CN114316798A - Dielectric multifunctional nano coating and preparation method and application thereof - Google Patents
Dielectric multifunctional nano coating and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a dielectric multifunctional nano coating and a preparation method and application thereof. The method comprises the following steps: weighing polydimethylsiloxane prepolymer, placing the polydimethylsiloxane prepolymer in n-hexane, and electrically stirring at room temperature to form a uniform solution; weighing nano particles and multi-walled carbon nanotubes, placing the nano particles and the multi-walled carbon nanotubes in the solution, stirring at normal temperature, and carrying out ultrasonic treatment for a certain time to finally form a suspension; adding PDMS curing agent into the solution, and continuing to perform ultrasonic treatment for a period of time; pretreating the surface of the substrate by using abrasive paper; spraying a nano coating: spraying the prepared solution on a substrate; the coated sample was cured in a vacuum oven at 100 ℃ for 4 hours; changing the mass percent of the nano particles, and repeating the steps to prepare the required nano coating with each concentration gradient. The coating disclosed by the invention is optimized in direct-current flashover strength, super-hydrophobic surface, self-cleaning capability and anti-icing performance.
Description
Technical Field
The invention relates to the technical field of materials and electrical engineering, in particular to a dielectric multifunctional nano coating and a preparation method and application thereof.
Background
Polymers have the advantages of high breakdown strength and light weight, and are commonly used as dielectric materials in electrical systems, electronic devices, pulse power equipment and spacecraft. The interface between different media such as gas/vacuum solids is a weak link in the insulation system, i.e. surface flashover occurs more easily than bulk breakdown. In particular, in High Voltage Direct Current (HVDC) transmission systems, insulators have the problem of surface charge accumulation under the action of dc stress, distorting the local electric field and promoting flashover at the dielectric interface. In addition, the increase of moisture or water droplets adhering to the surface of the medium may further deteriorate the flashover strength, indicating that the hydrophobicity is another important property of the medium. Therefore, the development of a surface with high dc flashover voltage and high hydrophobicity is an ideal condition for composite insulation systems. For dielectrics in outdoor applications, other properties such as mechanical durability, self-cleaning, Ultraviolet (UV) resistance, chemical stability, and resistance to icing, among others, should also be considered.
Suppressing the accumulation of surface charges by adjusting the surface characteristics of the insulator is an effective method for improving flashover performance. Therefore, several methods such as fluorination, plasma treatment, and doping of functional fillers have been proposed. It is generally believed that fluorination and plasma treatment change the chemical composition of the surface, accelerate the dissipation of surface charges, and improve flashover strength. However, the above techniques typically introduce chemical groups of high surface energy, thereby lowering the Contact Angle (CA) of water. Replacement of the precursor in the plasma treatment with tetraethoxysilane or trimethylsilane increases CA but rarely exceeds 100 °. In addition, surface coating is another method to improve the insulating properties of the surface, wherein the nano-filler is usually a non-linear conductive filler filled in a polymer matrix. And brushing a coating on the insulator to adjust the surface properties such as trap distribution, conductivity and the like and improve the charge accumulation behavior and the flashover strength. However, multifunctional coatings having superior surface insulating strength and superhydrophobicity while being suitable for indoor and outdoor devices have been rarely reported.
Creating artificial superhydrophobic surfaces and exploring their applications of waterproofing, anti-icing, self-cleaning, dust removal, etc. have become the leading edge of research. Changing the surface micro-nano structure or surface free energy is the main method to create superhydrophobic surfaces, e.g. by applying photolithography, etching, templating, chemical vapor deposition, solvent gel and surface coating methods. Among these methods, surface coating is a convenient method for easily producing a superhydrophobic surface. However, the current surface coating methods have the following drawbacks: the performance is single.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a dielectric multifunctional nano coating and a preparation method and application thereof.
A preparation method of a dielectric multifunctional nano coating comprises the following steps:
(1) weighing 1.88g of PDMS prepolymer, placing the PDMS prepolymer in 80mL of n-hexane, and electrically stirring at the room temperature at the speed of 500rad/min to form a uniform solution;
(2) weighing nano particles and MWCNTs in a certain mass percentage, placing the nano particles and the MWCNTs in the solution obtained in the step (1), stirring at normal temperature, and carrying out ultrasonic treatment for a certain time to finally form a suspension;
(3) adding 0.19g of PDMS curing agent into the solution, and continuing to perform ultrasonic treatment for a period of time;
(4) selecting a substrate, pretreating the surface by 1000Cw of grinding paper to improve the adhesive strength, and wiping the surface by using alcohol to clean the surface;
(5) and spraying a nano coating: spraying the solution prepared in step (3) onto the substrate;
(6) curing the coated sample in a vacuum oven at 100 ℃ for 4 hours;
(7) and (3) changing the mass percentage of the nanoparticles in the step (2), and repeating the steps (1) to (6) to prepare the required nano coating with each concentration gradient.
