WO2023236573A1 - Procédé de préparation de feuille d'électrode basse tension de volume spécifique élevé pour électronique d'automobile - Google Patents

Procédé de préparation de feuille d'électrode basse tension de volume spécifique élevé pour électronique d'automobile Download PDF

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WO2023236573A1
WO2023236573A1 PCT/CN2023/075328 CN2023075328W WO2023236573A1 WO 2023236573 A1 WO2023236573 A1 WO 2023236573A1 CN 2023075328 W CN2023075328 W CN 2023075328W WO 2023236573 A1 WO2023236573 A1 WO 2023236573A1
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foil
formation
controlled
minutes
dip
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PCT/CN2023/075328
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English (en)
Chinese (zh)
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王建中
陈辰
徐中均
周红炎
刘慧�
冒慧敏
何桂丽
王贵州
金学军
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南通海星电子股份有限公司
南通海一电子有限公司
宁夏海力电子有限公司
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Priority to KR1020237034833A priority Critical patent/KR20240009387A/ko
Publication of WO2023236573A1 publication Critical patent/WO2023236573A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/73—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process
    • C23C22/77—Controlling or regulating of the coating process
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/78—Pretreatment of the material to be coated
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/82—After-treatment
    • C23C22/83—Chemical after-treatment
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/12—Anodising more than once, e.g. in different baths
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/16—Pretreatment, e.g. desmutting
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C25D11/24—Chemical after-treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/04—Electrodes or formation of dielectric layers thereon
    • H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
    • H01G9/055—Etched foil electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T10/00—Road transport of goods or passengers
    • Y02T10/60—Other road transportation technologies with climate change mitigation effect
    • Y02T10/70—Energy storage systems for electromobility, e.g. batteries

Definitions

  • the invention relates to the technical field of electrode foil manufacturing, in particular to a preparation method of high specific volume and low voltage electrode foil for automotive electronics.
  • multi-stage formation of corroded foil is usually used to prepare electrode foil.
  • the general operation steps are: four-stage formation, one-stage formation: 7% ammonium adipate, 1% borate, temperature 70°C, time 7 minutes , after washing with water, enter the secondary formation: 5% ammonium adipate, 1% borate, temperature 70°C, time 6 minutes, third-level formation: 3% ammonium adipate, 1% borate, temperature 70°C, time 8min, after washing with water, carry out four-stage formation: 5% phosphate, temperature 70°C, time 15min, the latter one: 1% phosphate, temperature 80°C, time 12min, after washing with water, enter 7% phosphoric acid solution, time 5min, after washing High temperature (450-500°C) treatment for 1.5min, the last two: 3% phosphate, temperature 70°C, time 5min, the last three: 1% phosphate, temperature 70°C, time 5.5min, wash with water and dry.
  • the preparation process route is simple and the cost is low, the capacitance and boiling life of the prepared electrode foil are low, and the defective rate remains high.
  • the reason is that the aluminum oxide crystal content in the oxide film on the surface of the electrode foil is low, and a large number of defects remain on the oxide film after chemical conversion treatment. Therefore, technicians are urgently needed to solve the above problems.
