X-ray photon correlation spectrum sample experiment platform and regulation and control method thereof

Abstract

The invention provides an X-ray photon correlation spectrum sample experiment platform which is suitable for being used in combination with an X-ray and an X-ray detector and is coaxial with the X-ray. The experimental sample platform comprises an optical collimation laser instrument, a filter device, a first light limiting element, a second light limiting element, a sample table, a temperature control module and a photoelectric detector which are coaxially arranged in sequence in the X-ray diffraction direction; according to the regulation and control method of the X-ray photon correlation spectrum sample experiment platform, the coherence degree of incident light is improved by using light limiting elements such as a small-hole diaphragm and limiting the size of incident light spots, coherent X-rays are accurately irradiated on a sample by positioning the sample, and the problem that an XPCS experiment cannot be carried out by a synchrotron radiation light source in China at present is solved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of ray detection micron-level nanometer substance movement, in particular to an X-ray photon correlation spectroscopy sample experimental platform and a regulation method thereof. BACKGROUND

[0002] X-ray photon correlation spectroscopy (XPCS) has become one of the key probes for nanoscale dynamics in recent years, and is suitable for a wide range of condensed matter systems. XPCS produces a speckle pattern by making a coherent X-ray beam incident on a sample. Since the sample structure changes over time, the corresponding speckle distribution will also fluctuate over time. By analyzing the change of intensity correlation over time, the dynamic information of the sample can be obtained. The necessary conditions for XPCS experiment include: making the coherent light beam pass through the center of the sample, precisely controlling the sample temperature; however, the coherence of the X-ray generated by the third generation synchrotron cannot meet the experimental requirements, that is, the synchrotron cannot meet the conditions for carrying out XPCS experiment.

[0003] Therefore, in order to improve the correlation degree of the incident light to meet the requirements of XPCS experiment, and make it accurately pass through the sample stage and receive signals at the detector, it is urgent to develop an experimental platform to solve the above problems. SUMMARY

[0004] In view of the above-mentioned shortcomings of the prior art, the purpose of the present application is to provide an X-ray photon correlation spectroscopy sample experimental platform and a regulation method thereof, which is used to solve the technical problem that the synchrotron radiation source cannot carry out XPCS experiment in the prior art.

[0005] To achieve the above-mentioned purpose and other related purposes, the present application provides an X-ray photon correlation spectroscopy sample experimental platform, comprising: the X-ray photon correlation spectroscopy sample experimental platform is adapted to be used with X-ray and X-ray detector, with X-ray as the coaxial, the experimental sample platform includes optical collimation laser instrument, filter device, first light limiting element, second light limiting element, sample stage, temperature control module and photoelectric detector which are coaxially arranged in turn along the X-ray diffraction direction;

[0006] The first light limiting element is controlled by a first double motor to move in the vertical coaxial plane;

[0007] The second light limiting element is controlled by a second double motor to move in the vertical coaxial plane;

[0008] The temperature control module is closely connected with the sample stage;

[0009] The sample stage and the temperature control module are controlled by a third double motor to move in the vertical coaxial plane;

[0010] The photoelectric detector is controlled by a fourth double motor to move in a vertical coaxial plane;

[0011] The X-ray detector is adapted to be arranged coaxially behind the photoelectric detector.

[0012] In some embodiments of the present application, the distance between the optical collimating laser instrument and the filter device is 8-15 cm.

[0013] In some embodiments of the present application, the distance between the filter device and the first light limiting element is 4-8 cm.

[0014] In some embodiments of the present application, the distance between the first light limiting element and the second light limiting element is 7-12 cm.

[0015] In some embodiments of the present application, the distance between the second light limiting element and the sample stage is 1-3 cm.

[0016] In some embodiments of the present application, the distance between the sample stage and the photoelectric detector is 4-9 cm.

[0017] In some embodiments of the present application, the X-ray detector is adapted to be arranged at a position 20 m or more away from the photoelectric detector.

[0018] In some embodiments of the present application, the laser emitted by the optical collimating laser instrument is in the visible light band, and the size of the exit light spot is 0.9-1.1 mm.

