CN115538215B - Corona-resistant mica/aramid fiber composite material for new energy automobile and preparation method thereof - Google Patents
Corona-resistant mica/aramid fiber composite material for new energy automobile and preparation method thereof Download PDFInfo
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- CN115538215B CN115538215B CN202211286443.2A CN202211286443A CN115538215B CN 115538215 B CN115538215 B CN 115538215B CN 202211286443 A CN202211286443 A CN 202211286443A CN 115538215 B CN115538215 B CN 115538215B
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
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- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/10—Organic non-cellulose fibres
- D21H13/20—Organic non-cellulose fibres from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H13/26—Polyamides; Polyimides
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- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H15/00—Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution
- D21H15/02—Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution characterised by configuration
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/04—Hydrocarbons
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- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/06—Alcohols; Phenols; Ethers; Aldehydes; Ketones; Acetals; Ketals
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- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/37—Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
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- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
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- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/68—Water-insoluble compounds, e.g. fillers, pigments siliceous, e.g. clays
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- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/69—Water-insoluble compounds, e.g. fillers, pigments modified, e.g. by association with other compositions prior to incorporation in the pulp or paper
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- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
Abstract
The application discloses corona-resistant mica/aramid fiber composite material for new energy automobiles and a preparation method thereof, which belong to the technical field of mica composite materials, wherein the composite material comprises the following raw materials in percentage by weight: 40-60% of modified aramid fiber paper, 5-20% of adhesive and 40-60% of modified mica paper; wherein, the weight ratio of the modified aramid fiber paper to the modified mica paper is (1-1.5): 1, the adhesive comprises one or more of tetrafluoroethylene-perfluoro alkoxy vinyl ether copolymer, fluorinated ethylene propylene copolymer, ethylene-tetrafluoroethylene copolymer, polyether ether ketone and polyether imide. According to the modified aramid fiber paper and modified mica paper composite material, the modified aramid fiber paper and the modified mica paper with excellent corona resistance are compounded by using the adhesive, the overall compactness and paper inserting manufacturability, corona resistance, PDIV and temperature resistance of the composite material are improved, and the electrical insulation performance and long-term safe operation life of a new energy automobile motor can be remarkably improved.
Description
Technical Field
The application relates to a corona-resistant mica/aramid fiber composite material for a new energy automobile and a preparation method thereof, belonging to the technical field of mica composite materials.
Background
The prior high-temperature resistant H-grade or above slot insulation and interphase insulation paper for the new energy automobile motor is mostly aramid fiber pure paper or is formed by compounding aramid fiber paper with a polyimide film and using a high-temperature resistant adhesive, wherein a typical composite paper structure is Nomex fiber paper/PI film/Nomex fiber paper (NHN), and the composite adhesive is mostly epoxy, polyurethane or polyacrylate adhesive.
The aramid fiber pure paper or the NHN composite paper has higher heat resistance, is very excellent in performance of an insulation structure of a 400V voltage platform motor for a new energy automobile, however, for an 800V voltage platform motor, the highest safe voltage of the aramid fiber pure paper or the NHN composite paper can reach 2300V or even higher due to higher voltage level and the influence of environmental factors, which is far higher than the Partial Discharge Initial Voltage (PDIV) of the existing insulation material for the conventional piezoelectric motor, and the probability of generating partial discharge in the operation process of the motor is very high, so that corona resistance of the insulation material is required to be considered for the 800V voltage platform motor.
In the prior art, the corona-resistant service life of the composite paper is improved by adding mica components into the organic aramid fiber paper or by using epoxy, polyurethane or polyacrylate adhesive to compound the aramid fiber paper and the mica paper. However, the mica-containing composite paper prepared in the two modes generally has the problems of easy powder falling, easy fragmentation, layering and the like, has general corona resistance and high temperature resistance, and cannot meet the process requirements of the large-scale application of the new energy automobile motor.
Disclosure of Invention
In order to solve the problems, the corona resistant mica/aramid fiber composite material for the new energy automobile and the preparation method thereof are provided, the high temperature resistant, low dielectric constant adhesive such as the PFA-tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer, the FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer), the ETFE-ethylene-tetrafluoroethylene copolymer, the PEEK-polyether ether ketone, the PEI-polyether imide and the like is used for compounding the modified aramid fiber paper and the modified mica paper in a hot pressing manner, and meanwhile, the modified mica paper and the modified aramid fiber paper with excellent corona resistance are matched, so that the overall compactness and paper inserting manufacturability, corona resistance, partial Discharge Initiation Voltage (PDIV) and temperature resistant grade of the composite material can be improved, and the electrical insulation performance and long-term safe operation life of the new energy automobile motor can be remarkably improved by using the material as tank bottom insulation paper and interphase insulation paper.