Further, in the above-mentioned method, the stirring rate in the step (2) is 500 rad/min; stirring for 10 min; the ultrasonic treatment frequency is 40kHz, and the time is 20 min; the ultrasonic treatment frequency in the step (3) is 40 kHz; the time is 10 min.
Further, in the method described above, the matrix is epoxy resin, silicone rubber, nylon, polymethyl methacrylate, polytetrafluoroethylene, or insulating paper.
Further, in the method as described above, the conditions for spraying in the step (5) are: the pressure of the spray gun is 40psi, the distance between the substrate and the spray gun is 150mm, the spraying angle is 90 degrees, and the size and the flow of the needle head of the spraying device are respectively 0.3mm and 10 mL/min; the spraying time was 60 s.
Further, in the method as described above, the nanoparticles in the step (2) are zinc oxide, silicon dioxide or barium titanate; the size of the nanometer particle is not more than 100 nm.
Further, as described above, when the nanoparticles are SiO2When the mass percent of the prepolymer is 15-60% of that of the PDMS prepolymer in the step (1); when the nano-particles are ZnO or BaTiO3When the mass percent of the prepolymer is 25-150% with the mass percent of the PDMS prepolymer in the step (1); the mass percentage ranges of the MWCNTs and the PDMS prepolymer in the step (1) are as follows: 0.5 to 2.1 percent.
The dielectric multifunctional nanocoating prepared according to any one of the methods described above.
The dielectric multifunctional nano coating is applied to outdoor high-voltage power equipment.
Has the advantages that:
1. the coating prepared by the method can be widely applied to various insulating base materials.
2. The coating prepared by the method can simultaneously improve various properties: direct current surface flashover strength, super-hydrophobic surface, self-cleaning capability, anti-icing performance and the like.
3. The preparation process is simple, the spraying application is convenient, and the method is suitable for large-scale production and application.
4. The preparation process is short in time, and the achievement is quick.
The principle of improving the direct current surface flashover voltage is as follows: the nano filler has different electron transition energy levels, and the nano coating can form surface charge traps; for example, shallow traps formed by ZnO nanoparticles are beneficial to accelerating the dissipation of surface charges, so that the charges between the discharge electrodes are difficult to form a discharge channel, and the flashover voltage is further improved. Secondly, in the coating solution spraying process, a large number of micron-nanometer convex structures are formed on the surface of the coating, and in the flashover forming process, the charge movement further hinders the formation of a discharge channel due to the blocking effect of the convex structures, so that the flashover voltage is increased.
The reasons for improving the super-hydrophobic surface, self-cleaning and anti-icing performance are as follows: after the nano filler is sprayed on the coating material, a layer of compact micron-nanometer multi-scale convex structure is formed on the surface of the material, and the small protrusions reduce the contact area between water drops and the surface, so that the water contact angle is increased, and the super-hydrophobic performance requirement is gradually met. The self-cleaning performance and the anti-icing performance are both caused by the super-hydrophobic performance, water drops are not easy to stay on the surface of the material, dirt on the surface of the material can be taken away when the water drops roll off, and the self-cleaning effect is achieved. The anti-icing is caused by the fact that the contact area of the water drops on the super-hydrophobic surface and the material is small, and the temperature conduction efficiency is reduced. The freezing rate becomes slow.
Drawings
FIG. 1 is a flow chart for preparing a nano-insulation coating;
FIG. 2 is a graph comparing the flashover voltage of pure Epoxy (EP) and ZnO nanocoating, using as an example the nanocoating material prepared in example 3;
FIG. 3 is a comparative graph of the superhydrophobic performance test of the ZnO nano-coating, taking the nano-insulating coating material prepared in example 3 as an example;
FIG. 4 shows SiO, which is an example of the nano-insulation coating material prepared in example 12The self-cleaning performance test of the/MWCNTs nano coating is compared with a figure.
