Optical / electric / flow field vertical test equipment and method for X-ray scattering absorption

Abstract

The invention discloses optical / electric / flow field vertical test equipment and method for X-ray scattering absorption. The device comprises a device main body I, a device main body II, a fluid transmission pipeline, an electrode I and an electrode II, the first device main body and the second device main body are oppositely arranged, two groups of grooves which are perpendicular to each other are formed in the contact surfaces of the first device main body and the second device main body, and when the first device main body and the second device main body are assembled together, one group of grooves oppositely form a first channel for fluid to enter and exit, and the other group of grooves oppositely form a second channel for limiting the first electrode and the second electrode; the vertical intersection area of the first channel and the second channel is marked as an area O; the electrode I and the electrode II are respectively connected with a voltage source and are used for applying an electric field perpendicular to the flowing direction of fluid to the fluid flowing through the area O in the fluid transmission pipeline; the first device body and the second device body are each provided with a light through hole, and when the first device body and the second device body are assembled, the two light through holes face each other to form a third channel used for transmitting synchrotron radiation light to apply a light field perpendicular to the fluid flowing direction and the electric field to fluid flowing through the area O.

Description

Technical Field

[0001] The present invention belongs to the technical field of synchrotron radiation characterization, and particularly relates to a test device and method for perpendicular optical / electrical / current fields applicable to synchrotron radiation scattering absorption technology. Background Art

[0002] Synchrotron radiation is electromagnetic radiation generated by non-uniform motion of electrons with a speed close to the speed of light in a magnetic field. It has excellent characteristics such as a continuous wide spectrum (ranging from far infrared to hard X-rays), high brightness, and high collimation, and is considered by the scientific community as a characterization probe of extremely high quality, which is of great significance for scientific research in various fields such as condensed matter physics, catalytic chemistry, and biology. With the current upgrade and popularization construction of synchrotron radiation light sources in China, more and more synchrotron radiation X-ray characterization technologies for specific fields have been developed, and experimental equipment targeted at relevant research urgently needs to be developed.

[0003] Anisotropic dielectric particles dispersed in an insulating liquid form a complex fluid, and the mechanical properties of this complex fluid will change significantly with the change of an applied electric field. Studying the aggregation behavior of electrolyte particles dispersed therein is particularly important for understanding the electric field polarization response of these complex fluids. Existing experimental techniques do not have perfect experimental equipment and cannot perform X-ray characterization tests in-situ using synchrotron radiation while applying a perpendicular electric field to the flowing complex fluid. To meet the needs of experimental research, it is necessary to develop a test device for perpendicular optical / electrical / current fields applicable to synchrotron radiation X-ray scattering absorption technology. Summary of the Invention

[0004] The purpose of the present invention is to fill the gap in the technical field of synchrotron radiation characterization and provide a test device for perpendicular optical / electrical / current fields applicable to synchrotron radiation scattering absorption technology. An electric field perpendicular to the flow field of a flowing fluid is applied, and at the same time, the optical field of X-rays is made to be perpendicular to the above two fields for incidence, so as to conduct experimental research on one or more synchrotron radiation characterization technologies including but not limited to X-ray diffraction spectrum test, X-ray absorption spectrum test, and X-ray small-angle scattering test on the research object dispersed in the fluid.

[0005] The object of the present invention is achieved by the following technical solutions: A test device with three perpendicular fields of light / electricity / current applicable to synchrotron radiation scattering absorption technology, comprising a first device body, a second device body, a light incident window, a light exit window, a fluid input pipe, a fluid output pipe, a first electrode, a second electrode, bolts and nuts; The first device body and the second device body are arranged opposite to each other. Both the first device body and the second device body are provided with through holes along their axial directions as channels for synchrotron radiation to enter and exit. The light incident window and the light exit window respectively cover the through holes of the first device body and the second device body. On the surfaces of the first device body and the second device body that are in contact with each other, two sets of opposite grooves are opened as channels for fluid to enter and exit and channels for electrode sliding (used to limit the sliding of two opposite electrodes on the same straight line). The first electrode and the second electrode are arranged in the aforementioned set of opposite grooves and are connected to a voltage source. The fluid input pipe and the fluid output pipe are arranged in the aforementioned other set of opposite grooves and are connected to a fluid reservoir. Scales are engraved on the first electrode and the second electrode, and their insertion depths are controlled manually or electrically.