According to one aspect of the application, the corona-resistant mica/aramid fiber composite material for the new energy automobile is provided, and comprises the following raw materials in percentage by weight: 40-60% of modified aramid fiber paper, 5-20% of adhesive and 40-60% of modified mica paper;
wherein the weight ratio of the modified aramid fiber paper to the modified mica paper is (1-1.5): 1, the adhesive comprises one or more of tetrafluoroethylene-perfluoro alkoxy vinyl ether copolymer, fluorinated ethylene propylene copolymer, ethylene-tetrafluoroethylene copolymer, polyether ether ketone and polyether imide.
Preferably, the adhesive is FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer); preferably, the adhesive comprises FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer) and polyether ether ketone with a weight ratio of 3:1.
optionally, the modified mica paper is prepared from the following raw materials: mica powder, hydrochloric acid solution, ethanol, a silane coupling agent, methyl methacrylate, an initiator and toluene;
the mica powder consists of first mica powder, second mica powder and third mica powder, wherein the particle size of the first mica powder is 90-110 mu m, the particle size of the second mica powder is 130-150 mu m, and the particle size of the third mica powder is 200-230 mu m; the weight ratio of the first mica powder to the second mica powder to the third mica powder is sequentially 1: (3-5): (3-5).
Specifically, the concentration of the hydrochloric acid solution was 2mol/L.
Optionally, the weight ratio of the silane coupling agent to the mica powder is (0.05-0.08): 1, the weight ratio of the mica powder to the methyl methacrylate to the initiator is sequentially 1: (0.1-0.15): (0.002-0.005), the weight ratio of the mica powder to ethanol to toluene is 1: (6-8): (5-8).
Optionally, the preparation method of the modified mica paper comprises the following steps: adding a silane coupling agent into ethanol, regulating the pH value to 4 by using a hydrochloric acid solution, adding mica powder, heating to 60-80 ℃, stirring for 1-3h, filtering, washing and drying, adding the mixture into toluene, simultaneously adding methyl methacrylate and an initiator, reacting for 2-4h at 70-90 ℃, filtering, drying for 0.5-2h at 110-130 ℃, adding water, stirring uniformly to form slurry, and making paper by a paper forming machine to obtain the modified mica paper.
Specifically, the mass concentration of the slurry is 3-5%.
Optionally, the silane coupling agent is a171, and the initiator is benzoyl peroxide.
Optionally, the modified aramid fiber paper is prepared from meta-aramid chopped fibers and meta-aramid fibrids, wherein the lengths of the meta-aramid chopped fibers and the meta-aramid fibrids are 2-3mm, and the weight ratio of the meta-aramid chopped fibers to the meta-aramid fibrids is 1: (2-2.5).
Optionally, the preparation method of the modified aramid fiber paper comprises the following steps: and (3) carrying out fluffing dispersion on the meta-aramid chopped fibers and meta-aramid fibrids, adding water to prepare slurry, carrying out ultrasonic treatment, and carrying out papermaking by a paper sheet forming machine to obtain the modified aramid fiber paper.
Specifically, the mass concentration of the slurry is 0.1-0.5%.
Optionally, the ultrasonic treatment step is that each time is carried out for 10s, the interval is 3s, and the ultrasonic treatment is carried out for 6-9min; ultrasonic parameters: the frequency is 10-20kHz and the power is 500W.
According to another aspect of the application, a preparation method of the corona-resistant mica/aramid fiber composite material for the new energy automobile is provided, and the preparation method comprises the following steps:
(1) Unreeling two rolls of modified aramid fiber paper, and respectively coating adhesive on the surfaces of the two rolls of modified aramid fiber paper;
(2) Unreeling the modified mica paper, attaching the modified mica paper to one piece of modified aramid fiber paper coated with an adhesive, attaching another piece of Zhang Tufu modified aramid fiber paper with the adhesive to the other side of the modified mica paper, and drying;
(3) And hot-pressing the dried composite material by a hot roller to finally obtain the corona-resistant mica/aramid fiber composite material for the new energy automobile.
Optionally, the drying temperature is 120 ℃, the hot pressing temperature is 265-310 ℃, and the hot pressing pressure is 20MPa.
