CN107978453A - Chemical polymerization solution, conducting polymer solid sheet type aluminum electrolytic capacitor and preparation method thereof - Google Patents
Chemical polymerization solution, conducting polymer solid sheet type aluminum electrolytic capacitor and preparation method thereof Download PDFInfo
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- CN107978453A CN107978453A CN201711176799.XA CN201711176799A CN107978453A CN 107978453 A CN107978453 A CN 107978453A CN 201711176799 A CN201711176799 A CN 201711176799A CN 107978453 A CN107978453 A CN 107978453A
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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
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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
- H01G9/15—Solid electrolytic capacitors
Abstract
A kind of chemical polymerization solution, conducting polymer solid sheet type aluminum electrolytic capacitor and preparation method thereof, are related to conducting polymer solid sheet type aluminum electrolytic capacitor production technical field.Chemical polymerization solution weight percentage forms：0.1% 10% monomers；2% 20% oxidants；60% 93% solvents；0.5% 10% coupling agents, the stability of the chemical polymerization solution is good, the solid electrolyte layer controllable for performance to be made, so as to obtain the capacitor with estimated performance.The preparation method of the conducting polymer solid sheet type aluminum electrolytic capacitor is to carry out multiple chemical polymerization processing to aluminium foil using aqueous premix, chemical polymerization solution and mixed liquor, until aluminium foil surface forms the close uniform solid electrolyte layer of matter, capacitor is made again, this method is simple.Electrical parameter using conducting polymer solid sheet type aluminum electrolytic capacitor made from chemical polymerization solution is good, superior performance, can be applied in high power capacity product.
Description
Technical field
The present invention relates to conducting polymer solid sheet type aluminum electrolytic capacitor production technical field, and more particularly to one kindization
Learn polymeric solution, conducting polymer solid sheet type aluminum electrolytic capacitor and preparation method thereof.
Background technology
In recent years, cpu frequency is higher and higher, and the requirement of the high heat of generation to mainboard capacitance is also higher and higher, Ge great Zhu
Plate manufacturer has used solid electrolytic capacitor on the mainboard of production one after another so that the solid electrolytic capacitor city in global range
Field demand raises up rapidly and yields unusually brilliant results.Solid electrolytic capacitor is in the oxygen such as the valve metals such as aluminium, tantalum, niobium, titanium or columbium monoxide
The surface of compound generates oxide thin layer thing as electrolyte using oxidizing process, the capacitance formed using solid electrolyte as cathode
Device, conductive solid polymer capacitor refer to the capacitor that solid electrolyte is conducting polymer.And as global communication produces
Product enter " the high power, low resistance " epoch, conductive solid polymer capacitor because have excellent heat endurance, frequency characteristic,
Low ESR and high reliability, the terminal electronic product of electronic circuit and long-term effect suitable for low resistance demand.Together
When show with laptop, mobile phone, flat-panel monitor, digital switch, communication power supply, automotive electronics, instrument and meter and LCD
Show the expansion in device market, the demand of conductive solid polymer capacitor is also increasing.
Conducting polymer solid sheet type aluminum electrolytic capacitor is as a member in conductive solid polymer capacitor, it is not only
Have the impedance frequency characteristic of excellent electrical property, temperature stability and approximate ideal capacitor, also have concurrently miniaturization, chip type,
The good characteristics such as lightweight, make it be widely used in every field, and market demand is huge.Domestic each manufacturer mainly makes at present
The dielectric substrate of the conducting polymer solid sheet type aluminum electrolytic capacitor prepared with two step method, but the polymerization bar of conducting polymer
Part has a significant impact the property of its polymerization process and polymer, particularly has to the electric conductivity of reaction speed and conducting polymer
Material impact.Likewise, the solid electrolyte application this conducting polymer is electric in conducting polymer solid sheet type aluminum electrolytic
When in container, capacity, loss and the ESR of solid capacitor can not also obtain the solid of particular characteristic there are larger difference at present
Capacitor., can not and current conducting polymer solid sheet type aluminum electrolytic capacitor is mainly used in the product of 2V-6.3V
Applied in the product of other high power capacity.
Prepare that electrical parameter is good, and superior performance, can be applied to the conducting polymer in high power capacity product therefore, it is necessary to one kind
The method of solid sheet type aluminum electrolytic capacitor.
