CN113281380B - Dielectric trap state measurement and imaging system and method driven by friction nano generator - Google Patents
Dielectric trap state measurement and imaging system and method driven by friction nano generator Download PDFInfo
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
-
- H—ELECTRICITY
- H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
- H02N—ELECTRIC MACHINES NOT OTHERWISE PROVIDED FOR
- H02N1/00—Electrostatic generators or motors using a solid moving electrostatic charge carrier
- H02N1/04—Friction generators
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Testing Relating To Insulation (AREA)
Abstract
The invention relates to a dielectric trap state measurement and imaging system and method driven by a friction nano generator, and belongs to the technical field of dielectrics. The system comprises a trap excitation power supply device and a test sample chamber; the trap excitation power supply device comprises an independent layer rotary friction nano generator and a rotary motor, can output constant charge and high voltage, and excites micro-power dielectric barrier uniform discharge on the surface of a dielectric medium, so that electrons are fully trapped and detrapped, and detrapped current pulses with enough intensity and stability are generated; the test sample chamber is used for fixing the tested dielectric film and providing controllable filling gas; the test electrode structure is detachable, so that electrode groups in different measurement modes can be replaced; the air gap distance between the upper electrode and the lower electrode can be adjusted. The system has the advantages of no damage, accuracy and two-dimensional imaging, further obtains the detailed information of the trap state distribution of the surface of the high polymer film material, and is beneficial to the detection and improvement of various performances such as insulation, energy storage, micro-nano surface characteristics and the like of the functional material.
Description
Technical Field
The invention belongs to the technical field of dielectrics, and relates to a dielectric trap state measurement and imaging system and method driven by a friction nano generator.
Background
Trap states are a critical and widely-influencing mesoscopic concept. The trap state density and the trap energy level distribution are important basic parameters of energy generation, storage, transportation and transformation devices and materials under various energy scales. A number of studies have shown that surface trap states have a broad and significant impact on device performance from high polymer materials, such as electrically insulating polymer dielectrics used in electrical energy storage and high voltage applications, and solar thin film batteries capable of generating clean energy, various types of nano-generators, and the like. In the manufacturing process of the device, due to the intrinsic defects of the component materials and the action of the additive, a local state with the energy level in a forbidden band is formed inside the device, namely an electron trap state. The presence of the trap states causes defective sites in the material that allow carriers to stay and further causes space charge to accumulate, ultimately resulting in degradation of the device's electrical and mechanical properties. Therefore, the research on advanced characterization technology aiming at trap state density has important significance for improving the performance of energy materials and the safety of energy equipment and constructing efficient and reliable energy Internet.
In recent years, various methods for measuring trap state distribution have been proposed, such as isothermal surface potential decay method, thermal stimulated current method, photo-stimulated discharge method, electroacoustic pulse method, spectroscopic method, variable frequency conductance test, and drive level capacitance analysis method. The basic principle of the existing method is that an externally applied electric field or light excitation is utilized to form an embedded electron, then external excitation such as a variable frequency electric field, temperature rise, irradiation and the like is applied to the measured material, so that charges at the center energy level of the trap are detrapped, and experimental results related to detrapping current and equivalent circuit parameters thereof are measured, so that macroscopic trap state parameters of the whole sample are directly or indirectly calculated. However, since it is difficult to stably control the amounts of trapped and detrapped charges that have no intrinsic relation to the applied physical field in a single measurement, the test results obtained by the prior methods are often only useful for qualitative comparison and only for morphological interpretation, which limits the further development of the relevant disciplines to some extent. More importantly, the distributed imaging of the surface trap states still faces a great challenge, and the implementation of the method has a profound effect on the technical level of advanced energy material precision machining.
Disclosure of Invention
In view of the above, the present invention aims to provide a dielectric trap state measurement and imaging system and method driven by a friction nano generator, which can stably excite a detrapping current by using the friction nano generator in the system as a constant charge high voltage power supply, and perform single-point trap state parameter analysis and multi-point scanning trap state imaging according to the detrapping current signal.
In order to achieve the above purpose, the present invention provides the following technical solutions:
A dielectric trap state measurement and imaging system driven by a friction nano generator comprises a trap excitation power supply device, a test sample chamber and a trap state parameter extraction and analysis method;
The trap excitation power supply device comprises an independent layer rotary friction nano generator and a rotary motor, can output constant charge and high voltage, and excites micro-power uniform dielectric barrier discharge on the surface of a dielectric medium, so that electrons are fully trapped and detrapped, and detrapped current pulses with enough intensity and stability are generated;
The test sample chamber is used for fixing the tested dielectric film and providing controllable temperature, humidity, air pressure and different filling gases; the test electrode structure is detachable and electrode groups with different measurement modes can be replaced; the air gap distance between the upper electrode and the lower electrode can be adjusted;
The trap state parameter extraction and analysis method comprises a total discharge current acquisition method, a trap state current extraction method and a trap state parameter calculation method.