Benefits of the present application include, but are not limited to:
1. according to the corona-resistant mica/aramid fiber composite material for the new energy automobile, the PFA-tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer, the FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer), the copolymer of ETFE-ethylene and tetrafluoroethylene, PEEK-polyether ether ketone, PEI-polyether imide and other high-temperature resistant adhesives with low dielectric constant are used for hot-pressing and compounding the modified aramid fiber paper and the modified mica paper, and meanwhile, the modified mica paper and the modified aramid fiber paper with excellent corona resistance are matched, so that the overall compactness and paper inserting manufacturability, corona resistance, partial Discharge Initiation Voltage (PDIV) and temperature resistance grade of the composite material can be improved.
2. According to the corona-resistant mica/aramid fiber composite material for the new energy automobile, the mica powder is limited to be composed of three mica powder with different particle sizes, and the respective proportion is limited at the same time, so that the mica powder with large particle size is complete in lamellar, a good stress transfer effect can be achieved, the paper is prevented from being broken due to concentrated stress, meanwhile, the paper is endowed with a certain stiffness, small-particle-size mica with smaller particle size is filled among large mica flakes, and good strength performance can be endowed to the paper;
meanwhile, the regular arrangement of the two kinds of mica powder with larger particle sizes also endows paper with better flatness, the mica powder has larger diameter-thickness ratio, the high insulation effect of the lamellar Z direction has better blocking effect on current, the formation of a current channel is delayed, the electric arc spreading is effectively delayed, the carbonization damage of fibers is reduced, the size area of breakdown points is reduced, and the corona resistance is improved.
3. According to the corona-resistant mica/aramid fiber composite material for the new energy automobile, the silane coupling agent and the polymer monomer are used for compounding and modifying the mica paper, hydroxyl exists on the surface of mica powder, double bonds are introduced on the surface of the powder by using the silane coupling agent A171, then the monomer and the initiator are added into mica powder liquid for polymerization reaction, vinyl on the surface of the mica powder is copolymerized with the monomer, so that the surface graft polymer is realized, the dispersibility of the surface graft polymer in slurry is improved, and finally the interface bonding performance of the surface graft polymer and the modified aramid fiber paper is improved.
4. According to the corona-resistant mica/aramid fiber composite material for the new energy automobile, the grafting rate of the surface of the mica powder is improved by limiting the proportion of the silane coupling agent to the mica powder; by limiting the proportion of mica powder, monomer and initiator, the coating rate of the polymer is improved.
5. According to the corona-resistant mica/aramid fiber composite material for the new energy automobile, meta-aramid chopped fibers and meta-aramid fibrids are used, the length and the proportion of the meta-aramid chopped fibers are limited, the chopped fibers are of a rod-shaped structure, the fibrids are of a thin film shape, in the proportion range, the fibrids can adhere to the rod-shaped chopped fibers together, the chopped fibers are facilitated to form a bracket, the bracket is formed by the chopped fibers, the backbone of the fibrids is formed, when the backbone is subjected to external force, the effect of transferring stress can be achieved, and meanwhile, the network structure formed by interweaving the chopped fibers enables the composite material to be high in compactness, excellent in corona resistance and long in service life.
6. According to the corona-resistant mica/aramid fiber composite material for the new energy automobile, the surface fine fiber degree of the aramid fiber can be enhanced, the surface active groups and the surface energy are increased through ultrasonic modification of the mixed aramid fiber, so that the dispersion performance of the aramid chopped fiber is improved, meanwhile, the specific surface area and the surface roughness of the aramid fiber are improved, the interweaving force of the chopped fiber and the fibrid can be increased, the filament splitting and fibrillation phenomena of the aramid fiber are caused, the mechanical interlocking effect among fiber interfaces is enhanced, and the mechanical property and the high temperature resistance of the composite material are improved.
7. According to the preparation method of the corona-resistant mica/aramid fiber composite material for the new energy automobile, through high-temperature hot press molding and limiting the hot press temperature, the chopped fibers and the fibrids are fully softened and bonded, and meanwhile, the adhesive fully infiltrates into the pores of the modified aramid fiber paper and the modified mica paper to form an integrally compact composite material, so that the tensile strength of the composite material is improved, and the electrical property is good.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute an undue limitation to the application. In the drawings:
fig. 1 is a schematic structural diagram of a corona-resistant mica/aramid fiber composite material for a new energy automobile according to an embodiment of the application.
Reference numerals: 1. modified aramid fiber powder; 2. an adhesive; 3. modified mica paper.
Detailed Description
The present application is described in detail below with reference to examples, but the present application is not limited to these examples.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. The reagents or materials used in the present invention may be purchased in conventional manners, and unless otherwise indicated, they may be used in conventional manners in the art or according to the product specifications. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred methods and materials are presented in this patent for illustrative purposes only.
