CN113008920A - Small sample cavity for X-ray free electron laser device - Google Patents
Small sample cavity for X-ray free electron laser device Download PDFInfo
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- CN113008920A CN113008920A CN202110240266.3A CN202110240266A CN113008920A CN 113008920 A CN113008920 A CN 113008920A CN 202110240266 A CN202110240266 A CN 202110240266A CN 113008920 A CN113008920 A CN 113008920A
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Abstract
The invention relates to a small sample cavity for an X-ray free electron laser device, which comprises a sample cavity main body, an X-ray window, a temperature detection system, a temperature control system, an atmosphere control and vacuum system and a fluid control system, wherein the X-ray window is provided with a large-area high-purity thin diamond; the sample cavity body is a volume cavity with exposed front and back surfaces, the two X-ray windows are fixed in front and back and are sealed on the front and back exposed surfaces of the sample cavity body, the temperature control system, the atmosphere control and vacuum system and the fluid control system are all connected with the sample cavity body to provide a required experimental environment for the sample cavity body, X-rays are incident on a sample in the cavity body through the X-ray windows, and the temperature detection system tests the temperature in the sealed environment of the sample cavity body in real time. The cavity can realize various sample environments and is suitable for X-ray free electron laser characterization of various sample systems.
Description
Technical Field
The invention relates to a test device, in particular to a small sample cavity for an X-ray free electron laser device.
Background
An X-ray free electron laser device (XFEL) is a new generation X-ray light source capable of providing X-rays stronger than that of a synchrotron radiation device, and at present, an X-ray free electron laser device in ultraviolet and soft X-ray bands is already built in China, while a hard X-ray free electron laser device is also being actively built. Compared with a synchrotron radiation device which can provide strong X rays, the X-ray free electron laser device has the remarkable advantages of higher brightness, shorter pulse, stronger coherence and the like, and can provide a more advanced X-ray experimental characterization platform for scientific research and industrial users of multiple disciplines. Since the sample in the X-ray characterization often requires sample atmospheres such as normal pressure, low vacuum, helium, nitrogen, carbon dioxide, moisture, etc., on the synchrotron radiation device, the sample and the downstream of the optical path are often isolated by using an X-ray window to ensure that the high vacuum of the upstream and the downstream cannot be damaged by the sample atmosphere. However, the peak energy and the average energy of the pulse generated by the X-ray free electron laser device are high, and an X-ray window made of traditional materials such as beryllium and polymer is easily damaged due to the thermal effect and radiation damage of the XFEL pulse, and may have a certain adverse effect on the quality, especially coherence, of the X-ray. Diamond is an excellent material with high thermal conductivity and can withstand strong X-ray radiation, and thus an X-ray window made of diamond can withstand instantaneous and long-term X-ray radiation. In addition, diamond flakes, especially high purity nano-and mono-crystalline diamond flakes, do not substantially negatively impact the quality and intensity of the X-ray pulses. The X-ray window places high demands on the purity, size and thickness and crystallinity of diamond. In recent years, synthetic diamond technology has been significantly developed. The high-purity large-area sheet-shaped diamond required by the X-ray window is also successfully prepared by utilizing the technologies of chemical vapor deposition and the like, and is also applied to a plurality of X-ray free electron laser devices to a certain extent.
In the conventional design of an X-ray experiment station, in order to realize various sample environments and sample transportation modes, a heavy large-medium sample cavity is generally used, the weight of the sample cavity is generally about several tons, and the sample cavity is difficult to move in a large range. In addition, the large and medium-sized sample cavities have large volume, and certain limitation is caused to the space of the experiment station. Therefore, under the premise of basically meeting the sample environment required by the experiment, a small multifunctional sample chamber for an X-ray free electron laser device (XFLE) needs to be designed.
Disclosure of Invention
The invention provides a small sample cavity for an X-ray free electron laser device aiming at the problems of test convenience and compatibility improvement so as to meet the requirement of the X-ray free electron laser device on a small radiation-resistant multifunctional sample cavity.