The content of the invention
It is an object of the invention to provide a kind of chemical polymerization solution, its stability is good, and for being made, performance is controllable to be consolidated
Body dielectric substrate, so as to obtain the capacitor with estimated performance.
Another object of the present invention is to provide a kind of conducting polymer solid sheet type aluminum electrolytic capacitor, its electrical parameter is good
Good, superior performance, can be applied in high power capacity product.
Another object of the present invention is to provide a kind of preparation method of conducting polymer solid sheet type aluminum electrolytic capacitor,
Method is simple.
The present invention is solved its technical problem and is realized using following technical scheme.
The present invention proposes a kind of chemical polymerization solution, and percentage, it is mainly made of following raw material：
Wherein, one or more of mixtures of the coupling agent at least in silane coupling agent, titanate coupling agent.
Further, in present pre-ferred embodiments, monomer is pyrroles, N- methylpyrroles, N- N-ethyl pyrrole Ns, 3- decoyls
One or more of mixtures in base pyrroles thiophene, 3,4- ethylenedioxy thiophenes, 3- methoxythiophenes, 3- amoxy thiophene.
Further, in present pre-ferred embodiments, oxidant is iron chloride, p-methyl benzenesulfonic acid iron, ammonium persulfate, mistake
One or more of mixtures in sodium sulphate, potassium permanganate.
Further, in present pre-ferred embodiments, solvent is to contain saturated hydrocarbons, aromatic hydrocarbon or alcohol organic solvent
One or more of mixtures.
A kind of preparation method of conducting polymer solid sheet type aluminum electrolytic capacitor, it comprises the following steps：
Aluminium foil to be polymerized, is put into pretreatment fluid progress first stage surface modification treatment by S1, and pretreatment fluid is main
It is made of monomer, solvent and coupling agent, is taken out after 50-120s, dried, room temperature cooling, obtains pretreatment aluminium foil；
S2, by pretreatment aluminium foil be put into chemical polymerization solution as claimed in claim 1 progress second stage chemical polymerization, 3-
Take out, dry after 10s；
More times of S3, repeat step S2；
The obtained aluminium foils of step S3, is put into the mixed liquor of solvent and coupling agent progress phase III polymer improvement by S4
Handle, taken out after 5-15min, dried；
S5, the aluminium foil for obtaining step S4, using the different chemical polymerization solution of material rate, according to step S2-S4 weights
Handle 0-4 times again, until aluminium foil surface forms the close uniform solid electrolyte layer of matter；
S6, the aluminium foil progress aluminium foil repair process by the obtained covering solid electrolyte layers of step S5；
S7, in the solid electrolyte layer surfaces of the obtained aluminium foils of step S6 sequentially form carbon containing cathode layer, silver-contained cathode layer,
Monolithic capacitor element is made；
S8, by monolithic capacitor element stack and encapsulate, and conducting polymer solid sheet type aluminum electrolytic capacitor is made.
Further, in present pre-ferred embodiments, the total degree that second stage chemical polymerization carries out is 8-25 times.
Further, in present pre-ferred embodiments, the weight ratio of solvent, monomer and coupling agent in pretreatment fluid is
100：1-5：1-10；The weight ratio of solvent and coupling agent in mixed liquor is 5-10：1.
Further, in present pre-ferred embodiments, aluminium foil to be polymerized is will to wrap salic 14VF aluminium foils to cut
It is cut into the aluminium foil of effective area 3.6mm × 4.5mm and chemical remediation oxide-film obtains.
Further, in present pre-ferred embodiments, the furnace drying method after first stage surface modification treatment is：It is put into
50-65 DEG C of baking oven 8-12min, places into 110-125 DEG C of baking oven 8-12min；
Furnace drying method after second stage chemical polymerization is：It is put into 20-60 DEG C, the climatic chamber 2- of 35%-75%RH
15min；
Last time carry out phase III polymer improvement processing after furnace drying method be：It is put into 50-65 DEG C of baking oven 15-
20min, places into 110-125 DEG C of baking oven heat treatment 15-20min.