[0019] In some embodiments of the present application, the X-ray is a hard X-ray generated by a synchrotron radiation source, the energy is 5-15 keV, and the wavelength is 0.062-0.248 nm.

[0020] In some embodiments of the present application, the filter device is a switching type wheel disc including filter pieces with different attenuation rates, which is adapted to protect the photoelectric detector and the sample from being damaged.

[0021] In some embodiments of the present application, the first light limiting element is a pinhole diaphragm I, which is adapted to improve the coherence of the X-ray.

[0022] In some embodiments of the present application, the first light limiting element is an X-ray opaque material.

[0023] In some embodiments of the present application, the second light limiting element is a pinhole diaphragm II, which is adapted to reduce stray light generated by the diffraction effect of light and the edge of the pinhole diaphragm I.

[0024] In some embodiments of the present application, the second light limiting element is an X-ray opaque material.

[0025] In some embodiments of the present application, the sample stage is suitable for clamping samples with different appearances.

[0026] In some embodiments of the present application, the sample stage is made of stainless steel.

[0027] In some embodiments of the present application, the temperature control module is a heating and cooling integrated temperature control mechanism, which is suitable for accurately controlling the sample environment.

[0028] In some embodiments of the present application, the temperature control range of the temperature control module is -160℃-200℃.

[0029] In some embodiments of the present application, the response rate of the photodetector is 0.07-0.09 A / W.

[0030] The present application also provides a regulation method of the X-ray photon correlation spectroscopy sample experiment platform as described above, comprising the following steps:

[0031] 1) Adjust the optical collimation laser instrument to the same direction as the X-ray, move the sample stage, the temperature control module and the photodetector into the light path, rotate the filter device, and align the optical collimation laser instrument, the photodetector and the sample stage;

[0032] 2) Move in the first light limiting element, move it on the vertical coaxial plane to obtain the maximum value of the photodetector, realize the alignment of the first light limiting element, record the position of the first light limiting element and then remove it from the light path;

[0033] 3) Move in the second light limiting element, move it on the vertical coaxial plane to obtain the maximum value of the photodetector, realize the alignment of the second light limiting element, move the first light limiting element to the recorded position, and realize the coarse alignment of the optical collimation laser instrument, the first light limiting element and the second light limiting element;

[0034] 4) Turn off the optical collimation laser instrument, turn on the X-ray, move the first light limiting element on the vertical coaxial plane to obtain the maximum value of the photodetector, then move the second light limiting element on the vertical coaxial plane to obtain the maximum value of the photodetector; repeat 3-4 times to achieve fine alignment;

[0035] 5) Remove the photodetector from the light path, and according to the light spot pattern collected by the X-ray detector, finely adjust the first light limiting element and the second light limiting element, and complete the light adjustment.

[0036] The present application also provides a computer storage medium, comprising a readable storage medium and computer instructions, wherein the computer instructions are stored in the readable storage medium; and the computer instructions are used to realize the method of steps 1)-5) in the regulation method of claim 9.

[0037] As described above, the X-ray photon correlation spectroscopy sample experiment platform and the regulation method thereof have the following beneficial effects:

[0038] The X-ray photon correlation spectroscopy sample experiment platform integrates optical, mechanical and temperature control devices on a compact experiment platform, and can simultaneously realize two necessary conditions of XPCS experiment: passing a coherent light beam through the center of a sample and accurately controlling the temperature of the sample, thereby solving the problem that the domestic synchrotron radiation source cannot carry out XPCS experiment. BRIEF DESCRIPTION OF DRAWINGS

[0039] Figure 1 The overall schematic diagram of the X-ray photon correlation spectroscopy sample experiment platform is shown.

[0040] Figure 2 The XPCS experimental detection nanoparticle data image obtained without using the X-ray photon correlation spectroscopy sample experiment platform is shown.

[0041] Figure 3 The XPCS experimental detection nanoparticle data image obtained using the X-ray photon correlation spectroscopy sample experiment platform is shown.

[0042] Figure 4 The experimental data analysis result obtained without using the experimental condition of the present application is shown.