[0006] Preferably, the light incident window and the light exit window are transparent to X-rays. The incident light field passes through the through hole of the first device body and the light incident window and irradiates on the fluid, and then passes through the light exit window and the through hole of the second device body to leave the test device.

[0007] Preferably, on the side of the through holes of the first device body and the second device body that does not contact the fluid, there are large-angle chamfers shaped like horns to facilitate the collection of the outgoing light signal.

[0008] Preferably, the light incident window and the light exit window are covered on the through holes of the first device body and the second device body by means including but not limited to flange fixing, seal ring extrusion, and glue pasting to ensure the sealing of the test device and prevent fluid leakage.

[0009] Preferably, the first electrode and the second electrode are made of materials with good conductivity, and their bottom surfaces are facing each other and are smooth and flat to ensure that the electric field applied to the irradiated area of the incident light field is uniform.

[0010] Preferably, except for the first electrode and the second electrode, all other parts are made of insulating materials to prevent interference with the electric field applied to the sample.

[0011] Preferably, the first electrode and the second electrode are arranged on the first device body and the second device body by means including but not limited to flange fixing and seal ring extrusion, so that the first electrode and the second electrode can slide along the grooves on the first device body and the second device body, and ensure the sealing of the test device to prevent fluid leakage.

[0012] Preferably, the inner diameter and outer diameter of the fluid input pipe and the fluid output pipe are exactly the same, and their axes coincide, so as to ensure a uniform fluid flow field in the test device.

[0013] Preferably, the fluid input pipe and the fluid output pipe are fixed to the device body 1 and the device body 2 by means including but not limited to flange fixation, sealing ring extrusion, and glue pasting, so as to ensure the sealing of the test device and prevent fluid leakage.

[0014] Preferably, the axes of the light passing holes of the device body 1 and the device body 2, the axes of the electrode 1 and the electrode 2, and the axes of the fluid input pipe and the fluid output pipe are perpendicular to each other. The bottom surface shapes of the electrode 1 and the electrode 2 are exactly the same (or mirror images of each other).

[0015] A test method for a test device with perpendicular optical / electrical / current fields applicable to synchrotron radiation scattering absorption technology includes the following steps:

[0016] (1) Install the light incident window and the light exit window on the light passing holes of the device body 1 and the device body 2 respectively;

[0017] (2) Install the fluid input pipe, the fluid output pipe, the electrode 1 and the electrode 2 into the corresponding grooves respectively, and fix the device body 1 and the device body 2 with bolts and nuts;

[0018] (3) Set the positions and distances of the electrode 1 and the electrode 2, and connect them to the voltage source respectively; after the relative distance between the bottom surfaces of the two electrodes is determined, the shape of the electric field is determined; when the two electrodes slide while maintaining a fixed relative distance, the position of the test object in the electric field can be adjusted, and this adjustment is particularly important for non-uniform electric fields.

[0019] (4) Connect the fluid input pipe and the fluid output pipe to the fluid reservoir, and set the power source on the fluid input pipe;

[0020] (5) Install the test device on the synchrotron radiation beamline station so that the light incident window is perpendicular to the incident light field;

[0021] (6) Start the power source to input the fluid into the fluid input pipe, and set the voltage of the voltage source;