A kind of preparation method of conducting polymer solid sheet type aluminum electrolytic capacitor, it is according to above-mentioned conducting polymer
The preparation method of solid sheet type aluminum electrolytic capacitor is made.Chemical polymerization solution, the conducting polymer solid of the embodiment of the present invention
The beneficial effect of sheet type aluminum electrolytic capacitor and preparation method thereof is：The chemical polymerization solution percentage by weight of the embodiment of the present invention
Number meter is mainly made of following raw material：0.1%-10% monomers；2%-20% oxidants；60%-93% solvents；0.5%-10%
Coupling agent, the stability of the chemical polymerization solution is good, the solid electrolyte layer controllable for performance to be made, so as to obtain having pre-
The capacitor of phase performance.The preparation method of the conducting polymer solid sheet type aluminum electrolytic capacitor is using aqueous premix, changes
Learn polymeric solution and mixed liquor and multiple chemical polymerization processing is carried out to aluminium foil, until aluminium foil surface forms the close uniform solid electricity of matter
Matter layer is solved, then capacitor is made, this method is simple.Using conducting polymer solid sheet type aluminum electrolytic made from chemical polymerization solution
The electrical parameter of capacitor is good, superior performance, can be applied in high power capacity 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 solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer, is the conventional production that can be obtained by commercially available purchase
Product.
Below to the chemical polymerization solution, conducting polymer solid sheet type aluminum electrolytic capacitor and its system of the embodiment of the present invention
Preparation Method is specifically described.
The embodiment of the present invention provides a kind of chemical polymerization solution, and percentage, it is mainly made of following raw material：
0.1%-10% monomers；2%-20% oxidants；60%-93% solvents；0.5%-10% coupling agents.
Wherein, monomer is pyrroles, N- methylpyrroles, N- N-ethyl pyrrole Ns, 3- caprylyl pyrroles thiophene, 3,4- enedioxy thiophenes
One or more of mixtures in fen, 3- methoxythiophenes, 3- amoxy thiophene.
Oxidant is iron chloride, the one or more in p-methyl benzenesulfonic acid iron, ammonium persulfate, sodium peroxydisulfate, potassium permanganate
Mixture.
Solvent is one or more of mixtures containing saturated hydrocarbons, aromatic hydrocarbon or alcohol organic solvent.
One or more of mixtures of the coupling agent at least in silane coupling agent, titanate coupling agent.
The chemical polymerization solution of the embodiment of the present invention is used to carry out chemical polymerization processing to aluminium foil, to form conducting polymer
The solid electrolyte layer of solid sheet type aluminum electrolytic capacitor.Wherein, monomer is used with oxidant reaction generation conducting polymer, solvent
With dissolved dilution conducting polymer, coupling agent is used to connect different interfaces, the contact of the chemical polymerization solution of formation with aluminium foil
Property it is good, solution forms molecule particles are uniform, capacitance is big solid electrolyte layer in aluminium foil surface.
The embodiment of the present invention provides a kind of preparation method of conducting polymer solid sheet type aluminum electrolytic capacitor, it include with
Lower step：
Aluminium foil to be polymerized, be put into pretreatment fluid and carry out first stage performance modification by S1, and pretreatment fluid is main
It is made of monomer, solvent and coupling agent, is taken out after 50-120s, dries, be specifically put into 50-65 DEG C of baking oven 8-12min, then put
Enter 110-125 DEG C of baking oven 8-12min, room temperature cooling, obtains pretreatment aluminium foil.In the present embodiment, sun of the aluminium foil as capacitor
Pole, preprocessing solution handle aluminium foil surface, can improve the capacity extraction rate of aluminium foil.The present embodiment is usually that will first include aluminium oxide
14VF aluminium foils cut into the aluminium foil of effective area 3.6mm × 4.5mm and chemical remediation oxide-film obtains aluminium foil to be polymerized, in advance
The weight ratio of solvent, monomer and coupling agent in treatment fluid is 100：1-5：1-10, monomer is pyrroles, N- methylpyrroles, N- second
Base pyrroles, 3- caprylyl pyrroles thiophene, 3,4- ethylenedioxy thiophenes, 3- methoxythiophenes, one kind in 3- amoxy thiophene or
Several mixtures.Solvent is one or more of mixtures containing saturated hydrocarbons, aromatic hydrocarbon or alcohol organic solvent.Coupling agent
One or more of mixtures at least in silane coupling agent, titanate coupling agent.