  • the present invention relates to a preparation method of high specific volume low voltage electrode foil for automotive electronics, which includes the following steps:
  • Multi-level formation including the following sub-steps:
  • First-level formation immerse the corroded foil obtained in step S1 into a mixed solution containing 5-10wt% ammonium sulfate, 1-2wt% borate, and 0.5-1wt% amine salt, controlled at a temperature of 65-85°C. The formation is carried out at a voltage of 20 to 160V, and the time is controlled between 5 and 10 minutes, to produce a first-level formation foil;
  • Secondary formation Dip the primary formation foil processed in step S22 into a mixed solution containing 3-7wt% ammonium sulfate and 1-2wt% borate at a temperature controlled at 65-85°C, 20-160V The formation is carried out under voltage and the time is controlled between 5 and 10 minutes to produce a secondary formation foil;
  • Step S26 Intermediate treatment: Dip the tertiary chemical foil processed in step S25 into a quaternary ammonium salt solution with a temperature controlled at 40 to 60°C and 5 to 10 wt%, and the duration is controlled at 5 to 10 minutes;
  • step S27 Four-stage formation: Dip the three-stage formation foil obtained in step S26 into a solution containing 5-7wt% phosphate at a temperature controlled at 65-85°C, and perform the formation at a voltage of 20-160V, and the duration is controlled at 15-15%. 20 minutes to make a fourth-stage chemical foil;
  • Step S31 First-level post-processing: Dip the fourth-level chemical foil obtained in step S27 into a phosphate aqueous solution with a temperature controlled at 65-85°C and 1-5wt%, apply a voltage of 20-160V, and control the duration at 10-15 minutes. Made into primary treated foil;
  • Step S33 Pickling treatment: Dip the first-level treated foil treated in step S32 into a mixed solution containing 7 to 10 wt% phosphoric acid and oxidizing acid, and the time is controlled to 5 to 10 minutes;
  • step S34 Heat treatment: perform water washing and drying operations on the first-level treated foil obtained in step S33, and the drying temperature is controlled at 450 ⁇ 500°C, and the duration is controlled at 1 ⁇ 2 min;
  • Secondary post-processing Dip the primary-processed foil obtained in step S34 into a phosphate aqueous solution with a temperature controlled at 65-85°C and 1-5wt%, apply a voltage of 20-160V, and control the duration at 5-10 minutes. Made into secondary treated foil;
  • step S36 Third-level post-processing: Dip the secondary-processed foil obtained in step S35 into a phosphate aqueous solution with a temperature controlled at 65 to 85°C and 1 to 5 wt%, apply a voltage of 20 to 160 V, and control the duration to 5 to 10 minutes.
  • a temperature controlled at 65 to 85°C and 1 to 5 wt% a temperature controlled at 65 to 85°C and 1 to 5 wt%
  • apply a voltage of 20 to 160 V and control the duration to 5 to 10 minutes.
  • step S37 Surface cleaning: Wash and air-dry the three-level treated foil obtained in step S36 to obtain a high specific volume low-voltage electrode foil.
  • the borate is preferably any one of borax or sodium metaborate or a mixture thereof.
  • the amine salt is preferably hexylbenzylamine salt, dicyclohexylamine salt, bis-tert-butoxycarbonylhistidine dicyclohexylamine salt, dimethylamine hydrochloride, and triethanolamine , any one of piroctone ethanolamine salts or their mixtures.
  • the quaternary ammonium salt is preferably any one of sodium lauryl sulfate, dodecyl trimethyl ammonium bromide, ammonium lauryl alcohol ether sulfate or their combinations. mixture.
  • the phosphate is preferably any one of diammonium phosphate, sodium hexametaphosphate, disodium hydrogen phosphate or a mixture thereof.
  • the preparation method of high specific volume low-voltage electrode foil for automotive electronics has achieved at least the following beneficial effects:
  • a constant density of current is applied to the formation bath liquid to ensure that the oxide film is stably and rapidly formed on the surface of the corroded foil. , and the distribution shape of the formed channels in different areas is more balanced;
  • the voltage, temperature, time, and composition and ratio of the formation liquid used are adjusted so that the density of each layer of the formed oxide film becomes consistent, which is beneficial to improving the boiling properties of the electrode foil. life;
  • step S21 adding amine treatment liquid during the first-level formation can improve the concentration of the oxide film.
  • Figure 1 is a metallographic photograph of a shaped electrode foil prepared by conventional multi-stage formation as described in the background art.
  • Figure 2 is a metallographic photograph of the shaped electrode foil prepared by the method in Example 1.
  • Figure 3 is a metallographic photograph of the shaped electrode foil prepared by the method in Example 2.
  • Figure 4 is a metallographic photograph of the shaped electrode foil prepared by the method in Example 3.
  • Figure 5 is a metallographic photograph of the shaped electrode foil prepared by the method in Example 4.
  • the electrode foil is prepared with reference to the multi-stage formation method disclosed in the background art above.
