CN114262568A - Electroluminescent insulation defect self-diagnosis composite coating and preparation method thereof - Google Patents
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Abstract
The invention provides an electroluminescent insulation defect self-diagnosis composite coating and a preparation method thereof, wherein the method comprises the following steps: the electroluminescent composite coating is prepared by a coating method by using materials with good light transmittance such as Polydimethylsiloxane (PDMS) and the like as a polymer matrix, ZnS electroluminescent particles as a filler and insulating materials such as epoxy resin and the like as a base material. The composite coating shows excellent surface insulation strength and can improve the direct-current surface flashover voltage. In addition, the high electric field region generated by the insulation defect can be easily identified by the luminous distribution of the coating sample, thereby realizing self-diagnosis of the insulation defect.
Description
Technical Field
The invention relates to the field of material technology and electrical engineering, in particular to an electroluminescent insulation defect self-diagnosis composite coating and a preparation method thereof.
Background
Insulating materials are important components of electrical equipment, such as High Voltage (HV) power equipment, electronics, and advanced spacecraft applications. During the production, assembly and operation of these devices, insulation defects may occur, degrading or even failing the insulation material. Therefore, various insulation condition detection and diagnosis methods have been developed to detect potential defects in the equipment, but these methods generally require special detection equipment and sophisticated detection techniques, which may affect the safe operation of the equipment. For example, an ultraviolet imager is used for detecting corona discharge of an outdoor insulator, and a partial discharge detector based on a pulse current and ultrahigh frequency method is used for detecting insulation defects and the like of high-voltage equipment. However, most of these methods rely on expensive test equipment and require expert field knowledge to diagnose the insulation state. Therefore, the development of a new field insulation defect monitoring mode with the characteristics of no damage, intuition, real time and the like has great attraction for industrial application. Since the luminescent material has the advantages of high sensitivity, easy recognition and real-time response, if the luminescent material is applied to the insulating material, the insulating material can emit light under the stimulation of electric field enhancement or temperature, and self-detection and diagnosis of the defects are expected to be realized. Considering that most insulating materials are opaque and it is difficult to find insulation defects during operation, it is more feasible to develop self-diagnostic coatings in industrial applications. In addition, the surface charge accumulation of the insulator is serious under the action of a direct current electric field, the surface flashover voltage is reduced, and the introduction of the composite coating does not influence the insulating property of the insulator, particularly the surface flashover strength.
In summary, the defects existing at present are as follows:
1. when the insulation state detection and diagnosis method is adopted to detect potential defects in the equipment, a special detection device is usually needed, professional field knowledge is needed to diagnose the insulation state, and the safe operation of the equipment is easily influenced.
2. Under the action of the direct current electric field, the surface charges of the insulator are seriously accumulated, and the distribution of the electric field along the surface is distorted, so that the electric field becomes an extremely uneven electric field, and the flashover voltage along the surface of the insulator is reduced.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for preparing a luminescent coating with electroluminescent insulation defect self-diagnosis characteristics and high direct-current flashover strength performance.
An electroluminescent insulation defect self-diagnosis composite coating comprises the following raw materials: ZnS electroluminescent particles, a light-transmitting polymer and a polymer curing agent.
Further, in the electroluminescent insulation defect self-diagnosis composite coating, the ZnS-based electroluminescent particles are ZnS: Cu, ZnS: Mn or ZnS: cu or Al.
Further, according to the electroluminescent insulation defect self-diagnosis composite coating, the mol percentage of ZnS in the particles of Cu and Mn is 99%; the mol ratio of ZnS to Cu to Al in the ZnS to Cu and Al particles is as follows: 99: 0.67: 0.33.
further, according to the electroluminescent insulation defect self-diagnosis composite coating, the particle size of the ZnS electroluminescent particles is 9-30 nm.
Further, the electroluminescent insulation defect self-diagnosis composite coating is characterized in that the light-transmitting polymer is vinyl-terminated polydimethylsiloxane or epoxy resin.