[0022] (7) Start the test, introduce the synchrotron radiation light field, and collect the signals of the incident light and the outgoing light to obtain X-ray scattering (including small-angle X-ray scattering and wide-angle X-ray scattering) and X-ray absorption spectrum data. For example, Figure 4These are a set of two-dimensional small-angle X-ray scattering patterns obtained by testing with the present invention. This set of data reflects the evolution process of Bi2Fe4O9 nanosheets flowing in silicone oil from isotropic uniform orientation to orientation along the electric field direction as the externally applied electric field gradually increases; Figure 5 These are a set of two-dimensional wide-angle X-ray scattering patterns obtained by testing with the present invention. This set of data shows that as the concentration of Bi2Fe4O9 nanosheets in flowing silicone oil gradually increases under a fixed electric field, the wide-angle X-ray scattering signal of Bi2Fe4O9 nanosheets gradually increases; Figure 6 These are a set of one-dimensional wide-angle X-ray scattering spectra obtained by testing with the present invention. This set of spectra reflects the evolution process of the increasing number of Bi2Fe4O9 nanosheets aggregated along the electric field direction in flowing silicone oil as the externally applied electric field gradually increases; Figure 7 These are a set of X-ray absorption spectra obtained by testing with the present invention. This set of spectra reflects the evolution process of the local structure of Bi atoms in Bi2Fe4O9 nanosheets flowing in silicone oil as the externally applied electric field gradually increases.

[0023] Different concentrations of the fluid and different flow velocities determine the flow field of the sample; different magnitudes of the voltage and different distances between the electrodes determine the electric field applied to the sample; when both the flow field and the electric field are determined, the "state" of the sample is determined. At this time, the incident X-ray will generate various different signals, and corresponding data can be collected using different receiving devices - these data all reflect the "state" of the sample at this time. By adjusting the flow field and the electric field, samples in different "states" can be obtained, and various signals generated by the X-ray will change accordingly. Therefore, data in different "states" can be collected through the present invention.

[0024] The present invention has the following advantages over the prior art:

[0025] (1) The testing device of the present invention can realize in-situ monitoring of the aggregation behavior of dielectric particles in complex fluids under the influence of a flow field and an externally applied electric field using synchrotron radiation.

[0026] (2) During the process of dielectric polarization and aggregation, various signals including but not limited to X-ray transmission signals, fluorescence signals, diffraction signals, and scattering signals can be captured simultaneously.

[0027] (3) The present invention can change the flow field in the testing device by adjusting the flow velocity of the fluid or the concentration of the input fluid.

[0028] (4) The present invention can change the electric field distribution in the testing area by changing the voltage applied to the electrodes or adjusting the electrode distance.

[0029] (5) The testing device of the present invention has a simple structure, is convenient to assemble, and is easy to clean and reuse.

[0030] (6) The materials for manufacturing the various components of the test device of the present invention are common and easily available, facilitating popularization and use, and are of great significance for helping more researchers engage in the research on the aggregation behavior of nanoparticles in flowing complex fluids under an electric field. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 A perspective view of the test device with perpendicular optical / electric / current fields according to an embodiment of the present invention.

[0032] Figure 2 A schematic structural diagram of the test device with perpendicular optical / electric / current fields according to an embodiment of the present invention.

[0033] Figure 3 A schematic diagram of the working principle of the test device with perpendicular optical / electric / current fields according to an embodiment of the present invention.

[0034] Figure 4 The two-dimensional small-angle X-ray scattering pattern involved in an embodiment of the present invention, reflecting the orientation behavior of Bi2Fe4O9 nanosheets in flowing silicone oil under an external electric field;

[0035] (a) The two-dimensional small-angle X-ray scattering pattern collected when the applied electric field strength is 0 V / mm,

[0036] (b) The two-dimensional small-angle X-ray scattering pattern collected when the applied electric field strength is 10 V / mm,

[0037] (c) The two-dimensional small-angle X-ray scattering pattern collected when the applied electric field strength is 20 V / mm,

[0038] (d) The two-dimensional small-angle X-ray scattering pattern collected when the applied electric field strength is 40 V / mm,

[0039] (e) The two-dimensional small-angle X-ray scattering pattern collected when the applied electric field strength is 60 V / mm,

[0040] (f) The two-dimensional small-angle X-ray scattering pattern collected when the applied electric field strength is 120 V / mm.

