample 700, so as to calibrate the position of the X-ray, and to realize the function of guiding the X-ray to enter the preset position (for example, the center of the sample) of the sample 700 through the imaging spectrum of the CCD camera 101. Since the X-ray is invisible light, when the position of the X-ray is calibrated, a scintillation crystal (which can be fixed by a bracket) needs to be placed at a position where the sample 700 is to be placed before placing the sample 700, that is, the scintillation crystal and the sample 700 need to be placed at the same position, so that a visible light spot is generated after the X-ray irradiates the scintillation crystal, and then the visible light spot can be seen by the CCD camera 101, and the positions of the CCD camera 101 and the electric zoom lens barrel 102 are adjusted by the first electric platform 104, so that the visible light spot on the scintillation crystal is clear and moves to the center of the field of view of the CCD camera 101 (that is, the cross cursor), so that the center of the field of view of the CCD camera 101 is the incident position of the X-ray; then, only the scintillation crystal needs to be removed, the sample 700 is suspended, and the position of the ultrasonic suspension device 200 is adjusted to enable the sample 700 to be located at the center of the field of view of the CCD camera 101, so that the center of the field of view of the CCD camera 101 and the X-ray can be focused on the same point (i.e., the preset position) of the sample 700.
The CCD camera 101 may be electrically connected or communicatively connected to the control device 110, and the CCD camera 101 transmits the image of the sample 700 to the control device 110, and displays and stores the image in real time through a display device of the control device, so as to facilitate real-time observation and recording of test data. The control system of the laboratory station may also be electrically or communicatively connected to the first motorized stage 104 and the second motorized stage 105 to control their movements so as to adjust the light state of the sample 700 in real time (i.e., to ensure that the X-rays irradiate the preset position of the sample 700).
The plane mirror 103 may be mounted on an adjustment stage 108, and the adjustment stage 108 is used to adjust the pitch angle of the plane mirror 103 along the X-axis and the rotation angle around the Z-axis so that the X-ray can pass through the hole of the plane mirror 103 completely without being blocked by any position of the plane mirror 103. The adjusting platform 108 can be mounted on the second electric platform 105 through the supporting frame 109, for example, the supporting frame 109 is fixed on the second electric platform 105, and the adjusting platform 108 is fixed on the supporting frame 109, so that the position of the plane mirror 103 can be automatically adjusted to the intersection point of the first optical axis I and the second optical axis II through the second electric platform 105 to realize coarse adjustment, and then the pitch angle between the plane mirror 103 and the X axis and the rotation angle around the Z axis can be adjusted through the adjusting platform 108 to realize fine adjustment.
As shown in fig. 2, the adjusting platform 108 includes an inclination table 1081 and a rotation table 1082, the inclination table 1081 is connected to the supporting frame 109 through screws, so as to adjust the pitch angle of the mirror around the X axis, the rotation table 1082 is fixed on the inclination table through screws, so as to adjust the rotation angle of the mirror around the Z axis, and the supporting frame of the plane mirror 103 is fixed on the rotation table through screws, so as to adjust different postures of the plane mirror, and ensure that any position of the central through hole of the mirror surface of the plane mirror does not block X-rays. The tilt stage 1081 and the rotation stage 1082 are conventional devices in the art, and the detailed structure and principle thereof are not described herein.
With continued reference to fig. 1, the real-time inspection focusing apparatus 100 and the ultrasonic levitation apparatus 200 may be disposed on a support platform 600 of the laboratory station, the support platform 600 being parallel to the horizontal plane.
The real-time detection focusing device 100 may further include a housing 106, a ccd camera 101, an electric zoom lens barrel 102, a plane mirror 103, a first electric platform 104, a second electric platform 105, and the like all disposed in the housing 106, and the housing 106 is further provided with a through hole 1061 for X-rays to pass through, so that the components therein may be protected without affecting the passage of X-rays. In one embodiment, the housing 106 is secured to the base 107 and the base 107 is secured to the support platform 600. The housing 106 has a detachable front and rear bezel, which can be removed when the alignment is required, and then mounted after adjustment.
