CN111180147B - Ceramic insulator with microgrooves and self-assembled molecular film on surface and preparation method thereof - Google Patents

Ceramic insulator with microgrooves and self-assembled molecular film on surface and preparation method thereof Download PDF

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CN111180147B
CN111180147B CN202010005204.XA CN202010005204A CN111180147B CN 111180147 B CN111180147 B CN 111180147B CN 202010005204 A CN202010005204 A CN 202010005204A CN 111180147 B CN111180147 B CN 111180147B
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insulator
ceramic insulator
groove
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CN111180147A (en
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霍艳坤
刘文元
柯昌凤
陈昌华
程军
郭跃文
唐运生
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Northwest Institute of Nuclear Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B17/00Insulators or insulating bodies characterised by their form
    • H01B17/50Insulators or insulating bodies characterised by their form with surfaces specially treated for preserving insulating properties, e.g. for protection against moisture, dirt, or the like
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B17/00Insulators or insulating bodies characterised by their form
    • H01B17/42Means for obtaining improved distribution of voltage; Protection against arc discharges
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B19/00Apparatus or processes specially adapted for manufacturing insulators or insulating bodies
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B19/00Apparatus or processes specially adapted for manufacturing insulators or insulating bodies
    • H01B19/04Treating the surfaces, e.g. applying coatings

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Abstract

The invention relates to a ceramic insulator and a preparation method thereof, in particular to a ceramic insulator with a micro-groove and a self-assembled molecular membrane on the surface and a preparation method thereof, which solve the problems that the existing methods for modifying the surface of the ceramic insulator are single, the improvement effect of the flashover voltage on the vacuum surface is not obvious, the stability is poor and the ceramic insulator is difficult to put into practical application. The insulator is characterized in that: the surface of the ceramic insulator body is provided with a periodical and mutually parallel ten-micron-sized micro-groove array; the central axis of each micro-groove in the micro-groove array is vertical to the direction of the electric field; the array direction of the micro-groove array is parallel to the direction of the electric field; the microgrooves are made by laser etching; the surfaces of the ceramic insulator body and the micro-groove are covered with self-assembled molecular films; the self-assembly molecular membrane is a protective membrane generated by placing the ceramic insulator body in a silane coupling agent hydrolysis solution and standing still. The invention also provides a preparation method of the ceramic insulator with the microgrooves and the self-assembled molecular film on the surface.

Description

Ceramic insulator with microgrooves and self-assembled molecular film on surface and preparation method thereof
Technical Field
The invention relates to a ceramic insulator and a preparation method thereof, in particular to a ceramic insulator with a micro-groove and a self-assembled molecular film on the surface and a preparation method thereof.
Background
When the insulator is subjected to vacuum insulation, the phase and vacuum insulation strength of the insulator body is generally higher, and the insulation requirement under most conditions can be met; however, at the interface between the two, due to the existence of the Flashover phenomenon, the breakdown voltage along the Surface is lower and the dielectric strength is not as high as one tenth of the breakdown voltage of the insulator phase and the Vacuum, which severely limits the dielectric strength and the operation stability of the Vacuum high voltage equipment [ Li S, Nie Y, Min D, et al research development on Vacuum Surface flash of Solid Dielectrics [ J ]. transformations of Chinese electronic society.2017,32(8):1-9 ].
The ceramic insulator has higher surface secondary electron emission coefficient and lower surface compressive strength, so that the application requirement is difficult to meet; in vacuum high voltage equipment, polymer insulators are generally adopted, but the polymer insulators have relatively short insulation life due to the reasons of easy aging, easy ablation on the surface and the like. Therefore, the surface of the ceramic insulator is modified, and the improvement of the vacuum surface flashover voltage of the insulator has a high application value.
