CN108183034A - The preparation method of aluminium electrolutic capacitor high voltage anodization film - Google Patents
The preparation method of aluminium electrolutic capacitor high voltage anodization film Download PDFInfo
- Publication number
- CN108183034A CN108183034A CN201711284612.8A CN201711284612A CN108183034A CN 108183034 A CN108183034 A CN 108183034A CN 201711284612 A CN201711284612 A CN 201711284612A CN 108183034 A CN108183034 A CN 108183034A
- Authority
- CN
- China
- Prior art keywords
- high voltage
- aluminium
- electrolutic capacitor
- preparation
- foil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- H01G9/0032—Processes of manufacture formation of the dielectric layer
Abstract
The invention discloses a kind of preparation methods of aluminium electrolutic capacitor high voltage anodization film, it is that corrosive aluminum foil is placed in 90~100 DEG C of high purity water after reaction 5min, it is placed in progress high voltage anodization processing in 10% azelaic acid solution, that is the anode of aluminium foil connection high-voltage DC power supply, aluminium foil electrolytic bath connects the cathode of high-voltage DC power supply, after setting voltage being boosted to using constant dc, maintain constant pressure processing 10min, then it is heat-treated after being cleaned up with deionized water, i.e., forms Al on corrosive aluminum foil surface2O3High voltage anodization film.Corrosive aluminum foil is placed in progress high voltage anodization processing in the azelaic acid solution of 10wt% by the present invention, the structure and performance of anode oxide film can greatly be improved, improve the insulation performance of oxidation film, improve the content of crystal form oxidation film, so as to improve the specific capacitance of formed aluminum foil and proof voltage, formation efficiency is improved, achievees the purpose that reduce aluminium electrolutic capacitor volume.
Description
Technical field
The present invention relates to a kind of preparation methods of aluminium electrolutic capacitor high voltage anodization film, belong to aluminium electrolutic capacitor
Technical field.
Background technology
Aluminium electrolutic capacitor, also known as capacitance, a kind of energy-storage travelling wave tube, feature are that capacity is big, are the core members in electric equipment products
One of part is widely used in occasions such as energy storage conversion, liquid crystal display, integrated circuits, due to global electronic product not
Disconnected to update, global aluminium electrolutic capacitor demand is grown steadily in recent years with average more than 10% speed, industry prospect
It is very good.
Anode oxide film is the work dielectric of aluminium electrolutic capacitor, it is that aluminium foil passes through anodic oxidation in weak acid solution
And a kind of fine and close proof voltage film formed on surface, specific capacitance, heterogeneous microstructure are directly related to aluminium electroloysis electricity
Volume of a container and performance.The structure of anode oxide film is divided into amorphous Al2O3With crystal form γ-or γ '-Al2O3Two kinds.Crystal form
Oxidation film has larger relative dielectric constant and smaller pressure-resistant thickness, and capacitance is compared with amorphous oxide film height.
It is usually first to carry out corrosive aluminum foil and boiling water that modern industry, which prepares aluminium electrolutic capacitor with high voltage anodization film,
Reaction is in one layer of hydrated film of its Surface Creation, then carries out high voltage anodization in boric acid solution and the resistance to of hundreds of nanometers thickness is made
Ironed film.
In recent years, with the development that complete electronic set minimizes, user further reduces aluminium electrolutic capacitor volume and carries
The requirement of Fabrication of High Specific Capacitance is increasingly urgent, and also corresponding requirements have high quality and Fabrication of High Specific Capacitance to anode aluminium foil, therefore, it is necessary to how to carry
The performance of high oxidation film, the specific capacitance for improving electrode aluminium foil and resistance are studied.
Invention content
In view of this, in view of the deficiencies of the prior art, the present invention provides a kind of aluminium electrolutic capacitor high voltage anodization
The preparation method of film.