Further, the independent layer rotary friction nano generator comprises a transmission device and a power generation device, wherein the transmission device comprises a coupler and a linkage rotating shaft, the transmission device is used for fixedly connecting the friction nano generator with an external rotating motor, and mechanical energy required by the operation of the friction nano generator is provided by the external rotating motor; the power generation device comprises an upper stator disc, a lower stator disc, a middle rotor friction layer and a buffer layer between the stator and the rotor; two groups of electrode groups which are distributed in an internal and external complementary mode are arranged on one surface of the stator disc, which faces the rotor friction layer, the inner electrode groups extend towards the edge in a radial mode by taking the center of the disc as a center point, the outer electrode groups extend towards the center of the disc from the edge in opposite directions, adjacent electrodes belong to two different electrode groups, and the circle center angles of the electrodes are the same; the rotor friction layer comprises rotor blades and a modified flexible polymer film, the rotor blades and stator electrodes have the same area, and two groups of rotor blades are arranged in total and face up to the inner sides of the upper and lower stators respectively in a back-to-back mode; the modified flexible polymer film is coated on the rotor blade, and the outer side surface of the polymer film can completely cover one stator electrode without contacting with the adjacent electrode; the buffer layer between the stator and the rotor comprises buffer materials and supporting springs, wherein the buffer materials are filled between the rotor blades and the polymer film, and the supporting springs are fixed between the two groups of rotors, so that the sufficient contact between the stator and the rotors is maintained, the triboelectrification charge density is improved, and the triboelectrification charge density is kept stable.
Further, the stator electrode material is selected from a metal or an alloy, wherein the metal comprises gold, silver, platinum, palladium, aluminum, nickel, copper, titanium, chromium, selenium, iron, manganese, molybdenum, tungsten, or vanadium, and the alloy comprises an aluminum alloy, a titanium alloy, a magnesium alloy, a beryllium alloy, a copper alloy, a zinc alloy, a manganese alloy, a nickel alloy, a lead alloy, a tin alloy, a cadmium alloy, a bismuth alloy, an indium alloy, a gallium alloy, a tungsten alloy, a molybdenum alloy, a niobium alloy, or a tantalum alloy.
Further, the flexible polymer film and the flexible polymer material are both selected from any one of the following film materials: polydimethyl siloxane, polyethylene, polypropylene, polyvinylidene fluoride, vinylidene chloride acrylonitrile copolymer, polytetrafluoroethylene, polyvinyl chloride, fluorinated ethylene propylene copolymer, polytrifluoroethylene, polychloroprene, polyimide, aniline formaldehyde resin, polyoxymethylene, ethylcellulose, polyamide, melamine formaldehyde, polycarbonate, polyethylene glycol succinate, phenolic resin, neoprene, cellulose, natural rubber, ethylcellulose, cellulose acetate, polyethylene adipate, diallyl phthalate, rayon, polyethanol butyral, fibrous sponge, polyurethane elastomer, styrene propylene copolymer, styrene butadiene copolymer, polyethylene propylene carbonate, rayon, polystyrene, polymethacrylate, polyvinyl alcohol, polyester, polyisobutylene urethane flexible sponge, polydiphenol carbonate, polychloroether, polyethylene terephthalate, liquid crystal high molecular polymer and parylene, and the thickness of which is not less than 50 μm.
Further, the modified flexible polymer film refers to a nanowire structure prepared on the surface of the flexible polymer film by an inductively coupled plasma reaction etching method, and the preparation method comprises the following steps: washing the flexible polymer film with alcohol and deionized water and drying; depositing a layer of Au nano particles on the surface of perfluoroethylene propylene by using a sputtering instrument to serve as a mask for inducing the formation of nano wires; ar, O 2 and CF 4 gases were introduced at flow rates of 10.0sccm, 15.0sccm and 30.0sccm, respectively, and the surface of perfluoroethylene propylene was etched for 10 minutes using a high-density plasma generator and a plasma accelerator.
Further, the buffer layer material is any one of foaming polystyrene, foaming polyurethane, ethylene-vinyl acetate copolymer rubber or polyethylene chemical crosslinking high foaming material, and the supporting spring is any one of spring steel, stainless steel wires and brass wires.