[0041] Figure 5 The two-dimensional wide-angle X-ray scattering pattern involved in an embodiment of the present invention, reflecting the aggregation behavior of Bi2Fe4O9 nanosheets in flowing silicone oil under an external electric field;

[0042] (a) The two-dimensional small-angle X-ray scattering pattern collected when 0 vol% of Bi2Fe4O9 nanosheets are dispersed in silicone oil,

[0043] (b) The two-dimensional small-angle X-ray scattering pattern collected when 0.46 vol% of Bi2Fe4O9 nanosheets are dispersed in silicone oil,

[0044] (c) Two-dimensional small-angle X-ray scattering pattern collected when 4.12 vol% of Bi2Fe4O9 nanosheets are dispersed in silicone oil.

[0045] Figure 6 This is the one-dimensional wide-angle X-ray scattering spectrum involved in the embodiments of the present invention, which reflects the aggregation behavior of Bi2Fe4O9 nanosheets in flowing silicone oil under the action of an external electric field.

[0046] Figure 7 This is the X-ray absorption spectrum diagram involved in the embodiments of the present invention, which reflects the Bi atom near-neighbor structure of Bi2Fe4O9 nanosheets in flowing silicone oil under the action of an external electric field.

[0047] Reference numerals: 1 - Device main body 1, 2 - Device main body 2, 3 - Light incident window, 4 - Light exit window, 5 - Fluid input pipe, 6 - Fluid output pipe, 7 - Electrode 1, 8 - Electrode 2, 9 - Bolt, 10 - Nut. Detailed implementation manners

[0048] The present invention will be further described below in conjunction with the accompanying drawings and embodiments. This embodiment is implemented on the premise of the technical solution of the present invention, and detailed implementation manners and specific operation processes are given, but the protection scope of the present invention is not limited to the following embodiments.

[0049] As Figures 1-3 shown, the test equipment for the three-field perpendicular of light / electricity / current field for synchrotron radiation scattering absorption technology includes device main body 1, device main body 2, light incident window 3, light exit window 4, fluid input pipe 5, fluid output pipe 6, electrode 1 7, electrode 2 8, bolt 9, nut 10; the device main body 1 and the device main body 2 are arranged opposite to each other, and both the device main body 1 and the device main body 2 are provided with through holes penetrating along their axial directions as channels for synchrotron radiation light to enter and exit. The light incident window 3 and the light exit window 4 respectively cover the through holes of the device main body 1 and the device main body 2. The surfaces of the device main body 1 and the device main body 2 in contact with each other are provided with two groups of opposite grooves as channels for fluid to enter and exit and limits for electrode sliding. The electrode 1 7 and the electrode 2 8 are arranged in the aforementioned group of opposite grooves and are connected to a voltage source. The fluid input pipe 5 and the fluid output pipe 6 are arranged in the aforementioned other group of opposite grooves and are connected to a fluid reservoir.

[0050] Among them, the light incident window 3 and the light exit window 4 are made of materials with low X-ray absorption rates such as sapphire, silicon nitride glass, Kapton film, Mylar polyester film, and PET film. The device body 1, the device body 2, the fluid input pipe 5, the fluid output pipe 6, the bolt 9, and the nut 10 are all made of insulating materials such as PTFE and PEEK. The first electrode 7 and the second electrode 8 are made of metals with good electrical conductivity such as copper, aluminum, and silver. The light passing holes of the device body 1 and the device body 2 have large-angle chamfers shaped like horns on the side that does not contact the fluid, so as to facilitate the collection of the emitted optical signal. The light incident window 3 and the light exit window 4 are covered on the light passing holes of the device body 1 and the device body 2 by means including but not limited to flange fixation, seal ring extrusion, and glue pasting to ensure the sealing of the test device. The bottoms of the first electrode 1 and the second electrode 2 face each other and are smooth and flat to ensure that the electric field applied to the incident light field irradiation area is uniform. The first electrode 7 and the second electrode 8 are arranged on the device body 1 and the device body 2 by means including but not limited to flange fixation and seal ring extrusion, so that the first electrode 7 and the second electrode 8 can slide along the grooves on the device body 1 and the device body 2 and ensure the sealing of the test device. The inner diameters and outer diameters of the fluid input pipe 5 and the fluid output pipe 6 are exactly the same and their axes coincide to ensure a uniform flow field of the fluid in the test device. The fluid input pipe 5 and the fluid output pipe 6 are fixed to the device body 1 and the device body 2 by means including but not limited to flange fixation, seal ring extrusion, and glue pasting to ensure the sealing of the test device. The axes of the light passing holes of the device body 1 and the device body 2, the axes of the first electrode 7 and the second electrode 8, and the axes of the fluid input pipe 5 and the fluid output pipe 6 are perpendicular to each other.