[0043] Figure 5 The experimental data analysis result obtained using the experimental condition of the present application is shown.

[0044] Figure 6 The schematic diagram of the stereoscopic structure of the sample table is shown.

[0045] Figure 7 The schematic diagram of the first light limiting element or the first light limiting element is shown.

[0046] BRIEF DESCRIPTION OF DRAWINGS

[0047] 1 optical collimating laser instrument

[0048] 2 filter device

[0049] 3 first light limiting element

[0050] 4 second light limiting element

[0051] 5 sample table

[0052] 6 temperature control module

[0053] 7 photodetector

[0054] 8 X-ray detector DETAILED DESCRIPTION

[0055] The following specific examples illustrate the implementation of the present invention. Those skilled in the art can easily understand other advantages and effects of the present invention from the content disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and various details in this specification can also be modified or changed based on different viewpoints and applications without departing from the spirit of the present invention.

[0056] It should be noted that, in the description of the invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," "joining," and "fitting" should be interpreted broadly. For example, "connection" can be a fixed connection, a detachable connection, or an integral connection; it can be a direct connection or an indirect connection through an intermediate medium; it can be a connection within two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0057] Moreover, relational terms such as “first” and “second” are used merely to distinguish one component or method step from another that has the same name, and do not necessarily require or imply any such actual relationship or order between these components or method steps.

[0058] Please refer to the accompanying drawings. It should also be noted that the illustrations provided in this embodiment are only schematic representations of the basic concept of the present invention. Therefore, the drawings only show the components related to the present invention and are not drawn according to the actual number, shape and size of the components in the actual implementation. In the actual implementation, the form, quantity and proportion of each component can be arbitrarily changed, and the layout of the components may also be more complex.

[0059] In this invention, "several" means two or more.

[0060] like Figure 1 As shown, the first aspect of the present invention provides an X-ray photon correlation spectrum sample experimental platform, which is suitable for use with X-rays and an X-ray detector 8, with X-rays as the coaxial axis. The experimental sample platform includes an optical collimating laser 1, a filter device 2, a first light-limiting element 3, a second light-limiting element 4, a sample stage 5, a temperature control module 6, and a photodetector 7 arranged coaxially along the X-ray diffraction direction.

[0061] The first light-limiting element 3 is controlled by the first dual motors to move in a vertically coaxial plane;

[0062] The second light-limiting element 4 is controlled by the second dual motor to move in a vertically coaxial plane;

[0063] The temperature control module 6 is tightly connected to the sample stage 5;

[0064] The sample stage 5 and the temperature control module 6 are controlled by a third double motor to move in a vertical coaxial plane;

[0065] The photodetector 7 is controlled by a fourth double motor to move in a vertical coaxial plane;

[0066] The X-ray detector 8 is adapted to be arranged coaxially behind the photodetector 7.

[0067] The "behind" in the X-ray detector 8 adapted to be arranged coaxially behind the photodetector 7 means the arrangement order of each device in the coaxial. In the present application, the arrangement order in the X-ray coaxial is optical collimating laser instrument 1, filter device 2, first light limiting element 3, second light limiting element 4, sample stage 5, temperature control module 6, photodetector 7, X-ray detector 8.

[0068] The first double motor, the second double motor, the third double motor and the fourth double motor are all precision stepping motors. Further, the precision stepping motor has a division angle of 0.8°.

[0069] The distance between the optical collimating laser instrument 1 and the filter device 2 is 8-15 cm. For example, it is 8-9 cm, 9-10 cm, 10-11 cm, 11-12 cm, 12-13 cm, 13-14 cm or 14-15 cm. In the preferred embodiment of the present application, the distance between the optical collimating laser instrument 1 and the filter device 2 is 10 cm.

[0070] The distance between the filter device 2 and the first light limiting element 3 is 4-8 cm. For example, it is 4-5 cm, 5-6 cm, 6-7 cm or 7-8 cm. In the preferred embodiment of the present application, the distance between the filter device 2 and the first light limiting element 3 is 6 cm.