In order to improve the vacuum surface voltage resistance level of the ceramic insulator, Sudarshan et al prepared a layer of Cu with low secondary electron emission coefficient on the surface of the alumina ceramic material2O and Cr2O3The metal Oxide coating reduces the Surface secondary electron emission coefficient, so that the Flashover voltage of the Vacuum Surface of the ceramic insulator is improved to a certain extent, but the problem that the coating is easy to fall off and the like is faced [ Cross J D, Sudarshan T S].IEEE Transactions on Electrical Insulation.2007,EI-9(4):146-150.]. Put forward Cu in Kaikun et al2O and Cr2O3The metal oxide is doped in a processable alumina ceramic body to reduce the surface secondary electron emission coefficient, so that the vacuum surface flashover voltage of the insulator made of the material is improved to a certain degree [ in Kaikun, Zhangguanjun, Tianjie, and the like]The electrotechnical journal 2011,26(1):23-28.](ii) a Meanwhile, CO2 laser scribing treatment is carried out on the surface of the alumina ceramic insulator to obtain discontinuous etching lines, so that the vacuum surface flashover voltage can be improved to a certain degree [ open Kun, Zhangguanjun, Zhengnan, and the like]The electrotechnical journal 2009,24(1):28-34.]。
However, the existing methods for modifying the surface of the ceramic insulator are single, the vacuum surface flashover voltage improvement effect is not obvious, the stability is poor, and the method is difficult to put into practical application.
Disclosure of Invention
The invention aims to provide a ceramic insulator with microgrooves and a self-assembled molecular film on the surface and a preparation method thereof, and aims to solve the technical problems that the existing methods for modifying the surface of the ceramic insulator are single, the vacuum surface flashover voltage lifting effect is not obvious, the stability is poor, and the ceramic insulator is difficult to put into practical application.
The technical scheme adopted by the invention is that the ceramic insulator with the surface provided with the microgrooves and the self-assembled molecular film comprises a ceramic insulator body; it is characterized in that:
the surface of the ceramic insulator body is provided with a periodical and mutually parallel ten-micron-sized micro-groove array; the central axis of each micro-groove in the micro-groove array is vertical to the direction of the electric field; the array direction of the micro-groove array is parallel to the direction of the electric field; the micro-grooves are formed by laser etching;
self-assembled molecular films cover the surface of the ceramic insulator body and the surface of the micro-groove; the self-assembly molecular membrane is a layer of protective membrane generated after the ceramic insulator body is placed in a silane coupling agent hydrolysis solution for standing and molecular self-assembly reaction.
Further, in order to ensure that the self-assembled molecular film covered on the surface of the ceramic insulator has good adhesion performance and is not easy to fall off, the silane coupling agent hydrolysis solution is prepared by uniformly mixing and stirring a silane coupling agent, an organic solvent and deionized water according to the volume ratio of 1:20: 1-1: 500:1 and then hydrolyzing for 0.1-10 hours at room temperature;
the silane coupling agent is a bipolar molecule capable of being hydrolyzed, one end of the hydrolyzed silane coupling agent is polar silanol, and the other end of the hydrolyzed silane coupling agent is a nonpolar hydrocarbon chain.
Further, the silane coupling agent is KH-570, KH-550 or octadecyltrichlorosilane;
the organic solvent is toluene, acetone or absolute ethyl alcohol.
Further, the micro grooves have a V-shape, a width of 20 to 100 μm, a depth of 20 to 300 μm, and a period of 20 to 500 μm.
Further, the ceramic insulator body is made of alumina ceramic or silicate ceramic.
Meanwhile, the invention also provides a preparation method of the ceramic insulator with the microgrooves and the self-assembled molecular film on the surface, which is characterized by comprising the following steps:
step 1: processing a corresponding insulator original shape according to the size requirement of the ceramic insulator with the surface provided with the microgrooves and the self-assembled molecular film to be prepared;
step 2: opening a laser, and setting laser parameters according to the width, depth and cycle size of a micro groove required to be processed on the surface of the ceramic insulator with the micro groove and the self-assembled molecular film on the surface to be prepared; etching a microgroove on the surface of the insulator original sample processed in the step 1 through laser etching;
and step 3: ultrasonically cleaning the insulator original shape with a dilute acid solution after the microgrooves are etched on the surface in the step 2 to remove residual ceramic particles on the surface, cleaning the insulator original shape with deionized water, and drying the insulator original shape;
and 4, step 4: weighing a silane coupling agent, an organic solvent and deionized water according to a volume ratio of 1:20: 1-1: 500:1, mixing and stirring the silane coupling agent, the organic solvent and the deionized water uniformly, and hydrolyzing for 0.1-10 hours at room temperature to prepare a silane coupling agent hydrolysis solution;
and 5: placing the insulator with the micro grooves etched on the surface, dried in the step 3, in the silane coupling agent hydrolysis solution prepared in the step 4 for standing, and performing molecular self-assembly reaction for 12-36 hours;
step 6: sequentially carrying out ultrasonic cleaning on the insulator original sample subjected to the molecular self-assembly reaction in the step 5 by using ethanol and water, removing residues on the surface, and carrying out vacuum drying treatment at 50-70 ℃;
and 7: and (3) heating to 100-150 ℃, and carrying out high-temperature reaction on the insulator subjected to vacuum drying in the step (6) to obtain the ceramic insulator with the microgrooves and the self-assembled molecular film on the surface.