The technical scheme of the invention is as follows: a small sample chamber for an X-ray free electron laser device comprises a sample chamber main body, an X-ray window equipped with large-area high-purity thin-sheet diamond, a temperature detection system, a temperature control system, an atmosphere control and vacuum system and a fluid control system; the sample cavity body is a volume cavity with exposed front and back surfaces, the two X-ray windows are fixed in front and back and are sealed on the front and back exposed surfaces of the sample cavity body, the temperature control system, the atmosphere control and vacuum system and the fluid control system are all connected with the sample cavity body to provide a required experimental environment for the sample cavity body, X-rays are incident on a sample in the cavity body through the X-ray windows, and the temperature detection system tests the temperature in the sealed environment of the sample cavity body in real time.
Preferably, the X-ray window comprises a metal frame comprising the window outer portion and a large area high purity diamond face window embedded in the middle of the metal frame; wherein the diamond of the central diamond face window has an impurity content of less than 10ppm, a thermal conductivity of greater than 1800W/(mK), and an absorption of X-rays having a photon energy of 10keV of less than 20%.
Preferably, the sample cavity body is a cuboid, and the external geometric dimension of the sample cavity body is 30-100 mm long, 20-100 mm high and 5-50 mm wide; the thickness of the cavity wall is 10-20 mm; the geometric dimension of the diamond surface window is 30-60 mm long, 20-60 mm high and 0.05-1 mm thick.
Preferably, the temperature control system comprises a temperature control cavity, and the temperature control cavity is designed with a groove suitable for the insertion of the bottom of the sample cavity main body, so as to support and tightly wrap the bottom of the sample cavity main body; when an electric control mode is adopted, a temperature control resistor or a semiconductor temperature control element is embedded in the temperature control cavity and is connected with a temperature controller through a power line, and the temperature controller is connected with a controller for controlling a computer or a temperature sensor so as to carry out closed-loop control on the temperature; when liquid circulation is used for temperature control, a liquid flow circulation pipeline is embedded in the temperature control cavity, an inlet and an outlet of the pipeline are connected with an external liquid circulation system and a liquid temperature control system, wherein the liquid temperature control system is connected with a controller or a control computer of a temperature sensor to perform closed-loop temperature control.
Preferably, the upper surface of the sample cavity main body is provided with an airflow inlet and a gas outlet which are communicated with the cavity, and the gas inlet of the sample cavity main body is communicated with a gas source or a vacuum pump of an atmosphere control and vacuum system through a gas pipe; the gas outlet of the sample chamber body may be free of any means or connected to a special gas recovery means.
Preferably, a liquid inlet and a liquid outlet which are communicated with the cavity are arranged on two sides of the sample cavity main body, and the liquid inlet is connected with a liquid outlet of the fluid control system; the liquid outlet is connected with the liquid circulating device through a liquid pipe; the fluid control system provides configurable control of the fluid.
Preferably, the temperature detection system is a temperature sensor embedded at the bottom of the sample cavity and is used for detecting the temperature in the sample cavity in real time.
The invention has the beneficial effects that: the invention is used for the small sample cavity of the X-ray free electron laser device, can realize various sample environments and is suitable for X-ray free electron laser characterization of various sample systems.
Drawings
FIG. 1 is an exploded view of the components of a compact sample chamber for an X-ray free electron laser apparatus according to the present invention;
FIG. 2 is a schematic structural diagram of an embodiment of a sample chamber body in a small sample chamber for an X-ray free electron laser device according to the present invention;
FIG. 3 is a schematic structural diagram of a second embodiment of a sample chamber body in a small sample chamber for an X-ray free electron laser device according to the present invention;
fig. 4 is a graph showing the result of the irradiation resistance test of the diamond face window in the small sample chamber for the X-ray free electron laser device of the present invention.
Reference numerals: 1. a sample chamber body; 101. air holes; 102. a cavity; 103. a liquid flow aperture; 110. an airflow inlet; 111. a gas outlet; 112. a liquid inlet; 113. a liquid outlet; 114. a threaded hole; 115. a wire guide hole; 116-119, fixing holes; 120-121, fixing the spring piece; 2. an X-ray window; 201. a diamond face window; 202. a metal frame; 3. a temperature detection system; 4. a temperature control system; 401. a groove; 402. a power line; 403. a temperature controller; 5. atmosphere control and vacuum systems; 501. an air tube; 502. a gas source; 6. a fluid control system; 601. a liquid pipe; 602. and a liquid circulating device.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
As shown in fig. 1, the small sample chamber for X-ray free electron laser device, which is schematically illustrated in exploded view, mainly comprises a sample chamber body 1, an X-ray window 2 equipped with large-area high-purity thin-sheet diamond, a temperature detection system 3, a temperature control system 4, an atmosphere control and vacuum system 5, and a fluid control system 6. The sample cavity body 1 is a volume cavity body 102 with the front and the back exposed, the two X-ray windows 2 are fixed in front and back and are sealed on the front and back exposed surfaces of the sample cavity body 1, the temperature control system 4, the atmosphere control and vacuum system 5 and the fluid control system 6 are all connected with the sample cavity body 1 to provide a required experimental environment for the sample cavity body 1, X-rays are incident into a sample in the cavity body through the X-ray windows 2, and the temperature detection system 3 tests the temperature in the sealed environment of the sample cavity body 1 in real time.