[0071] The distance between the first light limiting element 3 and the second light limiting element 4 is 7-12 cm. For example, it is 7-8 cm, 8-9 cm, 9-10 cm, 10-11 cm or 11-12 cm. In the preferred embodiment of the present application, the distance between the first light limiting element 3 and the second light limiting element 4 is 10 cm.

[0072] The distance between the second light limiting element 4 and the sample stage 5 is 1-3 cm. For example, it is 1-1.5 cm, 1.5-2 cm, 2-2.5 cm or 2.5-3 cm. In the preferred embodiment of the present application, the distance between the second light limiting element 4 and the sample stage 5 is 2 cm.

[0073] The sample stage 5 and the temperature control module 6 are integrated.

[0074] The distance between the sample stage 5 and the photodetector 7 is 4-9 cm. For example, 4-5 cm, 5-6 cm, 6-7 cm, 7-8 cm, or 8-9 cm. In a preferred embodiment of the application, the distance between the sample stage 5 and the photodetector 7 is 7 cm.

[0075] The X-ray detector 8 is adapted to be located at a distance of more than 20 m from the photodetector 8. For example, 20-22 m, 22-24 m, 24-26 m, 26-28 m, 28-30 m, or more than 30 m.

[0076] In the X-ray photon correlation spectroscopy sample experiment platform of the application, the laser emitted by the optical collimating laser instrument 1 is in the visible light band, and the size of the exit light spot is 0.9-1.1 mm. For example, 0.9-0.95 mm, 0.95-1.0 mm, 1.0-1.05 mm, or 1.05-1.1 mm.

[0077] The wavelength of the laser emitted by the optical collimating laser instrument 1 is 630-680 nm. For example, 630-640 nm, 640-650 nm, 650-660 nm, 660-670 nm, or 670-680 nm.

[0078] In the X-ray photon correlation spectroscopy sample experiment platform of the application, the X-ray is a hard X-ray generated by a synchrotron radiation source, the energy is 5-15 keV, and the wavelength is 0.062-0.248 nm. The energy of the hard X-ray generated by the synchrotron radiation source can be 5-6 keV, 6-7 keV, 7-8 keV, 8-9 keV, 9-10 keV, 10-11 keV, 11-12 keV, 12-13 keV, 13-14 keV, or 14-15 keV. The wavelength of the X-ray can be 0.062-0.080 nm, 0.080-0.100 nm, 0.100-0.120 nm, 0.120-0.140 nm, 0.140-0.160 nm, 0.160-0.180 nm, 0.180-0.200 nm, 0.200-0.220 nm, 0.220-0.240 nm, or 0.240-0.248 nm.

[0079] In the X-ray photon correlation spectroscopy sample experiment platform of the present application, the filter device 2 is a switching wheel disc including several filters with different attenuation rates, which is suitable for protecting the photodetector and the sample from being damaged. The filters with different attenuation rates arranged on the filter device 2 can be switched in different environments to protect the photodetector 7 and the sample from being damaged. In the preferred embodiment of the present application, the filter device 2 is a switching wheel disc including four filters with different attenuation rates, and the attenuation rates of the four filters with different attenuation rates are 10% to 25%, 20% to 50%, 45% to 80% and 70% to 100% in sequence.

[0080] In the X-ray photon correlation spectroscopy sample experiment platform of the present application, the first light limiting element 3 is a pinhole diaphragm I, which is suitable for improving the coherence of X-rays. The structure of the first light limiting element 3 is shown in FIG. 2. Figure 7

[0081] In the X-ray photon correlation spectroscopy sample experiment platform of the present application, the first light limiting element 3 is a pinhole diaphragm I, which is suitable for improving the coherence of X-rays. The structure of the first light limiting element 3 is shown in FIG. 2.

[0082] In the X-ray photon correlation spectroscopy sample experiment platform of the present application, the second light limiting element 4 is a pinhole diaphragm II, which is suitable for reducing stray light generated by the diffraction effect of light and the edge of the pinhole diaphragm I. The structure of the second light limiting element 4 is shown in FIG. 3. Figure 7

[0083] In the X-ray photon correlation spectroscopy sample experiment platform of the present application, the second light limiting element 4 is a pinhole diaphragm II, which is suitable for reducing stray light generated by the diffraction effect of light and the edge of the pinhole diaphragm I. The structure of the second light limiting element 4 is shown in FIG. 3.

