WO2020048045A1 - 一种制备含TiO2介质层电子铝箔的前处理工艺 - Google Patents

一种制备含TiO2介质层电子铝箔的前处理工艺 Download PDF

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WO2020048045A1
WO2020048045A1 PCT/CN2018/121671 CN2018121671W WO2020048045A1 WO 2020048045 A1 WO2020048045 A1 WO 2020048045A1 CN 2018121671 W CN2018121671 W CN 2018121671W WO 2020048045 A1 WO2020048045 A1 WO 2020048045A1
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foil
dielectric layer
oven
immersed
solution
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PCT/CN2018/121671
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French (fr)
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王建中
冒慧敏
高志华
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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 KR1020207015398A priority Critical patent/KR102369396B1/ko
Publication of WO2020048045A1 publication Critical patent/WO2020048045A1/zh

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    • 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
    • C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/04—Electrodes or formation of dielectric layers thereon
    • H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
    • H01G9/045—Electrodes or formation of dielectric layers thereon characterised by the material based on aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/04—Electrodes or formation of dielectric layers thereon
    • H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
    • H01G9/055—Etched foil electrodes

Definitions

  • the invention relates to a pretreatment process for preparing an electronic aluminum foil containing a TiO 2 dielectric layer.
  • Formed foil is the core material of aluminum electrolytic capacitors, and its manufacturing process mainly includes two steps: light foil expansion and corrosion and corrosion foil formation.
  • the formation of foil determines most of the properties of the final product.
  • aluminum electrolytic capacitors as integrated components must also develop in the direction of high specific volume and miniaturization.
  • Expanded corrosion technology improves the specific volume of chemically formed foils by increasing the specific surface area of the etched foil, but this technology is now approaching its physical limit.
  • a dielectric with a high dielectric constant must be introduced into the alumina dielectric layer of chemically formed foils. Layers such as Ti, V, Ta and other valve metal oxides.
  • the corrosion foil or the corrosion foil subjected to one or more stages of chemical treatment was immersed in a mixed solution of titanium sulfate or sulfuric acid or a mixed solution of n-butyl titanate, ethanol, and acetone. After a certain period of time, heat treatment in a muffle furnace at 400 to 550 ° C for 10 to 30 minutes.
  • the main problems are: if the corrosion foil is directly immersed in the above titanium sulfate and sulfuric acid mixed solution, due to the lower pH value, the surface area of the corrosion foil after the expansion corrosion is extremely large, and the erosion is severe in the solution, and the thickness is reduced. Thin is not conducive to the improvement of specific volume.
  • the corrosion of the corroded foil formed by one or more stages is reduced due to the presence of the alumina dielectric layer, but at the same time, the reduction of the holes on the corroded foil is not conducive to the entry of Ti elements into the internal voids.
  • the mixed solution of n-butyl titanate, ethanol, and acetone has high stability, but the mixed solution has a high viscosity, and the corrosion foil immersed in it is difficult to fully wet, the content of the introduced Ti element is limited, and the mixed solution is It is difficult to thoroughly clean during the formation, which adversely affects the performance of the formation foil including hydration resistance and leakage current.
  • the heat treatment of the etched foil at 400 to 550 ° C for 10 to 30 minutes after dipping is difficult to achieve on current automated linkage forming machines. According to the conventional production speed, the muffle furnace is 10 to 50 meters long.
  • the purpose of the present invention is to overcome the above-mentioned shortcomings and provide a pretreatment process that is easy to implement on a forming machine, and achieves the purpose of introducing TiO 2 into the medium layer of the formed foil to improve the specific volume of the product without causing other properties of the formed foil. deterioration.
  • a pretreatment process for preparing an electronic aluminum foil containing a TiO 2 dielectric layer the steps are as follows:
  • Vf 240V ⁇ Vf ⁇ 690V
  • the pre-treated corrosion foil is immersed in different concentrations of sodium azelaic acid and azelaic acid solution, and it is converted to 0.3 by applying direct current.
  • Vf, 0.6Vf, 1.0Vf heat treatment in an oven at 450 ⁇ 500 °C for 2min; sodium azelate and azelaic acid solution continue to be transformed into 10-15min; immersed in 50 ⁇ 70g / L phosphoric acid solution for 5-10min after washing; 400 Heat treatment in an oven at ⁇ 450 °C for 2min; continue to form sodium azelate and azelaic acid solution for 10-15min; immerse in a 0.2% ⁇ 0.5% ammonium dihydrogen phosphate solution for 3-5min; and dry in a 120 °C oven.
  • the immersion treatment in step B is performed under ultrasonic conditions.
  • the present invention has the advantages of simple process flow and easy realization on the production line.
  • Example 1 A pre-treatment process for preparing an electronic aluminum foil containing a TiO 2 dielectric layer, the steps are as follows: the corrosion foil is pretreated in boiling water for 8 minutes, and then heat-treated in a 400 ° C muffle furnace for 30 seconds, and then taken out; then immersed in the pH value 1.2 In a mixed solution containing titanium sulfate, acetic acid, and sulfuric acid, where the Ti ion concentration is 0.1 mol / L, the solution temperature is 50 ° C, and the immersion time is 2 minutes; after taking out, wash with pure water and preheat to 300 ° C and place 2.45GHZ industrial microwave oven is heated for 2min; it is converted to the required voltage Vf (240V ⁇ Vf ⁇ 690V) according to the conventional production process, and the pre-treated corrosion foil is immersed in different concentrations of azelaic acid and azelaic acid solution and applied Direct current is chemically converted to 0.3Vf, 0.6Vf, 1.0Vf; heat treatment in an oven at
  • Embodiment 2 A pre-treatment process for preparing an electronic aluminum foil containing a TiO 2 dielectric layer, the steps are as follows: the corroded foil is pretreated in boiling water for 12 minutes, and then heat-treated in a 500 ° C.
  • Example 3 A pre-treatment process for preparing an electronic aluminum foil containing a TiO 2 dielectric layer, the steps are as follows: the corroded foil is pretreated in boiling water for 10 min, and then heat-treated in a muffle furnace at 450 ° C. for 75 s and taken out; then immersed in the pH value 1.6 in a mixed solution containing titanium sulfate, acetic acid, and sulfuric acid, where the concentration of Ti ions is 0.3mol / L, the solution temperature is 60 ° C, and the immersion time is 3.5min; after taking out, wash with pure water and preheat to 350 ° C.
  • Vf 240V ⁇ Vf ⁇ 690V

