CN110687146A - X-ray diffraction in-situ testing device for electrochromic film - Google Patents
X-ray diffraction in-situ testing device for electrochromic film Download PDFInfo
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- CN110687146A CN110687146A CN201910974887.7A CN201910974887A CN110687146A CN 110687146 A CN110687146 A CN 110687146A CN 201910974887 A CN201910974887 A CN 201910974887A CN 110687146 A CN110687146 A CN 110687146A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/20025—Sample holders or supports therefor
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Abstract
An X-ray diffraction in-situ testing device for an electrochromic film belongs to the field of X-ray diffraction. The method is characterized in that: taking electrochromic film lithium titanate as a research object, taking lithium titanate as a working electrode (6), and taking a reference electrode (4) as Ag/AgCl and an auxiliary electrode Pt (5); the working electrode (6) and the reference electrode (4) form a loop for determining the electrode potential; the working electrode (6) and the auxiliary electrode (5) form another loop for conducting current; the electrolyte is inorganic lithium salt powder-organic solvent electrolyte containing conductive lithium ions; the whole structure is divided into two parts; the upper part uses the sample groove (3) as a main body, the lower part is a lifting support, the testing device can assist a sample to be conveniently placed on a diffractometer, in-situ X diffraction of the sample under different voltage and current is realized, a sealing or light-transmitting system is not required to be considered, and real-time slight change in a short time can be observed.
Description
The technical field is as follows:
an X-ray diffraction testing technology relates to the field of large-scale instrument testing equipment. The invention relates to an X-ray diffraction in-situ testing device.
Background art:
with the continuous increase of scientific and technological development and scientific research investment, the X-ray diffraction in-situ test requirement is increasingly intense, and due to the complex equipment, the currently known in-situ X-ray diffraction is limited to three aspects of in-situ temperature change, in-situ stretching and in-situ battery. Only in-situ high-temperature devices are sold in the market, and only powder samples are subjected to complex operation, high price and limited use. Other in-situ devices are commonly found in universities and scientific research institutions, and are designed and manufactured by themselves in combination with self-demand. In-situ XRD devices generally need to take measures such as an overlying film or a sealed beryllium window because of the occurrence of many reactions in-situ experiments, but these measures affect the intensity of incident X-rays and do not obtain data with sufficient accuracy, which results in having to extend the measurement time, and thus are not suitable for observing subtle changes in real time in a short time. The in-situ X-ray diffraction testing device is designed because real-time monitoring of the performance and the structure of the electrochromic lithium titanate film under different voltage and current conditions and analysis of the lattice structure of the hysteresis effect of the electrochromic lithium titanate film are urgently needed through the research of the project. The first intention of our design and research is to try to control the electrode reaction, avoid and reduce other generation through the selection of the electrode and the preparation of the electrolyte.
The invention takes an electrochromic lithium titanate film as a research object. The electrochromic material can reversibly change optical properties (reflectivity, transmittance, absorptivity and the like) under an external electric field, and shows regular changes of color and transparency. When the film contacts the negative pole of the power supply, external ions enter the film and generate color together with electrons from the cathode, and when the film contacts the positive pole of the power supply, the ions leave and lose color. The invention relates to an X-ray diffraction in-situ testing device, which is used for on-site observation and real-time monitoring under different voltage and current. The device comprises a sample tank with a three-electrode system and lithium perchlorate-organic electrolyte, wherein a film sample is placed in the sample tank, the position of a light spot of the sample on a diffractometer is determined through a positioning column, and conductive lithium ions in the electrolyte are controlled to enter lithium titanate lattices through an external electric field of the electrode system. The movement of the conductive ions in the crystal lattice of the sample is controlled by different voltage and current, the change of the optical property of the film is observed, and the redox reaction and the crystal structure change brought by the migration of the conductive ions in the crystal lattice under different voltage and current are revealed by applying X diffraction.
The X-ray powder diffractometer disclosed by the invention does not need to be subjected to any structural modification, and does not need to be coated with a protective film or beryllium window for sealing, so that the diffraction intensity can be ensured, one datum can be acquired within a few minutes, the X-ray powder diffractometer is suitable for observing the real-time change and the hysteresis effect of a sample under a certain voltage and current, the X-ray powder diffractometer realizes the X-ray diffraction in-situ test of the sample in an electrochemical system, and the X-ray powder diffractometer is convenient to.