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 below clearly and completely, 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 utilizes multi-wall carbon nanotubes (MWCNTs) dispersed in Polydimethylsiloxane (PDMS) elastomer solution to prepare a multifunctional nano coating based on a combined polymer and nano filler. The nano filler coating has multiple functions, including accelerating charge dissipation by introducing surface shallow traps and enhancing surface conductivity to form a micro-nano scale layered surface structure. Therefore, the coating enables an insulating substrate and the like to have high direct current flashover strength, a super-hydrophobic surface, self-cleaning capability, good wear resistance, ultraviolet resistance and anti-icing performance. The nano-filler coating is very suitable for surface modification of dielectrics in indoor and outdoor high-voltage direct-current insulation systems. The method provides a new idea for simultaneously improving various surface properties of dielectric insulation.
As shown in fig. 1, a dielectric multifunctional nanocoating is prepared according to the procedure in fig. 1. 1.88g of PDMS prepolymer was electrically stirred in 80mL of n-hexane at room temperature at 500rad/min to form a homogeneous solution, and then dispersed and a certain amount of nanofiller was stirred and sonicated to form a suspension. Then, 0.19g of PDMS curing agent was added to the solution. The prepared solution was coated on a selected substrate (epoxy resin, silicone rubber, nylon, polymethylmethacrylate, polytetrafluoroethylene, and insulating paper) by a spray method, in which the surface of the substrate was pretreated with abrasive paper (1000Cw) to increase adhesive strength, and the surface was cleaned with alcohol wiping. The spray pressure (40psi), the distance between the substrate and the spray gun (about 150mm) and the spray angle (about 90 °) to balance the solvent evaporation time of the spray process. The needle size and flow rate of the spray device were 0.3mm and 10mL/min, respectively. The spraying time was selected to be 60 s. The coated samples were then cured in a vacuum oven at 100 ℃ for 4 hours.
The PDMS prepolymer is Polydimethylsiloxane (PDMS), and the raw material grade is as follows: analytically pure, raw material manufacturer: shanghai Kangning Co., Ltd. The curing agent of the PDMS is a matching product purchased by purchasing PDMS prepolymer.
Wherein the nanofiller typically has a particle size of no greater than 100 nm; the concentration of the nano particles is preferably different from that of the filler, and the nano particles are sprayed on the surface of the base material to form a compact nano coating. The mass ratio of nanoparticles to PDMS prepolymer is typically in the range: 15 to 150 percent.
According to the invention, by comprehensively considering a multi-aspect performance improvement mechanism and selecting a proper nano filler, the multi-aspect performances of direct-current surface flashover voltage, super-hydrophobicity, self-cleaning, ice coating prevention and the like of the insulating material are improved simultaneously; the coating can be prepared by spraying and drying the coating solution, and the preparation process is simple and convenient to implement.
The flashover voltage of the sample is tested, and finger electrodes are adopted for the fixing of the sample and the flashover voltage test of the coating surface. The distance between the two terminals is adjusted to be 10mm, and the experiment is carried out under the atmospheric condition. Wiping the surface of the sample with alcohol, fixing the sample on a support table after the sample is dried, and placing the support table on an insulating plate. Application of 1kVs was programmed using a positive polarity DC voltage-1The voltage is ramped up until flashover occurs, the flashover voltage value is recorded and the coating is repeated 15 times for different filler contents. The analysis of flashover intensity typically employs a framework of two-parameter weber statistics. The distribution rule of the flashover voltage can be embodied by the flashover voltage Weber distribution diagram. Because the distances between two terminals of the finger-shaped electrode are the same, the size of the abscissa in the distribution diagram can indicate the flashover voltage of the surface of the coating. Meanwhile, the slope of the fitted straight line can indicate the distribution condition of flashover voltage in the test process, and the distribution is more concentrated when the slope is larger. Taking the insulating coating prepared by ZnO nanoparticles and PDMS as an example, the sample was tested for flashover voltage, and the test results are shown in FIG. 2. Wherein the flashover voltage of the pure epoxy resin (EP) is 17.7kV, after the coating is added, the flashover voltage is gradually increased along with the increase of the concentration of the nano particles, when r isZnOWhen the voltage is 150%, the flashover voltage reaches 28.9kV, and is increased by 63%.
The water contact angle of the sample was tested using an experimental platform. The contact angle is an angle formed when a water droplet of about 5. mu.L is dropped on a horizontal surface of a material and two tangent lines of a gas-liquid interface and a liquid-solid interface are sandwiched between the two tangent lines at a solid-liquid-gas three-phase boundary on the surface of the material. The hydrophobic property of the surface of the coating is explored by using a JC2000 type contact angle measuring instrument, and a liquid drop image is collected and analyzed by combining a computer, an optical system and a CCD camera. And (3) dripping a proper amount of liquid by using a needle tube of the instrument, adjusting the angle and brightness of a lens, and collecting and storing the specimen. Taking the insulating coating prepared by ZnO nanoparticles and PDMS as an example, the water contact angle of the sample is tested, and the test result is shown in FIG. 3. The water contact angle gradually increases with the increase of the concentration of the nano-particles, when r isZnOWhen the water contact angle is 150 percent, the water contact angle reaches 152 degrees, and the requirement that the super-hydrophobic CA is more than 150 degrees is met.