The ultrasonic levitation device 200 comprises an ultrasonic generator 201, a horn 202, an emission end 203, a reflection end 204, a reflection end supporting platform 205 and a C-shaped frame 207, wherein the horn 202 and the emission end 203 are fixed at the top end of the C-shaped frame 207, the reflection end supporting platform 205 is arranged at the bottom end of the C-shaped frame 207, the reflection end 204 is arranged on the reflection end supporting platform 205, and the reflection end supporting platform 205 is used for adjusting the position of the reflection end 204 to ensure that the reflection end 204 is concentrically arranged with the horn 202 and the emission end 203 and is positioned right below the horn 202 and the emission end 203; the ultrasonic generator 201 is electrically connected to the horn 202 for generating and transmitting ultrasonic waves to the horn 202, and then the ultrasonic waves are emitted from the emitting end 203, and the ultrasonic waves are reflected on the end surface of the reflecting end 204, so that a sound field is formed between the end surfaces of the reflecting end 204 and the emitting end 203, and the sound field has a plurality of standing wave points, so that the sample 700 can be suspended at the standing wave points. The C-frame 207 may be fixed to a third motorized stage 206, and the third motorized stage 206 is used to adjust the X-axis and Z-axis positions of the C-frame 207 so that the sample 700 may be suspended on the first optical axis I. The structure and principle of the ultrasonic suspension device can be seen in the chinese utility model patent with publication number CN211062302U, which is not described herein again.
In some embodiments, the ultrasonic levitation sample stage may further include a heating device 300 and a temperature measuring device 400, which are both disposed on the supporting platform 600, wherein the heating device 300 is used to heat the sample 700, so as to facilitate the study of the microstructure evolution law of the sample 700 in the thermal external force action state (e.g., liquid evaporation, melt melting state); the temperature measuring device 400 is used to monitor the real-time temperature of the sample 700. The heating device 300 and the temperature measuring device 400 can be disposed beside the first optical axis I to avoid blocking X-rays.
In a specific embodiment, the heating device 300 may employ laser heating, and includes a laser 301 and a conditioning stage 302, the laser 301 is disposed on the conditioning stage 302, and the laser 301 is used to emit small laser beams formed by focusing in various stages to heat the sample 700; the adjustment stage 302 is used to adjust the position of the laser 301 so that the laser beam emitted by the laser 301 can be accurately irradiated on the sample 700. The heating device 300 may further include a protection plate 303, which may be disposed on the ultrasonic levitation device 200, for protecting the rest of the devices from the laser irradiation, thereby preventing damage. The shield plate 303 may be made of a material that is resistant to irradiation (does not deform and melt after laser irradiation), such as iron or stainless steel.
In this embodiment, the temperature control range that can be realized by the heating device 300 is room temperature to 200 ℃, and the temperature control accuracy is ± 1 ℃.
In one embodiment, the temperature measuring device 400 includes a thermal infrared imager 401 and a gimbal control stage 402, the thermal infrared imager 401 being mounted on the gimbal control stage 402, and the gimbal control stage 402 being used to adjust the attitude of the thermal infrared imager 401 to accurately measure the temperature of the sample 700.
The supporting platform 600 may further have a detector 500 for synchrotron radiation small-angle scattering, which is located on the first optical axis I and on a side of the ultrasonic levitation apparatus 200 away from the real-time detection and alignment apparatus 100 to receive a scattering signal from the sample.
In the experiment station, except the place of placing the ultrasonic suspension sample platform, vacuum pipelines are installed at other places, and X rays of the beam line station irradiate to the ultrasonic suspension sample platform through the vacuum pipelines so as to ensure that the X rays are always in a low vacuum state and avoid the sample signals from being weakened by air impurities. The thickness of the real-time detection light focusing device 100 can be as low as 9mm, the ultrasonic suspension device 200 is also thin, and the heating device 300 and the temperature measuring device 400 are arranged on the side surface of the optical path (namely the first optical axis I), so that the length of an air segment on the optical path is shortened as much as possible, the structure is compact, a sample signal is good, and the problem of spatial layout is well solved.
According to the ultrasonic suspension sample stage for the synchrotron radiation X-ray scattering test, disclosed by the embodiment of the invention, the sample 700 can be suspended during the scattering test through the ultrasonic suspension device 200, so that the influence of other supporting materials on a scattering signal is avoided; the optical device 100 is detected in real time, so that the optical path during testing is coaxial with the X-ray, the field difference is eliminated, and meanwhile, the X-ray can be ensured to irradiate the preset position of the sample 700 in real time; the sample 700 is heated by the heating device 300, so that the microstructure evolution law of the sample 700 in the state of the action of the external thermal force can be conveniently researched. The ultrasonic suspension sample table can be used as a conventional experimental liquid (melt) sample table for a small-angle scattering ray station, is favorable for improving the quality of liquid (melt) scattering data of the small-angle scattering ray station, and promotes the research results in related research fields.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.

