CN111004475A - Nonlinear composite insulating material with core-shell structure and preparation method thereof - Google Patents

Nonlinear composite insulating material with core-shell structure and preparation method thereof Download PDF

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CN111004475A
CN111004475A CN201911346516.0A CN201911346516A CN111004475A CN 111004475 A CN111004475 A CN 111004475A CN 201911346516 A CN201911346516 A CN 201911346516A CN 111004475 A CN111004475 A CN 111004475A
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core
insulating material
shell structure
composite insulating
silicon carbide
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韩永森
王婷婷
肖微
曾向军
孙健
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Harbin University of Science and Technology
Research Institute of Southern Power Grid Co Ltd
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Harbin University of Science and Technology
Power Grid Technology Research Center of China Southern Power Grid Co Ltd
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Abstract

A nonlinear composite insulating material with a core-shell structure and a preparation method thereof belong to the technical field of electric insulating material preparation. Weighing 1-15 g of silicon carbide powder with a core-shell structure, putting the silicon carbide powder into a beaker, adding 50-100 ml of acetone, adding 50-60 g of epoxy resin, ultrasonically dispersing for 5-10 min, stirring for 4-5 h in an oil bath environment at 50-60 ℃, adding 40-45 g of curing agent and 0.5-1 g of accelerator into the obtained mixed solution, stirring for 20-30 min under a vacuum condition, injecting the mixed solution into a mold, curing at a certain temperature, and naturally cooling to obtain the material. The volume conductivity of the invention is less than 6.5 multiplied by 10 in the electric field below 16kV/mm 14S/m, nonlinear threshold field strengthThe voltage is 16kV/mm, and the doping of the silicon carbide powder with the core-shell structure is more favorable for improving the nonlinear threshold field strength of the nonlinear composite insulating material.

Description

Nonlinear composite insulating material with core-shell structure and preparation method thereof
Technical Field
The invention belongs to the technical field of electric insulating material preparation; in particular to a nonlinear composite insulating material with a core-shell structure and a preparation method thereof.
Background
The nonlinear composite insulating material has the functions of inhibiting space charge accumulation and homogenizing electric field distribution, and has wide application prospect in the fields of cable terminals, motor corona-proof structures, basin-type insulators, high-voltage bushings and the like. Nonlinear composite insulating materials are typically formed by doping a polymer matrix with a semiconductor filler such as zinc oxide and silicon carbide. For the nonlinear composite insulating material doped with zinc oxide, the nonlinear electrical conductivity mainly originates from the grain boundary potential barrier inside zinc oxide particles, and the nonlinear electrical conductivity of the zinc oxide particles can be effectively regulated and controlled by adjusting the composition, sintering temperature, sintering time and other factors of the zinc oxide ceramic powder, so that the nonlinear electrical conductivity of the nonlinear composite insulating material doped with zinc oxide is improved. However, the dielectric loss of such nonlinear composite insulating materials is generally high, and the nonlinear composite insulating materials are mainly applied to medium and low voltage electrical equipment.
The non-linear composite insulating material doped with micron-sized silicon carbide is characterized in that the non-linear conductivity is formed by the contact between adjacent silicon carbide particles, the non-linear composite insulating material is widely applied to the insulation of a high-voltage power cable terminal and the end part of a high-voltage motor, and is one of key insulating materials for developing ultrahigh-voltage and ultrahigh-voltage electrical equipment. However, it is difficult to control the thickness of the interface region around the silicon carbide particles by this surface modification method, and the dielectric properties of the interface are difficult to quantitatively describe. The performance of the existing silicon carbide-doped epoxy resin-based nonlinear composite insulating material needs to be further improved.
Disclosure of Invention
The invention aims to provide a nonlinear composite insulating material with a core-shell structure, which is simple in preparation method and good in performance, and a preparation method thereof.