Further, in order to ensure that the self-assembled molecular film covered on the surface of the ceramic insulator has good adhesion performance and is not easy to fall off, in the step 3, the silane coupling agent is KH-570, KH-550 or octadecyl trichlorosilane; the organic solvent is toluene, acetone or absolute ethyl alcohol.
Further, in step 2, the micro grooves have a V-shape, a width of 20 to 100 μm, a depth of 20 to 300 μm, and a period of 20 to 500 μm.
Further, since the ceramic has a high hardness and is difficult to machine the micro-grooves, in step 2, the laser is an ultraviolet laser or a fiber laser.
Further, in step 1, the insulator is made of alumina ceramic or silicate ceramic.
The invention has the beneficial effects that:
(1) according to the invention, the micro-grooves are etched by using laser and then the molecular self-assembly reaction is carried out, structurally, secondary electron emission can be inhibited through the micro-groove array, and in terms of components, the ceramic surface with high secondary electron emission coefficient is replaced by the self-assembly molecular film, so that the secondary electron emission coefficient is reduced, and the double inhibition of the secondary electron emission coefficient on the surface of the ceramic insulator from the structure and the components is realized, therefore, the effect of improving the vacuum edge pressure strength of the insulator is obvious; in addition, the self-assembled molecular film covered on the surface of the ceramic insulator through the molecular self-assembly reaction has good adhesion performance and is not easy to fall off, so that the stability of the vacuum surface flashover voltage of the ceramic insulator is good; therefore, the invention solves the technical problems that the existing methods for modifying the surface of the ceramic insulator are single, the improvement effect of the flashover voltage of the vacuum surface is not obvious, the stability is poor and the method is difficult to put into practical application.
(2) According to the invention, the preferable silane coupling agent is a bipolar molecule capable of being hydrolyzed, one end of the hydrolyzed silane coupling agent is polar silanol, and the other end of the hydrolyzed silane coupling agent is a nonpolar hydrocarbon chain; thus, the polar end of the bipolar molecule is combined with the polar substrate, and the tails of the nonpolar hydrocarbon chains are mutually combined and arranged in order through Van der Waals force; during high-temperature treatment, silanol generated by hydrolysis and hydroxyl on the surface of a polar substrate are subjected to high-temperature etherification to generate chemical bonds, and the combination stability of self-assembly molecules and the substrate is enhanced, so that the self-assembly molecular film has good adhesion performance on the surface of the ceramic insulator and is not easy to fall off, and further, the vacuum edgewise flashover voltage of the ceramic insulator with the surface covered with the self-assembly molecular film has good stability.
(3) The invention only modifies the surface structure and components of the ceramic insulator, does not relate to the characteristics of the ceramic insulator body, can ensure that the mechanical properties such as strength, toughness and the like of the processed insulator are not changed, and has simple and easy operation and wide application range.
(4) The micro-groove is prepared by laser non-contact processing, the molecular membrane is prepared by self-assembly of molecules in the solution, and the two modes have lower requirements on the geometric appearance of the ceramic insulator and are suitable for insulators with most geometric shapes; and the experimental conditions are mild, mechanical extrusion and other stress processing are avoided, and the success rate of the insulator preparation is high.