[0084] In the X-ray photon correlation spectroscopy sample experiment platform of the present application, the sample stage 5 is suitable for clamping samples with different topographies. The structure of the sample stage 5 can be shown in FIG. 4. Figure 6

[0085] In the X-ray photon correlation spectroscopy sample experiment platform of the present application, the sample stage 5 is suitable for clamping samples with different topographies. The structure of the sample stage 5 can be shown in FIG. 4.

[0086] In the X-ray photon correlation spectroscopy sample experiment platform of the present application, the temperature control module 6 is a heating and cooling integrated temperature control mechanism, which is suitable for accurately controlling the sample environment. The temperature control module 6 adopts thermocouple heating and liquid nitrogen cooling. Figure 1

[0087] ​​​​The temperature control range of the temperature control module 6 is -160 DEG C to 200 DEG C, for example, -160 DEG C to -150 DEG C, -150 DEG C to -140 DEG C, -140 DEG C to -130 DEG C, -130 DEG C to -120 DEG C, -120 DEG C to -110 DEG C, -110 DEG C to -100 DEG C, -100 DEG C to -90 DEG C, -90 DEG C to -80 DEG C, -80 DEG C to -70 DEG C, -70 DEG C to -60 DEG C, -60 DEG C to -50 DEG C, -50 DEG C to -40 DEG C, -40 DEG C to -30 DEG C, -30 DEG C to -20 DEG C, -20 DEG C to -10 DEG C, -10 DEG C to 0 DEG C, 0 DEG C to 10 DEG C, 10 DEG C to 20 DEG C, 20 DEG C to 30 DEG C, 30 DEG C to 40 DEG C, 40 DEG C to 50 DEG C, 50 DEG C to 60 DEG C, 60 DEG C to 70 DEG C, 70 DEG C to 80 DEG C, 80 DEG C to 90 DEG C, 90 DEG C to 100 DEG C, 100 DEG C to 110 DEG C, 110 DEG C to 120 DEG C, 120 DEG C to 130 DEG C, 130 DEG C to 140 DEG C, 140 DEG C to 150 DEG C, 150 DEG C to 160 DEG C, 160 DEG C to 170 DEG C, 170 DEG C to 180 DEG C, 180 DEG C to 190 DEG C or 190 DEG C to 200 DEG C.

[0088] The error of the temperature control module 6 is within 0.1 DEG C, and the sample environment can be accurately controlled.

[0089] In the X-ray photon correlation spectroscopy sample experiment platform, the responsivity of the photodetector 7 is 0.07-0.09 A / W, for example, 0.07-0.08 A / W or 0.08-0.09 A / W.

[0090] The current signal collected by the photodetector 7 reflects the intensity of the transmitted light, which is fed back to the device adjustment end, and can be used to align all devices on the light path.

[0091] The second aspect of the application provides a regulation method suitable for the X-ray photon correlation spectroscopy sample experiment platform.

[0092] 1) The optical collimation laser instrument 1 is adjusted to the same direction as the X-ray, the sample stage 5, the temperature control module 6 and the photodetector 7 are moved into the light path, the filter device 2 is rotated, and the optical collimation laser instrument 1, the photodetector 7 and the sample stage 5 are aligned.

[0093] 2) The first light limiting element 3 is moved in, and is moved on the vertical coaxial plane to obtain the maximum value of the current signal measured by the photodetector 7, the first light limiting element 3 is aligned, and the position of the first light limiting element is recorded and then removed from the light path.