1. A sample chamber body:
the main function of the sample chamber body is to contain and support a solid sample or to contain a liquid sample and to provide a suitable gaseous or liquid environment and temperature for the sample. For a solid sample, a reflection type X-ray incidence scheme is mainly adopted, and a transmission type X-ray incidence scheme is also compatible, so that the sample can be updated in a mode of controlling a stepping motor to scan or in a manual sample changing mode. For the liquid sample, a manual sample feeding mode of direct dripping can be adopted, and dynamic automatic sample feeding can also be carried out by utilizing the fluid control system 6.
The sample chamber is rectangular in shape, and has external geometric dimensions of 30-100 mm long (x-axis), 20-100 mm high (z-axis), and 5-50 mm wide (y-axis). Wherein the z-axis is the vertical direction and the y-axis is the direction of the front X-ray incident sample chamber.
The material of the sample cavity can be various metal materials, such as steel, aluminum alloy and the like, and can also be a polymer material added with a heat-conducting filler, so that the cavity is ensured to have excellent mechanical property and heat-conducting property. The thickness of the cavity wall is 10-20 mm, and a perforation, a threaded hole or a spring clip is designed for fixing the X-ray window 2. In order to realize the atmosphere control and the vacuum acquisition, two air holes 101 are designed on the upper surface of the cavity. In order to cooperate with the fluid control system 6 to control the liquid environment and dynamically and automatically sample the liquid sample, a liquid flow hole 103 is respectively designed on the left and right sides (x direction) of the cavity. All of the openings may be closed when not in use. The bottom of the cavity 102 is embedded with a temperature sensor, which can realize real-time automatic temperature monitoring and can also realize accurate control of the sample temperature by cooperating with a temperature control system. Aiming at different fixing modes of the X-ray window 2, a plurality of through holes and a rectangular groove (with the depth of 0.2-2mm) or two spring clamps are further designed at the front end and the rear end (in the y direction) of the sample cavity and are respectively used for thread fixing or spring fixing of the X-ray window.
The inner space of the sample cavity is also a cuboid, the basic geometric dimension is 20-80 mm long, 10-80 mm high and 5-50 mm wide, and small special-shaped openings and threaded holes can be additionally designed for fixing samples. The solid sample can be prepared on the substrate and placed at the bottom, the middle part and the upper part of the sample cavity so as to perform the reflective X-ray experiment of the solid sample; the high-permeability substrate (such as silicon nitride) carrying the sample can be fixed in the sample cavity in the direction perpendicular to the X-ray optical path by using the threaded hole at the bottom, so that the transmission type X-ray experiment of the solid sample is realized. The two modes can realize that a plurality of solid samples are placed at one time, and the updating and scanning of the samples are realized by a mode of carrying out motor movement in a direction perpendicular to the incidence direction of the X-ray.
2. X-ray window equipped with large area high purity wafer diamond:
the main function of the X-ray window 2 equipped with a large area of high purity diamond is to allow the passage of X-ray pulses into the cavity 102 without affecting the X-ray pulse quality and intensity as much as possible. The X-ray window 2 comprises two parts of a window outer metal frame 202 and a large area high purity diamond face window 201 embedded in the middle of the metal frame. The metal frame can be made of various metal materials such as steel, aluminum alloy and the like, and the geometric dimension of the metal frame is 30-80 mm long (x axis), 20-80 mm high (z axis) and 0.2-2mm wide (y axis). While the central diamond face window 201 uses a large area of high purity synthetic diamond foil. Depending on the purpose of use, either single crystals or polycrystalline crystals of diamond may be used. The geometric dimension of the material is 30-60 mm long, 20-60 mm high and 0.05-1 mm thick. When the area of the window is larger than 20 mm × 20 mm, the current diamond preparation technology has difficulty in realizing such a large size, and can be realized by splicing a plurality of diamonds. In addition, in order to ensure the quality of transmitted X-rays and the long-term stable operation of the window, the impurity content of diamond needs to be lower than 10ppm, the thermal conductivity needs to be more than 1800W/(mK), and the absorptivity to X-rays with photon energy of 10keV is lower than 20%. Besides ensuring that the intensity and quality of transmitted light are basically not affected, namely high transmittance, the diamond surface window also needs to have good heat conduction capability and irradiation resistance capability so as to ensure that the diamond surface window is not damaged by irradiation of high-intensity X-ray free electron laser pulses.