(5) The invention realizes strong inhibition on flashover development by double inhibition of the surface structure and the components to secondary electrons, so that the surface insulation strength of the modified ceramic insulator is improved by 154-225 percent compared with that of the unmodified insulator.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment of a ceramic insulator with micro-grooves and a self-assembled molecular film on the surface according to the present invention;
FIG. 2 is a flow chart of a method for preparing a ceramic insulator having micro-grooves and a self-assembled molecular film on the surface thereof according to the present invention;
fig. 3 is a schematic view of the surface morphology of an original ceramic insulator and the surface morphology of the ceramic insulator in the process of preparing the ceramic insulator with the micro-grooves and the self-assembled molecular film on the surface, wherein:
(a) the surface appearance of the ceramic insulator is the original surface appearance of the ceramic insulator;
(b) the surface appearance of the ceramic insulator after the micro-groove is processed;
(c) ultrasonic cleaning is carried out on the insulator original shape with the surface etched with the microgrooves by dilute acid solution to remove residual ceramic particles on the surface, and the surface appearance of the ceramic insulator is cleaned by deionized water;
(d) the surface appearance of the ceramic insulator is provided with micro-grooves and a self-assembled molecular film on the surface;
FIG. 4 is a schematic diagram of the mechanism of suppressing secondary electron emission on the surface of a ceramic insulator with micro-grooves and a self-assembled molecular film on the surface.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Referring to fig. 1, the ceramic insulator with the surface having the micro-grooves and the self-assembled molecular film of the present invention includes a ceramic insulator body; the surface of the ceramic insulator body is provided with a periodical and mutually parallel ten-micron-sized micro-groove array; the central axis of each micro-groove in the micro-groove array is vertical to the direction of the electric field; the array direction of the micro-groove array is parallel to the direction of the electric field; the microgrooves are made by laser etching; the surface of the ceramic insulator body and the surface of the micro-groove are covered with self-assembled molecular films; the self-assembly molecular membrane is a layer of protective membrane generated after the ceramic insulator body is placed in a silane coupling agent hydrolysis solution for standing and molecular self-assembly reaction.
The silane coupling agent hydrolysis solution is prepared by mixing and stirring a silane coupling agent, an organic solvent and deionized water uniformly according to the volume ratio of 1:20: 1-1: 500:1, and hydrolyzing at room temperature for 0.1-10 hours; the silane coupling agent is a bipolar molecule capable of being hydrolyzed, one end of the hydrolyzed silane coupling agent is silanol with polarity, and the other end of the hydrolyzed silane coupling agent is a nonpolar hydrocarbon chain; the silane coupling agent may be KH-570 (Y-methacryloxypropyltrimethoxysilane), KH-550 (Y-aminopropyltriethoxysilane), or octadecyltrichlorosilane, or other bipolar molecule capable of hydrolysis. The organic solvent is toluene, acetone or absolute ethyl alcohol, or other solvents, the organic solvent mainly has the function of dissolving the bipolar molecules, and the deionized water molecules react with one polar end of the bipolar molecules to generate silanol. The shape of the micro grooves is preferably V-shaped, and the width of the grooves is 20 to 100 μm, the depth of the grooves is 20 to 300 μm, and the period of the grooves is 20 to 500 μm. The material of the ceramic insulator body is preferably alumina ceramic or silicate ceramic, and may be other ceramics.
Referring to fig. 2, the present invention further provides a method for preparing the ceramic insulator having the micro-grooves and the self-assembled molecular film on the surface, comprising the following steps:
step 1: processing a corresponding insulator original shape according to the size requirement of the ceramic insulator with the surface provided with the microgrooves and the self-assembled molecular film to be prepared; the surface topography of the insulator as it is, see fig. 3 (a);
step 2: opening a laser, and setting laser parameters according to the width, depth and cycle size of a micro groove required to be processed on the surface of the ceramic insulator with the micro groove and the self-assembled molecular film on the surface to be prepared; etching a microgroove on the surface of the insulator original sample processed in the step 1 through laser etching; the surface appearance of the ceramic insulator after the micro-grooves are etched is shown in fig. 3 (b);
and step 3: ultrasonically cleaning the insulator original shape with a dilute acid solution after the microgrooves are etched on the surface in the step 2 to remove residual ceramic particles on the surface, cleaning the insulator original shape with deionized water, and drying the insulator original shape; at this time, the surface morphology of the ceramic insulator is shown in fig. 3 (c);
and 4, step 4: weighing a silane coupling agent, an organic solvent and deionized water according to a volume ratio of 1:20: 1-1: 500:1, mixing and stirring the silane coupling agent, the organic solvent and the deionized water uniformly, and hydrolyzing for 0.1-10 hours at room temperature to prepare a silane coupling agent hydrolysis solution;
and 5: placing the insulator with the micro grooves etched on the surface, dried in the step 3, in the silane coupling agent hydrolysis solution prepared in the step 4 for standing, and performing molecular self-assembly reaction for 12-36 hours;
step 6: sequentially carrying out ultrasonic cleaning on the insulator original sample subjected to the molecular self-assembly reaction in the step 5 by using ethanol and water, removing residues on the surface, and carrying out vacuum drying treatment at 50-70 ℃;
and 7: and (3) heating to 100-150 ℃, and carrying out high-temperature reaction on the insulator subjected to vacuum drying in the step (6) to obtain the ceramic insulator with the microgrooves and the self-assembled molecular film on the surface. At this time, the surface morphology of the ceramic insulator is shown in fig. 3 (d).