[0094] 3) move the second light limiting element 4 to move in the vertical coaxial plane to obtain the maximum value of the current signal measured by the photodetector 7, realize the alignment of the second light limiting element 4, move the first light limiting element 3 to the recording position, and realize the coarse alignment of the optical collimation laser instrument 1, the first light limiting element 3 and the second light limiting element 4;

[0095] 4) turn off the optical collimation laser instrument 1, turn on the X-ray, move the first light limiting element 3 in the vertical coaxial plane to obtain the maximum value of the current signal measured by the photodetector 7, then move the second light limiting element 4 in the vertical coaxial plane to obtain the maximum value of the current signal measured by the photodetector 7, and repeat 3-4 times to achieve fine alignment;

[0096] 5) move the photodetector 7 out of the light path, and refer to the spot pattern collected by the X-ray detector 8 to perform the last fine adjustment on the first light limiting element 3 and the second light limiting element 4, and complete the light adjustment.

[0097] Wherein, the X-ray is provided by a specific working line station. It is only required that the X-ray is coaxial and in the same direction with the optical collimation laser beam.

[0098] The X-ray detector is used for collecting data in the experiment, and is the last measurement standard to achieve the experimental requirements. The appearance of the spot collected by the X-ray detector is observed, the previous devices are fine adjusted again, and the continuous collection of the coherent pattern is finally performed.

[0099] The last fine adjustment on the first light limiting element 3 and the second light limiting element 4 in the step 5) specifically includes: first adjusting the first light limiting element 3 and then adjusting the second light limiting element 4, so that the first light limiting element 3 and the second light limiting element 4 move in the XY plane.

[0100] The third aspect of the present application provides a computer storage medium, including a readable storage medium and computer instructions, the computer instructions are stored in the readable storage medium; the computer instructions are used for realizing the method of steps 1) to 5) in the regulation and control method. Optionally, the computer readable storage medium can include, but is not limited to, a floppy disk, an optical disk, a CD-ROM (compact disc read-only memory), a magneto-optical disk, a ROM (read only memory), a RAM (random access memory), an EPROM (erasable programmable read only memory), an EEPROM (electrically erasable programmable read only memory), a magnetic card or an optical card, a flash memory, or other types of media / machine readable media suitable for storing machine executable instructions. The computer readable storage medium can be a product not connected to a computer device, or a component connected to a computer device.

[0101] In the embodiment of the present application, the extension direction of the beam of the optical collimation laser instrument is the Z axis, the coaxial direction is the Z axis, and the plane perpendicular to the Z axis is the XY plane.

[0102] Example 1

[0103] The X-ray photon correlation spectroscopy sample experiment platform of the present application is regulated as follows:

[0104] 1) First, the optical collimation laser instrument 1 is used to coarsely adjust the experimental light path. The optical collimation laser instrument 1 is manually adjusted to the same direction as the X-ray light path (at this time, the X-ray is not turned on), the sample stage 5 and the temperature control module 6 and the photodetector 7 are moved into the light path, the filter device 2 is rotated to prevent damage to the detector due to exceeding the detection range (in general, a filter with a 50% attenuation rate is used, so it is not easy to exceed the range. If the range is exceeded, the output current of the photodetector will be very high (as compared with the photodetector manual), and the optical collimation laser instrument 1 can be turned off in time), and the optical collimation laser instrument 1, the photodetector 7 and the sample stage 5 are aligned.

[0105] 2) The first light limiting element 3 is moved in, and is moved in the XY plane to obtain the value of the photodetector 7. The position of the first light limiting element 3 when the current signal value of the photodetector 7 is maximum is found, the first light limiting element 3 is aligned, and the position is recorded. The first light limiting element 3 is removed from the light path.

[0106] 3) The second light limiting element 4 is moved in, and is moved in the XY plane to obtain the value of the photodetector 7. The position of the second light limiting element 4 when the current signal value of the photodetector 7 is maximum is found, the second light limiting element 4 is aligned, and the first light limiting element 3 is moved to the recorded position to achieve coarse alignment of the optical collimation laser instrument 1, the first light limiting element 3 and the second light limiting element 4.