The X-ray window 2 is independent of the sample chamber body 1 for ease of handling and manipulation. The integral assembly of the X-ray window 2 and the cavity can adopt a screw fixing scheme, a spring piece fixing scheme and a glue fixing scheme. The screw fixing scheme requires punching on the cavity and designing a groove for accommodating the window; the spring piece fixing scheme requires that a spring piece is arranged on a cavity; the glue fixing scheme does not need to be specially designed on the cavity body, but can cause the window to be not detachable, so that the glue fixing scheme is only suitable for liquid samples.
3. Temperature detection system:
as mentioned in the section of the sample chamber body 1 above, a temperature sensor is embedded in the bottom of the sample chamber, which can detect the temperature in the sample chamber in real time. The temperature sensor can adopt a platinum resistance temperature probe, and can also adopt other small temperature sensors. Typical temperature measurement ranges are-70 to 500 degrees celsius, and typical temperature measurement accuracy is ± (0.15+0.002xT) degrees celsius. The temperature sensor can be connected with the sensor controller to display the temperature, and can also be connected with the control computer to output the temperature data. When the temperature in the sample cavity does not need to be precisely controlled, the real-time temperature data output by the controller or the control computer can be independently used; when the temperature in the sample cavity needs to be precisely controlled, the output real-time temperature data is combined with a temperature control system to be described below to carry out closed-loop temperature control.
4. A temperature control system:
many samples for X-ray experiments have high requirements on temperature, and the structure and the properties of many samples for X-ray experiments have certain relation with the temperature. In both cases, a temperature control system is required to accurately control the temperature of the sample during the X-ray characterization experiment.
The real-time temperature input is provided by the temperature detection system 4, and the temperature can be controlled in two modes of electric control and liquid circulation temperature control. The temperature control chamber of the temperature control system is designed with a groove 401 into which the sample chamber body 1 is inserted, the size of the groove 401 depends on the length and thickness of the sample chamber body 1, and the depth of the groove is 5-40 mm, so as to support and tightly wrap the bottom of the sample chamber body 1. When the electric control mode is adopted, a temperature control resistor or a semiconductor temperature control element (Peltier module) is embedded in the temperature control chamber and is connected to the temperature controller 403 through a power line 402. The temperature controller 403 is connected to a control computer or a temperature sensor to perform closed-loop control of the temperature. When liquid circulation is used for temperature control, a liquid flow circulation pipeline needs to be buried inside the temperature control cavity, an inlet and an outlet of the pipeline are connected with an external liquid circulation system and a liquid temperature control system, and the liquid temperature control system is connected with a controller of a temperature sensor or a control computer to perform closed-loop temperature control.
5. Atmosphere control and vacuum system:
in order to realize the atmosphere control or vacuum acquisition in the sample cavity, the upper part of the sample cavity is provided with an inlet and an outlet of gas, and the diameter is 2-15 mm. The two outlets are connected to an atmosphere control system and a vacuum system to achieve (1) special atmosphere filling including helium, nitrogen, carbon dioxide in the sample chamber, (2) humidity control in the sample chamber, and (3) vacuum acquisition in the sample chamber.
In order to realize special atmosphere filling in the sample cavity, a gas inlet needs to be connected with a gas source 502 through a gas pipe 501; the gas outlet may be connected to no device or to a special gas recovery device.
In order to realize the humidity control in the sample chamber, the gas inlet needs to be connected with the output port of the humidity controller. Depending on the type of gas provided by the gas source, the humidity controller can output air, helium, nitrogen, carbon dioxide and other gases with certain humidity according to the setting; the gas outlet is designed with a small humidity detection device to monitor the humidity in the sample cavity in real time, and the device can be connected with a gas recovery device as the special atmosphere filling. The humidity controller can work independently and can also be connected with a control computer; the humidity sensor needs to be connected with a temperature controller or a control computer to output data, so that closed-loop control of humidity is realized.