In step 1, the insulator is preferably made of alumina ceramic or silicate ceramic. In the above step 2, the shape of the micro grooves is preferably V-shaped, and the width of the micro grooves is 20 μm to 100 μm, the depth of the micro grooves is 20 μm to 300 μm, and the period of the micro grooves is 20 μm to 500 μm; the laser is preferably an ultraviolet laser or a fiber laser; the laser parameters comprise laser energy, scribing density and laser spot size; according to the width, the depth and the cycle size of a micro groove required to be processed on the surface of a ceramic insulator with the micro groove and a self-assembled molecular film on the surface to be prepared, when laser parameters are set, the wider the width requirement of the micro groove is, the larger the laser spot is; the deeper the depth requirement of the microgrooves is, the higher the laser energy setting is; the smaller the requirement for the period value of the microgrooves, the greater the reticle density setting. In step 3, the silane coupling agent is preferably KH-570, KH-550 or octadecyltrichlorosilane, and may be other silane coupling agents; the organic solvent is toluene, acetone or absolute ethyl alcohol, and can also be other organic solvents.
The following three embodiments of the ceramic insulator with the surface provided with the microgrooves and the self-assembled molecular film are prepared by adopting the preparation method:
example 1:
(1) processing a cylindrical alumina ceramic insulator with the diameter of 30mm and the thickness of 10 mm;
(2) opening an ultraviolet laser, setting laser parameters, and etching a microgroove with the width of 20 microns, the depth of 20 microns and the period of 20 microns on the surface of the insulator original sample processed in the step 1 through laser etching;
(3) carrying out ultrasonic cleaning on the insulator original sample with the surface etched with the microgrooves for 30mins by using a dilute hydrochloric acid solution with the concentration of 5% by mass, removing residual ceramic particles on the surface, cleaning the insulator original sample with deionized water, and drying the insulator original sample in an oven at 80 ℃ for 12 hours;
(4) weighing Octadecyltrichlorosilane (OTS), toluene and deionized water according to the volume ratio of 1:20:1, mixing and stirring the weighed materials uniformly to prepare a toluene solution of the OTS, and hydrolyzing at room temperature for 0.1 hour to prepare a toluene hydrolysis solution of the OTS;
(5) placing the insulator with the micro grooves etched on the surface, dried in the step 3, in the OTS toluene hydrolysis solution prepared in the step 4 for standing, and carrying out molecular self-assembly reaction for 12 hours;
(6) sequentially carrying out ultrasonic cleaning on the insulator original sample subjected to the molecular self-assembly reaction by adopting methylbenzene, ethanol and water, removing residues on the surface, and carrying out vacuum drying treatment at 50 ℃ for 6 hours;
(7) and (3) heating to 100 ℃, keeping the temperature for 2 hours, and carrying out high-temperature reaction on the insulator subjected to vacuum drying to obtain the ceramic insulator with the surface provided with the microgrooves and the self-assembled molecular film, which is marked as a modified insulator 1.
