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Method for preparing high-dielectric composite film in combination with ALD (Atomic Layer Deposition)

A composite film, high dielectric technology, applied in the manufacture of capacitor electrodes, capacitor parts, electrolytic capacitors, etc., can solve the problems of small effective coating area, easy film shrinkage, and coating thickness, etc., to achieve increased coating area and tight fit Effect

Inactive Publication Date: 2016-02-24
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sol-gel method has the disadvantages of long production cycle, thick coating film and easy shrinkage of the film.
In 2005, Jinju Chen et al. prepared Al by hydrolysis deposition method. 2 o 3 / TiO 2 The composite film increases the specific capacity of corroded aluminum foil by 30%, but the process of hydrolytic deposition is not easy to control, and the coated particles are easy to agglomerate
The fundamental reason is that the coating is uneven, the film layer is not suitable for the substrate, the effective coating area is too small, and it has been heat-treated before anodizing, and the introduction of thermal aluminum oxide

Method used

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  • Method for preparing high-dielectric composite film in combination with ALD (Atomic Layer Deposition)
  • Method for preparing high-dielectric composite film in combination with ALD (Atomic Layer Deposition)
  • Method for preparing high-dielectric composite film in combination with ALD (Atomic Layer Deposition)

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Put a low-pressure etched aluminum foil in an atomic layer deposition chamber with a vacuum degree of 5hPa at 25°C, use nitrogen (99.99%) as the carrier gas, blow into the niobium source in the form of steam for 0.2S, and then blow in nitrogen for cleaning for 5S; Nitrogen was used as the carrier gas, and H was blown into the vapor form2 o 2 0.2S, and then pass nitrogen gas for cleaning for 5S; react for 500 cycles, and coat a layer of niobium oxide film. Then put the aluminum foil into a 5wt% ammonium pentaborate solution at 90°C, at 50V, 300mA / cm 2 formed under conditions. During the formation process, when the voltage reaches 50V, keep the voltage value unchanged, and reduce the current density to 0.3mA / cm 2 , and finally heat-treat the aluminum foil in an air atmosphere at 400°C for 10 minutes, and perform supplementary formation under the same conditions as the chemical formation process, until the current density drops to 0.2mA / cm 2 .

Embodiment 2

[0029] Put a low-pressure etched aluminum foil in an atomic layer deposition chamber with a vacuum degree of 15hPa at 80°C, use nitrogen (99.99%) as a carrier gas, blow into the hafnium source in the form of steam for 1.5S, and then blow in nitrogen for cleaning for 20S; Nitrogen was used as the carrier gas, and H was blown into the vapor form 2 O1.5S, and then pass nitrogen gas to clean for 20S; react for 400 cycles, and coat a layer of hafnium oxide film. Then put the aluminum foil into the 1.4wt‰ ammonium dihydrogen phosphate solution at 80°C, at 100V, 200mA / cm 2 formed under conditions. During the formation process, when the voltage reaches 100V, keep the voltage value unchanged and reduce the current density to 0.5mA / cm 2 , and finally heat-treat the aluminum foil in an air atmosphere at 450°C for 8 minutes, and perform supplementary formation under the same conditions as the chemical formation process, until the current density drops to 0.3mA / cm 2 .

Embodiment 3

[0031] Put a low-pressure etched aluminum foil in an atomic layer deposition chamber with a vacuum of 10hPa at 100°C, use nitrogen (99.99%) as the carrier gas, blow into the titanium source in the form of steam for 1S, and then blow in nitrogen for cleaning for 15S; As a carrier gas, H was blown in vapor form 2 O1S, and then pass nitrogen gas to clean for 15S; react for 300 cycles, and coat a layer of titanium oxide film. Then put the aluminum foil into 5wt% ammonium pentaborate solution at 70°C, at 150V, 100mA / cm 2 formed under conditions. During the formation process, when the voltage reaches 150V, keep the voltage value unchanged, and reduce the current density to 1mA / cm 2 , and finally heat-treat the aluminum foil in an air atmosphere at 500°C for 5 minutes, and perform supplementary formation under the same conditions as the chemical formation process, until the current density drops to 0.2mA / cm 2 .

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Abstract

The invention discloses a method for preparing a high-dielectric composite film in combination with ALD (Atomic Layer Deposition), and belongs to the technical field of electronic devices. The method comprises: putting a corrosive aluminum foil into an atomic layer deposition cavity of which the vacuum degree is 5-20hPa and the temperature is 25-400 DEG C, depositing a layer of high-dielectric metal oxide film on the surface of the corrosive aluminum foil by using a high-dielectric metal source as a precursor material, and performing anode oxidation to obtain the high-dielectric composite film. The composite film prepared by the method is closely attached to an aluminum substrate, a stripping phenomenon is eliminated, and compared with a traditional coating method, the effective coating area is greatly enlarged. The specific capacity of the corrosive aluminum foil treated by the method is 50-100% higher than that of the corrosive aluminum foil only treated by anode oxidation.

Description

technical field [0001] The invention belongs to the technical field of electronic devices, and in particular relates to a method for preparing a high-dielectric composite film in combination with ALD. Background technique [0002] With the rapid development of 3C (Computor, Communication, Control) technology, all kinds of electronic products are constantly developing towards miniaturization and portability. In order to meet this demand, electrolytic capacitors are developing in the direction of miniaturization, light weight, and high quality. The use of high specific capacity and high-performance anode aluminum foil is the key to realizing the miniaturization, light weight, and high quality of aluminum electrolytic capacitors. [0003] According to the specific volume formula C=ε·S·k -1 ·V -1 (where ε: dielectric constant of alumina; S: specific surface area of ​​electrode; k: formation constant of alumina; V: formation voltage of alumina) it can be seen that the high diel...

Claims

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Application Information

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IPC IPC(8): H01G9/04
CPCH01G9/0032H01G9/04
Inventor 杜显锋林白阁徐友龙
Owner XI AN JIAOTONG UNIV
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