For solution more than technical problem, technical scheme of the present invention employs a kind of aluminium electrolutic capacitor high-voltage anode oxygen
Change the preparation method of film, it includes the following steps：
(1) forming liquid is prepared：Azelaic acid powder is configured to the azelaic acid solution that mass fraction is 10% with high purity water to put
90 ± 2 DEG C are heated in aluminium foil electrolytic bath, keeps constant temperature；
(2) hydration-treated：Corrosive aluminum foil is placed in 90~100 DEG C of high purity water and reacts 5min；
(3) by step (2), treated that aluminium foil is placed in is carried out at high voltage anodization in the azelaic acid solution in step (1)
Reason：Aluminium foil connects the anode of high-voltage DC power supply, and aluminium foil electrolytic bath connects the cathode of high-voltage DC power supply, using constant dc
After boosting to setting voltage, constant pressure processing 10min is maintained；
(4) by step (3), treated is heat-treated after aluminium foil cleans up with deionized water, i.e., in corrosive aluminum foil table
Face forms Al2O3High voltage anodization film.
Further, it after step (4) heat treatment, further includes and is handled using the identical high voltage anodization of step (3)
Condition carries out aluminium foil the operation of supplement anodized.
Further, the time that constant pressure is handled in the supplement anodized is 5min.
Further, the corrosive aluminum foil is acid etch porous high-purity aluminium foil, and purity is more than 99.99%, average pore size 1
~2 μm.
Further, the resistivity of high purity water is 16M Ω cm in the step (1).
Further, the electric current of constant dc is 50 × 10 in the step (3)-3A/cm2。
Further, voltage is set as 500V in the step (3).
Further, heat treatment is to handle 2min in 500 DEG C of air atmospheres in the step (4).
Compared with prior art, corrosive aluminum foil is placed in progress high-voltage anode oxygen in the azelaic acid solution of 10wt% by the present invention
Change is handled, and can greatly improve the structure and performance of anode oxide film, improves the insulation performance of oxidation film, improves crystal form oxidation film
Content, so as to improve the specific capacitance of formed aluminum foil and proof voltage, improve formation efficiency, reach and reduce aluminium electrolutic capacitor volume
Purpose.
Description of the drawings
Fig. 1 current density and specific resistance change curve in azelaic acid solution mesohigh anode oxidation process for aluminium foil；
Current density and specific resistance variation in boric acid+azelaic acid solution mesohigh anode oxidation process are bent for aluminium foil by Fig. 2
Line chart；
Fig. 3 supplements current density and specific resistance change curve in anode oxidation process for aluminium foil in azelaic acid solution；
Fig. 4 supplements current density and specific resistance variation song in anode oxidation process for aluminium foil in boric acid+azelaic acid solution
Line chart.
Specific embodiment
In order to which those skilled in the art is made to more fully understand technical scheme of the present invention, With reference to embodiment
The present invention is described in further detail.
Embodiment 1：
A kind of preparation method of aluminium electrolutic capacitor high voltage anodization film, includes the following steps：
(1) forming liquid is prepared：Azelaic acid powder is configured to mass fraction with high purity water that resistivity is 16M Ω cm is
10% azelaic acid solution, which is placed in aluminium foil electrolytic bath, is heated to 90 ± 2 DEG C, keeps constant temperature；
(2) hydration-treated：Acid etch porous high-purity aluminium foil is cut into the sample that specification is 50mm × 10mm × 0.1mm to be placed in
5min is reacted in 90~100 DEG C of high purity water；
(3) by step (2), treated that aluminium foil is placed in is carried out at high voltage anodization in the azelaic acid solution in step (1)
Reason：Aluminium foil connects the anode of high-voltage DC power supply, and aluminium foil electrolytic bath connects the cathode of high-voltage DC power supply, using 50 × 10-3A/
cm2Constant dc boost to 500V setting voltage after, maintain constant pressure processing 10min；
(4) by step (3), treated is transferred in Muffle furnace after aluminium foil cleans up with deionized water, in 500 DEG C of skies
2min is handled in gas atmosphere, supplement sun is then carried out to aluminium foil using the identical high voltage anodization treatment conditions of step (3) again
Pole oxidation processes：50×10-3A/cm2Constant dc boost to constant pressure processing 5min after 500V, i.e., on corrosive aluminum foil surface
Form Al2O3High voltage anodization film.