The invention aims to provide an X-ray diffraction in-situ testing device for an electrochromic film. The case takes the Shimadzu diffractometer as an application object, and can also be used for other diffractometers by slightly changing the case. The testing device can assist a sample to be conveniently placed on a diffractometer, realizes in-situ X diffraction of the sample under different voltage and current, does not need to consider a sealing or light-transmitting system, and can observe real-time slight change in a short time.
The invention content is as follows:
the technical scheme includes that ① is a sample groove with an electrode as a main body, and comprises a positioning column, a positioning surface, a liftable support, an external lead and the like, the placement position of a sample is determined in advance through the designed in-situ testing device, the basic coincidence of the surface to be measured of the sample and a light spot position is realized while the testing device is fixed on the diffractometer, so that the test is convenient, ② three-electrode system determination and electrolyte allocation are performed, a research object lithium titanate is used as a working electrode, a reference electrode and an auxiliary electrode are determined according to the properties of lithium titanate, the basic requirement is that the electrode cannot influence the sample to be researched due to self reaction and does not react with the electrolyte, the reference electrode is finally determined to be an Ag/AgCl glass electrode and the auxiliary electrode to be a Pt metal electrode, the working electrode and the reference electrode form a loop for determining the electrode potential, the working electrode and the auxiliary electrode form another loop for conducting current, high-lithium-carbonate organic chlorate containing conductive lithium ions is placed in the groove, other organic solvents are doped as additives, the organic solvents are used as additives, the mixed solvent, the mixed solution is used for forming a short-free from a short-time, the research, the high-viscosity of the mixed reaction is kept, the high-free from the generation of the whole reaction, the research is not needed, the high-free of a smooth reaction, the research is not needed, the whole reaction, the high-free of a liquid-free from the open reaction, the research is not needed.
An X diffraction in-situ test device of an electrochromic film is characterized in that: taking electrochromic thin-film lithium titanate as a research object, taking lithium titanate as a working electrode (6), and taking a reference electrode (4) as Ag/AgCl and an auxiliary electrode Pt (5); the working electrode (6) and the reference electrode (4) form a loop for determining the electrode potential; the working electrode (6) and the auxiliary electrode (5) form another loop for conducting current; the electrolyte is inorganic lithium salt powder-organic solvent electrolyte containing conductive lithium ions;
the testing device is divided into two parts in the whole structure;
the upper part takes a sample groove (3) as a main body and comprises a positioning column (1), a positioning surface (2), a reference electrode (4), an auxiliary electrode (5), a working electrode (6), an electrode holder (7) and an external lead; the tail ends of the reference electrode (4), the auxiliary electrode (5) and the working electrode (6) are externally connected with leads and are connected with voltage and current control equipment outside the diffractometer;
the lower part is a lifting support which consists of a sample tank supporting plate (9), a nut (11), a screw (10), a supporting frame (12) and a base (13), and the supporting frame (12) is driven to extend upwards to play a role in bearing and changing the height of a sample by rotating the nut (11) and the screw (10);
the positioning column (1) is positioned at the front end of the sample groove (3) and plays a role in marking the position of the device relative to the diffractometer, and the marked diffraction spot surface (8) is flush with the surface to be measured of the sample;
the positioning surface (2) plays a role in marking the central position of the light spot.
The whole structure of the device can be divided into an upper part and a lower part: the upper part takes the sample groove as a main body, and sequentially comprises a positioning column, a positioning surface, a working electrode containing a sample, a reference electrode, an auxiliary electrode, an electrode holder and an external lead from front to back; the lower part is a lifting bracket.
The positioning is determined by the positioning column (1) at the forefront of the device. The location post (1) is used to determine the relative position of the diffractometer to the in-situ apparatus, and once the location of the location post (1) is determined, the sample position is automatically aligned with the diffractometer spot (8). The top surface of the positioning column (1) is flush with the plane where the light spot (8) of the diffractometer is located, and the positioning column is used for determining the height of the light spot (8). The positioning surfaces (2) are used for determining the positions of light spots, the midpoint of the connecting line of the centers of the two positioning surfaces is the center (8) of the light spots of the diffractometer, and the diffraction light spots are a circle with the center as the center and the diameter of 25 mm. The positioning surface cannot block incident light, so that some diffraction peaks cannot emerge.
