CN107731531A - Mixed polymerization solution, chip-type solid aluminium electrolutic capacitor and its hybrid polymerization technique - Google Patents
Mixed polymerization solution, chip-type solid aluminium electrolutic capacitor and its hybrid polymerization technique Download PDFInfo
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- CN107731531A CN107731531A CN201711175948.0A CN201711175948A CN107731531A CN 107731531 A CN107731531 A CN 107731531A CN 201711175948 A CN201711175948 A CN 201711175948A CN 107731531 A CN107731531 A CN 107731531A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/025—Solid electrolytes
- H01G9/028—Organic semiconducting electrolytes, e.g. TCNQ
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/0029—Processes of manufacture
- H01G9/0036—Formation of the solid electrolyte layer
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
- H01G9/045—Electrodes or formation of dielectric layers thereon characterised by the material based on aluminium
Abstract
A kind of mixed polymerization solution, chip-type solid aluminium electrolutic capacitor and its hybrid polymerization technique, are related to solid aluminum capacitor production technical field.Mixed polymerization solution includes chemical polymerization solution and dispersin polymerization liquid, and the mixed polymerization solution is used to be made uniform, fine and close, has the electroconductive polymer layer that proof voltage ability is strong, leakage current is small；The hybrid polymerization technique of chip-type solid aluminium electrolutic capacitor is to carry out multiple polymerization processing to aluminium foil using preprocessing solution, chemical polymerization solution and dispersin polymerization liquid, until aluminium foil surface forms the solid electrolyte layer of dense uniform, capacitor is made again, the technological operation is simple, obtained solid electrolyte layer is uniform, fine and close, strong with electrical conductivity height, proof voltage ability, leakage current is small, under high temperature the advantages of dependable performance；The ESR excellent performances of obtained chip-type solid aluminium electrolutic capacitor, proof voltage ability are strong, can prepare 20V and above product.
Description
Technical field
The present invention relates to solid aluminum capacitor production technical field, and more particularly to a kind of mixed polymerization solution, chip are solid
Body aluminium electrolutic capacitor and its hybrid polymerization technique.
Background technology
In recent years, as military electronic complete machine is fast-developing to miniaturization, high frequency, highly reliable direction, do not require nothing more than
Solid capacitor small volume, frequency characteristic are good, reliability is high, but also high pressure, low equivalent series are proposed to solid capacitor
The index requests such as resistance.Solid capacitor is in the use of the surface of the oxide such as the valve metals such as aluminium, tantalum, niobium, titanium or columbium monoxide
Oxidizing process generates oxide thin layer thing as electrolyte, the capacitor formed using solid electrolyte as negative electrode.Conducting polymer
Solid capacitor refers to the capacitor that solid electrolyte is conducting high polymers thing, chip-type solid aluminium electrolutic capacitor therein
Because of its small volume, in light weight, high frequency characteristics is good and high reliability be widely used in electronics, weapons, ship, communication and
All kinds of high-end electronic equipments such as medical electronics.
T/R components refer to the part between video and antenna in a wireless transceiver system, i.e. T/R components one terminate day
Line, a wireless transceiver system is formed once video processing unit in termination.Core of the T/R components as Connectors for Active Phased Array Radar
Part, with the continuous development in military radar field, it is proposed in terms of small size, high frequency, high-power and reliability
Higher requirement.Two generation T/R element bias voltages of a new generation's spaceborne, airborne and Shipboard Radar System application are from original 8V-
28V is arrived in 10V liftings, and this just proposes higher voltage request, but tradition to the chip-type solid aluminium electrolutic capacitor in T/R components
Chemical polymerization, electrochemical polymerization process be not suitable for produce high pressure sheet type aluminum electrolytic capacitor.
In order to meet two generation T/R component high pressures, small size, high frequency, high-power and high reliability requirement, high pressure is researched and developed
Chip-type solid aluminium electrolutic capacitor is very urgent.
The content of the invention
It is an object of the invention to provide a kind of mixed polymerization solution, and it is used to be made uniform, fine and close, has proof voltage energy
The electroconductive polymer layer that power is strong, leakage current is small.