Further, as for the electroluminescent insulation defect self-diagnosis composite coating described above, when the light-transmitting polymer is vinyl terminated polydimethylsiloxane, the polymer curing agent is Pt curing agent; when the light-transmitting polymer is an epoxy resin, the polymer curing agent is phthalic anhydride.
Further, in the electroluminescent insulation defect self-diagnosis composite coating as described above, the mass fraction of the ZnS-based electroluminescent particles in the coating is 20 wt% to 30 wt%.
A preparation method of an electroluminescent insulation defect self-diagnosis composite coating comprises the following steps: ZnS electroluminescent particles are used as filler, fully stirred and mixed with a light-transmitting polymer, and then added with a polymer curing agent, and stirred uniformly to prepare the material.
Further, the method as described above, comprising the steps of:
(1) mixing ZnS electroluminescent particles with a transparent polymer by stirring, adding a curing agent, and stirring to obtain a polymer matrix/ZnS electroluminescent particle mixture;
(2) taking an insulating material as a base material, and pretreating the base material by using 500Cw sand paper;
(3) uniformly coating the polymer matrix/ZnS electroluminescent particle mixture on the surface of a matrix, and shaping by using a scraper;
(4) curing was carried out in a vacuum oven at 120 ℃ for 4 hours.
Further, in the method described above, the substrate is silicone rubber, nylon, or polymethyl methacrylate.
The electroluminescent insulation defect self-diagnosis composite coating prepared by the invention can respond to a high electric field generated by insulation defects and can find various insulation defects, such as outdoor insulator pollution, cracks and surface particles.
Under the stimulation of an electric field, the ZnS type electroluminescent material can emit light with different colors (determined by trace metal doped in the ZnS type electroluminescent material), and the ZnS has better optical performance compared with other II-VI compounds and traditional organic dyes. The method prepares the composite coating with high flashover strength and self-diagnosis function by filling ZnS electroluminescent particles into a polymer with good light transmittance. The composite coating shows excellent surface insulation strength and can improve the direct-current surface flashover voltage. In addition, the high electric field region generated by the insulation defect can be easily identified by the luminous distribution of the coating sample, thereby realizing self-diagnosis of the insulation defect.
The composite coating can inhibit surface charge accumulation and improve flashover strength under direct current stress. ZnS is a semiconductive filler, and ZnS electroluminescent particles are filled in the composite coating, so that the dissipation of surface charges can be effectively accelerated, and the flashover strength can be improved.
Drawings
FIG. 1 is a flow chart of the preparation of ZnS electroluminescent coating with self-diagnosis and high flashover strength of the present invention and the verification of its performance;
FIG. 2(a) is a schematic diagram of the preparation of a sample of the PDMS/ZnS: Cu composite coating according to the present invention;
FIG. 2(b) is an experimental setup for testing the electroluminescent properties of the present invention;
FIG. 3 is a photomicrograph of the luminescence of the composite coating of the rod-plate electrode structure at different AC voltages and the discharge current of the composite coating of 31 wt% mass fraction of ZnS: Cu at different AC voltages;
FIG. 4 is a photomicrograph of the pin-plate electrode structure composite coating at different AC voltages and the discharge current of the composite coating with 31 wt% mass fraction of ZnS: Cu at different AC voltages;
FIG. 5 is a diagram showing the luminescence phenomenon when different minute defects are attached to the surface of a conical truncated cone epoxy resin insulator when the AC voltages applied to the electrodes are 5kV, 7kV and 8.5kV, respectively;
FIG. 6 is a plot of flashover voltage for different ZnS: Cu mass fraction samples; wherein, (a) is a direct current flashover voltage curve diagram; (b) is a graph of AC flashover voltage;
FIG. 7(a) is a graph of the isothermal surface potential decay after a sample of the present invention is being charged;
fig. 7(b) is a surface trap distribution diagram of different samples.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention takes a polymer with good light transmission as a coating substrate, adds a corresponding curing agent, selects ZnS particles with electroluminescence response characteristics as a filler, selects an epoxy resin sheet and an epoxy resin trapezoid round table as the substrate, and prepares the light-transmitting polymer/ZnS filler composite coating with different mass fractions by a coating method.