  • a method for preparing high specific volume low voltage electrode foil for automotive electronics which includes the following steps:
  • Multi-level formation including the following sub-steps:
  • First-level formation Immerse the corroded foil obtained in step S1 into a mixed solution containing 5wt% ammonium sulfate, 1wt% sodium metaborate, and 0.5wt% hexyl benzylamine salt, controlled at a temperature of 65 to 85°C, for 20 to The formation is carried out at a voltage of 160V and the time is controlled at 10 minutes to produce a first-level formation foil;
  • step S22 Surface cleaning: perform water washing and air-drying operations on the primary chemical foil obtained in step S21 (the air-drying temperature does not exceed 20°C);
  • Secondary formation Dip the primary formation foil processed in step S22 into a mixed solution containing 3wt% ammonium sulfate and 1wt% sodium metaborate at a temperature controlled at 65-85°C, and perform the formation at a voltage of 20-160V. , and the duration should be controlled at 10 minutes to make a secondary formation foil;
  • step S24 Tertiary formation: Dip the secondary formation foil obtained in step S23 into a mixed solution containing 3wt% ammonium sulfate and 1wt% sodium metaborate at a temperature controlled at 65-85°C, and perform the formation at a voltage of 20-160V, and The time is controlled at 15 minutes to make a three-stage chemical foil;
  • step S26 Intermediate treatment: Dip the tertiary chemical foil processed in step S25 into a 5wt% sodium dodecyl sulfate aqueous solution with a temperature controlled at 40-60°C, and the duration is controlled at 10 minutes;
  • step S27 Four-stage formation: Dip the three-stage formation foil obtained in step S26 into a solution containing 5wt% sodium hexametaphosphate and controlled at a temperature of 65 to 85°C. The formation is carried out at a voltage of 20 to 160V, and the duration is controlled to 20 minutes. Made into quaternary formation foil;
  • Step S31 First-level post-processing: Dip the fourth-level chemical foil obtained in step S27 into a 1wt% sodium hexametaphosphate aqueous solution with a temperature controlled at 65 to 85°C, apply a voltage of 20 to 160V, and control the time to 15 minutes to prepare Primary treatment foil;
  • Acid dipping treatment Dip the first-level treated foil treated in step S32 into an acidic mixed solution containing 7wt% phosphoric acid:perchloric acid in a ratio of 1:1, and the duration is controlled to 6 minutes;
  • step S34 Heat treatment: perform water washing and drying operations on the first-level treated foil obtained in step S33, and the drying temperature is controlled at 450 ⁇ 500°C, and the drying time is controlled at 1.5 minutes;
  • Secondary post-processing Dip the primary-processed foil obtained in step S34 into a 1wt% sodium hexametaphosphate aqueous solution controlled at a temperature of 65 to 85°C, apply a voltage of 20 to 160V, and control the duration to 10 minutes to prepare secondary treatment foil;
  • step S36 Third-level post-processing: Dip the secondary-processed foil obtained in step S35 into a 1wt% sodium hexametaphosphate aqueous solution with a temperature controlled at 65 to 85°C, apply a voltage of 20 to 160V, and control the duration to 10 minutes to prepare Tertiary treated foil;
  • step S37 Surface cleaning: Wash and air-dry the three-level treated foil obtained in step S36 to obtain a high specific volume low-voltage electrode foil.