[0051] A test method for a test device with perpendicular optical / electrical / current fields applicable to synchrotron radiation scattering absorption technology includes the following steps:

[0052] (1) Install the light incident window 3 and the light exit window 4 on the light passing holes of the device body 1 and the device body 2 respectively;

[0053] (2) Install the fluid input pipe 5, the fluid output pipe 6, the first electrode 7, and the second electrode 8 into the corresponding grooves respectively, and fix the device body 1 and the device body 2 with the bolt 9 and the nut 10;

[0054] (3) Set the positions and distances of the first electrode 7 and the second electrode 8 and connect them to the voltage source respectively; after the relative distance between the bottoms of the two electrodes is determined, the shape of the electric field is determined; when the two electrodes slide while maintaining a fixed relative distance, the position of the test object in the electric field can be adjusted, and this adjustment is particularly important for non-uniform electric fields.

[0055] (4) Connect the fluid input pipe 5 and the fluid output pipe 6 to the fluid reservoir, and set the peristaltic pump in the fluid input pipe 5;

[0056] (5) Install the test device on the synchrotron radiation beamline station so that the light incident window 3 is perpendicular to the incident light field;

[0057] (6) Start the peristaltic pump to input the fluid into the test device and set the voltage of the voltage source;

[0058] (7) Start the test, introduce the synchrotron radiation light field, and collect data including but not limited to X-ray absorption spectrum, X-ray fluorescence spectrum, X-ray diffraction spectrum, small angle X-ray scattering spectrum, etc.

[0059] The fluid input pipe 5 and the fluid output pipe 6 can be a complete fluid transmission pipe, connected to the fluid reservoir for transmitting the fluid to be tested, thereby avoiding fluid leakage in the pipe. At this time, the light incident window and the light output window can be omitted.

[0060] The above specific embodiments are only the preferred embodiments of the present invention and are not used to limit the present invention. Any other changes or other equivalent replacement methods made without departing from the spirit and principle of the present invention should be included within the protection scope of the present invention.

Claims

1. A light / electric / current field vertical test device for X-ray scattering absorption, characterized in that: It includes a device body 1, a device body 2, a fluid transmission pipeline, an electrode 1, and an electrode 2; The device body 1 and the device body 2 are arranged opposite to each other; the surfaces of the device body 1 and the device body 2 that contact each other are each provided with two groups of mutually perpendicular grooves; when the device body 1 and the device body 2 are assembled together, one group of grooves forms a first channel for fluid inlet and outlet; the other group of grooves forms a second channel for limiting the position of the electrode 1 and the electrode 2; the fluid transmission pipeline is inserted into the first channel, and the electrode 1 and the electrode 2 are respectively inserted into the second channel from both ends of the second channel; the area where the first channel and the second channel intersect vertically is recorded as area O; The fluid transmission pipeline is used to be connected to the fluid storage device and is used to transmit the fluid to be tested; The electrode 1 and the electrode 2 are respectively connected to a voltage source, and are used to apply an electric field perpendicular to the flow direction of the fluid to the fluid flowing through the area O in the fluid transmission pipeline; The device body 1 and the device body 2 are respectively provided with a light through hole. When the device body 1 and the device body 2 are assembled together, the two light through holes form a third channel relative to each other, which is used to transmit synchrotron radiation light to apply a light field perpendicular to the fluid flow direction and the electric field to the fluid flowing through the area O. The third channel is perpendicular to the first channel and the second channel respectively through the area O.