The invention is realized by the following technical scheme:
a preparation method of a nonlinear composite insulating material with a core-shell structure comprises the following steps:
step 1, preparing silicon carbide powder with a core-shell structure;
step 2, preparing the epoxy resin-based nonlinear composite insulating material doped with the silicon carbide with the core-shell structure: weighing 1-15 g of the silicon carbide powder with the core-shell structure prepared in the step 1, putting the silicon carbide powder into a beaker, adding 50-100 ml of acetone, then adding 50-60 g of epoxy resin, carrying out ultrasonic dispersion for 5-10 min, and then stirring for 4-5 h under an oil bath environment at 50-60 ℃ to obtain a mixed solution for later use;
and 3, adding 40-45 g of curing agent and 0.5-1 g of accelerator into the mixed solution obtained in the step 2, stirring for 20-30 min under a vacuum condition, then injecting the mixed solution into a mold, curing at a certain temperature, and naturally cooling to obtain the core-shell structured nonlinear composite insulating material.
The invention relates to a preparation method of a nonlinear composite insulating material with a core-shell structure, which comprises the following steps of 1:
step a, respectively weighing a certain amount of nano silicon carbide, tetraethoxysilane and 3-aminopropyltriethoxysilane according to a certain material-liquid ratio for later use;
b, adding distilled water and absolute ethyl alcohol with a certain volume into the nano silicon carbide weighed in the step a, uniformly stirring, performing ultrasonic dispersion, and dispersing to obtain a first mixed solution for later use;
step c, adding anhydrous ethanol with a certain volume into the tetraethoxysilane and the 3-aminopropyltriethoxysilane weighed in the step a, uniformly stirring, performing ultrasonic dispersion, and obtaining a second mixed solution for later use;
and d, slowly adding the second mixed solution obtained in the step c into the first mixed solution prepared in the step b, then adding deionized water with the volume of 0.8-3 times that of the first mixed solution, stirring and reacting for 10-12 hours at a certain temperature to obtain a third mixed solution, washing and centrifuging the third mixed solution with absolute ethyl alcohol and deionized water for three times respectively, and drying in vacuum to obtain silicon carbide powder with a core-shell structure.
The invention relates to a preparation method of a nonlinear composite insulating material with a core-shell structure, wherein in the step a, the feed-liquid ratio of nano silicon carbide, tetraethoxysilane and 3-aminopropyltriethoxysilane is 8-15 g: 16-30 ml: 1.2-2.25 ml.
The preparation method of the nonlinear composite insulating material with the core-shell structure comprises the following steps of (a) in step b, the ratio of nano silicon carbide, distilled water and absolute ethyl alcohol is 8-15 g: 40-100 ml: 5-10 ml, and 5-10 min of ultrasonic dispersion time.
According to the preparation method of the nonlinear composite insulating material with the core-shell structure, in the step c, 2-6 times of volume of absolute ethyl alcohol is added into weighed tetraethoxysilane and 3-aminopropyltriethoxysilane, and the ultrasonic dispersion time is 5-10 min.
According to the preparation method of the nonlinear composite insulating material with the core-shell structure, in the step d, the reaction condition is a 50 ℃ oil bath environment, and the vacuum drying condition is drying for 8 hours in a 100 ℃ vacuum drying oven.
According to the preparation method of the nonlinear composite insulating material with the core-shell structure, the epoxy resin in the step 2 is bisphenol A type epoxy resin.
According to the preparation method of the nonlinear composite insulating material with the core-shell structure, the curing agent in the step 3 is methyl tetrahydrophthalic anhydride, the accelerator is 2, 4, 6-tri (dimethylamine methyl) phenol, the curing condition is that the curing is carried out for 4 hours at 80 ℃, and then the temperature is raised to 120 ℃ for curing for 8 hours.
The nonlinear composite insulating material with the core-shell structure is prepared by the preparation method of the nonlinear composite insulating material with the core-shell structure, and the nonlinear composite insulating material with the core-shell structureThe volume conductivity of the nonlinear composite insulating material in an electric field below 16kV/mm is less than 6.5 multiplied by 10-14S/m, the nonlinear threshold field intensity is 16 kV/mm.