The sample groove (3) is square or rectangular, and the thickness of the groove wall is 1-2 mm. The width of the groove body is 50-52mm, the length of the groove body is 50mm or longer, the length of the reference electrode and the length of the diffractometer are actually determined, so that the three electrodes can be contained simultaneously, and the three electrodes are located outside an X-ray spot. The height of the sample groove (3) is not limited, and the sample groove is preferably 20-25mm, and the depth of three electrodes which are not in contact with each other can be accommodated.
The three electrodes are placed parallel to each other, horizontally, and perpendicular to the goniometer plane. The reference electrode (4) and the auxiliary electrode (5) are positioned near the bottom and on two sides of the tank, and the top end of the working electrode (6) clamps the sample, is near the liquid level and is positioned at the middle upper part of the tank body. The tail ends of the three electrodes are connected with voltage and current control equipment outside the diffractometer through external leads.
The electrode holder (7) is positioned outside the groove, and the position of the control electrode and the depth of the groove can be adjusted. The electrode is fixed by screws, and the horizontal state of the electrode can be finely adjusted.
The sample tank (3) is made of inert, pollution-free and easily-processed plastic and is formed by pouring and processing the plastic in a mold for one time, and is not influenced by electrode reaction and X-ray irradiation. The three electrodes are connected to the clamp holder (7) through metal rods wrapped with insulating plastic skins, the positions of the three electrodes are fixed through the clamp holder (7), and the connecting rods cannot react with electrolyte.
And the lifting support is positioned at the lower part of the in-situ measuring device. The lifting support consists of a sample groove supporting plate (9), a screw rod (10), a nut (11), a support frame (12) and a base (13); a nut (11) capable of driving the screw rod (10) to rotate is sleeved at one end of the screw rod (10) and rotates through the nut (11); the support frame (12) is positioned between the sample groove supporting plate (11) and the base (13), and the screw (10) which can drive the support frame (12) to move up and down is positioned on the support frame (12). The screw rod (10) is driven by manually rotating the nut (11) to be used as the power of the lifting platform and to adjust the approximate height position of the sample, so that the sample groove and the related accessories are supported, and the height of the sample is adjusted.
The sample groove supporting plate (9) and the base (13) are square or rectangular, bear the weight of the sample groove and all the components on the upper part, require the surface to be horizontal and cannot influence the horizontal state of the measuring reference surface. The length of the support frame (12) and the screw (10) between the supporting plate (9) and the base (13) is required to be not beyond the range of the supporting plate. For bearing, the sample tank supporting plate (9), the base (13), the supporting frame (12) and the screw (10) are required to be made of metal.
Drawings
The specific structural features and objects of the present invention are further described below in conjunction with the appended drawings.
Fig. 1 is a front view of the present invention.
Fig. 2 is a perspective view of the present invention.
Fig. 3 is a top view of the present invention.
1. Positioning column 2, positioning surface 3 and sample tank
4. Reference electrode 5, auxiliary electrode 6, working electrode
7. Electrode holder 8, X-ray spot 9 and sample groove support plate
10. Screw 11, nut 12, support frame
13. Base seat
Detailed Description
Referring to fig. 1, the present invention is a tool for realizing X-ray diffraction in-situ test of an electrochromic film on a diffractometer by combining a sample tank with a three-electrode system and a lifting bracket, wherein the tool comprises:
the positioning column (1) is positioned outside the sample groove (3) and in the middle of the foremost end, and the length and the width are required to be equal to 15mm multiplied by 8 mm. This is determined by the structure of the Shimadzu diffractometer. When the in-situ measuring device is arranged on a diffractometer, the front side surface of the positioning column is tightly attached to the inner wall of the goniometer, the upper top surface of the positioning column is tightly attached to the middle protruding part of the goniometer and just occupies the middle position of a sample clamp of the diffractometer, so that the whole in-situ measuring device is tightly attached to and perpendicular to the surface of the goniometer, and the positioning column is positioned on the vertical central axis surface of the goniometer.