Further, the combination method of the rotor blade and the stator disc of the independent layer rotary friction nano generator is as follows: the upper stator disc, the lower stator disc and the middle rotor blade are vertically arranged, the centers of the upper stator disc and the lower stator disc are aligned, the rotor and the rotating shaft are fixed in the vertical direction by using a bearing, the rotor and the inner circular hole of the rotor are stabilized by adopting a connecting pin, the two rotors are required to be kept from dislocation in the process, and then the two stator discs are rotated by an angle to enable the positions of electrodes above the two stator discs to correspond to each other; then, the vertical distance between the rotor blade and the upper and lower stator disks is adjusted, the buffer layer and the supporting spring are filled in and adhered and fixed, and the terminals on the two groups of stator electrodes are respectively connected in series by using copper wires, and a pair of extraction electrodes are formed.
Further, the test sample chamber comprises a shell, a test electrode and a gas regulating device; the shell of the test sample chamber is made of organic glass, has good light transmittance, the upper cover plate can be opened and closed, and the joint between the cover plate and the periphery adopts a rubber gasket seal ring, so that the closed test sample chamber has good air tightness; the test electrode is arranged at the center inside the shell and provided with a lead-out wiring terminal, and the test electrode is provided with two modules: single needle-plate and needle array-plate, for single point analysis and multi-point scanning imaging, respectively; the single needle-plate type test electrode module comprises an upper needle electrode, a needle electrode height adjusting knob and a bottom plate electrode, wherein the electrode material is brass, red copper or nichrome, the diameter of the tip end of the needle electrode is smaller than 30 microns, the top of the needle electrode is connected with a stud and the adjustable knob, the vertical position of the needle electrode is controlled through the knob, and the size of the plate electrode can be adjusted according to the size of a sample dielectric medium; the needle array-plate type test electrode module comprises an upper needle array electrode, a height adjusting knob and a bottom plate electrode, wherein the needle array electrode is made of an epoxy resin insulating material and is formed by fixing a certain number of metal micro-needles on the substrate to form array distribution, the diameter of a needle point is 0.5-10 microns, the plane distribution mode of the needle array is determined by trap state parameter imaging precision, the needle electrodes are mutually insulated, and the height adjusting knob and the bottom plate electrode are the same as the single needle-plate electrode module;
Further, the gas regulating device comprises a gas inlet ventilation valve, a gas outlet ventilation valve, a barometer and a gas guide pipe, and is arranged at a proper position of the shell, wherein the barometer is used for monitoring the pressure value in the sample chamber and needs to resist negative pressure; the air duct needs to penetrate through the wall of the shell and extend into the vicinity of the test electrode, so that the optimal ventilation effect is ensured; the part of the air duct outside the sample chamber can be made of rubber or nylon, and the part extending into the sample chamber is made of insulating materials such as epoxy resin or glass fiber reinforced epoxy resin, and the two materials are connected through an air inlet ventilation valve; the air outlet ventilation valve is arranged on the other side of the air inlet.
Further, the trap excitation power supply device is electrically connected with the test sample chamber in such a way that the leading-out end of the trap excitation power supply device is connected to the leading-out end of the test electrode, the output voltage is applied to the test electrode, an ammeter is connected in series in the test loop, and voltmeters are connected in parallel at two ends of the test electrode.
Further, the total discharge current collecting method is that the time sequence signals of the ammeter and the voltmeter are collected at the same time, the time domain waveform of the discharge current and the dielectric barrier discharge voltage during the existence period of the discharge current pulse are recorded.
Further, the detrap current extraction method is that the total discharge current is assumed to be composed of a blocking discharge current which is dominant by polarized charges and a detrap current which is dominant by detrap charges, a fluid model which takes into account the dynamic evolution of three carriers (electrons, ions and metastable particles) is established, boundary conditions are formed according to the actually measured dielectric surface charge density and dielectric blocking discharge voltage, the two-dimensional geometrical characteristics of a needle-plate structure of a test electrode are combined, and a poisson equation is taken as an electric field convergence condition to calculate a blocking discharge current waveform; then, the blocking discharge current is subtracted from the total discharge current to obtain a waveform of the detrapping current. Specific calculation formulas will be described in detail in the following detailed description.
Further, the trap state parameter calculating method is that trap state density and trap state energy level distribution of a test point are calculated according to an isothermal attenuation current theoretical formula according to the trap state current waveform obtained through calculation; in the imaging test, if a plurality of test points exist, the trap state parameters are sequentially obtained, and the two-dimensional distribution of the trap state parameters can be drawn according to the space coordinates of the trap state parameters.
The invention has the beneficial effects that: the system has the advantages of no damage, accuracy and two-dimensional imaging, further obtains the detailed information of the trap state distribution of the surface of the high polymer film material, and is beneficial to the detection and improvement of various performances such as insulation, energy storage, micro-nano surface characteristics and the like of the functional material.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objects and other advantages of the invention may be realized and obtained by means of the instrumentalities and combinations particularly pointed out in the specification.