S2, by pretreatment aluminium foil be put into above-mentioned chemical polymerization solution progress second stage chemical polymerization, is taken after 3-10s
Go out, dry, be specifically put into 20-60 DEG C, the climatic chamber 2-15min of 35%-75%RH.
More times of S3, repeat step S2, the total degree that second stage chemical polymerization carries out are generally 8-25 times.
The obtained aluminium foils of step S3, is put into solvent and progress phase III polymer in the mixed liquor of coupling agent composition by S4
Improvement is handled, and is taken out after 5-15min, is dried, is specifically put into 50-65 DEG C of baking oven 15-20min.In the present embodiment, in mixed liquor
The weight ratio of solvent and coupling agent is 5-10：1, solvent is one kind containing saturated hydrocarbons, aromatic hydrocarbon or alcohol organic solvent or several
The mixture of kind.One or more of mixtures of the coupling agent at least in silane coupling agent, titanate coupling agent.
S5, the aluminium foil for obtaining step S4, using the different chemical polymerization solution of material rate, according to step S2-S4 weights
Handle 0-4 times again, until aluminium foil surface forms the close uniform solid electrolyte layer of matter.The phase III polymer finally carried out changes
Conducting oneself well the furnace drying method after reason is：50-65 DEG C of baking oven 15-20min drying is put into, places into 110-125 DEG C of baking oven heat treatment 15-
20min。
For the present embodiment during solid electrolyte layer is formed, monomer, oxidant, solvent and coupling agent are selected can phase
Together, can not also be same；The present embodiment to conducting polymer by polymerizeing solution (pretreatment fluid, chemical polymerization solution, mixed liquor)
Proportioning, polymerization reaction time, the temperature humidity of polymerisation be controlled, it is ensured that cathode conducting polymer (i.e. solid electricity
Solve matter layer) polymerization process be controllable so that the performance for the solid electrolyte layer being prepared is also controllable, can solve
The stability of polymeric solution certainly existing in the prior art is poor, causes the property of conducting polymer solid sheet type aluminum electrolytic capacitor
The problem of desired value can be reached.
S6, the aluminium foil progress aluminium foil repair process by the obtained covering solid electrolyte layers (conducting polymer) of step S5.
S7, in the solid electrolyte layer surfaces of the obtained aluminium foils of step S6 sequentially form carbon containing cathode layer, silver-contained cathode layer,
Monolithic capacitor element is made.
S8, by monolithic capacitor element stack and encapsulate, and conducting polymer solid sheet type aluminum electrolytic capacitor is made.
The embodiment of the present invention provides a kind of preparation method of conducting polymer solid sheet type aluminum electrolytic capacitor, its be according to
The preparation method of above-mentioned conducting polymer solid sheet type aluminum electrolytic capacitor is made.Chemical polymerization provided in an embodiment of the present invention
Method is simply easily implemented, and can prepare uniform, fine and close, the electroconductive polymer layer with high conductivity, i.e. solid electrolyte layer,
So as to prepare the conducting polymer solid sheet type aluminum electrolytic capacitor of 2V-16V, and the capacity of product draws, small, ESR is lost
It is small, leakage current is small, dependable performance under high temperature.
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 conducting polymer solid sheet type aluminum electrolytic capacitor, it is according to following preparation method system
：
(1) preprocessing solution is prepared：2g N- methylpyrroles (monomer) and 2g silicon are added into 100g ethanol (solvent) respectively
Alkane coupling agent (coupling agent), magnetic agitation 3min.
Prepare chemical polymeric solution：8g silane coupling agents (coupling agent) are taken to add in 100g ethanol (solvent), magnetic agitation
3min, adds 8g p-methyl benzenesulfonic acid iron (oxide), magnetic agitation 1min, adds 2g N- methylpyrroles (monomer), magnetic force stirs
Mix 1min.
Prepare mixed liquor：60g ethanol (solvent) and 10g silane coupling agents (coupling agent) are uniformly mixed.