[0107] 4) The optical collimation laser instrument 1 is turned off, and the X-ray is turned on. The first light limiting element 3 is moved in the XY plane to obtain the value of the photodetector 7. The position of the first light limiting element 3 when the current signal is maximum is found. Then the second light limiting element 4 is moved in the XY plane to obtain the value of the photodetector 7. The position of the second light limiting element 4 when the current signal is maximum is found. The first light limiting element 3 and the second light limiting element 4 are adjusted three times to achieve precise alignment.

[0108] 5) The photodetector 7 is removed from the light path. The light spot pattern collected by the X-ray detector 8 is used as a reference (the reference is the light spot morphology. Whether there is shielding around the detected light spot and whether it is symmetrical are observed. If there is shielding, the first light limiting element 3 or the second light limiting element 4 is moved in the opposite direction), and the first light limiting element 3 and the second light limiting element 4 are finally adjusted: the first light limiting element 3 is adjusted first, and then the second light limiting element 4 is adjusted. They can be moved in the XY plane to complete the adjustment.

[0109] 6) Put in the sample, i.e. start the experiment, the sample is a silica sphere glycerol solution, the temperature of the temperature control module is 25℃; the obtained result is as shown in Figure 2 、 Figure 3 : Almost no stray light is observed, indicating that the XPCS sample experimental platform of the application can greatly improve the coherence of light and reduce stray light; Figure 2 The analysis spectrum result is simple and clear, and the contrast is improved to about 0.055, because the double-limit light element in the embodiment effectively improves the coherence of light and greatly removes stray light, and the temperature of the sample is accurately controlled, thereby improving the resolution of the XPCS experiment and improving the data quality of the experimental result.

[0110] Comparative Example 1

[0111] The sample, a silica sphere glycerol solution (the same as in Example 1), is measured, and in this experiment, the sample is not temperature-controlled, no light adjustment is performed using the XPCS experimental sample table of the application, and only the original X-ray of the line station is used.

[0112] The result is as shown in Figure 4 The experimental result image obtained in Comparative Example 1 has more stray light and is blurred, because the coherence of light is poor, and the temperature fluctuation makes the experiment unstable, the analysis spectrum result is not clear, the analysis spectrum relaxation curve is tortuous, and it is difficult to obtain information therefrom, as shown in Figure 5 .

[0113] In summary, the XPCS sample experimental platform of the application uses a small-aperture diaphragm and other limiting light elements, limits the size of the incident light spot, thereby improving the coherence of the incident light, and accurately positions the sample so that the coherent X-ray is accurately irradiated on the sample. The XPCS sample experimental platform of the application solves the problem that the domestic synchrotron radiation source cannot carry out XPCS experiments, can image the movement of a hundred nanometer solute solution, and has a wide application prospect in material science, nanotechnology and biology. Therefore, the application effectively overcomes the printing defects of the prior art, such as obvious scratches on the coated surface and poor coating quality of the slurry, and has high industrial utilization value.

[0114] The above embodiments only exemplarily illustrate the principles and effects of the application, and are not used to limit the application. Any person skilled in the art can modify or change the above embodiments without departing from the spirit and scope of the application. Therefore, all equivalent modifications or changes made by those skilled in the art without departing from the spirit and technical thought disclosed by the application should be covered by the claims of the application.

Claims

1. An X-ray photon correlation spectroscopy sample experiment platform, characterized in that, The X-ray photon correlation spectroscopy sample experimental platform is adapted to be used with an X-ray and an X-ray detector (8) coaxially, and the experimental sample platform comprises, in sequence along an X-ray diffraction direction, an optical collimating laser instrument (1), a filter device (2), a first light limiting element (3), a second light limiting element (4), a sample stage (5), a temperature control module (6), and a photoelectric detector (7); The first light limiting element (3) is controlled by a first double motor to move in a vertical coaxial plane; The second light limiting element (4) is controlled by a second double motor to move in a vertical coaxial plane; The temperature control module (6) is closely connected with the sample stage (5); The sample stage (5) and the temperature control module (6) are controlled by a third double motor to move in a vertical coaxial plane; The photoelectric detector (7) is controlled by a fourth double motor to move in a vertical coaxial plane; The X-ray detector (8) is adapted to be arranged coaxially behind the photoelectric detector (7).