Drawings
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in the following preferred detail with reference to the accompanying drawings, in which:
FIG. 1 is a schematic diagram of an independent layer rotary friction nano-generator;
FIG. 2 is a schematic diagram of a test sample chamber;
FIG. 3 is a schematic diagram of electrical connection for a trap state parameter test;
FIG. 4 is a flow chart of a method for extracting the trap current and calculating the trap state parameters;
FIG. 5 is a single point trap state parameter test result;
fig. 6 is a trap state parameter imaging result.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention. It should be noted that the illustrations provided in the following embodiments merely illustrate the basic idea of the present invention by way of illustration, and the following embodiments and features in the embodiments may be combined with each other without conflict.
Wherein the drawings are for illustrative purposes only and are shown in schematic, non-physical, and not intended to limit the invention; for the purpose of better illustrating embodiments of the invention, certain elements of the drawings may be omitted, enlarged or reduced and do not represent the size of the actual product; it will be appreciated by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.
The same or similar reference numbers in the drawings of embodiments of the invention correspond to the same or similar components; in the description of the present invention, it should be understood that, if there are terms such as "upper", "lower", "left", "right", "front", "rear", etc., that indicate an azimuth or a positional relationship based on the azimuth or the positional relationship shown in the drawings, it is only for convenience of describing the present invention and simplifying the description, but not for indicating or suggesting that the referred device or element must have a specific azimuth, be constructed and operated in a specific azimuth, so that the terms describing the positional relationship in the drawings are merely for exemplary illustration and should not be construed as limiting the present invention, and that the specific meaning of the above terms may be understood by those of ordinary skill in the art according to the specific circumstances.
The invention can be particularly applied to trap state parameter characterization and imaging test of polymer dielectric films, and provides effective optimization indexes for dielectric modification. The invention uses the low-frequency high voltage stably output by the friction nano generator, generates periodic dielectric barrier discharge on the dielectric surface through the needle-plate structure electrode, and drives electrons in the trap to get rid of the trap to participate in the discharge current; and further extracting a detrap current waveform from the discharge current, and quantitatively analyzing trap state parameters, so that single-point trap state parameter analysis and multi-point scanning trap state parameter imaging are realized. Suitable test dielectric materials are a wide range of materials including, but not limited to: various insulating high polymer dielectrics, conductive polymers, energy storage dielectrics, nano modified dielectrics, and the like.
Fig. 1 shows a self-contained layer rotary friction nano-generator structure. The independent layer rotary friction nano generator adopts a sandwich structure, two symmetrical stator-rotor combinations are vertically coupled on the same rotating shaft, and each group consists of a rotor with an electronegative surface and a stator with a copper material surface. The rotor is composed of insulated and light acrylic acid sheets, the sector parts of the rotor are respectively wrapped with a fluorinated ethylene propylene film to serve as a friction electrification layer, and a sponge material buffer layer and a spring array are introduced into the rotor, so that the fluorinated ethylene propylene film rotor friction layer on the rotor is kept in close electrical contact with a copper electrode on the stator, and the stability of output performance is ensured. The center angle of each fan-shaped unit is 18 deg., and the rotor has 5 units. The stator is composed of two groups of mutually insulated fan-shaped radial arrays, and the shape of the stator is the same as that of the rotor; thus, the two copper layers on the stator can be considered as two terminal electrodes. The distance between the rotor and the stator is sufficiently adjusted to maintain the electrical insulation on the one hand and to bring the fluorinated ethylene propylene film into full contact with only one electrode network on the other hand. In addition, the nanostructure is etched on the surface of the fluorinated ethylene propylene film by inductively coupled plasma so as to maintain higher friction charge density and output voltage. The two groups of stators and rotors of the independent layer rotary friction nano generator are in series connection, and the output end is led out by a copper wire. In the example, the open-circuit voltage of the independent layer rotary friction nano generator can reach more than 3 kV.
Fig. 2 shows a test sample chamber structure comprising a height-adjustable needle electrode, a circular plate electrode as a sample stage and a gas control means. The sample chamber was equipped with an air inlet pipe of 8mm diameter and an air valve for controlling the gas parameters. The top cover of the sample chamber is removable to allow for replacement of the barrier medium sample. The film sample was fixed to the plate electrode by a carbon conductive adhesive layer. After the sample is fixed, an upper cover plate with a sealing rubber ring is fixed on the sample chamber shell by using a screw so as to keep good air tightness. Before starting the test, the gas parameters of the sample chamber need to be reset, and after the air pressure is pumped to-0.05 MPa by using an air pump, any one of nitrogen, argon or helium with a certain pressure is introduced. In this example, 0.03MPa of high purity argon is introduced into the sample chamber to achieve the best dielectric barrier discharge effect.