In order to realize vacuum acquisition in the sample cavity, a gas inlet of the sample cavity is connected with a vacuum pump, and the vacuum pump is connected with a vacuum controller or a control computer. And a vacuum gauge is arranged at a gas outlet of the sample cavity to monitor the vacuum degree in the cavity in real time and needs to be sealed. The vacuum controller can work independently and can also be connected with a control computer; the vacuum gauge needs to be connected with a vacuum controller or a control computer to output data, so that closed-loop control of the vacuum degree is realized.
6. A fluid control system:
in order to cooperate with a fluid control system to control the liquid environment of a solid sample and dynamically and automatically sample a liquid sample, the left side and the right side (in the x direction) of the cavity are respectively provided with a liquid flow hole 103, and the diameter of the liquid flow hole is 0.5-10 mm. The liquid flow inlet is connected with a liquid outlet of the liquid control system. The fluid controller drives the syringe via an electric motor or controls the fluid pump to achieve controlled delivery of a single fluid, or controlled mixing and delivery of multiple fluids. The liquid outlet needs to be connected with the liquid circulation device 602 through a liquid pipe 601. The control of the fluid can be set by the fluid controller, and the fluid controller can also be connected with a control computer and then set by the control computer.
The invention is used for a small-sized multifunctional sample cavity of an X-ray free electron laser device (XFLE), can realize the control of various sample environments and is suitable for X-ray free electron laser characterization of various sample systems.
As shown in fig. 2, in an embodiment of the sample chamber body, a gas flow inlet 110 and a gas outlet 111 are arranged on the upper surface of the sample chamber body 1 and communicated with the chamber; the two sides of the sample cavity body 1 are provided with a liquid inlet 112 and a liquid outlet 113 which are communicated with the cavity body; a transmission type solid sample fixing screw hole 114 is formed at the bottom in the cavity of the sample cavity main body 1; the bottom of the outer surface of the sample cavity body 1 is provided with a temperature sensor wire hole 115 communicated with a cavity bottom temperature detection system; four corners of two sides of the outer surface of the sample cavity body 1 are provided with fixing holes 116-119 for fixing the X-ray window 2.
As shown in the schematic structural diagram of the second embodiment of the sample chamber body shown in FIG. 3, two fixing spring pieces 120-121 for fixing the X-ray window 2 are arranged on two sides of the outer surface of the sample chamber body 1.
The results of the irradiation resistance test of the diamond face window 201 are shown in fig. 4. There was almost no change in the scattering signal at the diamond face window after 1 hour of irradiation 30 minutes before irradiation with 10keV X-ray photons of light intensity power of 13 powers per second. The diamond window can thus withstand intense X-ray radiation over a long period of time.
Experimental example 1X-ray diffraction characterization of carbon dioxide reduction Process
Carbon dioxide can be reduced to carbon monoxide under the catalytic action of a catalyst, and the obtained carbon monoxide is an important energy source. Catalysts used in the carbon dioxide reduction process are typically elemental metals or compounds such as platinum and its compounds. During the carbon dioxide reduction reaction, the crystal structure of the catalyst also changes, and can be characterized by X-ray diffraction.
Firstly, preparing a catalyst on a substrate, wherein the substrate can be a material with high X-ray transmittance such as silicon nitride and the like, and can also be a material with low X-ray transmittance such as silicon single crystal and the like. Catalysts prepared on high transmittance substrates can be characterized by transmission X-ray diffraction, while catalysts prepared on low transmittance substrates can be characterized by reflection X-ray diffraction.
And secondly, fixing the front and rear X-ray windows 2 at two ends of the sample cavity body 1 by using screw nuts or spring pieces.
The third step requires setting the sample chamber to the temperature required for the catalytic reduction reaction before the reaction starts.
And fourthly, starting catalytic reaction through a gas controller or a control computer, namely starting to introduce carbon dioxide.
And fifthly, in the reduction process of the carbon dioxide, the acquisition of an X-ray diffraction pattern can be carried out once every certain time, so that the time resolution characterization of the crystal structure of the metal or metal compound catalyst is carried out.