Example 1:
the invention provides an electroluminescent composite coating, comprising: vinyl terminated Polydimethylsiloxane (PDMS) polymer, Pt curing agent, ZnS: Cu particles.
Wherein the particle diameter of ZnS: Cu particles is 10 μm. The mass of PDMS polymer was 1.88g, the mass of Pt curing agent was 0.19g, the mass of ZnS: Cu was: 0.188-1.316 g.
As shown in FIG. 1, the present invention also provides a method for preparing an electroluminescent composite coating, and FIG. 2(a) shows an explanatory view for preparing a PDMS/ZnS: Cu coating, which is prepared by coating a PDMS/ZnS: Cu mixture on the surface of an epoxy resin matrix using a matrix such as an epoxy resin sheet as an insulating material. The method comprises the following steps:
(1) different masses (0.188g, 0.564g, 0.94g, 1.316g) of ZnS: Cu filler were mixed with 1.88g PDMS with stirring, and 0.19g Pt curing agent was added and stirred to give a PDMS/ZnS: Cu mixture.
(2) Using epoxy resin (EP) as a base material, and carrying out pretreatment by using 500Cw sand paper;
(3) and uniformly coating the PDMS/ZnS-Cu mixture on the surface of an epoxy resin matrix, and shaping by using a scraper.
(4) The samples were cured in a dry box at 120 ℃ for 4 hours. Composite coatings with ZnS and Cu mass fractions of 8 wt%, 21 wt%, 31 wt% and 39 wt% were prepared, respectively.
The epoxy resin material can be replaced by silicon rubber, nylon, polymethyl methacrylate and other materials as a matrix. This example only represents epoxy resins.
The mentioned epoxy resin sheet is a circular sheet with the radius of 3cm and the thickness of 1.8 mm; the epoxy resin trapezoid round platform is a trapezoid round platform with the upper bottom radius of 1cm, the lower bottom radius of 2cm and the height of 2 cm.
The coating methods mentioned are: the epoxy resin matrix surface was pretreated with abrasive paper (500Cw) to improve the adhesion strength, then wiped with alcohol, air dried, and then uniformly spread on the epoxy resin matrix surface with a 1cm wide nylon brush and set with a spatula. Standing for a period of time, placing into a drying oven, drying at 120 deg.C for 4 hr, taking out after drying, and naturally cooling.
Example 2:
the present embodiment provides an electroluminescent composite coating comprising: PDMS polymer, Pt curing agent, ZnS, Cu and Al particles.
Wherein the particle diameter of ZnS, Cu and Al particles is 10 μm. Molar ratio of ZnS to Cu and Al in ZnS to Cu and Al particles is 99: 0.67: 0.33. the mass of PDMS polymer is 1.88g, the mass of Pt curing agent is 0.19g, the mass of ZnS, Cu and Al are as follows: 0.188-1.316 g.
The embodiment also provides a method for preparing polydimethylsiloxane PDMS/ZnS Cu and Al coating, which takes a substrate such as an epoxy resin sheet and the like as an insulating material, prepares a mixture of PDMS/ZnS Cu and Al and coats the mixture on the surface of the epoxy resin substrate, and specifically comprises the following steps:
(1) different masses (0.188g, 0.564g, 0.94g, 1.316g) of ZnS: Cu, Al filler were mixed with 1.88g PDMS with stirring, 0.19g Pt curing agent was added and stirring was carried out to obtain a PDMS/ZnS: Cu, Al mixture.
(2) Using epoxy resin (EP) as a base material, and carrying out pretreatment by using 500Cw sand paper;
(3) and uniformly coating the mixture of PDMS/ZnS, Cu and Al on the surface of an epoxy resin matrix, and shaping by using a scraper.