FIG. 3 is a schematic diagram of electrical connection for the trap state parameter test. The test sample chamber is connected to an independent layer rotary friction nano generator as an external load, and discharge voltage and current are collected by a high-voltage probe and an electrometer respectively. Relatively high sampling frequencies (above 10 kHz) should be employed to avoid aliasing of multiple discharge current waveforms. A thin film sample serving as a blocking medium was fixed on the bottom plate electrode with a gap of 1mm from the upper needle electrode. After the trap excitation power supply device starts to operate, dielectric barrier discharge is periodically generated in the sample chamber, and the presence criterion of the dielectric barrier discharge can be obtained by observing discharge pulse or discharge spectrum test. In this example, the rotating motor rotates at 100 rpm, the temperature of the sample chamber is room temperature, and the sample is an ethylene-tetrafluoroethylene copolymer film having a diameter of 50mm and a thickness of 0.1mm.
FIG. 4 is a flow chart of a method for extracting the trap current and calculating the trap state parameters. During the extraction process, the input parameters are derived from measured data of the discharge voltage, current waveform and boundary conditions related to the sample cell structure. The detrapping current involves three main types of carriers, including electrons, ions and metastable particles. The initial electric field distribution can be determined according to the initial boundary condition, and then the carrier distribution at different moments t is calculated iteratively by utilizing the two-dimensional electric field distribution of the needle-plate electrode structure. Therefore, when the potential of the needle electrode is kept positive, a barrier current in half a period (T/2) can be obtained. The time resolution of the calculation process is not lower than 0.1ms, and the time resolution is consistent with the sampling period of the measured data. The mathematical model of the dynamic evolution of carriers during dielectric barrier discharge involves the solution of three continuity equations, which can be expressed in terms of cylindrical coordinates:
Wherein subscripts e, i, m represent electron, ion, and metastable particles, respectively, n e,ni, and n m represent the densities of the three particles, respectively. D is the diffusion coefficient and μ is the carrier mobility, which can be obtained by investigation in the literature. In this example, electron mobility μ e＝987cm2V-1s-1, ion mobility μi=14 cm 2V-1s-1, electron diffusion coefficient de=5430 cm 2s-1, and mobility of ions and metastable particles di=0.354 cm 2s-1 and D m＝0.6cm2s-1, respectively. t and E are time and electric field strength, respectively. The k term represents the rate coefficient of generation and loss of each type of carrier, including the gradual ionization rate k em＝3.03×10-9×Ecm3s-1 and the recombination rate k rm＝7×105s-1,αi represent the reduced ionization coefficient, α ex is the excitation coefficient, both of which are related to the electric field strength E:
Thus, each of the left-hand side of formulas (1) through (3) represents in order the contributions of direct ionization or excitation, gradual ionization, and penning ionization, as well as the loss of metastable atoms due to the radiation and conversion processes. Poisson's equation determines the potential Can be described as:
Wherein the constant q c is 1.81×10 -6 Vcm. The boundary condition of the electric potential is the discharge voltage of the sample, and has important influence on the dynamic evolution of the electric field distribution. Considering the distortion of the electric field near the tip, for ease of calculation, it is assumed that the initial electron distribution at the tip is of the form:
Where n e0＝1.4×108cm-3, d is the electrode spacing and δ is the electric field distortion coefficient, which can be determined by measuring the charge density of the sample surface by electrostatic voltage. From the initial boundary conditions described above, the initial electric field distribution may be determined according to equation (5), and then equations (1) - (5) may be solved using finite flux techniques. Thus, the barrier discharge current can be further calculated by the following formula:
Where R d is the diameter of the dielectric sample and q is the amount of fundamental charge. The blocking discharge current calculated by equation (7) is then subtracted from the total discharge current to obtain the detrap current signal I DT for the different samples in each half-period.
Further, the energy level and density of the trap states can be further obtained from the detrapping current I DT data. It is assumed that the trapping process does not occur after the charge in a single discharge channel is detrapped and the recombination behavior of holes and electrons is ignored. Based on the trap parameter theory of the isothermal decay current method, the calculation formulas of the energy level E t and the density N t of the trap state are as follows:
Et＝kTln(νATE·t) (8)
where k is boltzmann constant, T is temperature, v ATE is electron escape frequency, and generally 10 12 is taken.