  • a method for preparing high specific volume low voltage electrode foil for automotive electronics which includes the following steps:
  • Multi-level formation including the following sub-steps:
  • step S21 First-level formation: immerse the corroded foil obtained in step S1 into a mixed solution containing 8wt% ammonium sulfate, 1.5wt% sodium metaborate, and 0.7wt% hexyl benzylamine salt at a temperature of 65 to 85°C, 20 The formation is carried out at a voltage of ⁇ 160V, and the time is controlled at 10 minutes, to produce a first-level formation foil;
  • step S22 Surface cleaning: perform water washing and air-drying operations on the primary chemical foil obtained in step S21 (the air-drying temperature does not exceed 20°C);
  • Secondary formation Dip the primary formation foil processed in step S22 into a mixed solution containing 5wt% ammonium sulfate and 1.5wt% sodium metaborate, controlled at a temperature of 65 to 85°C, and carried out at a voltage of 20 to 160V. Formation, and the time should be controlled within 10 minutes, to produce a secondary formation foil;
  • step S24 Tertiary formation: Dip the secondary formation foil obtained in step S23 into a mixed solution containing 4wt% ammonium sulfate and 1.5wt% sodium metaborate at a temperature controlled at 65-85°C, and perform the formation at a voltage of 20-160V. And the time is controlled at 15 minutes to make a three-stage chemical foil;
  • step S26 Intermediate treatment: Dip the tertiary chemical foil processed in step S25 into an 8wt% sodium dodecyl sulfate aqueous solution with a temperature controlled at 40-60°C, and the duration is controlled at 10 minutes;
  • step S27 Four-stage formation: Dip the three-stage formation foil obtained in step S26 into a solution containing 6wt% sodium hexametaphosphate at a temperature controlled at 65-85°C, and perform the formation at a voltage of 20-160V, and the duration is controlled at 20 minutes.
  • a solution containing 6wt% sodium hexametaphosphate at a temperature controlled at 65-85°C and perform the formation at a voltage of 20-160V, and the duration is controlled at 20 minutes.
  • Step S31 First-level post-processing: Dip the fourth-level chemical foil obtained in step S27 into a 3wt% sodium hexametaphosphate aqueous solution with a temperature controlled at 65 to 85°C, apply a voltage of 20 to 160V, and control the time to 15 minutes to prepare Primary treatment foil;
  • step S33 Pickling treatment: Dip the first-level treated foil treated in step S32 into an acidic mixed solution containing 8wt% phosphoric acid:perchloric acid in a ratio of 1:1, and the time is controlled to 6 minutes;
  • step S34 Heat treatment: perform water washing and drying operations on the first-level treated foil obtained in step S33, and the drying temperature is controlled at 450 ⁇ 500°C, and the drying time is controlled at 1.5 minutes;
  • Secondary post-processing Dip the primary-processed foil obtained in step S34 into a 3wt% sodium hexametaphosphate aqueous solution with a temperature controlled at 65 to 85°C, apply a voltage of 20 to 160V, and control the duration to 10 minutes to prepare secondary treatment foil;
  • step S36 Third-level post-processing: Dip the secondary-processed foil obtained in step S35 into a 3wt% sodium hexametaphosphate aqueous solution with a temperature controlled at 65 to 85°C, apply a voltage of 20 to 160V, and control the duration to 10 minutes to prepare Tertiary treated foil;
  • step S37 Surface cleaning: Wash and air-dry the three-level treated foil obtained in step S36 to obtain a high specific volume low-voltage electrode foil.
  • a method for preparing high specific volume low voltage electrode foil for automotive electronics which includes the following steps:
  • Multi-level formation including the following sub-steps:
  • step S21 First-level formation: immerse the corroded foil obtained in step S1 into a mixed solution containing 10wt% ammonium sulfate, 2wt% sodium metaborate, and 1wt% hexyl benzylamine salt at a temperature of 65 to 85°C, 20 to 160V Carry out formation under voltage and control the time to 10 minutes to make a first-level formation foil;
  • step S22 Surface cleaning: perform water washing and air-drying operations on the primary chemical foil obtained in step S21 (the air-drying temperature does not exceed 20°C);
  • Secondary formation Dip the primary formation foil processed in step S22 into a mixed solution containing 7wt% ammonium sulfate and 2wt% sodium metaborate at a temperature controlled at 65-85°C, and perform the formation at a voltage of 20-160V. , and the duration should be controlled at 10 minutes to make a secondary formation foil;
  • step S26 Intermediate treatment: Dip the tertiary chemical foil processed in step S25 into a 10wt% sodium dodecyl sulfate aqueous solution with a temperature controlled at 40-60°C, and the duration is controlled at 10 minutes;
  • step S27 Four-stage formation: Dip the three-stage formation foil obtained in step S26 into a solution containing 7wt% sodium hexametaphosphate at a temperature controlled at 65-85°C, and perform the formation at a voltage of 20-160V, and the duration is controlled at 20 minutes.