Abstract

本发明公开了一种制备含TiO2介质层化成箔的前处理工艺，将经过预化成处理的腐蚀箔400～500℃马弗炉中热处理30～120s后取出；然后浸渍于pH值1.2～2.0的含硫酸钛、醋酸、硫酸的混合溶液中，其中Ti元素浓度为0.1～0.5mol/L,溶液温度为50℃～70℃，浸渍时间为2～5min；取出后用纯水冲洗并预热至300～400℃，置于2.45GHZ工业微波炉中加热2～3min即可。将经过上述前处理的腐蚀箔按照常规的多级化成工艺进行化成即可制得含TiO2介质层的化成箔，在生产低电压段化成箔(Vf≦520V)时往往仅需要进行一次上述前处理即可，在生产较高电压段产品时可根据需要在各级化成工艺后增加上述前处理工艺。

Description

一种制备含TiO 2介质层电子铝箔的前处理工艺 技术领域
本发明涉及一种制备含TiO 2介质层电子铝箔的前处理工艺。
背景技术
化成箔是铝电解电容器的核心材料，其制造工艺主要包括光箔扩面腐蚀和腐蚀箔化成两个工序。化成箔决定了最终产品的绝大部分性能。随着电子整机的组装密度和集成化程度不断提高，作为集成元件的铝电解电容器也必须进一步向高比容、小型化方向发展。扩面腐蚀技术通过提高腐蚀箔比表面积来提高化成箔比容，但是该技术目前已经日益逼近其物理极限，为进一步提供比容必须在化成箔的氧化铝介质层中引入高介电常数的介质层如Ti，V，Ta等阀金属氧化物。
在此之前，为在介质层中引入Ti元素一般是将腐蚀箔或经过一级或多级化成处理的腐蚀箔浸渍于硫酸钛、硫酸混合溶液中或钛酸正丁酯、乙醇、丙酮混合溶液中一定时间后，置于400～550℃马弗炉中热处理10～30min。其存在的主要问题有，如将腐蚀箔直接浸渍于上述硫酸钛、硫酸混合溶液中，由于较低的pH值，经过扩面腐蚀的腐蚀箔表面积又极大，在溶液中侵蚀严重，厚度减薄不利于比容的提升。经过一级或多级化成的腐蚀箔由于氧化铝介质层的存在腐蚀情况减轻但同时也引起腐蚀箔上孔洞减小不利于Ti元素进入内部孔洞。钛酸正丁酯、乙醇、丙酮混合溶液具有较高的稳定性，但该混合溶液粘度较高浸渍于其中的腐蚀箔难以充分浸润，所引入的Ti元素含量受限，且该混合溶液在后续化成中难以彻底清洗，对化成箔包括耐水合性、漏电流在内的性能产生不利影响。此外在浸渍后将腐蚀箔在400～550℃中热处理10～30min在当前的自动化联动化成机上是难以实现的，按照常规生产速度所需马弗炉长达10～50米。
发明内容
本发明的目的在于克服以上不足之处，提供一种易于在化成机上实现的前处理工艺，达到在化成箔介质层中引入TiO 2提高产品比容的目的，同时又不引起化成箔其他性能的恶化。
本发明的目的通过以下技术方案来实现：一种制备含TiO 2介质层电子铝箔的前处理工艺，步骤如下：
A、将腐蚀箔在沸水中预处理8～12min后，在400～500℃马弗炉中热处理30～120s后取出；
B、然后浸渍于pH值1.2～2.0的含硫酸钛、醋酸、硫酸的混合溶液中，其中Ti离子浓度为0.1～0.5mol/L，溶液温度为50℃～70℃，浸渍时间为2～5min；
C、取出后经纯水清洗并预热至300～400℃后置于2.45GHZ工业微波炉中加热2～3min；
D、按照常规生产工艺化成至所需电压Vf(240V≦Vf≦690V)，将经前处理的腐蚀箔浸渍在不同浓度的壬二酸钠、壬二酸溶液中并施加直流电依次化化成至0.3Vf、0.6Vf、1.0Vf；450～500℃烘箱中热处理2min；壬二酸钠、壬二酸溶液中继续化成10～15min；水洗后浸于50～70g/L磷酸溶液中5～10min；400～450℃烘箱中热处理2min；壬二酸钠、壬二酸溶液中继续化成10～15min；浸渍于0.2％～0.5％磷酸二氢铵溶液中3～5min；120℃烘箱中烘干。