Another object of the present invention is to provide a kind of hybrid polymerization technique of chip-type solid aluminium electrolutic capacitor, operation
Simply, obtained solid electrolyte layer is uniform, fine and close, and strong with electrical conductivity height, proof voltage ability, leakage current is small, property under high temperature
Can be reliable the advantages of.
Another object of the present invention is to provide a kind of chip-type solid aluminium electrolutic capacitor, its ESR excellent performances, proof voltage
Ability is strong, can prepare 20V and above product.
The present invention is solved its technical problem and realized using following technical scheme.
The present invention proposes a kind of mixed polymerization solution, and it includes chemical polymerization solution and dispersin polymerization liquid, wherein, chemistry is poly-
Solution percentage is closed mainly to be made up of following raw material：0.1%-8% conductive high polymer monomers, 3%-20% oxidations
Agent, 70%-85% solvents, and 0.5%-10% coupling agents；Dispersin polymerization liquid is comprising poly- (2,5- thioxene), gathered
The dispersion liquid of (3- methoxythiophenes), one or more of mixtures in poly- (3-4- second diene thioxene).
Further, in present pre-ferred embodiments, above-mentioned conductive high polymer monomer is thiophene, 2,5- dimethyl thiophenes
One or more of mixtures in fen, 3- methoxythiophenes, 3-4- second diene thioxenes.
Further, in present pre-ferred embodiments, above-mentioned oxidant is iron chloride, p-methyl benzenesulfonic acid iron, persulfuric acid
One or more of mixtures in ammonium, sodium peroxydisulfate, potassium permanganate.
Further, in present pre-ferred embodiments, above-mentioned solvent is organic molten containing saturated hydrocarbons, aromatic hydrocarbon or alcohols
One or more of mixtures of agent.
Further, in present pre-ferred embodiments, above-mentioned coupling agent is in tetraethyl titanate coupling agent, silane coupler
One or more of mixtures.
Further, in present pre-ferred embodiments, the solid content of above-mentioned dispersin polymerization liquid is 3%-12%.
A kind of hybrid polymerization technique of chip-type solid aluminium electrolutic capacitor using above-mentioned mixed polymerization solution, it is wrapped
Include following steps：
S1, aluminium foil to be polymerized is put into preprocessing solution to progress material surface modifying processing, preprocessing solution is main
It is made up of solvent and coupling agent, is taken out after impregnating 8-12min, dried, obtains pre-processing aluminium foil；
S2, pretreatment aluminium foil is put into chemical polymerization solution progress first stage polymerization, taken out after impregnating 8-12min,
Drying；
S3, repeat step S2 are common 2-4 times；
S4, the obtained aluminium foils of step S3 are put into dispersin polymerization liquid to progress second stage polymerization, taken out after 8-12min,
Drying；
S5, repeat step S4 are common 10-15 times, at least again using a kind of different dispersin polymerization liquid of solid content in repetitive process
Carry out, until aluminium foil surface forms the close uniform solid electrolyte layer of matter；
S6, the solid electrolyte layer surface of the obtained aluminium foils of step S5 sequentially formed into carbon containing cathode layer, silver-contained cathode layer,
Monolithic capacitor element is made；
S7, by monolithic capacitor element stack, moulded package, chip-type solid aluminium electrolutic capacitor is made.
Further, in present pre-ferred embodiments, the weight ratio of solvent and coupling agent in above-mentioned preprocessing solution
For 100：3-7.
Further, in present pre-ferred embodiments, the furnace drying method after above-mentioned material surface modification treatment is：It is put into
110-125 DEG C of baking oven 20-40min；
First stage polymerization after furnace drying method be：It is put into 45-60 DEG C, 35%-55%RH climatic chamber 20-
40min；
Second stage polymerization after furnace drying method be：It is put into 110-125 DEG C of baking oven 20-60min.
A kind of chip-type solid aluminium electrolutic capacitor, it is according to the hybrid poly- of above-mentioned chip-type solid aluminium electrolutic capacitor
Technique is closed to be made.