Example 2:
(1) processing a cylindrical alumina porcelain insulator with the diameter of 30mm and the thickness of 10 mm;
(2) opening a fiber laser, setting laser parameters, and etching a microgroove with the width of 100 microns, the depth of 300 microns and the period of 500 microns on the surface of the insulator raw sample processed in the step 1 through laser etching;
(3) carrying out ultrasonic cleaning on the insulator original sample with the surface etched with the microgrooves for 30mins by using a dilute hydrochloric acid solution with the concentration of 5% by mass, removing residual ceramic particles on the surface, cleaning the insulator original sample with deionized water, and drying the insulator original sample in an oven at 80 ℃ for 12 hours;
(4) weighing KH-550, acetone and deionized water according to the volume ratio of 1:500:1, mixing and stirring the KH-550, acetone and acetone uniformly to prepare a KH-550 acetone solution, and hydrolyzing at room temperature for 1 hour to prepare a KH-550 acetone hydrolysis solution;
(5) placing the insulator with the micro grooves etched on the surface, dried in the step 3, in the acetone hydrolysis solution of KH-550 prepared in the step 4, standing, and performing molecular self-assembly reaction for 36 hours;
(6) sequentially carrying out ultrasonic cleaning on the insulator original sample subjected to the molecular self-assembly reaction by adopting methylbenzene, ethanol and water, removing residues on the surface, and carrying out vacuum drying treatment at 70 ℃ for 6 hours;
(7) and (3) heating to 150 ℃, keeping the temperature for 2 hours, and carrying out high-temperature reaction on the insulator subjected to vacuum drying to obtain the ceramic insulator with the surface provided with the microgrooves and the self-assembled molecular film, which is marked as a modified insulator 2.
Example 3:
(1) processing a cylindrical silicate porcelain insulator with the diameter of 30mm and the thickness of 5 mm;
(2) opening an ultraviolet laser, setting laser parameters, and etching a microgroove with the width of 50 microns, the depth of 150 microns and the period of 260 microns on the original surface of the insulator processed in the step 1 through laser etching;
(3) carrying out ultrasonic cleaning on the insulator original sample with the surface etched with the microgrooves for 30mins by using a dilute hydrochloric acid solution with the concentration of 5% by mass, removing residual ceramic particles on the surface, cleaning the insulator original sample with deionized water, and drying the insulator original sample in an oven at 80 ℃ for 12 hours;
(4) weighing KH570, absolute ethyl alcohol and deionized water according to the volume ratio of 1:200:1, uniformly mixing the absolute ethyl alcohol and the deionized water, adjusting the pH of the solution to 4.5-5.5 by using acetic acid, finally adding the KH570, and hydrolyzing at room temperature for 5 hours to prepare an ethanol hydrolysis solution of the KH 570;
(5) placing the insulator with the micro grooves etched on the surface, dried in the step 3, in the ethanol hydrolysis solution of KH570 prepared in the step 4, standing, and performing molecular self-assembly reaction for 20 hours;
(6) sequentially carrying out ultrasonic cleaning on the insulator original sample subjected to the molecular self-assembly reaction by adopting ethanol and water, removing residues on the surface, and carrying out vacuum drying treatment at 60 ℃ for 6 hours;
(7) and (3) heating to 120 ℃, keeping the temperature for 2 hours, and carrying out high-temperature reaction on the insulator subjected to vacuum drying to obtain the ceramic insulator with the surface provided with the microgrooves and the self-assembled molecular film, wherein the ceramic insulator is marked as a modified insulator 3.
The modified insulators and the corresponding ceramic insulators prepared in the above examples 1 to 3 were subjected to a vacuum flashover voltage test on a vacuum pulse surface flashover test bench having a pulse width of 500ns, as they were. The flashover voltage test results are shown in table 1:
table 1: comparison table for flashover voltage of original insulator and treated insulator
Figure BDA0002355009130000091
As can be seen from table 1, the vacuum flashover voltage of the modified insulator is increased by 154% to 225% compared with the original vacuum flashover voltage of the corresponding ceramic insulator, and the surface of the ceramic insulator having the micro-grooves and the self-assembled molecular film on the surface inhibits the secondary electron emission mechanism, as shown in fig. 4, the ceramic insulator having the micro-grooves and the self-assembled molecular film on the surface can greatly increase the flashover voltage of the insulator.

Claims (10)

1. A ceramic insulator with a micro-groove and a self-assembled molecular membrane on the surface comprises a ceramic insulator body; the method is characterized in that:
the surface of the ceramic insulator body is provided with a periodical and mutually parallel ten-micron-sized micro-groove array; the central axis of each micro-groove in the micro-groove array is vertical to the direction of the electric field; the array direction of the micro-groove array is parallel to the direction of the electric field; the micro-grooves are formed by laser etching;
self-assembled molecular films cover the surface of the ceramic insulator body and the surface of the micro-groove; the self-assembly molecular membrane is a layer of protective membrane generated after the ceramic insulator body is placed in a silane coupling agent hydrolysis solution for standing and molecular self-assembly reaction.