优选的是，B步骤中浸渍处理在超声波条件下进行。
综上所述，本发明具有工艺流程简单，易于在生产线实现的优点，在化成箔介质层中引入TiO 2提高产品比容的目的，同时又不引起化成箔其他性能的恶化。
具体实施方式
为了加深对本发明的理解，下面将结合实施例对本发明作进一步详述，该实施例仅用于解释本发明，并不构成对本发明保护范围的限定。
实施例1：一种制备含TiO 2介质层电子铝箔的前处理工艺，步骤如下：将腐蚀箔在沸水中预处理8min后，在400℃马弗炉中热处理30s后取出；然后浸渍于pH值1.2的含硫酸钛、醋酸、硫酸的混合溶液中，其中Ti离子浓度为0.1mol/L，溶液温度为50℃，浸渍时间为2min；取出后经纯水清洗并预热至300℃后置于2.45GHZ工业微波炉中加热2min；按照常规生产工艺化成至所需电压Vf(240V≦Vf≦690V)，将经前处理的腐蚀箔浸渍在不同浓度的壬二酸钠、壬二酸溶液中并施加直流电依次化化成至0.3Vf、0.6Vf、1.0Vf；450～500℃烘箱中热处理2min；壬二酸钠、壬二酸溶液中继续化成10～15min；水洗后浸于50～70g/L磷酸溶液中5～10min；400～450℃烘箱中热处理2min；壬二酸钠、壬二酸溶液中继续化成10～15min；浸渍于0.2％～0.5％磷酸二氢铵溶液中3～5min；120℃烘箱中烘干。
实施例2：一种制备含TiO 2介质层电子铝箔的前处理工艺，步骤如下：将腐蚀箔在沸水中预处理12min后，在500℃马弗炉中热处理120s后取出；然后浸渍于pH值2.0的含硫酸钛、醋酸、硫酸的混合溶液中，其中Ti离子浓度为0.5mol/L，溶液温度为70℃，浸渍时间为5min；取出后经纯水清洗并预热至400℃后置于2.45GHZ工业微波炉中加热3min；按照常规生产工艺化成至所需电压Vf(240V≦Vf≦690V)，将经前处理的腐蚀箔浸渍在不同浓度的壬二酸钠、壬二酸溶液中并施加直流电依次化化成至0.3Vf、0.6Vf、1.0Vf；450～500℃烘箱中热处理2min；壬二酸钠、壬二酸溶液中继续化成10～15min；水洗后浸于50～70g/L磷酸溶液中5～10min；400～450℃烘箱中热处理2min；壬二酸钠、壬二酸溶液中继续化成10～15min；浸渍于0.2％～0.5％磷酸二氢铵溶液中3～5min；120℃烘箱中烘干。
实施例3：一种制备含TiO 2介质层电子铝箔的前处理工艺，步骤如下：将腐蚀箔在沸水中预处理10min后，在450℃马弗炉中热处理75s后取出；然后浸渍于pH值1.6的含硫酸钛、醋酸、硫酸的混合溶液中，其中Ti离子浓度为0.3mol/L，溶液温度为60℃，浸渍时间为3.5min；取出后经纯水清 洗并预热至350℃后置于2.45GHZ工业微波炉中加热2.5min；按照常规生产工艺化成至所需电压Vf(240V≦Vf≦690V)，将经前处理的腐蚀箔浸渍在不同浓度的壬二酸钠、壬二酸溶液中并施加直流电依次化化成至0.3Vf、0.6Vf、1.0Vf；450～500℃烘箱中热处理2min；壬二酸钠、壬二酸溶液中继续化成10～15min；水洗后浸于50～70g/L磷酸溶液中5～10min；400～450℃烘箱中热处理2min；壬二酸钠、壬二酸溶液中继续化成10～15min；浸渍于0.2％～0.5％磷酸二氢铵溶液中3～5min；120℃烘箱中烘干。