2. The X-ray photon correlation spectroscopy sample stage of claim 1, wherein, One or more of the following features are also included: a) The distance between the optical collimating laser instrument (1) and the filter device (2) is 8-15 cm; b) The distance between the filter device (2) and the first light limiting element (3) is 4-8 cm; c) The distance between the first light limiting element (3) and the second light limiting element (4) is 7-12 cm; d) The distance between the second light limiting element (4) and the sample stage (5) is 1-3 cm; e) The distance between the sample stage (5) and the photoelectric detector (7) is 4-9 cm; f) The X-ray detector (8) is adapted to be arranged at a position more than 20 m away from the photoelectric detector (7).

3. The X-ray photon correlation spectroscopy sample stage of claim 1, wherein, The laser emitted by the optical collimating laser instrument (1) is visible light, and the size of the exit spot is 0.9-1.1 mm.

4. The X-ray photon correlation spectroscopy sample stage of claim 1, wherein, The X-ray is a hard X-ray generated by a synchrotron radiation source, with an energy of 5-15 keV and a wavelength of 0.062-0.248 nm.

5. The X-ray photon correlation spectroscopy sample stage of claim 1, wherein, The filter device (2) is a switching type wheel disc comprising a plurality of filter discs with different attenuation rates, which is adapted to protect the photoelectric detector and the sample from being damaged.

6. The X-ray photon correlation spectroscopy sample stage of claim 1, wherein, The first light limiting element (3) is a pinhole diaphragm I, which is adapted to improve the coherence of the X-ray; And / or, the first light limiting element (3) is made of X-ray opaque material.

7. The X-ray photon correlation spectroscopy sample platform according to claim 6, characterized in that, The second light limiting element (4) is a pinhole diaphragm II, which is adapted to reduce stray light generated by the diffraction effect of light and the edge of the pinhole diaphragm I; And / or, the second light limiting element (4) is made of X-ray opaque material.

8. The X-ray photon correlation spectroscopy sample stage of claim 1, wherein, The sample stage (5) is adapted to clamp samples with different morphologies; And / or, the sample stage (5) is made of stainless steel; And / or, the temperature control module (6) is a heating and cooling integrated temperature control mechanism, which is adapted to accurately control the sample environment; And / or, the temperature control range of the temperature control module (6) is -160℃-200℃; And / or, the response rate of the photoelectric detector (7) is 0.07-0.09 A / W.

9. A method for regulating the X-ray photon correlation spectroscopy sample experimental platform according to any one of claims 1-8, characterized in that, The following steps are included: 1) Adjust the optical collimating laser instrument (1) to the same direction as the X-ray, move the sample stage (5), temperature control module (6), photodetector (7) into the light path, rotate the filter device (2), align the optical collimating laser instrument (1), photodetector (7), sample stage (5); 2) Move in the first light limiting element (3), move it in the vertical coaxial plane to obtain the maximum value of the photodetector, realize the alignment of the first light limiting element (3), record the position of the first light limiting element (3) and then remove it from the light path; 3) Move in the second light limiting element (4), move it in the vertical coaxial plane to obtain the maximum value of the photodetector, realize the alignment of the second light limiting element (4), move the first light limiting element (3) to the recorded position, realize the coarse alignment of the optical collimating laser instrument (1), the first light limiting element (4) and the second light limiting element (4); 4) Turn off the optical collimating laser instrument (1), turn on the X-ray, move the first light limiting element (3) in the vertical coaxial plane to obtain the maximum value of the photodetector, then move the second light limiting element (4) in the vertical coaxial plane to obtain the maximum value of the photodetector; Repeat 3-4 times to achieve precise alignment; 5) Remove the photodetector (7) from the light path, take the spot pattern collected by the X-ray detector (8) as the reference, fine-tune the first light limiting element (3) and the second light limiting element (4) for the last time, and complete the light adjustment.

10. A computer storage medium, characterized in that, The computer readable storage medium and computer instructions, the computer instructions are stored in the computer readable storage medium; The computer instructions are used for realizing the method of step 1) to step 5) in the regulation method of claim 9.

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