The mixed polymerization solution of the embodiment of the present invention, chip-type solid aluminium electrolutic capacitor and its hybrid polymerization technique have
Beneficial effect is：The mixed polymerization solution of the embodiment of the present invention includes chemical polymerization solution and dispersin polymerization liquid, wherein, chemical polymerization
Solution percentage is mainly made up of following raw material：0.1%-8% conductive high polymer monomers, 3%-20% oxidants,
70%-85% solvents, and 0.5%-10% coupling agents；Dispersin polymerization liquid is to include poly- (2,5- thioxene), poly- (3- first
Epoxide thiophene), the dispersion liquid of one or more of mixtures in poly- (3-4- second diene thioxene), the mixed polymerization solution
It is uniform, fine and close for being made, there is the electroconductive polymer layer that proof voltage ability is strong, leakage current is small；Chip-type solid alminium electrolytic condenser
The hybrid polymerization technique of device is that aluminium foil is repeatedly polymerize using preprocessing solution, chemical polymerization solution and dispersin polymerization liquid
Processing, until aluminium foil surface forms the solid electrolyte layer of dense uniform, then capacitor is made, the technological operation is simple, is made
Solid electrolyte layer uniformly, it is fine and close, have that electrical conductivity is high, proof voltage ability is strong, leakage current is small, and dependable performance is excellent under high temperature
Point；The ESR excellent performances of obtained chip-type solid aluminium electrolutic capacitor, proof voltage ability are strong, can prepare 20V and above product.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, it is the conventional production that can be obtained by commercially available purchase
Product.
Mixed polymerization solution to the embodiment of the present invention, chip-type solid aluminium electrolutic capacitor and its hybrid polymerization work below
Skill is specifically described.
The embodiment of the present invention provides a kind of mixed polymerization solution, and it includes chemical polymerization solution and dispersin polymerization liquid.Chemistry
Polymeric solution percentage is mainly made up of following raw material：0.1%-8% conductive high polymer monomers, 3%-20% oxidations
Agent, 70%-85% solvents, and 0.5%-10% coupling agents.Wherein, conductive high polymer monomer is thiophene, 2,5- dimethyl thiophenes
One or more of mixtures in fen, 3- methoxythiophenes, 3-4- second diene thioxenes.Oxidant is iron chloride, right
One or more of mixtures in toluenesulfonic acid iron, ammonium persulfate, sodium peroxydisulfate, potassium permanganate.Solvent is to contain saturated hydrocarbons, virtue
One or more of mixtures of fragrant hydrocarbon or alcohol organic solvent, can be deionized water and absolute ethyl alcohol, butanol, hexanol, third
One or more of mixtures in alcohol, propane diols, glycerine etc..Coupling agent is in tetraethyl titanate coupling agent, silane coupler
One or more of mixtures.
Dispersin polymerization liquid is to include poly- (2,5- thioxene), poly- (3- methoxythiophenes), poly- (3-4- second diene diformazans
Base thiophene) in one or more of mixtures dispersion liquid, the solid content of dispersin polymerization liquid is 3%-12%.Dispersin polymerization liquid can
Be by one kind in poly- (2,5- thioxene), poly- (3- methoxythiophenes), poly- (3-4- second diene thioxene) or
Several mixtures are scattered in the dispersion liquid formed in solvent, and solvent is one containing saturated hydrocarbons, aromatic hydrocarbon or alcohol organic solvent
Kind or several mixtures.
The mixed polymerization solution of the embodiment of the present invention is used to carry out polymerization processing to aluminium foil, wherein, coupling agent is handling
Aluminium foil surface, improve its capacity extraction rate；Dispersion liquid is pressure-resistant to strengthen the intensity of electroconductive polymer layer and lifting product.
The embodiment of the present invention also provides a kind of chip-type solid aluminium electrolutic capacitor using above-mentioned mixed polymerization solution
Hybrid polymerization technique, it comprises the following steps：
S1, aluminium foil to be polymerized is put into preprocessing solution to progress material surface modifying processing, preprocessing solution is main
It is made up of solvent and coupling agent, is taken out after impregnating 8-12min, dries, be specifically put into 110-125 DEG C of baking oven 20-40min, obtain
To pretreatment aluminium foil.In the present embodiment, the weight ratio of solvent and coupling agent in preprocessing solution is 100：3-7, solvent be containing
There are one or more of mixtures of saturated hydrocarbons, aromatic hydrocarbon or alcohol organic solvent.Coupling agent is tetraethyl titanate coupling agent, silane
One or more of mixtures in coupling agent.