Embodiment 2：
A kind of preparation method of aluminium electrolutic capacitor high voltage anodization film, includes the following steps：
(1) forming liquid is prepared：By electron level boric acid powder, azelaic acid powder and high purity water of the resistivity for 16M Ω cm
The forming liquid that mass fraction is+5% azelaic acid solution of 5% boric acid solution is configured to be placed in aluminium foil electrolytic bath and be heated to 90 ± 2
DEG C, keep constant temperature；
(2) hydration-treated：Acid etch porous high-purity aluminium foil is cut into the sample that specification is 50mm × 10mm × 0.1mm to be placed in
5min is reacted in 90~100 DEG C of high purity water；
(3) by step (2) treated aluminium foil is placed in progress high voltage anodization processing in the forming liquid in step (1)：
Aluminium foil connects the anode of high-voltage DC power supply, and aluminium foil electrolytic bath connects the cathode of high-voltage DC power supply, using 50 × 10-3A/cm2
Constant dc boost to 500V setting voltage after, maintain constant pressure processing 10min；
(4) by step (3), treated is transferred in Muffle furnace after aluminium foil cleans up with deionized water, in 500 DEG C of skies
2min is handled in gas atmosphere, supplement sun is then carried out to aluminium foil using the identical high voltage anodization treatment conditions of step (3) again
Pole oxidation processes：50×10-3A/cm2Constant dc boost to constant pressure processing 5min after 500V, i.e., on corrosive aluminum foil surface
Form Al2O3High voltage anodization film.
It is the oxidation film that 500v constant pressures 10min is obtained when aoxidizing for the first time to Examples 1 and 2 high voltage anodization
Into electric current and resistance change measurement, curve graph is obtained referring to shown in Fig. 1, Fig. 2.As seen from the figure, azelaic acid solution and 5% boric acid+
The current resistor variation tendency of 5% azelaic acid solution, two solution is close, electric current downward trend and resistance ascendant trend all than very fast,
All to peaking when 8min or so.In azelaic acid solution, specific resistance reaches 460 Ω cm after final chemical conversion-2Left and right, and
There was only 260 Ω cm in+5% azelaic acid solution of 5% boric acid-2.Being higher by for resistance ratio the latter after the former aoxidizes will by about one time, says
The insulating properties of film for aoxidizing formation in bright azelaic acid solution is more preferable, i.e. crystalline content higher.Due to chemical conversion resistance and anodic oxidation
The thickness of film is related, and the Waste Acid From Hua Cheng Foil proof voltage formed in azelaic acid solution can be speculated than in+5% azelaic acid solution of 5% boric acid
Height.
The oxidation film that 500v constant pressures 5min is obtained when being second of oxidation to Examples 1 and 2 supplement anodic oxidation
Into electric current and resistance change measurement, curve graph is obtained referring to shown in Fig. 3, Fig. 4.As seen from the figure, under preceding 4min current densities continue
Drop, peak value is reached in 4min, specific resistance reaches about 320 Ω cm in azelaic acid solution-2, in+5% azelaic acid solution of 5% boric acid
About 230 Ω cm of specific resistance-2, the former is higher by nearly 40% than the chemical conversion resistance of the latter, illustrates in azelaic acid solution after secondary chemical conversion
Crystalline content is high.
Compared with prior art, corrosive aluminum foil is placed in progress high-voltage anode oxygen in the azelaic acid solution of 10wt% by the present invention
Change is handled, and can greatly improve the structure and performance of anode oxide film, improves the insulation performance of oxidation film, improves crystal form oxidation film
Content, so as to improve the specific capacitance of formed aluminum foil and proof voltage, improve formation efficiency, reach and reduce aluminium electrolutic capacitor volume
Purpose.
It should be pointed out that the above embodiment is not construed as limitation of the present invention, protection scope of the present invention should
It is subject to claim limited range.For those skilled in the art, do not departing from the present invention's
In spirit and scope, several improvements and modifications can also be made, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of aluminium electrolutic capacitor high voltage anodization film, it is characterised in that：Include the following steps：
(1) forming liquid is prepared：Azelaic acid powder and high purity water are configured to the azelaic acid solution that mass fraction is 10% and are placed in aluminium
90 ± 2 DEG C are heated in foil electrolytic bath, keeps constant temperature；
(2) hydration-treated：Corrosive aluminum foil is placed in 90~100 DEG C of high purity water and reacts 5min；
(3) by step (2) treated aluminium foil is placed in progress high voltage anodization processing in the azelaic acid solution in step (1)：
Aluminium foil connects the anode of high-voltage DC power supply, and aluminium foil electrolytic bath connects the cathode of high-voltage DC power supply, using constant dc liter
After being depressed into setting voltage, constant pressure processing 10min is maintained；
(4) by step (3), treated is heat-treated after aluminium foil cleans up with deionized water, i.e., in corrosive aluminum foil surface shape
Into Al2O3High voltage anodization film.
