CN115116754A - Preparation method of reinforced solid-liquid mixed conductive polymer capacitor - Google Patents
Preparation method of reinforced solid-liquid mixed conductive polymer capacitor Download PDFInfo
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- CN115116754A CN115116754A CN202210940708.XA CN202210940708A CN115116754A CN 115116754 A CN115116754 A CN 115116754A CN 202210940708 A CN202210940708 A CN 202210940708A CN 115116754 A CN115116754 A CN 115116754A
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- 239000003990 capacitor Substances 0.000 title claims abstract description 63
- 229920001940 conductive polymer Polymers 0.000 title claims abstract description 38
- 239000007788 liquid Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000011049 filling Methods 0.000 claims abstract description 64
- 239000000853 adhesive Substances 0.000 claims abstract description 59
- 230000001070 adhesive effect Effects 0.000 claims abstract description 59
- 229920005989 resin Polymers 0.000 claims abstract description 38
- 239000011347 resin Substances 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 31
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 19
- 239000012745 toughening agent Substances 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 239000003085 diluting agent Substances 0.000 claims abstract description 18
- 229920001971 elastomer Polymers 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000003292 glue Substances 0.000 claims abstract description 17
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 16
- 239000000654 additive Substances 0.000 claims abstract description 15
- 230000000996 additive effect Effects 0.000 claims abstract description 15
- 239000003999 initiator Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000007789 sealing Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 32
- 238000006243 chemical reaction Methods 0.000 claims description 24
- -1 aromatic acid ester Chemical class 0.000 claims description 19
- 238000009775 high-speed stirring Methods 0.000 claims description 14
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 11
- 229920000570 polyether Polymers 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 239000011541 reaction mixture Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 239000003822 epoxy resin Substances 0.000 claims description 7
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- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 6
- 229920002635 polyurethane Polymers 0.000 claims description 6
- 239000004814 polyurethane Substances 0.000 claims description 6
- 229920001296 polysiloxane Polymers 0.000 claims description 5
- 125000005456 glyceride group Chemical group 0.000 claims description 4
- 150000004982 aromatic amines Chemical class 0.000 claims description 3
- 239000003792 electrolyte Substances 0.000 claims description 3
- 230000002159 abnormal effect Effects 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 239000003973 paint Substances 0.000 description 6
- 238000009472 formulation Methods 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 3
- 229920000459 Nitrile rubber Polymers 0.000 description 3
- 229920000180 alkyd Polymers 0.000 description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000004642 Polyimide Substances 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
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- 238000001179 sorption measurement Methods 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/15—Solid electrolytic capacitors
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J167/00—Adhesives based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Adhesives based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/15—Solid electrolytic capacitors
- H01G9/153—Skin fibre
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention relates to a preparation method of a reinforced solid-liquid mixed conductive polymer capacitor, which is characterized by comprising the following steps of: the method comprises the following steps: preparing a solid-liquid mixed conductive polymer capacitor body; step two: the filling adhesive capable of reinforcing the capacitor structure is prepared and comprises the following raw materials: main materials of resins, a curing agent, a defoaming agent, a silane coupling agent, a resin toughening agent, a diluent, an initiator and an additive; step three: injecting the filling adhesive point to the opening of the shell on the solid-liquid mixed conductive polymer capacitor body to obtain a filling adhesive sealing layer covering the opening of the shell; drying and curing in a high-temperature environment; so that the filling glue is adhered to the contact surface of the glue cover and the shell to form a whole. The problem that in the prior art, after the capacitor is subjected to thermal impact force, the rubber cover slides up and down to cause various electrical parameters of the capacitor to be abnormal, and particularly leakage current is large is solved.
Description
Technical Field
The invention belongs to the field of capacitors, and particularly relates to a preparation method of a reinforced solid-liquid mixed conductive polymer capacitor.