(2) salic 14VF aluminium foils will be wrapped to cut into the aluminium foil of effective area 3.6mm × 4.5mm and be melted into reparation oxygen
After changing film, then aluminium foil to be polymerized is immersed in preprocessing solution and is taken out after 60s, be put into 60 DEG C of baking oven 10min, place into 120
DEG C baking oven 10min, room temperature cooling, obtains pretreatment aluminium foil.
(3) pretreatment aluminium foil is immersed in chemical polymerization solution and is taken out after 5s, be put into 50 DEG C, the climatic chamber of 40%RH
Taken out after 2min.
(4) repeat step (3) 22 times.
(5) aluminium foil that step (4) obtains is immersed in mixed liquor and is taken out after 10min, be put into 60 DEG C of baking oven 15min drying,
Plough under 120 DEG C of baking ovens heat treatment 15min again, after the completion of chemical polymerization process, aluminium foil surface forms the close uniform solid electrolytic of matter
Matter layer.
(6) aluminium foil of the step (5) covered with conducting polymer is subjected to aluminium foil repair process.
(7) the solid electrolyte layer outer surface of the aluminium foil obtained in step (6) sequentially forms carbon containing cathode layer, containing silver cathode
Layer, is made monolithic capacitor element.
(8) by monolithic capacitor element stack and encapsulate, conducting polymer solid sheet type aluminum electrolytic capacitor is made.
Embodiment 2
The present embodiment provides a kind of conducting polymer solid sheet type aluminum electrolytic capacitor, it is according to following preparation method system
：
(1) preprocessing solution is prepared：2g N- methylpyrroles (monomer) and 2g silicon are added into 100g ethanol (solvent) respectively
Alkane coupling agent (coupling agent), magnetic agitation 3min.
Prepare the first chemical polymerization solution：8g silane coupling agents (coupling agent) are taken to add in 100g ethanol (solvent), magnetic force
3min is stirred, adds 8g p-methyl benzenesulfonic acid iron (oxide), magnetic agitation 1min, adds 2g N- methylpyrroles (monomer), magnetic
Power stirs 1min.
Prepare the second chemical polymerization solution：6g silane coupling agents (coupling agent) are taken to add in 100g ethanol (solvent), magnetic force
3min is stirred, adds 12g p-methyl benzenesulfonic acid iron (oxide), magnetic agitation 1min, adds 4g N- methylpyrroles (monomer),
Magnetic agitation 1min.
Prepare mixed liquor：60g ethanol (solvent) and 10g silane coupling agents (coupling agent) are uniformly mixed.
(2) salic 14VF aluminium foils will be wrapped to cut into the aluminium foil of effective area 3.6mm × 4.5mm and be melted into reparation oxygen
After changing film, then aluminium foil to be polymerized is immersed in prepared preprocessing solution and is taken out after 60s, be put into 60 DEG C of baking oven 10min, then
120 DEG C of baking oven 10min are put into, room temperature cooling, obtains pretreatment aluminium foil.
(3) pretreatment aluminium foil is immersed in the first chemical polymerization solution and is taken out after 5s, be put into 50 DEG C, the constant temperature perseverance of 40%RH
Taken out after wet tank 2min.
(4) repeat step (3) 10 times.
(5) aluminium foil for obtaining step (4) immerses 10min in mixed liquor and takes out, and is put into 60 DEG C of baking oven 15min drying.
(6) aluminium foil that step 5 obtains is immersed in the second chemical polymerization solution and is taken out after 5s, be put into 50 DEG C, 40%RH
Taken out after climatic chamber 2min.
(7) repeat step (6) 11 times.
(8) aluminium foil for obtaining step (7) immerses 10min in mixed liquor and takes out, and is put into 60 DEG C of baking oven 15min drying, then
It is put into 120 DEG C of baking ovens heat treatment 15min, after the completion of chemical polymerization process, aluminium foil surface forms the close uniform solid electrolyte of matter
Layer.
(9) aluminium foil of the step (8) covered with conducting polymer is subjected to aluminium foil repair process.
(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, is made monolithic capacitor element.
(11) by monolithic capacitor element stack and encapsulate, conducting polymer solid sheet type aluminum electrolytic capacitor is made.
Embodiment 3
The present embodiment provides a kind of conducting polymer solid sheet type aluminum electrolytic capacitor, it is according to following preparation method system
：
(1) preprocessing solution is prepared：2g N- methylpyrroles (monomer) and 2g silicon are added into 100g ethanol (solvent) respectively
Alkane coupling agent (coupling agent), magnetic agitation 3min.