S2, pretreatment aluminium foil is put into chemical polymerization solution progress first stage polymerization, taken out after impregnating 8-12min,
Drying, is specifically put into 45-60 DEG C, 35%-55%RH climatic chamber 20-40min.
S3, repeat step S2 are common 2-4 times.
S4, the obtained aluminium foils of step S3 are put into dispersin polymerization liquid to progress second stage polymerization, taken out after 8-12min,
Drying, is specifically put into 110-125 DEG C of baking oven 20-60min.
S5, repeat step S4 are common 10-15 times, at least again using a kind of different dispersin polymerization liquid of solid content in repetitive process
Carry out, until aluminium foil surface forms the close uniform solid electrolyte layer of matter.
The present embodiment first uses solid content repeatedly to be polymerize to aluminium foil for a dispersin polymerization liquid A, then use solid content for
The dispersin polymerization liquid C that b dispersin polymerization liquid B and solid content is c is repeatedly polymerize to aluminium foil circulation.It can also first use and contain admittedly
Measure and aluminium foil is repeatedly polymerize for a dispersin polymerization liquid A, then use solid content repeatedly to be gathered for b dispersin polymerization liquid B
Close.
S6, the solid electrolyte layer surface of the obtained aluminium foils of step S5 sequentially formed into carbon containing cathode layer, silver-contained cathode layer,
Monolithic capacitor element is made.
S7, by monolithic capacitor element stack, moulded package, chip-type solid aluminium electrolutic capacitor is made.
In the present embodiment, the chemical polymerization process carried out using chemical polymerization solution can be prepared uniform, fine and close, have
The electroconductive polymer layer of high conductivity, draw the capacity of capacitor finished product, loss is small, and ESR is small, and uses dispersin polymerization liquid
The polymerization technique of progress can make that the conductive polymer layer proof voltage ability of preparation is strong, leakage current is small, dependable performance under high temperature.
The embodiment of the present invention also provides a kind of chip-type solid aluminium electrolutic capacitor, and it is according to above-mentioned chip-type solid aluminium electricity
The hybrid polymerization technique of electrolysis condenser is made.Conductive polyelectrolyte is specifically prepared using hybrid polymerization technique, with
Obtain ESR excellent performances, the strong conducting polymer chip solid aluminum electrolytic capacitor of proof voltage ability, can prepare 20V and 20V with
Upper product.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of chip-type solid aluminium electrolutic capacitor, and it is made according to following preparation method：
(1) preprocessing solution is prepared：It is (molten that 50g silane couplers (coupling agent) are added to 1000g ethanol solutions
Agent) in, magnetic agitation 10min.
Prepare chemical polymeric solution：It is (molten that 100g p-methyl benzenesulfonic acid iron (oxide) is added to 1000g ethanol solutions
Agent) in, magnetic agitation 10min, 8g silane couplers (coupling agent) are added, magnetic agitation 5min, add 12g 2,5- dimethyl
Thiophene (conductive high polymer monomer), magnetic agitation 5min.
Dispersin polymerization liquid A, dispersin polymerization liquid B, dispersin polymerization liquid C are prepared respectively：Dispersin polymerization liquid A is by poly- (2,5- bis-
Methylthiophene) dispersion liquid formed in ethanol solution (solvent) is scattered in, its solid content is 3.5%；Dispersin polymerization liquid B is
Poly- (2,5- thioxene) is scattered in the dispersion liquid formed in ethanol solution (solvent), its solid content is 8.5%；Point
It is that poly- (2,5- thioxene) is scattered in the dispersion liquid formed in ethanol solution (solvent) to dissipate polymer fluid C, and it contains admittedly
Measure as 10.5%.
(2) with the trade mark：Y100LN02-67VF, specific volume：19.1μF/cm2Aluminium foil is aluminium foil to be polymerized, will be pre-processed molten
Liquid is poured into dipping tank, is put into aluminium foil to be polymerized, impregnates 10min, is then placed in 120 DEG C of drying 30min in baking oven.