Claims (2)

  1. 一种制备含TiO 2介质层电子铝箔的前处理工艺，其特征在于：步骤如下：
    A、将腐蚀箔在沸水中预处理8～12min后，在400～500℃马弗炉中热处理30～120s后取出；
    B、然后浸渍于pH值1.2～2.0的含硫酸钛、醋酸、硫酸的混合溶液中，其中Ti离子浓度为0.1～0.5mol/L，溶液温度为50℃～70℃，浸渍时间为2～5min；
    C、取出后经纯水清洗并预热至300～400℃后置于2.45GHZ工业微波炉中加热2～3min；
    D、按照常规生产工艺化成至所需电压Vf(240V≦Vf≦690V)，将经前处理的腐蚀箔浸渍在不同浓度的壬二酸钠、壬二酸溶液中并施加直流电依次化化成至0.3Vf、0.6Vf、1.0Vf；450～500℃烘箱中热处理2min；壬二酸钠、壬二酸溶液中继续化成10～15min；水洗后浸于50～70g/L磷酸溶液中5～10min；400～450℃烘箱中热处理2min；壬二酸钠、壬二酸溶液中继续化成10～15min；浸渍于0.2％～0.5％磷酸二氢铵溶液中3～5min；120℃烘箱中烘干。
  2. 权利要求1所述的一种制备含TiO 2介质层电子铝箔的前处理工艺，其特征在于：所述B步骤中浸渍处理在超声波条件下进行。
PCT/CN2018/121671 2018-09-06 2018-12-18 一种制备含TiO2介质层电子铝箔的前处理工艺 WO2020048045A1 (zh)

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