Fig. 5 and 6 are single point trap state parameter test results and trap state parameter imaging results, respectively. After the discharge voltage and discharge current signals of the tested sample are analyzed according to the process, the relation between the energy level E t and the density N t of the trap state, namely the energy level distribution of the trap state parameters, can be obtained. The test result is similar to the thermal stimulation current method, and the accuracy of the method is demonstrated. After further multi-point scanning by using the needle array-plate electrode, two-dimensional distribution of trap state parameters in space is generated. In this example, the test points of each needle electrode are conducted in turn and insulated from each other by the epoxy resin substrate, and the discharge processes of each point are not interfered with each other. In this embodiment, the detection range of the trap state energy level is 0.5-0.8 eV, corresponding to the shallow trap level of the medium surface.
The embodiment also provides a preparation method of each module, and firstly, a specific manufacturing method of the independent layer rotary friction nano generator for driving dielectric barrier discharge is described. The independent layer rotary friction nano generator is respectively composed of an upper electrode layer, a lower electrode layer and a middle rotor friction layer. Specifically, the upper electrode layer and the lower electrode layer are formed by stator discs with equal areas, two groups of copper electrodes which are complementarily distributed are respectively arranged on the upper electrode layer and the lower electrode layer, the two groups of electrodes are separated by a cutting groove, and electric insulation is ensured. The middle rotor friction layer consists of double layers of 5 pairs of rotor blades and a flexible polymer material perfluoroethylene propylene film, and the polymer film can cover the stator electrode. The electrode plate is made of acrylic material, the outer diameter size is 25 cm-30 cm, the inner hole is the same as the rotating shaft, and the thickness is 12mm. And cutting and groove processing are carried out on the electrode plate by using a laser cutting machine, and then a copper foil tape is attached to the corresponding position to form a conductive layer.
The modification of the flexible polymer material is to grow the nanowire structure on the surface of the perfluoroethylene propylene film by adopting a plasma etching method. Washing a 50 mu m-thick perfluoroethylene propylene film with alcohol and deionized water, drying, and depositing a layer of Au nano particles on the surface of perfluoroethylene propylene by using a sputtering instrument to serve as a mask for inducing the formation of nano wires; ar, O2 and CF4 gases were then introduced at flow rates of 10.0sccm, 15.0sccm and 30.0sccm, respectively, and the surface of perfluoroethylene propylene was etched for 10 minutes using a high-density plasma generator (400W) and a plasma accelerator (100W) to obtain a perfluoroethylene propylene film modified with a nanowire structure.
The combined method of the rotor and the stator of the independent layer rotary friction nano generator comprises the steps of vertically arranging an upper stator disc, a lower stator disc and two middle rotor blades, aligning the centers, fixing the rotor and a rotating shaft in the vertical direction by using a bearing, stabilizing the rotor and a circular hole in the rotor by using a connecting pin, keeping the two rotors from dislocation in the process, and rotating the angles of the two stator discs to enable the positions of electrodes above the two stator discs to correspond to each other; then, the vertical distance between the rotor blade and the upper and lower stator disks is adjusted, the buffer layer and the supporting spring are filled in and adhered and fixed, and the terminals on the two groups of stator electrodes are respectively connected in series by using copper wires, and a pair of extraction electrodes are formed. And finally, stud structures are introduced into four corners of the stator to play a role in supporting and fixing.
The whole length and width of the test sample chamber are 300mm, and the height is 200mm; the shell is made of organic glass material and has a thickness of 15mm; the height adjustable range of the electrode is 20mm, and the precision is 0.05mm; the circular plate electrode is made of red copper, has the diameter of 60mm and the thickness of 10mm; the red copper material of the single needle electrode has a needle tip diameter of 35 mu m; the needle array electrode substrate is transparent epoxy resin, the diameter is 60mm, the thickness is 10mm, 24 nichrome test needle electrodes are uniformly distributed, the diameter of a needle handle is 0.5mm, and the diameter of a needle tip is 0.5mm. The high voltage probe used in the test procedure was TektronixP a, the static meter was Keithley6514, and the sampling frequency was 10kHz.
Finally, it is noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the present invention, which is intended to be covered by the claims of the present invention.