2. The ceramic insulator with the surface provided with the micro grooves and the self-assembled molecular film according to claim 1, wherein:
the silane coupling agent hydrolysis solution is prepared by mixing and stirring a silane coupling agent, an organic solvent and deionized water uniformly according to the volume ratio of 1:20: 1-1: 500:1, and hydrolyzing at room temperature for 0.1-10 hours;
the silane coupling agent is a bipolar molecule capable of being hydrolyzed, one end of the hydrolyzed silane coupling agent is polar silanol, and the other end of the hydrolyzed silane coupling agent is a nonpolar hydrocarbon chain.
3. The ceramic insulator with the surface provided with the micro grooves and the self-assembled molecular film according to claim 2, wherein:
the silane coupling agent is KH-570, KH-550 or octadecyl trichlorosilane;
the organic solvent is toluene, acetone or absolute ethyl alcohol.
4. The ceramic insulator having the micro-grooves and the self-assembled molecular film on the surface thereof according to any one of claims 1 to 3, wherein: the micro-groove is V-shaped, the width of the micro-groove is 20-100 μm, the depth of the micro-groove is 20-300 μm, and the period of the micro-groove is 20-500 μm.
5. The ceramic insulator with the surface provided with the micro grooves and the self-assembled molecular film according to claim 4, wherein: the ceramic insulator body is made of alumina ceramic or silicate ceramic.
6. A preparation method of a ceramic insulator with microgrooves and a self-assembled molecular film on the surface is characterized by comprising the following steps:
step 1: processing a corresponding insulator original shape according to the size requirement of the ceramic insulator with the surface provided with the microgrooves and the self-assembled molecular film to be prepared;
step 2: opening a laser, and setting laser parameters according to the width, depth and cycle size of a micro groove required to be processed on the surface of the ceramic insulator with the micro groove and the self-assembled molecular film on the surface to be prepared; etching a microgroove on the surface of the insulator original sample processed in the step 1 through laser etching;
and step 3: ultrasonically cleaning the insulator original shape with a dilute acid solution after the microgrooves are etched on the surface in the step 2 to remove residual ceramic particles on the surface, cleaning the insulator original shape with deionized water, and drying the insulator original shape;
and 4, step 4: weighing a silane coupling agent, an organic solvent and deionized water according to a volume ratio of 1:20: 1-1: 500:1, mixing and stirring the silane coupling agent, the organic solvent and the deionized water uniformly, and hydrolyzing for 0.1-10 hours at room temperature to prepare a silane coupling agent hydrolysis solution;
and 5: placing the insulator with the micro grooves etched on the surface, dried in the step 3, in the silane coupling agent hydrolysis solution prepared in the step 4 for standing, and performing molecular self-assembly reaction for 12-36 hours;
step 6: sequentially carrying out ultrasonic cleaning on the insulator original sample subjected to the molecular self-assembly reaction in the step 5 by using ethanol and water, removing residues on the surface, and carrying out vacuum drying treatment at 50-70 ℃;
and 7: and (3) heating to 100-150 ℃, and carrying out high-temperature reaction on the insulator subjected to vacuum drying in the step (6) to obtain the ceramic insulator with the microgrooves and the self-assembled molecular film on the surface.
7. The method for preparing a ceramic insulator with micro-grooves and a self-assembled molecular film on the surface according to claim 6, wherein the method comprises the following steps: in the step 3, the silane coupling agent is KH-570, KH-550 or octadecyl trichlorosilane; the organic solvent is toluene, acetone or absolute ethyl alcohol.
8. The method for preparing a ceramic insulator with micro-grooves and a self-assembled molecular film on the surface according to claim 7, wherein the method comprises the following steps: in the step 2, the micro-groove is V-shaped, the width of the micro-groove is 20-100 μm, the depth of the micro-groove is 20-300 μm, and the period of the micro-groove is 20-500 μm.
9. The method for preparing a ceramic insulator having micro grooves and a self-assembled molecular film on the surface thereof according to any one of claims 6 to 8, wherein: in the step 2, the laser is an ultraviolet laser or a fiber laser.
10. The method for preparing a ceramic insulator having micro grooves and a self-assembled molecular film on the surface thereof according to claim 9, wherein: in the step 1, the original insulator material is alumina ceramic or silicate ceramic.
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