(3) chemical polymerization solution is poured into another dipping tank, is put into the aluminium foil that step (2) obtains, impregnate 10min, so
50 DEG C are put into afterwards, 30min in 40%RH climatic chamber.
(4) repeat step (3) 2 times.
(5) dispersion liquid A is poured into another dipping tank, is put into the aluminium foil that step (4) obtains, impregnated 10min, be then placed in
120 DEG C of drying 30min in baking oven.
(6) repeat step (5) 4 times.
(7) dispersion liquid B is poured into another dipping tank, is put into the aluminium foil that step (6) obtains, impregnated 5min, be then placed in
120 DEG C of drying 60min in baking oven.
(8) dispersion liquid C is poured into another dipping tank, is put into the aluminium foil that step (7) obtains, impregnated 5min, be then placed in
120 DEG C of drying 60min in baking oven.
(9) repeat step (7)-(8) 4 times, aluminium foil surface form fine and close, uniform solid electrolyte layer.
(10) it is cloudy to sequentially form carbon containing cathode layer, argentiferous for the solid electrolyte layer outer surface of the aluminium foil obtained in step (9)
Pole layer, monolithic capacitor element is made.
(11) by 2 layers of monolithic capacitor element stack, moulded package, chip-type solid aluminium electrolutic capacitor is made.
Embodiment 2
The present embodiment provides a kind of chip-type solid aluminium electrolutic capacitor, and it is made according to following preparation method：
(1) preprocessing solution is prepared：It is (molten that 50g silane couplers (coupling agent) are added to 1000g ethanol solutions
Agent) in, magnetic agitation 10min.
Prepare chemical polymeric solution：It is (molten that 100g p-methyl benzenesulfonic acid iron (oxide) is added to 1000g ethanol solutions
Agent) in, magnetic agitation 10min, 8g silane couplers (coupling agent) are added, magnetic agitation 5min, add 12g 2,5- dimethyl
Thiophene (conductive high polymer monomer), magnetic agitation 5min.
Dispersin polymerization liquid A, dispersin polymerization liquid B, dispersin polymerization liquid C are prepared respectively：Dispersin polymerization liquid A is by poly- (2,5- bis-
Methylthiophene) dispersion liquid formed in ethanol solution (solvent) is scattered in, its solid content is 3.5%；Dispersin polymerization liquid B is
Poly- (2,5- thioxene) is scattered in the dispersion liquid formed in ethanol solution (solvent), its solid content is 8.5%；Point
It is that poly- (2,5- thioxene) is scattered in the dispersion liquid formed in ethanol solution (solvent) to dissipate polymer fluid C, and it contains admittedly
Measure as 10.5%.
(2) with the trade mark：Y100LN02-67VF, specific volume：19.1μF/cm2Aluminium foil is aluminium foil to be polymerized, will be pre-processed molten
Liquid is poured into dipping tank, is put into aluminium foil to be polymerized, impregnates 10min, is then placed in 120 DEG C of drying 30min in baking oven.
(3) chemical polymerization solution is poured into another dipping tank, is put into the aluminium foil that step (2) obtains, impregnate 10min, so
50 DEG C are put into afterwards, 30min in 40%RH climatic chamber.
(4) repeat step (3) 2 times.
(5) dispersion liquid A is poured into another dipping tank, is put into the aluminium foil that step (4) obtains, impregnated 10min, be then placed in
120 DEG C of drying 30min in baking oven.
(6) repeat step (5) 4 times.
(7) dispersion liquid B is poured into another dipping tank, is put into the aluminium foil that step (6) obtains, impregnated 5min, be then placed in
120 DEG C of drying 60min in baking oven.
(8) repeat step (7) 4 times.
(9) dispersion liquid C is poured into another dipping tank, is put into the aluminium foil that step (8) obtains, impregnated 5min, be then placed in
120 DEG C of drying 60min in baking oven.
(10) repeat step (9) 4 times, aluminium foil surface form fine and close, uniform solid electrolyte layer.
(11) it is cloudy to sequentially form carbon containing cathode layer, argentiferous for the solid electrolyte layer outer surface of the aluminium foil obtained in step (10)
Pole layer, monolithic capacitor element is made.