Compared with micron silicon carbide, the nano silicon carbide used in the preparation method of the nonlinear composite insulating material with the core-shell structure has larger specific surface area, the interaction between the nano silicon carbide and the polymer matrix is stronger, and the small-size effect of the nano silicon carbide increases the contact probability among silicon carbide particles, so that even under the condition of lower content of nano silicon carbide filler, the conductivity of the nonlinear composite insulating material doped with the nano silicon carbide also has obvious nonlinear characteristics.
According to the preparation method of the nonlinear composite insulating material with the core-shell structure, the epoxy resin is a typical insulating material and is widely applied to corona-proof structures at the end parts of high-voltage bushings, basin-type insulators and motor wire rods. The nonlinear electrical conductivity of the nonlinear composite insulating material with the epoxy resin as the matrix and the nano silicon carbide as the filler is closely related to the interface between the nano silicon carbide particles and the epoxy resin matrix besides the nano silicon carbide particles. The method can effectively regulate and control the thickness of an interface region between the silicon carbide particles and the epoxy resin matrix and the dielectric property parameters of the interface, and compared with the traditional doping of silicon carbide, the doping of the silicon carbide powder with the core-shell structure is more favorable for improving the nonlinear threshold field strength of the nonlinear composite insulating material.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a transmission electron microscope photograph of a nonlinear composite insulating material with a core-shell structure prepared by a method according to an embodiment;
fig. 3 is an X-ray diffraction contrast diagram of silicon carbide powder having a core-shell structure prepared by the method of the embodiment.
Detailed Description
The first embodiment is as follows:
a preparation method of a nonlinear composite insulating material with a core-shell structure comprises the following steps:
step 1, preparing silicon carbide powder with a core-shell structure;
step 2, preparing the epoxy resin-based nonlinear composite insulating material doped with the silicon carbide with the core-shell structure: weighing 9.05g of the silicon carbide powder with the core-shell structure prepared in the step 1, putting the silicon carbide powder into a beaker, adding 50ml of acetone, then adding 50g of epoxy resin, carrying out ultrasonic dispersion for 5min, and then stirring for 5h in an oil bath environment at 60 ℃ to obtain a mixed solution for later use;
and 3, adding 40g of curing agent and 0.5g of accelerator into the mixed solution obtained in the step 2, stirring for 30min under a vacuum condition, then injecting the mixed solution into a mold, curing at a certain temperature, and naturally cooling to obtain the core-shell structured nonlinear composite insulating material.
The preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment 1 is a preparation method of silicon carbide powder having a core-shell structure, and includes the following steps:
step a, respectively weighing a certain amount of nano silicon carbide, tetraethoxysilane and 3-aminopropyltriethoxysilane according to a certain material-liquid ratio for later use;
b, adding distilled water and absolute ethyl alcohol with a certain volume into the nano silicon carbide weighed in the step a, uniformly stirring, performing ultrasonic dispersion, and dispersing to obtain a first mixed solution for later use;
step c, adding anhydrous ethanol with a certain volume into the tetraethoxysilane and the 3-aminopropyltriethoxysilane weighed in the step a, uniformly stirring, performing ultrasonic dispersion, and obtaining a second mixed solution for later use;
and d, slowly adding the second mixed solution obtained in the step c into the first mixed solution prepared in the step b, then adding deionized water with the volume being 2.45 times that of the first mixed solution, stirring and reacting for 12 hours at a certain temperature to obtain a third mixed solution, washing and centrifuging the third mixed solution for three times respectively by using absolute ethyl alcohol and deionized water, and drying in vacuum to obtain silicon carbide powder with a core-shell structure.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, in the step a, the material-to-liquid ratio of the nano silicon carbide, the tetraethoxysilane and the 3-aminopropyltriethoxysilane is 8 g: 16 ml: 1.2 ml.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, in the step b, the material-to-liquid ratio of the nano silicon carbide, the distilled water and the absolute ethyl alcohol is 8 g: 40 ml: 5ml, and the ultrasonic dispersion time is 5 min.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, in the step c, 3.5 times of volume of absolute ethyl alcohol is added into weighed tetraethoxysilane and 3-aminopropyltriethoxysilane, and the ultrasonic dispersion time is 5 min.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, the reaction condition in the step d is a 50 ℃ oil bath environment, and the vacuum drying condition is drying in a 100 ℃ vacuum drying oven for 8 hours.