Background
The solid electrolytic capacitor comprises an anode, a dielectric layer formed on the anode, a cathode and a solid electrolyte, and is packaged to form an electronic component. The capacitor is generally formed by packaging an element, an aluminum shell and a glue cover, wherein the element is placed in the aluminum shell, the element is sealed in the aluminum shell by the glue cover, and an electrode is externally led out through a guide pin or a guide foil to form the capacitor. The rubber cover is inserted into the opening of the aluminum shell and sealed, and the tightness between the opening of the aluminum shell and the rubber cover is better through the girdling process. However, after a long time use, the rubber cap may be aged and shrunk or thermally shocked, which may result in poor sealing performance and movement of the rubber cap. The mechanical stress of the existing solid-liquid mixed conductive polymer capacitor with the small size of 4 phi/5 phi/6.3 phi and the like is easily conducted into the capacitor during processing, or after the capacitor passes through a high-temperature environment of 250 ℃, the rubber cover slides up and down after the capacitor is subjected to the thermal impact force, so that various electrical parameters of the capacitor are abnormal, particularly leakage current is caused.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a reinforced solid-liquid mixed conductive polymer capacitor, which is used for solving the problem that in the prior art, after the capacitor is subjected to thermal impact force, a rubber cover slides up and down to cause abnormal electrical parameters of the capacitor, especially large leakage current.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a preparation method of a reinforced solid-liquid mixed conductive polymer capacitor is characterized by comprising the following steps:
the method comprises the following steps: preparing a solid-liquid mixed conductive polymer capacitor body; the solid-liquid mixed conductive polymer capacitor body consists of a shell, a rubber cover, an anode body with a dielectric layer on the surface, a cathode body and electrolyte between the anode body and the cathode body;
step two: preparing filling adhesive capable of reinforcing a capacitor structure, wherein the filling adhesive comprises the following raw materials: main materials of resins, a curing agent, a defoaming agent, a silane coupling agent, a resin toughening agent, a diluent, an initiator and an additive;
step three: injecting filling glue to the opening of the shell on the solid-liquid mixed conductive polymer capacitor body to obtain a filling glue sealing layer covering the opening of the shell; drying and curing in a high-temperature environment; so that the filling adhesive is bonded with the contact surface of the adhesive cover and the shell into a whole.
Further, the filling adhesive comprises the following raw materials in percentage: 60-70% of main material resins, 5-8% of curing agent, 0.3% of defoaming agent, 7-10% of silane coupling agent, 5-10% of resin toughening agent, 0.5-1% of diluent, 2% of initiator and 0.7% of additive.
Furthermore, the temperature for drying and curing the filling adhesive in the third step is controlled to be 100-130 ℃.
Further, the main material resins are as follows: one or more of epoxy resin, polyurethane, aromatic acid ester and glyceride.
Further, the defoaming agent is: one or more of silicon, polyether and polyether modified polysiloxane.
Further, the curing agent is: one or a mixture of two or more of aliphatic amines, aromatic amines, and amidoamines.
Further, the preparation method of the filling adhesive comprises the following steps:
and (3) SI: weighing main material resin compounds, a defoaming agent and a resin toughening agent, and putting the main material resin compounds, the defoaming agent and the resin toughening agent into a low-temperature reaction kettle at the temperature of-5 ℃ to maintain the temperature of the main material at-5 ℃;
s2: adding the weighed material curing agent, the silane coupling agent, the diluent, the initiator and the additive into a reaction kettle, and uniformly stirring at a high speed under a vacuum condition;
s3: transferring the reaction mixture to a constant-temperature homogenizer at the temperature of-5 ℃ to accelerate the micronization of the mixture particles, so that the mixture is more uniform;
s4: and transferring the mixture into an original reaction kettle, carrying out vacuum high-speed stirring again to avoid bubbles, and carrying out high-speed stirring and mixing at a low temperature of-5 ℃ for 1h to obtain the filling adhesive with good fluidity, high hardness and high temperature resistance.
The invention has the advantages and positive effects that:
according to the preparation method of the reinforced solid-liquid mixed conductive polymer capacitor, the technical scheme is adopted, the resin toughening agent is mainly used for increasing the toughness and hardness of the curing agent, the diluent is used for adjusting the viscosity of the curing agent, the multi-component mixing is easy to generate bubbles, and the defoaming agent can reduce the generation of bubbles. The initiator can enable the resin and the curing agent to generate polymerization reaction at the high temperature of about 80 ℃ to form a high-molecular aggregate, and the high-molecular aggregate is bonded with the aluminum shell and the rubber cover of the contact surface, so that the curing effect is achieved. After the capacitor is filled with the glue and hardened, the filled glue does not expand with heat and contract with cold like a glue cover to cause structural deformation at the high temperature of 250 ℃. The problem of among the prior art, the condenser receives the phenomenon that the lid appears sliding from top to bottom after the thermal shock power, leads to the condenser each electric parameter unusual, especially the leakage current is big is solved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a flow chart of the manufacturing process of the present invention.