(4) The samples were cured in a dry box at 120 ℃ for 4 hours. Composite coatings with the mass fractions of ZnS, Cu, Al of 8 wt%, 21 wt%, 31 wt% and 39 wt% are respectively prepared.
Experimental example 1:
the experimental example used the ZnS-Cu composite coating of example 1 to perform the following experiment, wherein the particle diameters of the ZnS-Cu and Al particles were 10 μm, the added PDMS mass was 1.88g, the Pt curing agent mass was 0.19g, and the ZnS-Cu and Al masses were respectively: 0.188g, 0.564g, 0.94g and 1.316g, wherein the final ZnS composite coating comprises the following ZnS, Cu and Al in mass fraction: 8 wt%, 21 wt%, 31 wt%, 39 wt%, and blank 0 wt%.
Processing rod-plate, needle-plate and other typical structure electrodes, observing the luminescence characteristics of the composite coating under different structures, testing the electroluminescence performance when small metal defects are attached to the surface of the conical truncated cone insulator, comparing and analyzing the relevance between the luminescence distribution characteristics and the electric field distribution, and verifying the self-diagnosis effect of the composite coating.
The coatings were tested for their electroluminescent properties in both rod-plate and pin-plate typical electrode configurations, with the experimental setup shown in fig. 2 (b). The composite coating is excited to emit light under the alternating voltages of 5kV, 8kV, 11kV and 14kV respectively. The luminescence photographs at different applied voltages were recorded with a digital camera (canon EOS 80D) and the discharge current was measured using a 50 Ω resistor connected in series in the ground line. The lowest voltage at which blue and green light can be observed with the naked eye is defined as the starting voltage. Fig. 3 and 4 are photographs of the luminescence of the rod-plate electrode and pin-plate electrode composite coatings, respectively, at different ac voltages. It can be seen that for the coating added samples, only a weak blue-green halo was observed under the rod electrode at the starting voltage. When the alternating voltage reaches 8kV, the light-emitting area is obviously enlarged and is further enlarged along with the applied voltage. With the continuous increase of the alternating voltage, the light-emitting area of the composite coating is continuously increased, and the brightness is also continuously increased. The brightness near the high voltage electrode is close to saturation, showing the characteristics of white light, and gradually decreases as the distance from the high voltage electrode increases. For uncoated epoxy resins, only at applied voltages above 11kV, a faint violet light is produced due to corona discharge around the high voltage electrode. The uncoated epoxy resin was less luminous than the sample with the coating added and was difficult to observe with the naked eye.
Discharge current detection is considered to be an effective method for finding insulation defects. Therefore, we also measured the discharge current of the composite coating layer having ZnS: Cu mass fraction of 31 wt%, as shown in FIG. 3. It can be seen that as the applied voltage increases, both the amplitude and the repetition frequency of the discharge current increase, which is consistent with the enhancement of the brightness of the composite coating. In addition, by comparing the discharge current waveform and the luminescence photo under different voltages, the electroluminescent self-diagnosis coating of the invention can be found to have better detection sensitivity than the traditional pulse current method. Blue-green light was observed at 2.1kV starting voltage, while the pulse current method failed to detect the discharge signal. In addition, fig. 3 and 4 show that the luminescence intensity of the sample increases with increasing mass fraction of ZnS: Cu filler at the same alternating voltage. The composite coating with high ZnS-Cu mass fraction has high brightness and a large white light saturation area.
Experimental example 2:
and testing the electroluminescent performance of the conical truncated cone epoxy resin insulator when the surface is attached with the metal defect so as to investigate the effectiveness of the ZnS-Cu coating in identifying the insulation defect. Fig. 5 shows a luminescence photograph and a discharge current of the coating surface. And a copper wire with the length of 3.1mm and the diameter of 0.15mm is placed on the coating to simulate the insulation defect. When the applied voltage was increased to 5.0kV, a distinct light emitting area was observed around the wire defect tip, indicating a higher electric field strength. Due to the addition of the fine copper wire, the field strength near the copper wire is enhanced, thereby generating luminescence near the defect. In addition, the ZnS: Cu coating has better detection sensitivity than the pulse current method. These results indicate that the fluorescence signal of PDMS/ZnS: Cu coatings can be used to find insulation defects.