2. a kind of preparation method of aluminium electrolutic capacitor high voltage anodization film according to claim 1, feature exist
In：After step (4) heat treatment, further include and aluminium foil is carried out using step (3) identical high voltage anodization treatment conditions
Supplement the operation of anodized.
3. a kind of preparation method of aluminium electrolutic capacitor high voltage anodization film according to claim 2, feature exist
In：The time that constant pressure is handled in the supplement anodized is 5min.
4. a kind of preparation method of aluminium electrolutic capacitor high voltage anodization film according to claim 1, feature exist
In：The corrosive aluminum foil is acid etch porous high-purity aluminium foil, and purity is more than 99.99%, and average pore size is 1~2 μm.
5. a kind of preparation method of aluminium electrolutic capacitor high voltage anodization film according to claim 1, feature exist
In：The resistivity of high purity water is 16M Ω cm in the step (1).
6. a kind of preparation method of aluminium electrolutic capacitor high voltage anodization film according to claim 1, feature exist
In：The electric current of constant dc is 50 × 10 in the step (3)-3A/cm2。
7. a kind of preparation method of aluminium electrolutic capacitor high voltage anodization film according to claim 1, feature exist
In：Voltage is set as 500V in the step (3).
8. a kind of preparation method of aluminium electrolutic capacitor high voltage anodization film according to claim 1, feature exist
In：Heat treatment is to handle 2min in 500 DEG C of air atmospheres in the step (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711284612.8A CN108183034A (en) | 2017-12-07 | 2017-12-07 | The preparation method of aluminium electrolutic capacitor high voltage anodization film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711284612.8A CN108183034A (en) | 2017-12-07 | 2017-12-07 | The preparation method of aluminium electrolutic capacitor high voltage anodization film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108183034A true CN108183034A (en) | 2018-06-19 |
Family
ID=62545858
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711284612.8A Pending CN108183034A (en) | 2017-12-07 | 2017-12-07 | The preparation method of aluminium electrolutic capacitor high voltage anodization film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108183034A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111330535A (en) * | 2020-03-25 | 2020-06-26 | 南通海星电子股份有限公司 | Novel adsorption material for water treatment and preparation method thereof |
| CN113948315A (en) * | 2021-09-28 | 2022-01-18 | 西安交通大学 | Multi-stage high-specific-volume high-pressure aluminum foil formation method |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1366094A (en) * | 2001-01-19 | 2002-08-28 | 江苏中联科技集团有限公司 | Three-stage process for preparing electrode foil used for middle-and high-voltage aluminium-electrolytic capacitor |
| CN1438662A (en) * | 2003-03-05 | 2003-08-27 | 西安交通大学 | Technology for preparing ande foil of aluminium electrolytic capacitor |
| CN1667767A (en) * | 2005-04-05 | 2005-09-14 | 江苏中联科技集团有限公司 | Process for preparing high voltage long life electrode foil for aluminum electrolytic capacitors |
| CN1873865A (en) * | 2006-04-05 | 2006-12-06 | 江苏中联科技集团有限公司 | Manufacturing method for raising specific volume of electrode foil in use for aluminium electrolytic capacitor |
| JP2007036048A (en) * | 2005-07-28 | 2007-02-08 | Nichicon Corp | Manufacturing method of electrode foil for aluminum electrolytic capacitor |
| CN103151174A (en) * | 2013-03-06 | 2013-06-12 | 佛山科学技术学院 | Manufacturing method of electrode foil for high-voltage aluminium electrolytic capacitor |
| CN106065488A (en) * | 2016-05-19 | 2016-11-02 | 西安交通大学 | A kind of method utilizing positive negative pulse stuffing anodizing to prepare anode aluminium foil |
-
2017
- 2017-12-07 CN CN201711284612.8A patent/CN108183034A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1366094A (en) * | 2001-01-19 | 2002-08-28 | 江苏中联科技集团有限公司 | Three-stage process for preparing electrode foil used for middle-and high-voltage aluminium-electrolytic capacitor |
| CN1438662A (en) * | 2003-03-05 | 2003-08-27 | 西安交通大学 | Technology for preparing ande foil of aluminium electrolytic capacitor |