  • a solution containing 7wt% sodium hexametaphosphate at a temperature controlled at 65-85°C and perform the formation at a voltage of 20-160V, and the duration is controlled at 20 minutes.
  • Step S31 First-level post-processing: Dip the fourth-level chemical foil obtained in step S27 into a 5wt% sodium hexametaphosphate aqueous solution with a temperature controlled at 65 to 85°C, apply a voltage of 20 to 160V, and control the time to 15 minutes to prepare Primary treatment foil;
  • Acid dipping treatment Dip the first-level treated foil treated in step S32 into an acidic mixed solution containing 10wt% phosphoric acid: perchloric acid in a ratio of 1:1, and the duration is controlled to 6 minutes;
  • step S34 Heat treatment: perform water washing and drying operations on the first-level treated foil obtained in step S33, and the drying temperature is controlled at 450 ⁇ 500°C, and the drying time is controlled at 1.5 minutes;
  • Secondary post-processing Dip the primary-processed foil obtained in step S34 into a 5wt% sodium hexametaphosphate aqueous solution with a temperature controlled at 65 to 85°C, apply a voltage of 20 to 160V, and control the duration to 10 minutes to prepare secondary treatment foil;
  • step S36 Third-level post-processing: Dip the secondary-processed foil obtained in step S35 into a 5wt% sodium hexametaphosphate aqueous solution with a temperature controlled at 65 to 85°C, apply a voltage of 20 to 160V, and control the duration to 10 minutes to prepare Tertiary treated foil;
  • step S37 Surface cleaning: Wash and air-dry the three-level treated foil obtained in step S36 to obtain a high specific volume low-voltage electrode foil.
  • a method for preparing high specific volume low voltage electrode foil for automotive electronics which includes the following steps:
  • Multi-level synthesis including the following sub-steps:
  • First-level formation Immerse the corroded foil obtained in step S1 into a mixed solution containing 5wt% ammonium sulfate, 1wt% sodium metaborate, and 0.5wt% hexyl benzylamine salt, controlled at a temperature of 65 to 85°C, for 20 to The formation is carried out at a voltage of 160V and the time is controlled at 5 minutes to produce a first-level formation foil;
  • step S22 Surface cleaning: perform water washing and air-drying operations on the primary chemical foil obtained in step S21 (the air-drying temperature does not exceed 20°C);
  • Secondary formation Dip the primary formation foil processed in step S22 into a mixed solution containing 3wt% ammonium sulfate and 1wt% sodium metaborate at a temperature controlled at 65-85°C, and perform the formation at a voltage of 20-160V. , and the time should be controlled at 5 minutes to make a secondary formation foil;
  • step S24 Tertiary formation: Dip the secondary formation foil obtained in step S23 into a mixed solution containing 3wt% ammonium sulfate and 1wt% sodium metaborate at a temperature controlled at 65-85°C, and perform the formation at a voltage of 20-160V, and The time is controlled at 7 minutes to produce a three-stage chemical foil;
  • step S26 Intermediate treatment: Dip the tertiary chemical foil processed in step S25 into a 5wt% sodium dodecyl sulfate aqueous solution with a temperature controlled at 40-60°C, and the duration is controlled at 10 minutes;
  • step S27 Four-stage formation: Dip the three-stage formation foil obtained in step S26 into a solution containing 5wt% sodium hexametaphosphate at a temperature controlled at 65-85°C, and perform the formation at a voltage of 20-160V, and the duration is controlled at 15 minutes.
  • a solution containing 5wt% sodium hexametaphosphate at a temperature controlled at 65-85°C and perform the formation at a voltage of 20-160V, and the duration is controlled at 15 minutes.