Experimental raw materials:
1. three particle size mica powder: and (3) adopting a ball mill to prepare mica raw materials with different particle diameters by wet grinding, controlling the ball-to-material ratio to be 4:1, the matching mass ratio of small balls to medium balls to be 1:1, setting the rotating speed to be 300rmp, and adopting a laser particle size analyzer to measure the particle diameters and particle size distribution of the mica to prepare three mica slurries with different particle diameters.
2. Instrument: ball mill: TCXQM-2, tianchuang powder Co., ltd; laser particle size analyzer: BT-9300H, baite instruments Co., ltd; squeezer: CHYZ-01, initial creation of an electromechanical system; tensile strength tester: SE-062, lorentzen Wether, sweden; fluffer: ZQS4 Lorentzen Wether, sweden; a paper sheet forming machine, shenzhen Puyun, PY-Y814B.
3. Reagent: mica: hubei safety electric materials Co., ltd; silane coupling agent A171, U.S. Michael drawing; methyl methacrylate, shandong Xin Shun New Material Co., ltd; benzoyl peroxide, jiangsu Qiangsheng functional chemical Co., ltd; aramid fiber: japanese emperor.
Example 1 composite 1#
The composite material 1# is prepared from the following raw materials in percentage by weight: 40% of modified aramid fiber paper, 5% of adhesive and 40% of modified mica paper, wherein the adhesive is FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer).
The modified mica paper is prepared from the following raw materials: mica powder, hydrochloric acid solution, ethanol, a silane coupling agent, methyl methacrylate, an initiator and toluene; the mica powder consists of first mica powder, second mica powder and third mica powder, wherein the particle size of the first mica powder is 90 mu m, the particle size of the second mica powder is 130 mu m, and the particle size of the third mica powder is 200 mu m; the weight ratio of the first mica powder to the second mica powder to the third mica powder is sequentially 1:3:3, a step of; the weight ratio of the silane coupling agent to the mica powder is 0.05:1, the weight ratio of the mica powder to the methyl methacrylate to the initiator is sequentially 1:0.1:0.002, the weight ratio of the mica powder to the ethanol to the toluene is sequentially 1:6:5, a step of; the preparation method of the modified mica paper comprises the following steps: adding a silane coupling agent A171 into ethanol, regulating the pH value to 4 by using a hydrochloric acid solution, adding mica powder, heating to 60 ℃, stirring for 1h, filtering, washing and drying, adding the mixture into toluene, simultaneously adding methyl methacrylate and benzoyl peroxide, reacting for 2h at 70 ℃, filtering, drying for 0.5h at 110 ℃, adding water, stirring uniformly to form slurry with the mass concentration of 3%, and carrying out papermaking by a paper sheet forming machine to obtain the modified mica paper.
The modified aramid fiber paper is prepared from meta-aramid chopped fibers and meta-aramid fibrids, wherein the lengths of the meta-aramid chopped fibers and the meta-aramid fibrids are 2mm, and the weight ratio of the meta-aramid chopped fibers to the meta-aramid fibrids is 1:2; the preparation method of the modified aramid fiber paper comprises the following steps: the method comprises the steps of carrying out fluffing dispersion on meta-aramid chopped fibers and meta-aramid fibrids, adding water to prepare slurry with the mass concentration of 0.1%, carrying out ultrasonic treatment, and carrying out papermaking by a paper sheet forming machine to obtain modified aramid fiber paper with the thickness of 0.05mm; the ultrasonic treatment step is that each time is carried out for 10s, the interval is 3s, and the ultrasonic treatment is carried out for 6min; ultrasonic parameters: the frequency was 10kHz and the power was 500W.
The preparation method of the composite material 1# comprises the following steps:
(1) Unreeling two rolls of modified aramid fiber paper, and respectively coating adhesive on the surfaces of the two rolls of modified aramid fiber paper;
(2) Unreeling the modified mica paper, attaching the modified mica paper to one piece of modified aramid fiber paper coated with an adhesive, attaching another piece of Zhang Tufu modified aramid fiber paper with the adhesive to the other side of the modified mica paper, and drying;
(3) And hot-pressing the dried composite material by a hot roller to finally obtain the corona-resistant mica/aramid fiber composite material No. 1 with the thickness of 0.25mm for the new energy automobile.
Wherein the drying temperature is 120 ℃, the hot pressing temperature is 270 ℃, and the hot pressing pressure is 20MPa.
Example 2 composite 2#
The composite material 2# is prepared from the following raw materials in percentage by weight: 50% of modified aramid fiber paper, 10% of adhesive and 40% of modified mica paper, wherein the adhesive is FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer).