2. A light / electric / current field vertical test device for X-ray scattering absorption, characterized in that: It includes a device body 1, a device body 2, a light incident window, a light exit window, a fluid input pipeline, a fluid output pipeline, an electrode 1, and an electrode 2; The device body 1 and the device body 2 are arranged opposite to each other; the surfaces of the device body 1 and the device body 2 that contact each other are each provided with two groups of mutually perpendicular grooves; when the device body 1 and the device body 2 are assembled together, one group of grooves forms a first channel for fluid inlet and outlet; the other group of grooves forms a second channel for limiting the position of the electrode 1 and the electrode 2; the fluid input pipeline and the fluid output pipeline are respectively inserted into the first channel from both ends of the first channel, and the electrode 1 and the electrode 2 are respectively inserted into the second channel from both ends of the second channel; The area where the first channel and the second channel intersect vertically is recorded as area O; The fluid input pipeline and the fluid output pipeline are used to be connected to the fluid reservoir, and the fluid in the fluid reservoir enters the area O through the fluid input pipeline and then flows back to the fluid reservoir through the fluid output pipeline; The electrode 1 and the electrode 2 are respectively connected to a voltage source, and are used to apply an electric field perpendicular to the flow direction of the fluid to the fluid flowing through the region O and prevent the fluid in the region O from flowing out through the second channel; the fluid is an insulator; A light through hole is respectively provided on the device body one and the device body two. When the device body one and the device body two are assembled together, the two light through holes form a third channel relative to each other, which is used to transmit synchrotron radiation light to apply a light field perpendicular to the fluid flow direction and the electric field to the fluid flowing through the area O. The third channel is perpendicular to the first channel and the second channel respectively through the area O; the light incident window and the light exit window respectively cover the two light through holes, which are used to prevent the fluid in the area O from flowing out through the third channel.

3. The device according to claim 2, characterized in that The light incident window and the light exit window respectively cover one end of the two light through holes close to the area O.

4. The device according to claim 2, characterized in that The inner diameter and outer diameter of the fluid input pipeline and the fluid output pipeline are the same, and the axes coincide with each other.

5. The device according to claim 2, characterized in that The fluid input pipeline and the fluid output pipeline are respectively fixed to the assembly of the device body 1 and the device body 2 by means including but not limited to flange fixing, sealing ring extrusion, and adhesive bonding to prevent fluid leakage.

6. The device according to claim 1 or 2, characterized in that The electrode one and the electrode two are respectively arranged on the device body one and the device body two by means including but not limited to flange fixing and sealing ring extrusion, so that the electrode one and the electrode two can slide in the second channel and prevent fluid leakage.

7. The device according to claim 1 or 2, characterized in that The second channel is used to restrict the sliding of the electrode 1 and the electrode 2 on the same straight line; the bottom surfaces of the electrode 1 and the electrode 2 have the same shape or are mirror images of each other, and are used to provide a uniform electric field.

8. The device according to claim 1 or 2, characterized in that The electrode 1 and the electrode 2 are engraved with scales for controlling the depth of insertion into the second channel.

9. A testing method for the optical / electrical / current field vertical testing device for X-ray scattering absorption according to claim 1 or 2, the steps comprising: 1) Setting the positions and distances of electrode 1 and electrode 2, and connecting them to voltage sources respectively; 2) connecting the fluid input pipeline and the fluid output pipeline to the fluid reservoir, and setting the power source in the fluid input pipeline; 3) Installing the optical / electrical / current field vertical testing device for X-ray scattering absorption as described in claim 1 or 2 on a synchrotron radiation line station to vertically incident the incident light field into the third channel; 4) starting the power source to input the fluid into the fluid input pipeline, and setting the voltage of the voltage source; 5) When the test starts, the synchrotron radiation is vertically incident on the third channel to irradiate the fluid, and an electric field is applied to the fluid. Then the outgoing light signal is collected to obtain X-ray scattering absorption data.

10. The method according to claim 9, characterized in that When adjusting the positions of electrode one and electrode two in the second channel, the relative distance between the bottom surfaces of electrode one and electrode two is kept unchanged; the X-ray scattering absorption data includes but is not limited to small-angle X-ray scattering, wide-angle X-ray scattering, X-ray absorption spectrum or X-ray fluorescence spectrum.

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