(12) by 2 layers of monolithic capacitor element stack, moulded package, chip-type solid aluminium electrolutic capacitor is made.
Embodiment 3
The present embodiment provides a kind of chip-type solid aluminium electrolutic capacitor, and it is made according to following preparation method：
(1) preprocessing solution is prepared：It is (molten that 50g silane couplers (coupling agent) are added to 1000g ethanol solutions
Agent) in, magnetic agitation 10min.
Prepare chemical polymeric solution：It is (molten that 100g p-methyl benzenesulfonic acid iron (oxide) is added to 1000g ethanol solutions
Agent) in, magnetic agitation 10min, 8g silane couplers (coupling agent) are added, magnetic agitation 5min, add 12g 2,5- dimethyl
Thiophene (conductive high polymer monomer), magnetic agitation 5min.
Dispersin polymerization liquid A, dispersin polymerization liquid B are prepared respectively：Dispersin polymerization liquid A is that poly- (2,5- thioxene) is scattered
The dispersion liquid formed in ethanol solution (solvent), its solid content are 3.5%；Dispersin polymerization liquid B is by poly- (2,5- diformazans
Base thiophene) dispersion liquid formed in ethanol solution (solvent) is scattered in, its solid content is 8.5%.
(2) with the trade mark：Y100LN02-67VF, specific volume：19.1μF/cm2Aluminium foil is aluminium foil to be polymerized, will be pre-processed molten
Liquid is poured into dipping tank, is put into aluminium foil to be polymerized, impregnates 10min, is then placed in 120 DEG C of drying 30min in baking oven.
(3) chemical polymerization solution is poured into another dipping tank, is put into the aluminium foil that step (2) obtains, impregnate 10min, so
50 DEG C are put into afterwards, 30min in 40%RH climatic chamber.
(4) repeat step (3) 2 times.
(5) dispersion liquid A is poured into another dipping tank, is put into the aluminium foil that step (4) obtains, impregnated 10min, be then placed in
120 DEG C of drying 30min in baking oven.
(6) repeat step (5) 6 times.
(7) dispersion liquid B is poured into another dipping tank, is put into the aluminium foil that step (6) obtains, impregnated 5min, be then placed in
120 DEG C of drying 60min in baking oven.
(8) repeat step (7) 6 times, aluminium foil surface form fine and close, uniform solid electrolyte layer.
(9) the solid electrolyte layer outer surface of the aluminium foil obtained in step (8) sequentially forms carbon containing cathode layer, containing silver cathode
Layer, monolithic capacitor element is made.
(10) by 2 layers of monolithic capacitor element stack, moulded package, chip-type solid aluminium electrolutic capacitor is made.
Embodiment 4
The present embodiment provides a kind of chip-type solid aluminium electrolutic capacitor, and its preparation method and the preparation method of embodiment 1 are big
Cause identical, difference is：Chemical polymerization solution uses butanol as solvent.
Embodiment 5
The present embodiment provides a kind of chip-type solid aluminium electrolutic capacitor, and its preparation method and the preparation method of embodiment 1 are big
Cause identical, difference is：When preparing chemical polymeric solution, 4g silane couplers, 4g tetraethyl titanate coupling agent conducts are added
Coupling agent, 24g 2 is added, 5- thioxenes are as conductive high polymer monomer.
The properties of the chip-type solid aluminium electrolutic capacitor in embodiment 1-5 are detected below by way of experiment, had
Body method is to select 5 samples at random from the product of each embodiment, and numbering is 1,2,3,4,5 respectively, then detects theirs
Capacity C, loss tangent tan δ, equivalent series resistance ESR, leakage current LC, concrete outcome are as shown in the table.
The properties of the chip-type solid aluminium electrolutic capacitor of table 1
As can be seen from the above table, the solid electrolytic capacitor produced according to the hybrid polymerization technique of the embodiment of the present invention
The excellent performances such as the capacity of device, loss, ESR, leakage current.