The modified mica paper is prepared from the following raw materials: mica powder, hydrochloric acid solution, ethanol, a silane coupling agent, methyl methacrylate, an initiator and toluene; the mica powder consists of first mica powder, second mica powder and third mica powder, wherein the particle size of the first mica powder is 110 mu m, the particle size of the second mica powder is 150 mu m, and the particle size of the third mica powder is 230 mu m; the weight ratio of the first mica powder to the second mica powder to the third mica powder is sequentially 1:5:5, a step of; the weight ratio of the silane coupling agent to the mica powder is 0.08:1, the weight ratio of the mica powder to the methyl methacrylate to the initiator is sequentially 1:0.15:0.005, the weight ratio of the mica powder to the ethanol to the toluene is sequentially 1:8:8, 8; the preparation method of the modified mica paper comprises the following steps: adding a silane coupling agent A171 into ethanol, regulating the pH value to 4 by using a hydrochloric acid solution, adding mica powder, heating to 80 ℃, stirring for 3 hours, filtering, washing and drying, adding the mixture into toluene, simultaneously adding methyl methacrylate and benzoyl peroxide, reacting for 4 hours at 90 ℃, filtering, drying for 2 hours at 130 ℃, adding water, stirring uniformly to form slurry with the mass concentration of 4%, and making by a paper sheet forming machine to obtain the modified mica paper.
The modified aramid fiber paper is prepared from meta-aramid chopped fibers and meta-aramid fibrids, wherein the lengths of the meta-aramid chopped fibers and the meta-aramid fibrids are 3mm, and the weight ratio of the meta-aramid chopped fibers to the meta-aramid fibrids is 1:2.5; the preparation method of the modified aramid fiber paper comprises the following steps: the meta-aramid chopped fiber and meta-aramid fibrid are fluffed, dispersed and added with water to prepare slurry with the mass concentration of 0.3%, and the slurry is subjected to ultrasonic treatment and manufactured by a paper forming machine to obtain modified aramid fiber paper with the thickness of 0.05mm; the ultrasonic treatment step is that each time is carried out for 10s, the interval is 3s, and the ultrasonic treatment is carried out for 9min; ultrasonic parameters: the frequency was 20kHz and the power was 500W.
The preparation method of the composite material No. 2 comprises the following steps:
(1) Unreeling two rolls of modified aramid fiber paper, and respectively coating adhesive on the surfaces of the two rolls of modified aramid fiber paper;
(2) Unreeling the modified mica paper, attaching the modified mica paper to one piece of modified aramid fiber paper coated with an adhesive, attaching another piece of Zhang Tufu modified aramid fiber paper with the adhesive to the other side of the modified mica paper, and drying;
(3) And hot-pressing the dried composite material by a hot roller to finally obtain the corona-resistant mica/aramid fiber composite material No. 2 with the thickness of 0.25mm for the new energy automobile.
Wherein the drying temperature is 120 ℃, the hot pressing temperature is 265 ℃, and the hot pressing pressure is 20MPa.
Example 3 composite 3#
The composite material 3# is prepared from the following raw materials in percentage by weight: 60% of modified aramid fiber paper, 20% of adhesive and 40% of modified mica paper, wherein the adhesive is PFA-tetrafluoroethylene-perfluoro alkoxy vinyl ether copolymer.
The modified mica paper is prepared from the following raw materials: mica powder, hydrochloric acid solution, ethanol, a silane coupling agent, methyl methacrylate, an initiator and toluene; the mica powder consists of first mica powder, second mica powder and third mica powder, wherein the particle size of the first mica powder is 100 mu m, the particle size of the second mica powder is 140 mu m, and the particle size of the third mica powder is 220 mu m; the weight ratio of the first mica powder to the second mica powder to the third mica powder is sequentially 1:4:4, a step of; the weight ratio of the silane coupling agent to the mica powder is 0.06:1, the weight ratio of the mica powder to the methyl methacrylate to the initiator is sequentially 1:0.12:0.003, the weight ratio of the mica powder to the ethanol to the toluene is sequentially 1:7:6, preparing a base material; the preparation method of the modified mica paper comprises the following steps: adding a silane coupling agent A171 into ethanol, regulating the pH value to 4 by using a hydrochloric acid solution, adding mica powder, heating to 70 ℃, stirring for 2 hours, filtering, washing and drying, adding the mixture into toluene, simultaneously adding methyl methacrylate and benzoyl peroxide, reacting for 3 hours at 80 ℃, filtering, drying for 1 hour at 120 ℃, adding water, stirring uniformly to form slurry with the mass concentration of 5%, and making by a paper sheet forming machine to obtain the modified mica paper.