Prepare the first chemical polymerization solution：8g silane coupling agents (coupling agent) are taken to add in 100g ethanol (solvent), magnetic force
3min is stirred, adds 8g p-methyl benzenesulfonic acid iron (oxide), magnetic agitation 1min, adds 2g N- methylpyrroles (monomer), magnetic
Power stirs 1min.
Prepare the second chemical polymerization solution：6g silane coupling agents (coupling agent) are taken to add in 100g ethanol (solvent), magnetic force
3min is stirred, adds 12g p-methyl benzenesulfonic acid iron (oxide), magnetic agitation 1min, adds 4g N- methylpyrroles (monomer),
Magnetic agitation 1min.
Prepare the 3rd chemical polymerization solution：4g silane coupling agents (coupling agent) are taken to add in 100g ethanol (solvent), magnetic force
3min is stirred, adds 16g p-methyl benzenesulfonic acid iron (oxide), magnetic agitation 1min, adds 6g N- methylpyrroles (monomer),
Magnetic agitation 1min.
Prepare mixed liquor：60g ethanol (solvent) and 10g silane coupling agents (coupling agent) are uniformly mixed.
(2) salic 14VF aluminium foils will be wrapped to cut into the aluminium foil of effective area 3.6mm × 4.5mm and be melted into reparation oxygen
After changing film, then aluminium foil to be polymerized is immersed in prepared preprocessing solution and is taken out after 60s, be put into 60 DEG C of baking oven 10min, then
120 DEG C of baking oven 10min are put into, room temperature cooling, obtains pretreatment aluminium foil.
(3) pretreatment aluminium foil is immersed in the first chemical polymerization solution and is taken out after 5s, be put into 50 DEG C, the constant temperature perseverance of 40%RH
Taken out after wet tank 2min.
(4) repeat step (3) 7 times.
(5) aluminium foil that step (4) obtains is immersed in mixed liquor and is taken out after 10min, be put into 60 DEG C of baking oven 15min drying.
(6) aluminium foil that step (5) obtains is immersed in the second chemical polymerization solution and is taken out after 5s, be put into 50 DEG C, 40%RH
Climatic chamber 2min after take out.
(7) repeat step (6) 7 times.
(8) aluminium foil that step (7) obtains is immersed in mixed liquor and is taken out after 10min, be put into 60 DEG C of baking oven 15min drying,
Place into 120 DEG C of baking oven 15min heat treatments.
(9) aluminium foil that step (8) obtains is immersed in the 3rd chemical polymerization solution and is taken out after 5s, be put into 50 DEG C, 40%RH
Climatic chamber 2min after take out.
(10) repeat step (9) 7 times.
(11) aluminium foil that step (10) obtains is immersed in the mixed liquor of mixed liquor and is taken out after 10min, be put into 60 DEG C of baking ovens
15min is dried, and is placed into 120 DEG C of baking oven 15min and is heat-treated, and after the completion of chemical polymerization process, it is close uniformly that aluminium foil surface forms matter
Solid electrolyte layer.
(12) aluminium foil covered with conducting polymer for obtaining step (11) carries out aluminium foil repair process.
(13) 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 (12)
Pole layer, is made monolithic capacitor element.
(14) by monolithic capacitor element stack and encapsulate, conducting polymer solid sheet type aluminum electrolytic capacitor is made.
Embodiment 4
The present embodiment provides a kind of conducting polymer solid sheet type aluminum electrolytic capacitor, its preparation method and embodiment 1
Preparation method is roughly the same, and difference is：First chemical polymerization solution uses butanol as solvent.
Embodiment 5
The present embodiment provides a kind of conducting polymer solid sheet type aluminum electrolytic capacitor, its preparation method and embodiment 2
Preparation method is roughly the same, and difference is：First chemical polymerization solution, the second chemical polymerization solution use butanol as molten
Agent.
Embodiment 6
The present embodiment provides a kind of conducting polymer solid sheet type aluminum electrolytic capacitor, its preparation method and embodiment 3
Preparation method is roughly the same, and difference is：First chemical polymerization solution, the second chemical polymerization solution, the 3rd chemical polymerization
Solution uses butanol as solvent.