FIG. 2 is a schematic cross-sectional view of the capacitor of the present invention.
Description of the drawings: 1. a housing; 2. a rubber cover; 3. filling glue; 4. an anode body; 5. a cathode body.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In some embodiments of the present invention, a filling adhesive is injected at the sealing position of the outer shell of the solid-liquid mixed conductive polymer capacitor. Firstly, preparing a solid-liquid mixed conductive polymer capacitor, assembling the capacitor to a package through each process, and preparing filling adhesive capable of reinforcing a capacitor structure, wherein the filling adhesive comprises the following raw materials in proportion: main materials of resins, a curing agent, a defoaming agent, a silane coupling agent, a resin toughening agent, a diluent, an initiator and an additive. The raw materials are stirred and mixed at a high speed for 1h at a low temperature of-5 ℃ to obtain filling adhesive, then the curing agent is injected on the capacitor by using a point injection mode, and the curing agent is hardened after drying. Wherein the main materials of the resins are as follows: one or more of epoxy resin, polyurethane, aromatic acid ester and glyceride. The defoaming agent is: one or a mixture of two or more of silicon, polyether, and polyether-modified polysiloxane. Bubbles are easily generated in the case where a plurality of substance components are mixed, but the generation of bubbles can be reduced in the case where an antifoaming agent is added; so that the prepared filling adhesive has better compactness. The thinner is added and mixed, so that the thinning effect is achieved, the viscosity is reduced, the filling adhesive has better fluidity, and better permeability is achieved when the filling adhesive is injected into the capacitor, so that the filling adhesive can fully permeate and cover the gap between the shell and the adhesive cover, and the filling adhesive has better adsorption force and air tightness. The resin toughening agent is added, the resin toughening agent is effectively combined with the main material resins, the toughness and hardness of the filling adhesive are increased, and the initiator can enable the resin and the curing agent to perform polymerization reaction at high temperature to form a high-molecular aggregate which is bonded with the contact surface of the shell and the rubber cover, so that the curing effect is achieved. After the capacitor is fixedly filled with the glue and hardened, the filled glue can not expand with heat and contract with cold like a rubber cover to cause structural deformation at a high temperature of 250 ℃, so that a reinforcing effect is achieved, and the problem that in the prior art, after the capacitor is subjected to thermal impact force, the rubber cover slides up and down to cause various electrical parameters of the capacitor to be abnormal, particularly leakage current to be large is solved.
The embodiments of the invention will be described in further detail with reference to the accompanying drawings:
a preparation method of a reinforced solid-liquid mixed conductive polymer capacitor is characterized by comprising the following steps:
the method comprises the following steps: preparing a solid-liquid mixed conductive polymer capacitor body; the solid-liquid mixed conductive polymer capacitor body consists of a shell, a rubber cover, an anode body with a dielectric layer on the surface, a cathode body and electrolyte between the anode body and the cathode body;
step two: preparing filling adhesive capable of reinforcing a capacitor structure, wherein the filling adhesive comprises the following raw materials: main materials of resins, a curing agent, a defoaming agent, a silane coupling agent, a resin toughening agent, a diluent, an initiator and an additive;
step three: injecting filling glue to the opening of the shell on the solid-liquid mixed conductive polymer capacitor body to obtain a filling glue sealing layer covering the opening of the shell; drying and curing in a high-temperature environment; so that the filling adhesive is bonded with the contact surface of the adhesive cover and the shell into a whole.