The modified aramid fiber paper is prepared from meta-aramid chopped fibers and meta-aramid fibrids, wherein the lengths of the meta-aramid chopped fibers and the meta-aramid fibrids are 2mm, and the weight ratio of the meta-aramid chopped fibers to the meta-aramid fibrids is 1:2.2; the preparation method of the modified aramid fiber paper comprises the following steps: the meta-aramid chopped fiber and meta-aramid fibrid are fluffed, dispersed and added with water to prepare slurry with the mass concentration of 0.5%, and the slurry is subjected to ultrasonic treatment and manufactured by a paper forming machine to obtain modified aramid fiber paper with the thickness of 0.05mm; the ultrasonic treatment step is that each time is carried out for 10s, the interval is 3s, and the ultrasonic treatment is carried out for 7min; ultrasonic parameters: the frequency was 15kHz and the power was 500W.
The preparation method of the composite material 3# comprises the following steps:
(1) Unreeling two rolls of modified aramid fiber paper, and respectively coating adhesive on the surfaces of the two rolls of modified aramid fiber paper;
(2) Unreeling the modified mica paper, attaching the modified mica paper to one piece of modified aramid fiber paper coated with an adhesive, attaching another piece of Zhang Tufu modified aramid fiber paper with the adhesive to the other side of the modified mica paper, and drying;
(3) And hot-pressing the dried composite material by a hot roller to finally obtain the corona-resistant mica/aramid fiber composite material 3# for the new energy automobile, wherein the thickness is 0.25mm.
Wherein the drying temperature is 120 ℃, the hot pressing temperature is 310 ℃, and the hot pressing pressure is 20MPa.
Example 4 composite 4#
Example 4 differs from example 1 in that: the adhesive in example 4 was a fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer) and a polyetheretherketone in a weight ratio of 3:1, which are identical to each other.
Comparative example 1 comparative composite 1#
Comparative example 1 differs from example 3 in that: the adhesive in comparative example 1 was a methylated amino resin, the remainder being the same.
Comparative example 2 comparative composite 2#
Comparative example 2 differs from example 3 in that: the aramid fiber of comparative example 2 was not modified and the rest was the same.
Comparative example 3 comparative composite 3#
Comparative example 3 is different from example 3 in that: the mica powder in comparative example 3 was two kinds of mica powder having particle diameters of 50 μm and 90 μm in a weight ratio of 1:3, and the remainder were the same.
Comparative example 4 comparative composite 4#
Comparative example 4 differs from example 3 in that: the weight ratio of the first mica powder, the second mica powder and the third mica powder in comparative example 4 is 1:1.5:1.2, the remainder being identical.
Comparative example 5 comparative composite 5#
Comparative example 5 differs from example 3 in that: the weight ratio of the silane coupling agent to the mica powder in comparative example 5 was 0.12:1, the remainder being identical.
Comparative example 6 comparative composite 6#
Comparative example 6 differs from example 3 in that: in comparative example 6, only the silane coupling agent KH550 was used to modify the mica powder, and the remainder was the same.
Comparative example 7 comparative composite 7#
Comparative example 7 differs from example 3 in that: the aramid fiber used in comparative example 7 was para-aramid fibrid and the rest were the same.
Comparative example 8 comparative composite 8#
Comparative example 8 differs from example 3 in that: the length of the intermediate aramid chopped fiber and the meta-aramid fibrid of comparative example 8 are 5mm, and the rest are the same.
Comparative example 9 comparative composite 9#
Comparative example 9 differs from example 3 in that: comparative example 9 the weight ratio of the intermediate aramid chopped fiber to the para aramid fibrid is 1:1, the remainder being identical.
Comparative example 10 comparative composite 10#
Comparative example 10 differs from example 3 in that: the hot press molding temperature was 360℃in comparative example 10, and the rest were the same.
Comparative example 11 comparative composite 11#
Comparative example 11 is meta-aramid fiber paper plain paper, 0.25mm thick.
Comparative example 12 comparative composite 12#
Comparative example 12 is a composite material (commercially available material name NHN) prepared by compounding 0.05mm thick meta-aramid fiber paper on both sides of a polyimide film using polyurethane as an adhesive, and has a thickness of 0.25mm.
Experimental example
1. Electrical performance
Breakdown voltage: the test is carried out according to national standard GB/T1408.1-2006, the thickness of a sample is 0.25mm, a phi 25 mm/phi 75mm cylindrical electrode system is adopted, the test times are 5 times, and the average value is obtained.
PDIV (partial discharge initiation voltage): the test is carried out according to national standard GB/T7354-2018, the alternating voltage frequency: 50hz; boost speed: 50V/s; taking the partial discharge quantity 10PC as an initial discharge voltage point; experimental temperature: 21-25 ℃, humidity: 45-55%.