Claims (7)
1. A tribo-nano-generator driven dielectric trap state measurement and imaging device, characterized by: the device comprises a trap excitation power supply device and a test sample chamber;
The trap excitation power supply device comprises an independent layer rotary friction nano generator and a rotary motor, can output constant charge and high voltage, and excites micro-power dielectric barrier uniform discharge on the surface of a dielectric medium, so that electrons are fully trapped and detrapped, and detrapped current pulses with enough intensity and stability are generated;
The test sample chamber is used for fixing the tested dielectric film and providing controllable temperature, humidity, air pressure and different filling gases; the test electrode structure is detachable, so that electrode groups in different measurement modes can be replaced; the air gap distance between the upper electrode and the lower electrode can be adjusted;
the independent layer rotary friction nano generator comprises a transmission device and a power generation device;
The transmission device comprises a coupler and a linkage rotating shaft, and is used for fixedly connecting the friction nano generator with an external rotating motor, and mechanical energy required by the operation of the friction nano generator is provided by the external rotating motor;
the power generation device comprises an upper stator disc, a lower stator disc, a middle rotor friction layer and a buffer layer between the stator and the rotor;
Two groups of electrode groups which are distributed in an internal and external complementary mode are arranged on one surface of the stator disc, which faces the rotor friction layer, the inner electrode groups extend towards the edge in a radial mode by taking the center of the disc as a center point, the outer electrode groups extend towards the center of the disc from the edge in opposite directions, adjacent electrodes belong to two different electrode groups, and the circle center angles of the electrodes are the same;
The rotor friction layer comprises rotor blades and a modified flexible polymer film;
The rotor blades and the stator electrodes have the same area, and two groups of rotor blades are arranged in total and face to the inner sides of the upper and lower stators respectively in a back-to-back mode;
the modified flexible polymer film is coated on the rotor blade, and the outer side surface of the polymer film can cover one stator electrode and is not contacted with the adjacent electrode;
The buffer layer between the stator and the rotor comprises a buffer material and a supporting spring, wherein the buffer material is filled between the rotor blade and the polymer film, and the supporting spring is fixed between the two groups of rotors, so that the sufficient contact between the stator and the rotors is maintained, the triboelectrification charge density is improved, and the triboelectrification charge density is kept stable;
In the independent layer rotary friction nano generator, the combination form of the rotor blade and the stator disc is as follows: the upper stator disc, the lower stator disc and the middle rotor blade are vertically arranged, the centers of the upper stator disc and the lower stator disc are aligned, the rotor and the rotating shaft are fixed in the vertical direction by using a bearing, the rotor and the inner circular hole of the rotor are stabilized by adopting a connecting pin, the two rotors are required to be kept from dislocation in the process, and then the two stator discs are rotated by an angle to enable the positions of electrodes above the two stator discs to correspond to each other; then, adjusting the vertical distance between the rotor blade and the upper and lower stator disks, filling a buffer layer and a supporting spring, bonding and fixing the buffer layer and the supporting spring, connecting terminals on the two groups of stator electrodes in series by using copper wires, and forming a pair of extraction electrodes;
the test sample chamber comprises a shell, a test electrode and a gas regulating device;
The test sample chamber shell is made of organic glass, the upper cover plate can be opened and closed, and a rubber gasket seal ring is adopted at the joint of the cover plate and the periphery, so that the test sample chamber shell has good air tightness after being closed;
The test electrode is arranged at the central position inside the shell and is provided with a lead-out wiring terminal, and the test electrode is provided with two modules: the single-needle-plate type test electrode module and the needle array-plate type test electrode module are respectively used for single-point analysis and multi-point scanning imaging; the single needle-plate type test electrode module comprises an upper needle electrode, a needle electrode height adjusting knob and a bottom plate electrode, wherein the electrode material is brass, red copper or nichrome, the diameter of the tip end of the needle electrode is smaller than 30 microns, the top of the needle electrode is connected with a stud and the adjustable knob, the vertical position of the needle electrode is controlled through the knob, and the size of the plate electrode can be adjusted according to the size of a sample dielectric medium; the needle array-plate type test electrode module comprises an upper needle array electrode, a height adjusting knob and a bottom plate electrode, wherein the needle array electrode is made of an epoxy resin insulating material and is formed by fixing a certain number of metal micro-needles on the substrate to form array distribution, the diameter of a needle point is 0.5-10 microns, the plane distribution mode of the needle array is determined by trap state parameter imaging precision, the needle electrodes are mutually insulated, and the height adjusting knob and the bottom plate electrode are the same as the single needle-plate type test electrode module;
The air regulating device comprises an air inlet ventilation valve, an air outlet ventilation valve, an air pressure gauge and an air duct, and is arranged at a proper position of the shell, wherein the air pressure gauge is used for monitoring the air pressure value in the sample chamber and needs to resist negative pressure; the air duct needs to penetrate through the wall of the shell and extend into the vicinity of the test electrode, so that ventilation is ensured; the part of the air duct outside the sample chamber is made of rubber or nylon, the part extending into the sample chamber is made of epoxy resin or glass fiber reinforced epoxy resin insulating material, and the two parts are connected through an air inlet air exchange valve; the air outlet ventilation valve is arranged on the other side of the air inlet.