The preparation method of the filling adhesive comprises the following steps:
and (3) SI: weighing main material resin compounds, a defoaming agent and a resin toughening agent, and putting the main material resin compounds, the defoaming agent and the resin toughening agent into a low-temperature reaction kettle at the temperature of-5 ℃ to maintain the temperature of the main material at-5 ℃;
s2: adding the weighed material curing agent, the silane coupling agent, the diluent, the initiator and the additive into a reaction kettle, and uniformly stirring at a high speed under a vacuum condition;
s3: transferring the reaction mixture to a constant-temperature homogenizer at the temperature of-5 ℃ to accelerate the micronization of the mixture particles, so that the mixture is more uniform;
s4: and transferring the mixture into an original reaction kettle, carrying out vacuum high-speed stirring again to avoid bubbles, and carrying out high-speed stirring and mixing at a low temperature of-5 ℃ for 1h to obtain the filling adhesive with good fluidity, high hardness and high temperature resistance.
The following are specific examples.
Example 1
And (3) SI: weighing 60% of epoxy resin, 0.3% of silicon and 5% of nitrile rubber, and putting the epoxy resin, the silicon and the nitrile rubber into a low-temperature reaction kettle at the temperature of-5 ℃ to keep the temperature of the main material at-5 ℃;
s2: adding 5% of weighed aliphatic amine, 7% of silane coupling agent, 0.5% of epoxy paint diluent, 2% of acyl peroxide and 0.7% of additive into a reaction kettle, and uniformly stirring at high speed under a vacuum condition;
s3: transferring the reaction mixture to a constant-temperature homogenizer at the temperature of-5 ℃ to accelerate the micronization of the mixture particles, so that the mixture is more uniform;
s4: and transferring the mixture into an original reaction kettle, carrying out vacuum high-speed stirring again to avoid bubbles, and carrying out high-speed stirring and mixing at a low temperature of-5 ℃ for 1h to obtain the filling adhesive with good fluidity, high hardness and high temperature resistance.
After the filling adhesive is prepared, the filling adhesive is injected to the opening of the shell on the solid-liquid mixed conductive polymer capacitor body in a point mode to obtain a filling adhesive sealing layer covering the opening of the shell; drying and curing in a high-temperature environment.
Example 2
And (3) SI: weighing 60% of polyurethane, 0.3% of polyether and 5% of polysulfide rubber, and putting the materials into a low-temperature reaction kettle at the temperature of-5 ℃ to keep the temperature of the main material at-5 ℃;
s2: adding 5% of aromatic amine, 7% of silane coupling agent, 0.5% of alkyd paint diluent, 2% of ketone peroxide and 0.7% of additive into a reaction kettle, and uniformly stirring at high speed under a vacuum condition;
s3: transferring the reaction mixture to a constant-temperature homogenizer at the temperature of-5 ℃ to accelerate the micronization of the mixture particles, so that the mixture is more uniform;
s4: and transferring the mixture into the original reaction kettle, stirring at high speed in vacuum again to avoid bubbles, and stirring and mixing at high speed for 1h at the low temperature of-5 ℃ to obtain the filling adhesive with good fluidity, high hardness and high temperature resistance.
After the filling adhesive is prepared, the filling adhesive is injected to the opening of the shell on the solid-liquid mixed conductive polymer capacitor body in a point mode to obtain a filling adhesive sealing layer covering the opening of the shell; drying and curing in a high-temperature environment.
Example 3
And (3) SI: weighing 65% of aromatic acid ester, 0.3% of polyether modified polysiloxane and 7% of polyether, and putting the materials into a low-temperature reaction kettle at the temperature of-5 ℃ to keep the temperature of the main materials at-5 ℃;
s2: adding 7 percent of acylamino amine, 7 percent of silane coupling agent, 0.5 percent of alkyd paint diluent, 2 percent of azo and 0.7 percent of additive into a reaction kettle, and uniformly stirring at high speed under a vacuum condition;
s3: transferring the reaction mixture to a constant-temperature homogenizer at the temperature of-5 ℃ to accelerate the micronization of the mixture particles, so that the mixture is more uniform;
s4: and transferring the mixture into an original reaction kettle, carrying out vacuum high-speed stirring again to avoid bubbles, and carrying out high-speed stirring and mixing at a low temperature of-5 ℃ for 1h to obtain the filling adhesive with good fluidity, high hardness and high temperature resistance.