2. Experiment of temperature resistance
The experimental method comprises the following steps: the test is carried out according to national standard GB/T4074.7-2009, and the heat resistance grade of the material is evaluated by adopting a three-point method.
3. Tensile Strength
The experimental method comprises the following steps: measured according to national standards GB/T20629.2-2013 and GB/T5591.2-2017.
4. Corona resistant life of square wave
The experimental method comprises the following steps: the test was performed according to the T/CEEIA 415-2019 standard, test conditions: peak-to-peak voltage Vp-p=3000V, temperature 155±3 ℃, frequency=20 KHz, rising edge 100±10ns, duty cycle 50%.
The composite material 1# -4# and the comparative composite material 1# -12# were sampled and tested in the above four experiments, and the experimental results are shown in table 1.
TABLE 1
From the experimental data, the composite material 1# -4 prepared by the raw materials and the method defined by the application has the advantages of good electrical property, long corona resistant life of square waves, excellent high temperature resistance and excellent mechanical property.
Compared with the composite material 1# which is a commercially available common adhesive, the final result has general electrical performance and general high temperature resistance; compared with the composite material No. 2, the aramid fiber is not modified, and the final result has general electrical performance, and the analysis reason is that the aramid fiber has higher inertia and has poorer boundary bonding effect with other matrix materials.
Compared with the composite material 3# in which the particle size of the mica powder is smaller than the range defined by the application, the final result is general in electrical performance and low in breakdown voltage, more mica fragments are generated due to the small-particle mica, most of the mica fragments are added into paper to serve as sediment components, the paper is loose in structure and increased in thickness due to irregular arrangement, the paper mixing structure is damaged, the mechanical property of the paper is reduced, meanwhile, the paper pores are increased, and when the paper is acted by external voltage, electron beams are blocked by the reduction of high insulation on Z directions of large mica sheets, so that the paper is broken down more easily.
The ratio of small-particle-size mica powder in the comparative composite material No. 4 exceeds the range defined by the application, the final result is general in electrical performance, the analysis reason is that the integrity of mica layer sheets is destroyed along with the increase of mica with smaller particle size, the size of the mica layer sheets in a longitudinal structure is increased, fine particles are increased and gradually accumulated, the mica sheet arrangement is changed from tiling to recumbent, and the mechanical property is reduced; meanwhile, due to damage of a mica sheet structure, small-particle-size mica with a large proportion presents particles, a large number of pores are generated by stacking of the particles, so that the mica has a limited insulation effect, when the paper is subjected to electric breakdown, the current is blocked less, the current channel is shorter, and the overall insulation performance of the paper is reduced.
The ratio of the silane coupling agent to the mica powder in the comparative composite material No. 5 exceeds the range defined by the application, and the final result has general electrical performance, and the analysis reason is that the excessive amount of the coupling agent can reduce the coupling efficiency due to condensation reaction, the grafting rate is low, the modification effect is poor, and the amount of the coupling agent is small, so that the amount of the coupling agent grafted on the surface is small.
Compared with the composite material 6# only uses the silane coupling agent to modify the mica powder, the final result has general electrical performance, and the analysis reason is that the dispersion performance after modification is still limited, and the interface bonding performance with other materials is not high.
Compared with the composite material 7# which uses para-aramid fibrid, the final result has better mechanical property, but the electrical property is general, the analysis reason is that the para-molecular structure is excellent in mechanical property, but the electrical property is poorer than that of the meta-structure, and meanwhile, the fibrid has poor cladding property on chopped fibers.
The length of the fibers used in the comparative composite material 8# exceeds the range defined by the application, and the final result is that the electrical performance is general, and the analysis reasons are that the lengthening of the fibers increases the probability of intertwining among the fibers, is not suitable for dispersion, increases the non-uniformity of the hot-pressed composite paper, and further influences the overall strength of the paper.
The ratio of fibrids to chopped fibers used in comparative composite material 9# is less than the range defined in the application, and the final result is generally electrical performance, and the analysis is that the chopped fibers are inserted in the paper structure, so that the paper is easy to form pores easily, the bonding effect with the chopped fibers is poor due to the smaller ratio of fibrids, and the electrical performance and the thermal performance of the composite material are difficult to develop.
The final result, electrical properties are generally, for comparison of composite 10# with hot press forming temperatures above the ranges defined herein, with the analysis being that the temperature is too high resulting in aging of the raw materials and a decrease in the bonding force of the aramid fibers and fibrids. Compared with the composite material 11# -12# which is a common composite material sold in the market, the composite material has the advantages of general high temperature resistance, corona resistance and short service life.