In the method for preparing the nonlinear composite insulating material with the core-shell structure according to the embodiment, the epoxy resin in the step 2 is bisphenol a epoxy resin.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, the curing agent in step 3 is methyl tetrahydrophthalic anhydride, the accelerator is 2, 4, 6-tris (dimethylaminomethyl) phenol, and the curing condition is that the curing is performed for 4 hours at 80 ℃, and then the temperature is raised to 120 ℃ for curing for 8 hours.
In the nonlinear composite insulating material with a core-shell structure prepared by the preparation method of the nonlinear composite insulating material with a core-shell structure according to the embodiment of the present invention, the volume conductivity of the nonlinear composite insulating material with a core-shell structure in an electric field of 16kV/mm or less is less than 6.5 × 10-14S/m, the nonlinear threshold field intensity is 16 kV/mm.
In the method for preparing the nonlinear composite insulating material with the core-shell structure according to the embodiment, a transmission electron microscope photograph of the prepared nonlinear composite insulating material with the core-shell structure is shown in fig. 2, and as can be seen from fig. 2, the obvious core-shell structure is shown, an outer shell material is silicon dioxide, an inner core material is silicon carbide, and the size of the nonlinear composite insulating material with the core-shell structure is about 25 nm.
In the method for preparing the nonlinear composite insulating material with the core-shell structure according to the embodiment, an X-ray diffraction contrast spectrum of the prepared core-shell structure is shown in fig. 3. As can be seen from fig. 3, in the silicon carbide powder with the core-shell structure obtained by the core-shell structure preparation method, three characteristic peaks (2 θ located at 35.7 °, 60.1 ° and 71.7 °) of silicon carbide do not undergo significant changes, which indicates that the crystal structure of silicon carbide is not changed by the core-shell process. However, in the 2 θ range of 20 ° to 30 °, a relatively broad characteristic peak, which is a characteristic peak of silica, is observed. Therefore, a core-shell structure silicon carbide powder having a silicon carbide core and a silicon dioxide shell was successfully prepared.
The second embodiment is as follows:
a preparation method of a nonlinear composite insulating material with a core-shell structure comprises the following steps:
step 1, preparing silicon carbide powder with a core-shell structure;
step 2, preparing the epoxy resin-based nonlinear composite insulating material doped with the silicon carbide with the core-shell structure: weighing 15g of the silicon carbide powder with the core-shell structure prepared in the step 1, putting the silicon carbide powder into a beaker, adding 100ml of acetone, then adding 60g of epoxy resin, ultrasonically dispersing for 10min, and then stirring for 5h under an oil bath environment at 50-60 ℃ to obtain a mixed solution for later use;
and 3, adding 45g of curing agent and 1g of accelerator into the mixed solution obtained in the step 2, stirring for 30min under a vacuum condition, then injecting the mixed solution into a mold, curing at a certain temperature, and naturally cooling to obtain the core-shell structured nonlinear composite insulating material.
The preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment 1 is a preparation method of silicon carbide powder having a core-shell structure, and includes the following steps:
step a, respectively weighing a certain amount of nano silicon carbide, tetraethoxysilane and 3-aminopropyltriethoxysilane according to a certain material-liquid ratio for later use;
b, adding distilled water and absolute ethyl alcohol with a certain volume into the nano silicon carbide weighed in the step a, uniformly stirring, performing ultrasonic dispersion, and dispersing to obtain a first mixed solution for later use;
step c, adding anhydrous ethanol with a certain volume into the tetraethoxysilane and the 3-aminopropyltriethoxysilane weighed in the step a, uniformly stirring, performing ultrasonic dispersion, and obtaining a second mixed solution for later use;
and d, slowly adding the second mixed solution obtained in the step c into the first mixed solution prepared in the step b, then adding 3 times of volume of deionized water, stirring and reacting for 12 hours at a certain temperature to obtain a third mixed solution, washing and centrifuging the third mixed solution for three times respectively by using absolute ethyl alcohol and deionized water, and drying in vacuum to obtain the silicon carbide powder with the core-shell structure.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, in the step a, the material-to-liquid ratio of the nano silicon carbide, the tetraethoxysilane and the 3-aminopropyltriethoxysilane is 15 g: 30 ml: 2.25 ml.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, in the step b, the material-to-liquid ratio of the nano silicon carbide, the distilled water and the absolute ethyl alcohol is 15 g: 100 ml: 10ml, ultrasonic dispersion time is 10 min.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, in the step c, absolute ethyl alcohol with the volume 6 times that of the weighed tetraethoxysilane and 3-aminopropyltriethoxysilane is added, and the ultrasonic dispersion time is 10 min.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, the reaction condition in the step d is a 50 ℃ oil bath environment, and the vacuum drying condition is drying in a 100 ℃ vacuum drying oven for 8 hours.
In the method for preparing the nonlinear composite insulating material with the core-shell structure according to the embodiment, the epoxy resin in the step 2 is bisphenol a epoxy resin.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, the curing agent in step 3 is methyl tetrahydrophthalic anhydride, the accelerator is 2, 4, 6-tris (dimethylaminomethyl) phenol, and the curing condition is that the curing is performed for 4 hours at 80 ℃, and then the temperature is raised to 120 ℃ for curing for 8 hours.
In the nonlinear composite insulating material with a core-shell structure prepared by the preparation method of the nonlinear composite insulating material with a core-shell structure according to the embodiment of the present invention, the volume conductivity of the nonlinear composite insulating material with a core-shell structure in an electric field of 16kV/mm or less is less than 6.5 × 10-14S/m, the nonlinear threshold field intensity is 16kV/mm, which is far higher than the nonlinear threshold field intensity of the common silicon carbide doped nonlinear composite insulating material (S/m)<10kV/mm)), the nonlinear coefficient was 3.2.
The third concrete implementation mode:
a preparation method of a nonlinear composite insulating material with a core-shell structure comprises the following steps:
step 1, preparing silicon carbide powder with a core-shell structure;
step 2, preparing the epoxy resin-based nonlinear composite insulating material doped with the silicon carbide with the core-shell structure: weighing 1-15 g of the silicon carbide powder with the core-shell structure prepared in the step 1, putting the silicon carbide powder into a beaker, adding 50-100 ml of acetone, then adding 50-60 g of epoxy resin, carrying out ultrasonic dispersion for 5-10 min, and then stirring for 4-5 h under an oil bath environment at 50-60 ℃ to obtain a mixed solution for later use;
and 3, adding 40-45 g of curing agent and 0.5-1 g of accelerator into the mixed solution obtained in the step 2, stirring for 20-30 min under a vacuum condition, then injecting the mixed solution into a mold, curing at a certain temperature, and naturally cooling to obtain the core-shell structured nonlinear composite insulating material.
The preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment 1 is a preparation method of silicon carbide powder having a core-shell structure, and includes the following steps:
step a, respectively weighing a certain amount of nano silicon carbide, tetraethoxysilane and 3-aminopropyltriethoxysilane according to a certain material-liquid ratio for later use;
b, adding distilled water and absolute ethyl alcohol with a certain volume into the nano silicon carbide weighed in the step a, uniformly stirring, performing ultrasonic dispersion, and dispersing to obtain a first mixed solution for later use;
step c, adding anhydrous ethanol with a certain volume into the tetraethoxysilane and the 3-aminopropyltriethoxysilane weighed in the step a, uniformly stirring, performing ultrasonic dispersion, and obtaining a second mixed solution for later use;
and d, slowly adding the second mixed solution obtained in the step c into the first mixed solution prepared in the step b, then adding deionized water with the volume of 0.8-3 times that of the first mixed solution, stirring and reacting for 10-12 hours at a certain temperature to obtain a third mixed solution, washing and centrifuging the third mixed solution with absolute ethyl alcohol and deionized water for three times respectively, and drying in vacuum to obtain silicon carbide powder with a core-shell structure.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, in the step a, the material-to-liquid ratio of the nano silicon carbide, the tetraethoxysilane and the 3-aminopropyltriethoxysilane is 8-15 g: 16-30 ml: 1.2-2.25 ml.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, in the step b, the material-liquid ratio of the nano silicon carbide, the distilled water and the absolute ethyl alcohol is 8-15 g: 40-100 ml: 5-10 ml, and 5-10 min of ultrasonic dispersion time.
In the preparation method of the core-shell structured nonlinear composite insulating material, in the step c, 2-6 times of volume of absolute ethyl alcohol is added into weighed tetraethoxysilane and 3-aminopropyltriethoxysilane, and the ultrasonic dispersion time is 5-10 min.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, the reaction condition in the step d is a 50 ℃ oil bath environment, and the vacuum drying condition is drying in a 100 ℃ vacuum drying oven for 8 hours.
In the method for preparing the nonlinear composite insulating material with the core-shell structure according to the embodiment, the epoxy resin in the step 2 is bisphenol a epoxy resin.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, the curing agent in step 3 is methyl tetrahydrophthalic anhydride, the accelerator is 2, 4, 6-tris (dimethylaminomethyl) phenol, and the curing condition is that the curing is performed for 4 hours at 80 ℃, and then the temperature is raised to 120 ℃ for curing for 8 hours.
In the preparation method of the core-shell structured nonlinear composite insulating material according to the embodiment, compared with the micron silicon carbide, the nano silicon carbide used in the preparation method has a larger specific surface area, the interaction between the nano silicon carbide and the polymer matrix is also stronger, and the small-size effect of the nano silicon carbide increases the contact probability between silicon carbide particles, so that even under the condition of low nano silicon carbide filler content, the conductivity of the nano silicon carbide-doped nonlinear composite insulating material has an obvious nonlinear characteristic.
In the preparation method of the nonlinear composite insulating material with the core-shell structure according to the embodiment, the epoxy resin is a typical insulating material and is widely applied to corona-proof structures at the ends of high-voltage bushings, basin-type insulators and motor wire rods. The nonlinear electrical conductivity of the nonlinear composite insulating material with the epoxy resin as the matrix and the nano silicon carbide as the filler is closely related to the interface between the nano silicon carbide particles and the epoxy resin matrix besides the nano silicon carbide particles. The method can effectively regulate and control the thickness of the interface region between the silicon carbide particles and the epoxy resin matrix and the dielectric property parameters of the interface, and compared with the traditional doping of silicon carbide, the doping of the silicon carbide powder with the core-shell structure in the embodiment is more favorable for improving the nonlinear threshold field strength of the nonlinear composite insulating material.

Claims (9)

1. A preparation method of a nonlinear composite insulating material with a core-shell structure is characterized by comprising the following steps: the method comprises the following steps:
step 1, preparing silicon carbide powder with a core-shell structure;
step 2, preparing the epoxy resin-based nonlinear composite insulating material doped with the silicon carbide with the core-shell structure: weighing 1-15 g of the silicon carbide powder with the core-shell structure prepared in the step 1, putting the silicon carbide powder into a beaker, adding 50-100 ml of acetone, then adding 50-60 g of epoxy resin, carrying out ultrasonic dispersion for 5-10 min, and then stirring for 4-5 h under an oil bath environment at 50-60 ℃ to obtain a mixed solution for later use;
and 3, adding 40-45 g of curing agent and 0.5-1 g of accelerator into the mixed solution obtained in the step 2, stirring for 20-30 min under a vacuum condition, then injecting the mixed solution into a mold, curing at a certain temperature, and naturally cooling to obtain the core-shell structured nonlinear composite insulating material.