Experimental example 2 time-resolved grazing X-ray diffraction (GIXD) characterization of multilayer phospholipid membranes
The structure of the multilayer phospholipid membrane can be characterized by grazing (small reflection angle) X-ray diffraction. The structure and phase of the phospholipid membrane are easily influenced by the environment in which the phospholipid membrane is positioned, the structure or phase of the phospholipid membrane can be changed by introducing air with different humidity into a sample cavity, or introducing solutions with different physiological conditions (mainly changing the solute content and the type of the aqueous solution), or changing the temperature of the sample cavity, and then the process of changing the structure and phase is subjected to dynamic time resolution characterization through grazing X-ray diffraction.
In the first step, the multilayer phospholipid membrane is firstly prepared on a substrate which can be made of silicon, glass and the like, and then the substrate is fixed on the special-shaped opening for reflective X-ray characterization.
And secondly, fixing the front and rear X-ray windows 2 at two ends of the sample cavity by using screws, nuts or spring pieces.
And thirdly, adding a required solution (optional) into the sample cavity through the openings on two sides.
And fourthly, controlling the temperature of the multilayer phospholipid membrane through a temperature control system 4, controlling the atmosphere, the vacuum degree or the humidity (optional) in the sample cavity through an atmosphere control system and a vacuum system, and controlling the liquid environment (optional) in the sample cavity through a fluid control system 6.
And the fifth step is to collect the static X-ray diffraction pattern, or the dynamic X-ray diffraction pattern can be collected by changing the environmental condition of the sample through any one of the three systems.
Experimental example 3X-ray Scattering characterization of silica pellet solids and dispersions (colloids)
The silica spheres are important X-ray standard samples and are multipurpose materials which are widely applied in scientific research and industry. The structure and morphology of the silica spheres can be well characterized through transmission type X-ray scattering, the selection of the scattering angle of the X-ray scattering depends on the characteristic dimension of the silica spheres, the small characteristic dimension uses wide-angle X-ray scattering (WAXS), and the large characteristic dimension uses small-angle X-ray scattering (SAXS).
X-ray scattering characterization of silica pellet solids:
firstly, preparing silicon dioxide pellets on a substrate which can be made of silicon, glass and the like, and then fixing the substrate on a special-shaped opening for reflective X-ray scattering or fixing the substrate on a threaded hole at the bottom for transmissive X-ray scattering.
And secondly, fixing the front and rear X-ray windows 2 at two ends of the sample cavity by using screws, nuts or spring pieces.
And thirdly, controlling the temperature of the sample cavity through a temperature control system 4 (optional), controlling the atmosphere, the vacuum degree or the humidity in the sample cavity through an atmosphere control system and a vacuum system (optional), and controlling the liquid environment in the sample cavity through a fluid control system 6 (optional).
And the fourth step is to collect the static X-ray diffraction pattern, or the dynamic X-ray diffraction pattern can be collected by changing the environmental condition of the sample through any one of the three systems.
X-ray scattering characterization of silica bead dispersion:
the first step is to first disperse the silica spheres in a suitable solution, which may be water or an organic solvent, to which the desired solute may also be added.
And secondly, fixing the front and rear X-ray windows at two ends of the sample cavity by using screw nuts or spring pieces.
In the third step, the silicon dioxide pellet dispersion is added through the openings on the two sides of the sample cavity, and the fluid control system 6 can also be used for sample injection.
And fourthly, controlling the temperature (optional) of the sample cavity through a temperature control system 4, and controlling the atmosphere, the vacuum degree or the humidity (optional) in the sample cavity through an atmosphere control and vacuum system 5.
Fifthly, performing a static transmission type solution X-ray scattering experiment step by step to obtain a static X-ray scattering pattern; the temperature or the composition of the dispersion can be changed by the control of the temperature control system 4 or the fluid control system 6, and then the dynamic X-ray diffraction scattering experiment is carried out to obtain the dynamic X-ray scattering pattern.
Experimental example 4 scanning X-ray Scattering, diffraction and imaging of cells
Depending on the type of cell and the characterization content of the experiment, the structure of the cell can be characterized by a variety of X-ray techniques such as X-ray scattering, diffraction and imaging. Scanning X-ray characterization techniques such as scanning X-ray scattering, diffraction and imaging can provide both high spatial resolution and a large field of view to characterize the fine structure of whole cells and even multiple cells.