The foregoing is merely exemplary of the present application, and the scope of the present application is not limited to the specific embodiments, but is defined by the claims of the present application. Various modifications and changes may be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the technical ideas and principles of the present application should be included in the protection scope of the present application.
Claims (9)
1. The corona-resistant mica/aramid fiber composite material for the new energy automobile is characterized by comprising the following raw materials in percentage by weight: 40-60% of modified aramid fiber paper, 5-20% of adhesive and 40-60% of modified mica paper;
wherein the weight ratio of the modified aramid fiber paper to the modified mica paper is (1-1.5): 1, the adhesive comprises one or more of tetrafluoroethylene-perfluoro alkoxy vinyl ether copolymer, fluorinated ethylene propylene copolymer, ethylene-tetrafluoroethylene copolymer, polyether ether ketone and polyether imide;
the modified mica paper is prepared from the following raw materials: mica powder, hydrochloric acid solution, ethanol, a silane coupling agent, methyl methacrylate, an initiator and toluene; the mica powder consists of first mica powder, second mica powder and third mica powder, wherein the particle size of the first mica powder is 90-110 mu m, the particle size of the second mica powder is 130-150 mu m, and the particle size of the third mica powder is 200-230 mu m; the weight ratio of the first mica powder to the second mica powder to the third mica powder is sequentially 1: (3-5): (3-5).
2. The corona resistant mica/aramid fiber composite material for new energy automobiles according to claim 1, wherein the weight ratio of the silane coupling agent to the mica powder is (0.05-0.08): 1, the weight ratio of the mica powder to the methyl methacrylate to the initiator is sequentially 1: (0.1-0.15): (0.002-0.005), the weight ratio of the mica powder to ethanol to toluene is 1: (6-8): (5-8).
3. The corona resistant mica/aramid fiber composite material for new energy automobiles according to claim 2, wherein the preparation method of the modified mica paper comprises the following steps: adding a silane coupling agent into ethanol, regulating the pH value to 4 by using a hydrochloric acid solution, adding mica powder, heating to 60-80 ℃, stirring for 1-3h, filtering, washing and drying, adding the mixture into toluene, simultaneously adding methyl methacrylate and an initiator, reacting for 2-4h at 70-90 ℃, filtering, drying for 0.5-2h at 110-130 ℃, adding water, stirring uniformly to form slurry, and making paper by a paper forming machine to obtain the modified mica paper.
4. The corona resistant mica/aramid fiber composite material for new energy automobiles according to claim 3, wherein the silane coupling agent is a171 and the initiator is benzoyl peroxide.
5. The corona resistant mica/aramid fiber composite material for new energy vehicles according to claim 1, wherein the modified aramid fiber paper is prepared from meta-aramid chopped fibers and meta-aramid fibrids, the lengths of the meta-aramid chopped fibers and the meta-aramid fibrids are 2-3mm, and the weight ratio of the meta-aramid chopped fibers to the meta-aramid fibrids is 1: (2-2.5).
6. The corona resistant mica/aramid fiber composite material for new energy automobiles according to claim 5, wherein the preparation method of the modified aramid fiber paper comprises the following steps: and (3) carrying out fluffing dispersion on the meta-aramid chopped fibers and meta-aramid fibrids, adding water to prepare slurry, carrying out ultrasonic treatment, and carrying out papermaking by a paper sheet forming machine to obtain the modified aramid fiber paper.
7. The corona resistant mica/aramid fiber composite material for new energy automobiles according to claim 6, wherein the ultrasonic treatment step is 10s ultrasonic treatment each time, 3s interval and 6-9min ultrasonic treatment altogether; ultrasonic parameters: the frequency is 10-20kHz and the power is 500W.
8. A method for preparing the corona resistant mica/aramid fiber composite material for new energy automobiles according to any one of claims 1 to 7, which is characterized by comprising the following steps:
(1) Unreeling two rolls of modified aramid fiber paper, and respectively coating adhesive on the surfaces of the two rolls of modified aramid fiber paper;
(2) Unreeling the modified mica paper, attaching the modified mica paper to one piece of modified aramid fiber paper coated with an adhesive, attaching another piece of Zhang Tufu modified aramid fiber paper with the adhesive to the other side of the modified mica paper, and drying;
(3) And hot-pressing the dried composite material by a hot roller to finally obtain the corona-resistant mica/aramid fiber composite material for the new energy automobile.
9. The method according to claim 8, wherein the drying temperature is 120 ℃, the hot pressing temperature is 265-310 ℃, and the hot pressing pressure is 20MPa.
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