Embodiment 7
The present embodiment provides a kind of conducting polymer solid sheet type aluminum electrolytic capacitor, its preparation method and embodiment 3
Preparation method is roughly the same, and difference is：3rd chemical polymerization solution uses butanol as solvent.
Embodiment 8
The present embodiment provides a kind of conducting polymer solid sheet type aluminum electrolytic capacitor, its preparation method and embodiment 3
Preparation method is roughly the same, and difference is：Second chemical polymerization solution, the 3rd chemical polymerization solution use butanol as molten
Agent.
Embodiment 9
The present embodiment provides a kind of conducting polymer solid sheet type aluminum electrolytic capacitor, its preparation method and embodiment 1
Preparation method is roughly the same, and difference is：Coupling agent is used as using titanate coupling agent.
Embodiment 10
The present embodiment provides a kind of conducting polymer solid sheet type aluminum electrolytic capacitor, its preparation method and embodiment 4
Preparation method is roughly the same, and difference is：Coupling agent is used as using titanate coupling agent.
Embodiment 11
The present embodiment provides a kind of conducting polymer solid sheet type aluminum electrolytic capacitor, its preparation method and embodiment 1
Preparation method is roughly the same, and difference is：Aluminium foil is immersed in the first chemical polymerization solution and is taken out after 5s, be put into 55 DEG C,
Taken out after the climatic chamber 2min of 40%RH.
Embodiment 12
The present embodiment provides a kind of conducting polymer solid sheet type aluminum electrolytic capacitor, its preparation method and embodiment 1
Preparation method is roughly the same, and difference is：Aluminium foil is immersed in the first chemical polymerization solution and is taken out after 5s, be put into 35 DEG C,
Taken out after the climatic chamber 2min of 40%RH.
Properties below by way of experiment to the conducting polymer solid sheet type aluminum electrolytic capacitor in embodiment 1-12
It is detected, mainly detects their capacitance C, loss tan δ, ESR, leakage current LC, concrete outcome is as shown in the table.
The properties of 1 conducting polymer solid sheet type aluminum electrolytic capacitor of table
As can be seen from the above table, the electricity for the solid electrolytic capacitor produced according to the polymerization technique of the embodiment of the present invention
The excellent performances such as capacity, loss, ESR, leakage current.
In conclusion the stability of the chemical polymerization solution of the embodiment of the present invention is good, the solid controllable for performance to be made
Dielectric substrate, so as to obtain the capacitor with estimated performance.Using conducting polymer solid piece made from chemical polymerization solution
The electrical parameter of formula aluminium electrolutic capacitor is good, superior performance, can be applied in high power capacity product.The conducting polymer solid sheet type
The method of the preparation method of aluminium electrolutic capacitor is simple.
Embodiments described above is part of the embodiment of the present invention, instead of all the 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 embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of chemical polymerization solution, it is characterised in that percentage, it is mainly made of following raw material：
Wherein, one or more of mixtures of the coupling agent at least in silane coupling agent, titanate coupling agent.
2. chemical polymerization solution according to claim 1, it is characterised in that the monomer is pyrroles, N- methylpyrroles, N-
One kind in N-ethyl pyrrole N, 3- caprylyl pyrroles thiophene, 3,4- ethylenedioxy thiophenes, 3- methoxythiophenes, 3- amoxy thiophene
Or several mixture.
3. chemical 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. chemical 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. a kind of preparation method of conducting polymer solid sheet type aluminum electrolytic capacitor, it is characterised in that it comprises the following steps：
Aluminium foil to be polymerized, is put into pretreatment fluid progress first stage surface modification treatment by S1, and the pretreatment fluid is main
It is made of monomer, solvent and coupling agent, is taken out after 50-120s, dried, room temperature cooling, obtains pretreatment aluminium foil；
The pretreatment aluminium foil, is put into chemical polymerization solution as claimed in claim 1 that to carry out second stage chemistry poly- by S2
Close, taken out after 3-10s, dried；
More times of S3, repeat step S2；
S4, by the obtained aluminium foils of step S3 be put into the mixed liquor of solvent and coupling agent carry out phase III polymer improvement at
Manage, taken out after 5-15min, dried；
S5, the aluminium foil for obtaining step S4, using the different chemical polymerization solution of material rate, at step S2-S4 repetitions
Reason 0-4 times, until aluminium foil surface forms the close uniform solid electrolyte layer of matter；
S6, the aluminium foil progress aluminium foil repair process by the obtained covering solid electrolyte layers of step S5；
S7, in the solid electrolyte layer surfaces of the obtained aluminium foils of step S6 sequentially form carbon containing cathode layer, silver-contained cathode layer, is made
Monolithic capacitor element；
S8, by the monolithic capacitor element stack and encapsulate, and conducting polymer solid sheet type aluminum electrolytic capacitor is made.