  • Step S31 First-level post-processing: Dip the fourth-level chemical foil obtained in step S27 into a 1wt% sodium hexametaphosphate aqueous solution with a temperature controlled at 65 to 85°C, apply a voltage of 20 to 160V, and control the time to 10 minutes to prepare Primary treatment foil;
  • Acid dipping treatment Dip the first-level treated foil treated in step S32 into an acidic mixed solution containing 7wt% phosphoric acid:perchloric acid in a ratio of 1:1, and the duration is controlled to 6 minutes;
  • step S34 Heat treatment: perform water washing and drying operations on the first-level treated foil obtained in step S33, and the drying temperature is controlled at 450 ⁇ 500°C, and the drying time is controlled at 1.5 minutes;
  • Secondary post-processing Dip the primary-processed foil obtained in step S34 into a 1wt% sodium hexametaphosphate aqueous solution with a temperature controlled at 65 to 85°C, apply a voltage of 20 to 160V, and control the duration to 5 minutes to prepare secondary treatment foil;
  • step S36 Third-level post-processing: Dip the secondary-processed foil obtained in step S35 into a 1wt% sodium hexametaphosphate aqueous solution controlled at a temperature of 65 to 85°C, apply a voltage of 20 to 160V, and control the duration to 5 minutes to prepare Tertiary treated foil;
  • step S37 Surface cleaning: Wash and air-dry the three-level treated foil obtained in step S36 to obtain a high specific volume low-voltage electrode foil.
  • Table 1 is a summary of the performance test results of the electrode foils obtained in Comparative Examples and Examples 1 to 4.
  • Vfe the final voltage applied during the forming process of the unformed foil
  • a constant density of current is applied to the formation bath liquid to ensure that the oxide film is stably and rapidly formed on the surface of the corroded foil. , and the distribution shape of the formed channels in different areas is more balanced;
  • the voltage, temperature, time, and composition and ratio of the formation liquid used are adjusted so that the density of each layer of the formed oxide film becomes consistent, which is beneficial to improving the boiling properties of the electrode foil. life;
  • step S21 adding amine treatment liquid during the first-level formation can improve the concentration of the oxide film.
  • defects formed on the oxide film during chemical formation can be effectively and fully repaired, and can also be significantly improved. Improve the specific capacitance of aluminum electrode foil.
  • the cathode Due to the presence of strong oxidizing acid, the cathode is
  • borates such as borax and a mixture of sodium metaborate and borax can also be selected according to the actual situation;
  • dicyclohexylamine salt or dicyclohexylamine salt or di-tert-butoxycarbonyl histidine dicyclohexylamine can also be selected according to the actual situation.
  • Any one of amine salts such as dimethylamine hydrochloride, triethanolamine, piroctone ethanolamine salt, or mixtures thereof;
  • dodecyltrimethylammonium bromide and lauryl alcohol ether can also be selected according to the actual situation. Any one of quaternary ammonium salts such as ammonium sulfate or their mixture;
  • any one of the phosphates such as diammonium phosphate, disodium hydrogen phosphate or the like can also be selected according to the actual situation. Their mixture.

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Abstract

La présente invention concerne un procédé de préparation d'une feuille d'électrode basse tension de volume spécifique élevé pour l'électronique d'automobile. Le procédé comprend les étapes suivantes consistant à : tout d'abord, réaliser séquentiellement des opérations de formation de premier étage, de formation de deuxième étage, de formation de troisième étage et de formation quatrième étage sur une feuille de gravure, et ajuster respectivement la tension, la température, le temps et les composants et la proportion du liquide de formation utilisé pendant la réalisation d'une formation unique ; ajouter une solution de traitement d'amine pendant la formation du premier étage pour augmenter considérablement la teneur en cristaux d'oxyde d'aluminium dans un film d'oxyde formé ; puis tremper la feuille formée dans une solution de phosphate de multiples fois pour effectuer une opération de post-traitement de façon à réparer des points défectueux résiduels sur le film d'oxyde formé. De cette manière, non seulement la durée de vie à l'ébullition d'une feuille d'électrode peut être efficacement prolongée, mais une bonne base est également posée pour améliorer considérablement le volume spécifique électrique d'une feuille d'électrode en aluminium.
PCT/CN2023/075328 2022-06-07 2023-02-10 Procédé de préparation de feuille d'électrode basse tension de volume spécifique élevé pour électronique d'automobile WO2023236573A1 (fr)

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