Experimental example 3:
a typical finger electrode structure is adopted, alternating current and direct current voltages are applied, and the surface flashover characteristic is tested under the atmospheric condition. The surface trap distribution of the coating samples was measured using Isothermal Surface Potential Decay (ISPD). And (3) investigating the influence of the content of ZnS and Cu particles on trap distribution characteristics and surface flashover voltage.
A typical finger electrode structure is adopted, alternating current and direct current voltages are applied, and the surface flashover characteristic is tested under the atmospheric condition. Firstly, wiping the surface of a sample with alcohol, and setting the boosting speed to be 1kV per second for testing flashover voltage after the sample is dried. The electrodes used were typical finger electrodes with a spacing of 10.7mm and a radius of the electrode tip of 10 mm. FIG. 6 is a Weibull plot of DC and AC flashover voltages for different samples. The dc flashover voltage of the sample without the added coating was the lowest, about 17.5 kV. With the increase of the mass fraction of ZnS to Cu, the direct current flashover voltage is increased firstly and then reduced. The maximum DC flashover voltage of the composite coating containing 31 wt% of ZnS and Cu is 22.8kV, which is improved by 30.3% compared with a sample without the coating. At a mass fraction of ZnS: Cu of 39 wt%, the flashover voltage of the sample was reduced by about 10.1% as compared to that at a mass fraction of ZnS: Cu of 31 wt%. The flashover probability plots for the ac flashover voltages for the different ZnS: Cu mass fraction samples are shown in fig. 6 (b). With the increase of the mass fraction of ZnS to Cu, the alternating current flashover voltage firstly rises and then falls. But different from direct current flashover, the overall improvement range of the flashover voltage of the composite coating under the alternating voltage is small. For the coating with the largest ac flashover improvement, the lift rate is only around 3%.
Selecting samples with different ZnS: Cu mass fractions and blank samples, lightly wiping the surfaces with alcohol, and testing the isothermal surface potential attenuation and surface trap distribution characteristics of the samples. Firstly, the surface of a sample is subjected to needle and grid corona discharge. The needle and the metal mesh were charged at 6kV and 2kV dc voltages, respectively. After charging for 5 minutes, the sample was moved under a kelvin probe (Trek 347), and the decay curve of the surface potential with time was measured. Throughout the measurement, the sample was heated with a heating plate and the temperature was maintained at 50 ℃. The level and density of traps can be determined according to the Isothermal Discharge Current (IDC) theory proposed by Simmons. The surface potential decay curves and the surface trap distribution results for the different ZnS: Cu mass fraction samples were calculated as shown in fig. 7(a) - (b). It can be seen that the addition of the ZnS composite coating increases the rate of surface potential decay of the sample. The trap energy becomes shallower compared to the untreated surface. The trap depth of the pure epoxy resin without the added coating layer was 1.04eV, and the trap depth decreased first and then increased as the ZnS: Cu concentration increased, and was the smallest at 0.96eV when the ZnS: Cu mass fraction was 31 wt%. Typically, the charge in the shallower traps is released first, and the charge in the deeper traps is released later. Due to the nonlinear conductivity of the ZnS: Cu particles, carriers migrate rapidly in the ZnS: Cu particles, and thus, as the filler concentration increases, carriers are more easily transported in the path formed by the ZnS: Cu filler, thereby accelerating the dissipation of charges. Due to the difference in dielectric constant and conductivity between the epoxy spacer layer and the composite coating, the interface between them provides another charge accumulation region, thereby increasing the trap density. Therefore, when the mass fraction of ZnS: Cu is 39 wt%, the increase in trap energy is likely to be due to enhancement of interface charge accumulation.