To SiO2Insulating coating prepared from nano particles, MWCNTs and PDMS, and test sampleSelf-cleaning capability of. Spreading sand on the surface of the coating simulates the surface fouling of the insulator, and water drops can easily roll off the super-hydrophobic surface at an inclination angle of about 5 degrees while carrying away the sand deposited on the surface. The test results are shown in fig. 4.
Example 1:
as shown in fig. 1, the present embodiment includes the following steps:
(1) weighing 1.88g of PDMS prepolymer, and electrically stirring the PDMS prepolymer in 80mL of n-hexane at room temperature of 500rad/min to form a uniform solution;
(2) weighing 0.28g (r)SiO2＝15％)SiO2Nanoparticles and 0.01g (r)CNT0.5%) MWCNTs, placed in the solution of step (1), and formed into a suspension by stirring at 500rad/min for 10min and sonication at 40kHz frequency for 20min at room temperature. Wherein r isSiO2And rCNTRespectively represent SiO2Nanoparticles and the mass ratio of MWCNTs to PDMS prepolymer.
(3) 0.19g of PDMS curing agent was added to the solution and sonication was continued at 40kHz for 10 min.
(4) The epoxy resin was selected as the substrate, the surface was pretreated with abrasive paper (1000Cw) to increase the adhesive strength, and the surface was cleaned with alcohol wiping.
(5) And spraying a nano coating: the spray gun pressure was 40psi, the distance between the substrate and the spray gun was 150mm and the spray angle was 90 deg., balancing the solvent evaporation time of the spray process. The needle size and flow rate of the spray device were 0.3mm and 10mL/min, respectively. The spraying time was selected to be 60 s.
(6) The coated sample was cured in a vacuum oven at 100 ℃ for 4 hours.
(7) Repeating the steps 1-6, and adding r in the step 2SiO2And rCNTRespectively setting as follows: 15%, 30%, 45%, 60% and 0.5%, 1.1%, 1.6%, 2.1%, four concentration gradient coatings were prepared.
Example 2:
the embodiment comprises the following steps:
(1) weighing 1.88g of PDMS prepolymer, and electrically stirring the PDMS prepolymer in 80mL of n-hexane at room temperature of 500rad/min to form a uniform solution;
(2) weighing 0.47g (r)ZnO25%) ZnO nanoparticles and 0.01g (r)CNT0.5%) MWCNTs, placed in the solution of step 1, and formed into a suspension by stirring at 500rad/min for 10min at room temperature and sonicating at 40kHz for 20 min.
(3) 0.19g of PDMS curing agent was added to the solution and sonication was continued at 40kHz for 10 min.
(4) The epoxy resin was selected as the substrate, the surface was pretreated with abrasive paper (1000Cw) to increase the adhesive strength, and the surface was cleaned with alcohol wiping.
(5) And spraying a nano coating: the spray gun pressure was 40psi, the distance between the substrate and the spray gun was 150mm and the spray angle was 90 deg., balancing the solvent evaporation time of the spray process. The needle size and flow rate of the spray device were 0.3mm and 10mL/min, respectively. The spraying time was selected to be 60 s.
(6) The coated sample was cured in a vacuum oven at 100 ℃ for 4 hours.
(7) Repeating the steps 1-6, and adding r in the step 2ZnOAnd rCNTRespectively setting as follows: 25%, 50%, 75%, 100% and 0.5%, 1.1%, 1.6%, 2.1%, four concentration gradient coatings were prepared.
Example 3:
the embodiment comprises the following steps:
(1) weighing 1.88g of PDMS prepolymer, and electrically stirring the PDMS prepolymer in 80mL of n-hexane at room temperature of 500rad/min to form a uniform solution;
(2) weighing 0.47g (r)ZnO25%) ZnO nanoparticles, placed in the solution of step 1, and formed into a suspension by stirring at 500rad/min for 10min at room temperature and sonicating at 40kHz frequency for 20 min.
(3) 0.19g of PDMS curing agent was added to the solution and sonication was continued at 40kHz for 10 min.
(4) The epoxy resin was selected as the substrate, the surface was pretreated with abrasive paper (1000Cw) to increase the adhesive strength, and the surface was cleaned with alcohol wiping.