In the first step, cells are firstly fixed on an X-ray substrate with high transmittance, and the substrate is fixed on a threaded hole at the bottom of a sample cavity, wherein a sample is vertical to the incident direction of the X-ray.
And secondly, fixing the front and rear X-ray windows 2 at two ends of the sample cavity by using screws, nuts or spring pieces.
A third step of adding a suitable solution (optional) through the sample chamber opening or the fluid control system;
and fourthly, controlling the temperature of the sample cavity through a temperature control system 4 (optional), controlling the atmosphere, the vacuum degree or the humidity in the sample cavity through an atmosphere control and vacuum system 5 (optional), and controlling the liquid environment in the sample cavity through a fluid control system 6 (optional).
The fifth step performs scanning perpendicular to the X-ray incidence direction by the stepping motor, and performs collection of X-ray scattering or diffraction images at each position.
And sixthly, performing overall data analysis on the obtained multiple images by combining different data analysis methods of different methods.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (7)
1. A compact sample chamber for X-ray free electron laser devices, characterized by comprising a sample chamber body (1), an X-ray window (2) equipped with large area high purity wafer diamond, a temperature detection system (3), a temperature control system (4), an atmosphere control and vacuum system (5) and a fluid control system (6); sample chamber main part (1) is the exposed volume cavity of front and back face, two X ray windows (2) are fixed and airtight on sample chamber main part (1) front and back exposure face, temperature control system (4), atmosphere control and vacuum system (5) and fluid control system (6) all are connected with sample chamber main part (1), provide required experimental environment for sample chamber main part (1), X ray passes through X ray window (2) and incides on the sample in the cavity, temperature detection system (3) real-time test sample chamber main part (1) temperature in the airtight environment.
2. The compact sample chamber for X-ray free electron laser devices according to claim 1, characterized in that the X-ray window (2) comprises a large area high purity diamond face window (201) comprising a window outer metal frame (202) and embedded in the middle of the metal frame; wherein the impurity content of the central diamond face window (201) is less than 10ppm, the thermal conductivity is more than 1800W/(mK), and the absorptivity to X-rays with photon energy of 10keV is less than 20%.
3. The small-sized sample cavity for the X-ray free electron laser device according to claim 2, characterized in that the sample cavity body (1) is a cuboid, and the external geometric dimension is 30-100 mm long, 20-100 mm high and 5-50 mm wide; the thickness of the cavity wall is 10-20 mm; the geometric dimension of the diamond surface window (201) is 30-60 mm long, 20-60 mm high and 0.05-1 mm thick.
4. The compact sample chamber for X-ray free electron laser devices according to claim 1, characterized by the fact that the temperature control system (4) comprises a temperature controlled chamber designed with a recess (401) suitable for the insertion of the bottom of the sample chamber body (1) in order to support and tightly wrap the bottom of the sample chamber body (1); when an electric control mode is adopted, a temperature control resistor or a semiconductor temperature control element is embedded in the temperature control cavity and is connected with a temperature controller through a power line, and the temperature controller is connected with a controller for controlling a computer or a temperature sensor so as to carry out closed-loop control on the temperature; when liquid circulation is used for temperature control, a liquid flow circulation pipeline is embedded in the temperature control cavity, an inlet and an outlet of the pipeline are connected with an external liquid circulation system and a liquid temperature control system, wherein the liquid temperature control system is connected with a controller or a control computer of a temperature sensor to perform closed-loop temperature control.
5. The compact sample chamber for X-ray free electron laser device according to claim 1, characterized in that the upper surface of the sample chamber body (1) has a gas inlet and a gas outlet which are communicated with the chamber, the gas inlet of the sample chamber body (1) is communicated with the gas source or the vacuum pump of the atmosphere control and vacuum system (5) through a gas pipe; the gas outlet of the sample chamber body (1) may be connected to no device or to a special gas recovery device.
6. The miniature sample chamber for X-ray free electron laser device according to claim 1, wherein the sample chamber body (1) has a liquid inlet and a liquid outlet on both sides communicating with the chamber body, the liquid inlet is connected with the liquid outlet of the fluid control system (6); the liquid outlet is connected with the liquid circulating device through a liquid pipe; the fluid control system (6) performs configurable control on the fluid.
7. The compact sample chamber for X-ray free electron laser device according to claim 1, characterized in that the temperature detection system (3) is a temperature sensor embedded in the bottom of the sample chamber for real-time detection of the temperature in the sample chamber.
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