Claims (10)

1. An ultrasonic suspension sample stage for synchrotron radiation X-ray scattering test is characterized by comprising a real-time detection light focusing device and an ultrasonic suspension device which are sequentially arranged on a first optical axis along the incident direction of X-rays, wherein the ultrasonic suspension device is arranged to suspend a sample on the first optical axis;
the real-time detection light-focusing device comprises a CCD camera, an electric zoom lens barrel and a plane reflector which are sequentially arranged on a second optical axis vertical to the first optical axis, wherein the plane reflector is positioned at the intersection of the first optical axis and the second optical axis;
and the plane reflector is provided with a through hole for X-rays to pass through.
2. The ultrasonically suspended sample stage for synchrotron X-ray scattering testing of claim 1, wherein the real-time alignment detection apparatus further comprises a first motorized stage and a second motorized stage, the first motorized stage being disposed on the second motorized stage, the CCD camera and the motorized zoom lens barrel being disposed on the first motorized stage, the second motorized stage being configured to adjust X-axis and Z-axis positions of the first motorized stage, the first motorized stage being configured to adjust positions of the CCD camera and the motorized zoom lens barrel in a lens focusing axis and a Y-axis.
3. The ultrasonic levitation sample stage for synchrotron radiation X-ray scattering test of claim 2, wherein the second motorized stage comprises an X-axis slide and a Z-axis slide, the Z-axis slide being disposed on the X-axis slide or the X-axis slide being disposed on the Z-axis slide, the X-axis slide being configured to be movable on the X-axis, and the Z-axis slide being configured to be movable on the Z-axis.
4. The ultrasonic levitation sample stage for synchrotron radiation X-ray scattering testing of claim 2, wherein an adjustment platform is disposed on the second motorized platform, and the planar mirror is disposed on the adjustment platform, and the adjustment platform is configured to adjust the tilt angle of the planar mirror with respect to the X-axis and the rotation angle about the Z-axis such that X-rays can pass completely through the through hole in the planar mirror.
5. The ultrasonically suspended sample stage for synchrotron X-ray scattering testing of claim 4, wherein the conditioning stage comprises a tilt stage and a rotary stage, the tilt stage is mounted on the second motorized stage by a support frame, the rotary stage is disposed on the tilt stage, the plane mirror is disposed on the rotary stage, the tilt stage is configured to adjust a pitch angle of the plane mirror with respect to the X-axis, and the rotary stage is configured to adjust a rotation angle of the plane mirror about the Z-axis.
6. The ultrasonic suspended sample stage for synchrotron radiation X-ray scattering test of claim 2, wherein the real-time detection focusing device further comprises a housing, the CCD camera, the electric zoom lens barrel, the plane mirror, the first electric platform and the second electric platform are all disposed in the housing, and a through hole for X-ray to pass through is opened on the housing.
7. The ultrasonically suspended sample stage for synchrotron radiation X-ray scattering testing of claim 1, further comprising a control device, wherein said control device is electrically or communicatively connected to said CCD camera.
8. The ultrasonic suspended sample stage for synchrotron radiation X-ray scattering testing of claim 1, wherein said plane mirror is elliptical; and/or, the plane reflector is plated with a film; and/or the included angle between the plane reflector and the first optical axis and the included angle between the plane reflector and the second optical axis are both 45 degrees.
9. The ultrasonic levitation sample stage for synchrotron radiation X-ray scattering test of claim 1, wherein the ultrasonic levitation device comprises an ultrasonic generator, an amplitude transformer, a transmitting end, a reflecting end support platform and a C-shaped frame, the ultrasonic generator is electrically connected with the amplitude transformer, the amplitude transformer and the transmitting end are fixed at the top end of the C-shaped frame, the reflecting end support platform is arranged at the bottom end of the C-shaped frame, the reflecting end is arranged on the reflecting end support platform, and the reflecting end support platform is arranged to adjust the position of the reflecting end, so that the reflecting end is concentrically arranged with the amplitude transformer and the transmitting end and is located right below the amplitude transformer and the transmitting end.
10. The ultrasonically suspended sample stage for synchrotron radiation X-ray scattering testing of claim 1, further comprising a heating device configured to heat the sample and a temperature measuring device configured to monitor a real-time temperature of the sample.
CN202211346061.4A 2022-10-31 2022-10-31 Ultrasonic suspension sample table for synchrotron radiation X-ray scattering test Pending CN115616011A (en)

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CN202211346061.4A CN115616011A (en) 2022-10-31 2022-10-31 Ultrasonic suspension sample table for synchrotron radiation X-ray scattering test

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CN202211346061.4A CN115616011A (en) 2022-10-31 2022-10-31 Ultrasonic suspension sample table for synchrotron radiation X-ray scattering test

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CN115616011A true CN115616011A (en) 2023-01-17

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