2. The preparation method of the nonlinear composite insulating material with the core-shell structure according to claim 1, characterized in that: step 1 is a preparation method of silicon carbide powder with a core-shell structure, which comprises the following steps:
step a, respectively weighing a certain amount of nano silicon carbide, tetraethoxysilane and 3-aminopropyltriethoxysilane according to a certain material-liquid ratio for later use;
b, adding distilled water and absolute ethyl alcohol with a certain volume into the nano silicon carbide weighed in the step a, uniformly stirring, performing ultrasonic dispersion, and dispersing to obtain a first mixed solution for later use;
step c, adding anhydrous ethanol with a certain volume into the tetraethoxysilane and the 3-aminopropyltriethoxysilane weighed in the step a, uniformly stirring, performing ultrasonic dispersion, and obtaining a second mixed solution for later use;
and d, slowly adding the second mixed solution obtained in the step c into the first mixed solution prepared in the step b, then adding deionized water with the volume of 0.8-3 times that of the first mixed solution, stirring and reacting for 10-12 hours at a certain temperature to obtain a third mixed solution, washing and centrifuging the third mixed solution with absolute ethyl alcohol and deionized water for three times respectively, and drying in vacuum to obtain silicon carbide powder with a core-shell structure.
3. The preparation method of the nonlinear composite insulating material with the core-shell structure according to claim 2, characterized in that: in the step a, the material-to-liquid ratio of the nano silicon carbide, the ethyl orthosilicate and the 3-aminopropyltriethoxysilane is 8-15 g: 16-30 ml: 1.2-2.25 ml.
4. The preparation method of the nonlinear composite insulating material with the core-shell structure according to claim 2, characterized in that: in the step b, the feed-liquid ratio of the nano silicon carbide, the distilled water and the absolute ethyl alcohol is 8-15 g: 40-100 ml: 5-10 ml, and 5-10 min of ultrasonic dispersion time.
5. The preparation method of the nonlinear composite insulating material with the core-shell structure according to claim 2, characterized in that: and c, adding 2-6 times of volume of absolute ethyl alcohol into the weighed tetraethoxysilane and 3-aminopropyltriethoxysilane, and performing ultrasonic dispersion for 5-10 min.
6. The preparation method of the nonlinear composite insulating material with the core-shell structure according to claim 2, characterized in that: in the step d, the reaction condition is 50 ℃ oil bath environment, and the vacuum drying condition is drying for 8 hours in a vacuum drying oven at 100 ℃.
7. The preparation method of the nonlinear composite insulating material with the core-shell structure according to claim 1, characterized in that: the epoxy resin in the step 2 is bisphenol A type epoxy resin.
8. The preparation method of the nonlinear composite insulating material with the core-shell structure according to claim 1, characterized in that: the curing agent in the step 3 is methyl tetrahydrophthalic anhydride, the accelerator is 2, 4, 6-tri (dimethylamine methyl) phenol, the curing condition is that the curing is carried out for 4 hours at the temperature of 80 ℃, and then the temperature is raised to 120 ℃ for curing for 8 hours.
9. A nonlinear composite insulating material with a core-shell structure prepared by the preparation method of the nonlinear composite insulating material with a core-shell structure according to any one of claims 1 to 8, which is characterized in that: the volume conductivity of the nonlinear composite insulating material with the core-shell structure in an electric field below 16kV/mm is less than 6.5 multiplied by 10-14S/m, the nonlinear threshold field intensity is 16 kV/mm.
CN201911346516.0A 2019-12-24 2019-12-24 Nonlinear composite insulating material with core-shell structure and preparation method thereof Pending CN111004475A (en)

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