The length of the positioning surface (2) is 25mm, the positioning surface is just equal to the diameter of the circular light spot (8) of the diffractometer, and the distance from the front end of the positioning surface to the outermost side of the front edge of the sample groove (3) is 7.5 mm. The middle point of the connecting line of the centers of the two positioning surfaces is 35mm away from the straight line of the most front end of the positioning column and is just positioned at the position of the diffraction light spot (8). When the sample is placed, the placement position of the sample can be determined by the midpoint of the positioning plane.
In order to avoid the contact of incident X-rays, the reference electrode (4) and the auxiliary electrode (5) are arranged at the depth of the sample groove (3); in order to facilitate the sample to receive incident X-ray and generate diffraction, the working electrode (6) is arranged on the upper surface of the sample groove (3) near the liquid level. Due to the size of the working electrode (6) and the thickness of the connecting column, the working electrode needs to be positioned at a position with a certain depth in the sample groove (3) when being placed for firm placement, so that two sides of the sample groove (3) can block incident X-ray, and a concave plane which allows the X-ray to penetrate needs to be cut at two sides of the sample groove (3). The width of the surface, which is located on the path of the incident X-ray beam, corresponds exactly to the size of the spot, which corresponds to one of the cross-sections of the sample chamber, i.e. the locating surface (2).
The height of the positioning surface (2) determines the highest position of the liquid level of the electrolyte in the sample tank. In the experiment, conductive ions and electrons are conducted through the electrolyte, and the sample is required to be in direct contact with the electrolyte, so that the liquid level of the electrolyte is required to be higher than the surface to be measured of the sample, namely the position of the positioning surface (2) is required to be higher than the light spot surface; but not too high, which would block the incident X-rays by the sample wells on both sides. According to theoretical calculation and experimental verification, under the test conditions of a general sample, when the incidence angle 2 theta is 5 degrees, 10 degrees and 20 degrees, the distribution range of the incident X-ray on the spot surface (8) is concentrated in the distances of 12.5mm, 8mm and 2.5mm from the center of the spot along the optical path direction. The first diffraction line position of lithium titanate is 18 °, and the height of the positioning surface with respect to the spot is calculated as follows: the tangent of the angle θ of incidence of the X-ray with the horizontal plane is multiplied by the distance from the center of the spot to the sides of the sample well-the observed distance of the incident X-ray range from the center of the spot at this angle. When the width of the groove is about 50mm, the height of the positioning surface relative to the spot surface is preferably 2.5mm in consideration of not blocking the incidence of the X-ray.
The working electrode (6) consists of a top plastic sample clamp, a central metal rod and an outer insulating plastic skin, and the tail end of the electrode is connected with an external lead. The plastic sample clamp consists of an upper horizontal sheet (a lower metal surface) and a lower inclined sheet, the sample is connected and fixed through a rotary screw, and the metal surface is in contact with the film and is connected with an external lead through a central metal rod. The film sample is prepared by taking glass as a substrate, plating a thin film on the substrate, and taking the film surface as the surface to be detected of the sample. When in test, the surface to be tested of the sample is superposed with the diffraction spot surface (8), so that the sample clamp clamps the film sample, and the lower metal surface of the plastic clamp horizontal sheet is attached to the surface to be tested of the sample, namely, the lower metal surface of the plastic clamp horizontal sheet is flush with the light spot (8) when in test. Therefore, when the in-situ measuring device is designed, firstly, the height and the width of the sample groove (3) are estimated according to the sizes and the placing positions of the three electrodes, the electrodes and the sample rack are ensured to be firmly and horizontally placed, and then the heights of the positioning columns (1) and the positioning surfaces (2) are determined so as to achieve the optimal sample testing position.
The in-situ device has the following use process:
selection of electrodes and preparation of electrolyte: the system is a three-electrode system, a research object is lithium titanate, the research object is set as a working electrode, and a reference electrode and an auxiliary electrode are determined according to the working electrode. The basic requirements for selection are: the electrode itself does not react with the sample to be studied and does not react with the electrolyte. Finally, the reference electrode is determined to be an Ag/AgCl glass electrode and the auxiliary electrode is determined to be a Pt metal electrode.