| CN1667767A (en) * | 2005-04-05 | 2005-09-14 | 江苏中联科技集团有限公司 | Process for preparing high voltage long life electrode foil for aluminum electrolytic capacitors |
| JP2007036048A (en) * | 2005-07-28 | 2007-02-08 | Nichicon Corp | Manufacturing method of electrode foil for aluminum electrolytic capacitor |
| CN1873865A (en) * | 2006-04-05 | 2006-12-06 | 江苏中联科技集团有限公司 | Manufacturing method for raising specific volume of electrode foil in use for aluminium electrolytic capacitor |
| CN103151174A (en) * | 2013-03-06 | 2013-06-12 | 佛山科学技术学院 | Manufacturing method of electrode foil for high-voltage aluminium electrolytic capacitor |
| CN106065488A (en) * | 2016-05-19 | 2016-11-02 | 西安交通大学 | A kind of method utilizing positive negative pulse stuffing anodizing to prepare anode aluminium foil |
Non-Patent Citations (1)
| Title |
|---|
| 韦佳等: ""五硼酸铵在高压铝阳极箔化成液中的作用机理"", 《电子元件与材料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111330535A (en) * | 2020-03-25 | 2020-06-26 | 南通海星电子股份有限公司 | Novel adsorption material for water treatment and preparation method thereof |
| CN113948315A (en) * | 2021-09-28 | 2022-01-18 | 西安交通大学 | Multi-stage high-specific-volume high-pressure aluminum foil formation method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108172402A (en) | The preparation method of aluminium electrolutic capacitor high voltage anodization film | |
| CN108221024A (en) | The preparation method of aluminium electrolutic capacitor high voltage anodization film | |
| CN110819965B (en) | Energy-saving preparation method of anode aluminum foil for aluminum electrolytic capacitor | |
| CN110714218B (en) | Method for preparing MXenes by using electrochemical cation intercalation | |
| Xing et al. | Influence of substrate morphology on the growth and properties of TiO2 nanotubes in HBF4-based electrolyte | |
| CN102864479A (en) | Low-energy method for preparing high-insulativity anodised aluminium film by using two-step method | |
| CN108658064B (en) | Nitrogen-doped graphene and preparation method thereof | |
| CN108183034A (en) | The preparation method of aluminium electrolutic capacitor high voltage anodization film | |
| TWI516640B (en) | Graphite oxide and graphene preparation method | |
| CN102360954B (en) | Method capable of improving specific volume of anode foil of aluminum electrolytic capacitor | |
| CN106744898A (en) | A kind of modifies three-dimensional grapheme powder of nitrogen plasma and its preparation and application | |
| CN106340404B (en) | A kind of preparation method of the high dielectric nano complex oxide film anode foils of low-voltage aluminum electrolytic capacitor | |
| TWI676593B (en) | Graphite Composite Conductive Bar Material And Method For Producing Graphene Using The Same | |
| CN111364016B (en) | Method for preparing porous anode aluminum foil by aid of ALD (atomic layer deposition) assisted nitrogen-doped micro-nano aluminum powder | |
| CN105977030A (en) | Preparation method for ultra-high-capacity tantalum capacitor | |
| CN107799313B (en) | A kind of Waste Acid From Hua Cheng Foil and its production technology | |
| CN105513802B (en) | A kind of manufacture method of the low-pressure chemical synthesis foil containing composite dielectric film | |
| CN105624757B (en) | A kind of industrial frequency AC anodizing of aluminium electrolutic capacitor anode aluminium foil | |
| Ning et al. | High-quality graphene grown directly on stainless steel meshes through CVD process for enhanced current collectors of supercapacitors | |
| CN108648915A (en) | A kind of electrode aluminum foil preparation for high power capacity aluminium electrolutic capacitor | |
| CN106384671B (en) | A kind of mixed acid electrolyte | |
| CN104157457A (en) | Aluminium electrolytic capacitor formed foil production device and production line thereof | |
| CN107731530A (en) | A kind of electric aluminum foil complex media production technology | |
| CN204102723U (en) | A kind of process units of aluminum electrolysis capacitor formed foil and production line thereof | |
| CN107974701A (en) | A kind of pre-treating method of anode aluminium foil chemical conversion |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180619 |
|
| RJ01 | Rejection of invention patent application after publication |