After the filling adhesive is prepared, the filling adhesive is injected to the opening of the shell on the solid-liquid mixed conductive polymer capacitor body in a point mode to obtain a filling adhesive sealing layer covering the opening of the shell; drying and curing in a high-temperature environment.
Example 4
And (3) SI: weighing 70% of epoxy resin and polyurethane, 0.3% of silicon and polyether, and 7% of polyimide and nano titanium dioxide, and placing the epoxy resin and polyurethane, the silicon and polyether and the polyimide and nano titanium dioxide into a low-temperature reaction kettle at the temperature of-5 ℃ to keep the temperature of the main material at-5 ℃;
s2: adding 7% of aliphatic amine, 8% of silane coupling agent, 1% of epoxy paint diluent, 2% of acyl peroxide and ketone peroxide and 0.7% of additive into a reaction kettle, and uniformly stirring at high speed under a vacuum condition;
s3: transferring the reaction mixture to a constant-temperature homogenizer at the temperature of-5 ℃ to accelerate the micronization of the mixture particles, so that the mixture is more uniform;
s4: and transferring the mixture into an original reaction kettle, carrying out vacuum high-speed stirring again to avoid bubbles, and carrying out high-speed stirring and mixing at a low temperature of-5 ℃ for 1h to obtain the filling adhesive with good fluidity, high hardness and high temperature resistance.
After the filling adhesive is prepared, the filling adhesive is injected to the opening of the shell on the solid-liquid mixed conductive polymer capacitor body in a point mode to obtain a filling adhesive sealing layer covering the opening of the shell; drying and curing in a high-temperature environment.
Example 5
And (3) SI: weighing 70% of aromatic acid ester and glyceride, 0.3% of polyether modified polysiloxane, and 10% of nitrile rubber and polyvinyl alcohol, and placing the materials into a low-temperature reaction kettle at-5 ℃ to keep the temperature of the main material at-5 ℃;
s2: adding 8 percent of weighed aliphatic amine and acylamino amine, 10 percent of weighed silane coupling agent, 1 percent of weighed epoxy paint diluent and alkyd paint diluent, 2 percent of weighed acyl peroxide and 0.7 percent of weighed additive into a reaction kettle, and uniformly stirring at high speed under a vacuum condition;
s3: transferring the reaction mixture to a constant-temperature homogenizer at the temperature of-5 ℃ to accelerate the micronization of the mixture particles, so that the mixture is more uniform;
s4: and transferring the mixture into an original reaction kettle, carrying out vacuum high-speed stirring again to avoid bubbles, and carrying out high-speed stirring and mixing at a low temperature of-5 ℃ for 1h to obtain the filling adhesive with good fluidity, high hardness and high temperature resistance.
After the filling adhesive is prepared, the filling adhesive is injected to the opening of the shell on the solid-liquid mixed conductive polymer capacitor body in a dispensing manner to obtain a filling adhesive sealing layer covering the opening of the shell; drying and curing in a high-temperature environment.
Comparative example 1
Comparative example 1 differs from example 1 in that comparative example 1 does not include a resin toughening agent and an initiator in the formulation of the underfill composition, and the other ingredients and formulation conditions are the same as in example 1.
Comparative example 2
Comparative example 2 differs from example 2 in that comparative example 2 does not include an antifoaming agent, a resin toughening agent, a silane coupling agent, a diluent, and an initiator in the formulation of the underfill composition, and other components and formulation conditions are the same as those of example 2.
Table one:
the table shows the specific test parameters of the examples and comparative examples
As can be seen from Table 1, the solid-liquid mixed conductive polymer capacitor has an obvious effect of reducing leakage current after the filling adhesive is injected.
It can be known from comparative examples 1 to 5 that the low leakage current of the solid-liquid mixed conductive polymer capacitor can be affected by injecting the filling glue with different proportions, wherein example 1 is the best proportion.
Comparing example 1 with comparative example 1, it can be seen that the addition of the resin toughening agent and the initiator according to the present invention can significantly improve the hardness of the underfill, the contact effect of the underfill and the housing, and the hardness of the 250 ℃ high temperature underfill.