And obtaining the ZnS-Cu filler concentration ratio coating with comprehensively optimal physical and chemical properties under various conditions according to the comprehensive test result.
By filling electroluminescent ZnS and Cu filler, the composite coating with self-diagnosis of insulation defects and high flashover strength is developed. The composite coating can be applied to the surfaces of insulating materials such as epoxy resin and the like, and the composite coating emits light before corona discharge starts, and the luminous intensity of the composite coating is far higher than that of the corona discharge. The results show that the high electric field region generated by the insulation defect can be easily identified by the luminous distribution of the coating sample, and self-diagnosis of the insulation defect is realized. In addition, by effectively dissipating surface charges, the composite coating can improve the surface flashover strength of the insulator, and the direct current flashover voltage and the alternating current flashover voltage are respectively improved by 30.3% and 3% to the maximum. In consideration of improvement of ac/dc flashover strength and electroluminescence performance, we consider that this excellent composite material has a potential for application to self-diagnosis of insulation defects of high-voltage facilities such as outdoor insulators and gas insulation equipment.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. An electroluminescent insulation defect self-diagnosis composite coating is characterized by comprising the following raw materials: ZnS electroluminescent particles, a light-transmitting polymer and a polymer curing agent.
2. The electroluminescent insulation defect self-diagnosis composite coating according to claim 1, characterized in that the ZnS-based electroluminescent particles are ZnS: Cu, ZnS: Mn, or ZnS: cu or Al.
3. The electroluminescent insulation defect self-diagnosis composite coating according to claim 1, wherein the molar percentage of ZnS in the ZnS: Cu and ZnS: Mn particles is 99%; the mol ratio of ZnS to Cu to Al in the ZnS to Cu and Al particles is as follows: 99: 0.67: 0.33.
4. the electroluminescent insulation defect self-diagnosis composite coating according to claim 1, wherein the particle size of the ZnS-based electroluminescent particles is 9 to 30 nm.
5. The electroluminescent insulation defect self-diagnosis composite coating according to claim 1, characterized in that the light-transmitting polymer is vinyl terminated polydimethylsiloxane or epoxy resin.
6. The electroluminescent insulation defect self-diagnosis composite coating according to claim 4, wherein when the light-transmitting polymer is vinyl terminated polydimethylsiloxane, the polymer curing agent is a Pt curing agent; when the light-transmitting polymer is an epoxy resin, the polymer curing agent is phthalic anhydride.
7. The electroluminescent insulation defect self-diagnosis composite coating according to claim 1, wherein the mass fraction of the ZnS-based electroluminescent particles in the coating is 20 to 30 wt%.
8. A preparation method of an electroluminescent insulation defect self-diagnosis composite coating is characterized by comprising the following steps: ZnS electroluminescent particles are used as filler, fully stirred and mixed with a light-transmitting polymer, and then added with a polymer curing agent, and stirred uniformly to prepare the material.
9. The method of claim 7, comprising the steps of:
(1) mixing ZnS electroluminescent particles with a transparent polymer by stirring, adding a curing agent, and stirring to obtain a polymer matrix/ZnS electroluminescent particle mixture;
(2) taking an insulating material as a base material, and pretreating the base material by using 500Cw sand paper;
(3) uniformly coating the polymer matrix/ZnS electroluminescent particle mixture on the surface of a matrix, and shaping by using a scraper;
(4) curing was carried out in a vacuum oven at 120 ℃ for 4 hours.
10. The method of claim 9, wherein the substrate is silicone rubber, nylon, or polymethylmethacrylate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210064929.5A CN114262568A (en) | 2022-01-20 | 2022-01-20 | Electroluminescent insulation defect self-diagnosis composite coating and preparation method thereof |
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| CN114907672A (en) * | 2022-06-01 | 2022-08-16 | 合肥工业大学 | Epoxy composite material with insulation fault indication function and preparation method thereof |
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