In summary, the mixed polymerization solution of the embodiment of the present invention is used to be made uniform, fine and close, has proof voltage ability
By force, the small electroconductive polymer layer of leakage current；The hybrid polymerization technique of chip-type solid aluminium electrolutic capacitor it is simple to operate, be made
Solid electrolyte layer uniformly, it is fine and close, have that electrical conductivity is high, proof voltage ability is strong, leakage current is small, and dependable performance is excellent under high temperature
Point；The ESR excellent performances of chip-type solid aluminium electrolutic capacitor, proof voltage ability are strong, can prepare 20V and above product.
Embodiments described above is part of the embodiment of the present invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
- A kind of 1. mixed polymerization solution, it is characterised in that it includes chemical polymerization solution and dispersin polymerization liquid, wherein, describedization Polymeric solution percentage is learned mainly to be made up of following raw material：0.1%-8% conductive high polymer monomers, 3%-20% oxygen Agent, 70%-85% solvents, and 0.5%-10% coupling agents；The dispersin polymerization liquid is to include poly- (2,5- dimethyl thiophenes Fen), poly- (3- methoxythiophenes), the dispersion liquid of one or more of mixtures in poly- (3-4- second diene thioxene).
- 2. mixed polymerization solution according to claim 1, it is characterised in that the conductive high polymer monomer be thiophene, 2, One or more of mixtures in 5- thioxenes, 3- methoxythiophenes, 3-4- second diene thioxenes.
- 3. mixed polymerization solution according to claim 1, it is characterised in that the oxidant is iron chloride, to toluene sulphur One or more of mixtures in sour iron, ammonium persulfate, sodium peroxydisulfate, potassium permanganate.
- 4. mixed polymerization solution according to claim 1, it is characterised in that the solvent is to contain saturated hydrocarbons, aromatic hydrocarbon Or one or more of mixtures of alcohol organic solvent.
- 5. mixed polymerization solution according to claim 1, it is characterised in that the coupling agent be tetraethyl titanate coupling agent, One or more of mixtures in silane coupler.
- 6. mixed polymerization solution according to claim 1, it is characterised in that the solid content of the dispersin polymerization liquid is 3%- 12%.
- A kind of 7. hybrid polymerization of chip-type solid aluminium electrolutic capacitor using mixed polymerization solution as claimed in claim 1 Technique, it is characterised in that it comprises the following steps：S1, aluminium foil to be polymerized is put into preprocessing solution to progress material surface modifying processing, the preprocessing solution is main It is made up of solvent and coupling agent, is taken out after impregnating 8-12min, dried, obtains pre-processing aluminium foil；S2, the pretreatment aluminium foil is put into chemical polymerization solution progress first stage polymerization, taken out after impregnating 8-12min, Drying；S3, repeat step S2 are common 2-4 times；S4, the obtained aluminium foils of step S3 are put into dispersin polymerization liquid to progress second stage polymerization, take out, dry after 8-12min；S5, repeat step S4 are common 10-15 times, are at least entered again using a kind of different dispersin polymerization liquid of solid content in repetitive process OK, until aluminium foil surface forms the close uniform solid electrolyte layer of matter；S6, the solid electrolyte layer surface of the obtained aluminium foils of step S5 sequentially formed into carbon containing cathode layer, silver-contained cathode layer, be made Monolithic capacitor element；S7, by the monolithic capacitor element stack, moulded package, chip-type solid aluminium electrolutic capacitor is made.
- 8. the hybrid polymerization technique of chip-type solid aluminium electrolutic capacitor according to claim 7, it is characterised in that described The weight ratio of solvent and coupling agent in preprocessing solution is 100：3-7.
- 9. the hybrid polymerization technique of chip-type solid aluminium electrolutic capacitor according to claim 7, it is characterised in that material Furnace drying method after surface modification treatment is：It is put into 110-125 DEG C of baking oven 20-40min；First stage polymerization after furnace drying method be：It is put into 45-60 DEG C, 35%-55%RH climatic chamber 20-40min；Second stage polymerization after furnace drying method be：It is put into 110-125 DEG C of baking oven 20-60min.
- 10. a kind of chip-type solid aluminium electrolutic capacitor, it is characterised in that it is according to as any one of claim 7 to 9 The hybrid polymerization technique of chip-type solid aluminium electrolutic capacitor be made.
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