(5) And spraying a nano coating: the spray gun pressure was 40psi, the distance between the substrate and the spray gun was 150mm and the spray angle was 90 deg., balancing the solvent evaporation time of the spray process. The needle size and flow rate of the spray device were 0.3mm and 10mL/min, respectively. The spraying time was selected to be 60 s.
(6) The coated sample was cured in a vacuum oven at 100 ℃ for 4 hours.
(7) Repeating the steps 1-6, and adding r in the step 2ZnOThe method comprises the following steps: 25%, 50%, 75%, 100%, 150%, preparing five concentration gradient coatings.
Example 4:
the embodiment comprises the following steps:
(1) weighing 1.88g of PDMS prepolymer, and electrically stirring the PDMS prepolymer in 80mL of n-hexane at room temperature of 500rad/min to form a uniform solution;
(2) weighing 0.47g (r)BaTiO3＝25％)BaTiO3Nanoparticles were placed in the solution of step 1 and suspended by stirring at 500rad/min for 10min and sonication at 40kHz for 20min at room temperature.
(3) 0.19g of PDMS curing agent was added to the solution and sonication was continued at 40kHz for 10 min.
(4) The epoxy resin was selected as the substrate, the surface was pretreated with abrasive paper (1000Cw) to increase the adhesive strength, and the surface was cleaned with alcohol wiping.
(5) And spraying a nano coating: the spray gun pressure was 40psi, the distance between the substrate and the spray gun was 150mm and the spray angle was 90 deg., balancing the solvent evaporation time of the spray process. The needle size and flow rate of the spray device were 0.3mm and 10mL/min, respectively. The spraying time was selected to be 60 s.
(6) The coated sample was cured in a vacuum oven at 100 ℃ for 4 hours.
(7) Repeating the steps 1-6, and adding r in the step 2BaTiO3The method comprises the following steps: 25%, 50%, 75% and 100%, and preparing four concentration gradient coatings.
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 (8)
1. A preparation method of a dielectric multifunctional nano coating is characterized by comprising the following steps:
(1) weighing 1.88g of PDMS prepolymer, placing the PDMS prepolymer in 80mL of n-hexane, and electrically stirring at the room temperature at the speed of 500rad/min to form a uniform solution;
(2) weighing nano particles and MWCNTs in a certain mass percentage, placing the nano particles and the MWCNTs in the solution obtained in the step (1), stirring at normal temperature, and carrying out ultrasonic treatment for a certain time to finally form a suspension;
(3) adding 0.19g of PDMS curing agent into the solution, and continuing to perform ultrasonic treatment for a period of time;
(4) selecting a substrate, pretreating the surface by 1000Cw of grinding paper to improve the adhesive strength, and wiping the surface by using alcohol to clean the surface;
(5) and spraying a nano coating: spraying the solution prepared in step (3) onto the substrate;
(6) curing the coated sample in a vacuum oven at 100 ℃ for 4 hours;
(7) and (3) changing the mass percentage of the nanoparticles in the step (2), and repeating the steps (1) to (6) to prepare the required nano coating with each concentration gradient.
2. The method according to claim 1, wherein the stirring rate in step (2) is 500 rad/min; stirring for 10 min; the ultrasonic treatment frequency is 40kHz, and the time is 20 min; the ultrasonic treatment frequency in the step (3) is 40 kHz; the time is 10 min.
3. The method of claim 1, wherein the matrix is epoxy, silicone rubber, nylon, polymethylmethacrylate, polytetrafluoroethylene, or insulating paper.
4. The method according to claim 1, wherein the conditions for spraying in step (5) are: the pressure of the spray gun is 40psi, the distance between the substrate and the spray gun is 150mm, the spraying angle is 90 degrees, and the size and the flow of the needle head of the spraying device are respectively 0.3mm and 10 mL/min; the spraying time was 60 s.
5. The method according to claim 1, wherein the nanoparticles in step (2) are zinc oxide, silica or barium titanate; the size of the nanometer particle is not more than 100 nm.
6. The method of claim 5, wherein the nanoparticles are SiO2When the mass percent of the prepolymer is 15-60% of that of the PDMS prepolymer in the step (1); when the nano-particles are ZnO or BaTiO3When the mass percent of the prepolymer is 25-150% with the mass percent of the PDMS prepolymer in the step (1); the mass percentage ranges of the MWCNTs and the PDMS prepolymer in the step (1) are as follows: 0.5 to 2.1 percent.
7. The dielectric multifunctional nanocoating prepared according to any one of claims 1-6.
8. Use of the dielectric multifunctional nanocoating of claim 7 in outdoor high voltage power equipment.
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