6. the preparation method of conducting polymer solid sheet type aluminum electrolytic capacitor according to claim 5, it is characterised in that
The total degree that the second stage chemical polymerization carries out is 8-25 times.
7. the preparation method of conducting polymer solid sheet type aluminum electrolytic capacitor according to claim 5, it is characterised in that
The weight ratio of solvent, monomer and coupling agent in the pretreatment fluid is 100：1-5：1-10；Solvent in the mixed liquor with
The weight ratio of coupling agent is 5-10：1.
8. the preparation method of conducting polymer solid sheet type aluminum electrolytic capacitor according to claim 5, it is characterised in that
Aluminium foil to be polymerized is will to wrap that salic 14VF aluminium foils cut into the aluminium foil of effective area 3.6mm × 4.5mm and chemistry is repaiied
What multiple oxide-film obtained.
9. the preparation method of conducting polymer solid sheet type aluminum electrolytic capacitor according to claim 5, it is characterised in that
Furnace drying method after first stage surface modification treatment is：50-65 DEG C of baking oven 8-12min is put into, places into 110-125 DEG C of baking oven
8-12min；
Furnace drying method after second stage chemical polymerization is：It is put into 20-60 DEG C, the climatic chamber 2- of 35%-75%RH
15min；
Last time carry out phase III polymer improvement processing after furnace drying method be：It is put into 50-65 DEG C of baking oven 15-
20min, places into 110-125 DEG C of baking oven heat treatment 15-20min.
10. a kind of conducting polymer solid sheet type aluminum electrolytic capacitor, it is characterised in that it is according in such as claim 5 to 9
The preparation method of any one of them conducting polymer solid sheet type aluminum electrolytic capacitor is made.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110190281A (en) * | 2019-06-11 | 2019-08-30 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | A kind of electrode material and preparation method thereof and aluminium electrolutic capacitor |
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|---|---|---|---|---|
| CN1032263A (en) * | 1987-08-05 | 1989-04-05 | 三洋电机株式会社 | Solid aluminium electrolytic capacitor and manufacture method thereof |
| CN1649053A (en) * | 2005-02-05 | 2005-08-03 | 西安交通大学 | Method for producing solid sheet type electrolytic capacitor |
| CN101350253A (en) * | 2008-09-17 | 2009-01-21 | 中国振华（集团）新云电子元器件有限责任公司 | Solid electrolyte capacitor with ultra-low equivalent series resistance and manufacturing method thereof |
| CN104409212A (en) * | 2014-11-12 | 2015-03-11 | 深圳新宙邦科技股份有限公司 | Formed foil post-processing method, electrode foil and capacitor |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1032263A (en) * | 1987-08-05 | 1989-04-05 | 三洋电机株式会社 | Solid aluminium electrolytic capacitor and manufacture method thereof |
| CN1649053A (en) * | 2005-02-05 | 2005-08-03 | 西安交通大学 | Method for producing solid sheet type electrolytic capacitor |
| CN101350253A (en) * | 2008-09-17 | 2009-01-21 | 中国振华（集团）新云电子元器件有限责任公司 | Solid electrolyte capacitor with ultra-low equivalent series resistance and manufacturing method thereof |
| CN104409212A (en) * | 2014-11-12 | 2015-03-11 | 深圳新宙邦科技股份有限公司 | Formed foil post-processing method, electrode foil and capacitor |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110190281A (en) * | 2019-06-11 | 2019-08-30 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | A kind of electrode material and preparation method thereof and aluminium electrolutic capacitor |
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