2. The tribo-nano-generator driven dielectric trap state measurement and imaging device of claim 1, wherein: the electrode material of the stator is selected from single metal or alloy;
wherein the single metal comprises gold, silver, platinum, palladium, aluminum, nickel, copper, titanium, chromium, selenium, iron, manganese, molybdenum, tungsten, or vanadium;
The alloy includes aluminum alloy, titanium alloy, magnesium alloy, beryllium alloy, copper alloy, zinc alloy, manganese alloy, nickel alloy, lead alloy, tin alloy, cadmium alloy, bismuth alloy, indium alloy, gallium alloy, tungsten alloy, molybdenum alloy, niobium alloy, or tantalum alloy.
3. The tribo-nano-generator driven dielectric trap state measurement and imaging device of claim 1, wherein: the flexible polymer film and the flexible polymer material are selected from any one of the following film materials: polydimethyl siloxane, polyethylene, polypropylene, polyvinylidene fluoride, vinylidene chloride acrylonitrile copolymer, polytetrafluoroethylene, polyvinyl chloride, fluorinated ethylene propylene copolymer, polytrifluoroethylene, polychloroprene, polyimide, aniline formaldehyde resin, polyoxymethylene, ethylcellulose, polyamide, melamine formaldehyde, polycarbonate, polyethylene glycol succinate, phenolic resin, neoprene, cellulose, natural rubber, cellulose acetate, polyethylene adipate, diallyl phthalate, rayon, polyvinyl butyral, fibrous sponge, polyurethane elastomer, styrene propylene copolymer, styrene butadiene copolymer, polyethylene propylene carbonate, polystyrene, polymethacrylate, polyvinyl alcohol, polyester, polyisobutylene, polyurethane flexible sponge, polydiphenol carbonate, polychloroether, polyethylene terephthalate, liquid crystalline high molecular polymer and parylene, with a thickness of not less than 50 μm.
4. The tribo-nano-generator driven dielectric trap state measurement and imaging device of claim 1, wherein: the modified flexible polymer film is prepared on the surface of the flexible polymer film by an inductively coupled plasma reaction etching method to prepare a nanowire structure, and the preparation method comprises the following steps: washing the flexible polymer film with alcohol and deionized water and drying; depositing a layer of Au nano particles on the surface of perfluoroethylene propylene by using a sputtering instrument to serve as a mask for inducing the formation of nano wires; ar, O 2 and CF 4 gases were introduced at flow rates of 10.0 sccm, 15.0 sccm and 30.0 sccm, respectively, and the surface of perfluoroethylene propylene was etched for 10 minutes using a high density plasma generator and a plasma accelerator.
5. The tribo-nano-generator driven dielectric trap state measurement and imaging device of claim 1, wherein: the buffer material is any one of foaming polystyrene, foaming polyurethane, ethylene-vinyl acetate copolymer rubber or polyethylene chemical crosslinking high foaming material, and the supporting spring is any one of spring steel, stainless steel wires and brass wires.
6. The tribo-nano-generator driven dielectric trap state measurement and imaging device of claim 1, wherein: the trap excitation power supply device is electrically connected with the test sample chamber in such a way that the leading-out end of the trap excitation power supply device is connected to the leading-out end of the test electrode, the output voltage is applied to the test electrode, an ammeter is connected in series in the test loop, and the voltmeters are connected in parallel at two ends of the test electrode.
7. Dielectric trap state measurement and imaging method based on the measurement and imaging device of any one of claims 1 to 6: the method comprises a total discharge current acquisition method, a trap current extraction method and a trap state parameter calculation method;
The total discharge current collecting method is that time sequence signals of an ammeter and a voltmeter are collected simultaneously, time domain waveforms of the discharge current and dielectric barrier discharge voltage in the period of the discharge current pulse are recorded;
The method for extracting the detrap current comprises the steps of assuming that the total discharge current consists of a blocking discharge current dominated by polarized charges and a detrap current dominated by detrap charges, establishing a fluid model for taking into account dynamic evolution of three carriers of electrons, ions and metastable particles, forming boundary conditions according to the actually measured dielectric surface charge density and dielectric blocking discharge voltage, combining the two-dimensional geometric characteristics of a needle-plate structure of a test electrode, and calculating a blocking discharge current waveform by taking a poisson equation as an electric field convergence condition; then, subtracting the blocking discharge current from the total discharge current to obtain a waveform of the detrapping current;
The trap state parameter calculation method is that trap state density and trap state energy level distribution of a test point are calculated according to an isothermal attenuation current theoretical formula according to the trap current waveform obtained through calculation; in the imaging test, if a plurality of test points exist, the trap state parameters are sequentially obtained, and the two-dimensional distribution of the trap state parameters is drawn according to the space coordinates.
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