In conclusion, it can be shown that after the filling adhesive is injected to the seal of the solid-liquid mixed conductive polymer capacitor, the contact effect and hardness between the filling adhesive and the housing are improved, the sliding phenomenon of the rubber cover in a high-temperature environment is avoided, good sealing performance is achieved, the solid-liquid mixed conductive polymer capacitor has the capability of bearing external force or high-temperature thermal impact, the sliding of the rubber cover is avoided, and the effect of reducing leakage current is achieved.
It should be emphasized that the embodiments described herein are illustrative rather than restrictive, and thus the present invention is not limited to the embodiments described in the detailed description, but other embodiments derived from the technical solutions of the present invention by those skilled in the art are also within the scope of the present invention.
Claims (7)
1. A preparation method of a reinforced solid-liquid mixed conductive polymer capacitor is characterized by comprising the following steps:
the method comprises the following steps: preparing a solid-liquid mixed conductive polymer capacitor body; the solid-liquid mixed conductive polymer capacitor body consists of a shell, a rubber cover, an anode body with a dielectric layer on the surface, a cathode body and electrolyte between the anode body and the cathode body;
step two: preparing filling adhesive capable of reinforcing a capacitor structure, wherein the filling adhesive comprises the following raw materials: main materials of resins, a curing agent, a defoaming agent, a silane coupling agent, a resin toughening agent, a diluent, an initiator and an additive;
step three: injecting filling glue to the opening of the shell on the solid-liquid mixed conductive polymer capacitor body to obtain a filling glue sealing layer covering the opening of the shell; drying and curing in a high-temperature environment; so that the filling adhesive is bonded with the contact surface of the adhesive cover and the shell into a whole.
2. The method for preparing the reinforced solid-liquid mixed conductive polymer capacitor as claimed in claim 1, wherein the method comprises the following steps: the filling adhesive comprises the following raw materials in percentage: 60-70% of main material resins, 5-8% of curing agent, 0.3% of defoaming agent, 7-10% of silane coupling agent, 5-10% of resin toughening agent, 0.5-1% of diluent, 2% of initiator and 0.7% of additive.
3. The method for preparing the reinforced solid-liquid mixed conductive polymer capacitor as claimed in claim 1, wherein the method comprises the following steps: and in the third step, the drying and curing temperature of the filling adhesive is controlled to be 100-130 ℃.
4. The method for preparing the reinforced solid-liquid mixed conductive polymer capacitor as claimed in claim 1, wherein the method comprises the following steps: the main material resins are as follows: one or more of epoxy resin, polyurethane, aromatic acid ester and glyceride.
5. The method for preparing the reinforced solid-liquid mixed conductive polymer capacitor as claimed in claim 1, wherein the method comprises the following steps: the defoaming agent is: one or more of silicon, polyether and polyether modified polysiloxane.
6. The method for preparing the reinforced solid-liquid mixed conductive polymer capacitor as claimed in claim 1, wherein the method comprises the following steps: the curing agent is: one or more of aliphatic amines, aromatic amines, and amidoamines.
7. The method for preparing the reinforced solid-liquid mixed conductive polymer capacitor as claimed in claim 1, wherein the method comprises the following steps: the preparation method of the filling adhesive comprises the following steps:
and (3) SI: weighing main material resin compounds, a defoaming agent and a resin toughening agent, and putting the main material resin compounds, the defoaming agent and the resin toughening agent into a low-temperature reaction kettle at the temperature of-5 ℃ to maintain the temperature of the main material at-5 ℃;
s2: adding the weighed material curing agent, the silane coupling agent, the diluent, the initiator and the additive into a reaction kettle, and uniformly stirring at a high speed under a vacuum condition;
s3: transferring the reaction mixture to a constant-temperature homogenizer at the temperature of-5 ℃ to accelerate the micronization of the mixture particles, so that the mixture is more uniform;
s4: and transferring the mixture into an original reaction kettle, carrying out vacuum high-speed stirring again to avoid bubbles, and carrying out high-speed stirring and mixing at a low temperature of-5 ℃ for 1h to obtain the filling adhesive with good fluidity, high hardness and high temperature resistance.
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| US20150322309A1 (en) * | 2013-01-23 | 2015-11-12 | Henkel IP & Holding GmbH | Underfill composition and packaging process using the same |
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