The organic electrolyte of lithium perchlorate is placed in the groove, and the effects of providing conductive lithium ions and transmitting charges are achieved. Lithium perchlorate requires high purity and moisture<0.01 percent. Because lithium perchlorate is strong in hygroscopicity, proper powder needs to be obtained by dehydration and drying before experiments. The preparation of lithium perchlorate organic electrolyte is commonly used acrylate, and the conductivity of the acrylate solution of lithium perchlorate can reach 7.3x10-3s/cm. Other solvents such as nitrile solvents can be added in appropriate amounts to increase viscosity and increase conductivity. Crushing the lithium perchlorate powder, adding the crushed lithium perchlorate powder into an organic solvent, uniformly stirring,the steady state was reached by 24 hours of standing. During the preparation and test process, certain attention must be paid to avoid the moisture incorporation, which can cause electrode reaction and gas generation.
Sample installation: the sample cell was placed on the diffractometer platform and the sample was inserted into the sample holder. And adjusting the insertion length of the working electrode, rotating to enable the surface to be measured of the sample to be horizontally upward, and finally enabling the sample to be in the range of the expected diffraction light spots and enabling the plastic to be clamped outside the diffraction light spots. Care was taken to keep the working electrode and sample on a horizontal plane.
Installation of a measuring device: the liftable support is placed below the sample tank, the positioning column and the liftable support are placed close to the surface of the goniometer and perpendicular to the surface of the goniometer, the positioning column and the liftable support are positioned on the axis of the surface of the goniometer, the nut on the sample support is rotated to enable the sample support to slowly rise, the height and the position of the measuring device are adjusted until the front side surface of the positioning column is close to the diffractometer and the upper top surface just props against the position right below the middle protruding part of the goniometer. To this end, the position of the measuring device relative to the diffractometer is determined.
And (3) testing the measurement position: and (3) inspecting and finely adjusting the position of the sample by adopting the silicon single crystal wafer until the surface to be measured of the sample is matched with the diffraction surface of the light spot.
Measurement is started: and (4) putting a sample, and slowly adding the prepared electrolyte to ensure that the electrolyte just submerges the surface of the sample to be detected. And connecting an external lead, starting the circuit voltage control equipment, and then starting the measurement work.
Claims (4)
1. An X diffraction in-situ test device of an electrochromic film is characterized in that: taking electrochromic film lithium titanate as a research object, taking lithium titanate as a working electrode (6), and taking a reference electrode (4) as Ag/AgCl and an auxiliary electrode Pt (5); the working electrode (6) and the reference electrode (4) form a loop for determining the electrode potential; the working electrode (6) and the auxiliary electrode (5) form another loop for conducting current; the electrolyte is inorganic lithium salt powder-organic solvent electrolyte containing conductive lithium ions;
the testing device is divided into two parts in the whole structure;
the upper part takes a sample groove (3) as a main body and comprises a positioning column (1), a positioning surface (2), a reference electrode (4), an auxiliary electrode (5), a working electrode (6), an electrode holder (7) and an external lead; the tail ends of the reference electrode (4), the auxiliary electrode (5) and the working electrode (6) are externally connected with leads and are connected with voltage and current control equipment outside the diffractometer;
the lower part is a lifting support which consists of a sample tank supporting plate (9), a nut (11), a screw (10), a support frame (12) and a base (13), and the support frame (12) is driven to extend upwards to play a role in bearing and changing the height of a sample by rotating the nut (11) and the screw (10);
the positioning column (1) is positioned at the front end of the sample groove (3) and plays a role in marking the position of the device relative to the diffractometer, and the marked diffraction spot surface (8) is flush with the surface to be measured of the sample;
the positioning surface (2) plays a role in marking the central position of the light spot.
2. A measuring device according to claim 1, wherein the height of the positioning surface (2) relative to the spot surface (8) is suitably 2.5mm for a sample well having a width of 50 mm.
3. The measuring device according to claim 1, wherein the sample well (3) is open at the top and is free of an overlying light-transmissive film or beryllium window seal.
4. The measuring device according to claim 1, the sample holder (3) having a size, length or width of 50-52mm and a height of 20-25 mm.
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| CN113311012A (en) * | 2021-05-26 | 2021-08-27 | 西湖大学 | Electrochemical detection device based on polycrystalline X-ray diffractometer and test method thereof |
| WO2021238043A1 (en) * | 2020-05-23 | 2021-12-02 | 北京工业大学 | Experiment apparatus for measuring electrical signals produced by liquid mixing and dripping |
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