CN101651046B - Preparation method of Al2O3/TiO2 compound dielectric film aluminum electrode foil - Google Patents

Preparation method of Al2O3/TiO2 compound dielectric film aluminum electrode foil Download PDF

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CN101651046B
CN101651046B CN2009100600688A CN200910060068A CN101651046B CN 101651046 B CN101651046 B CN 101651046B CN 2009100600688 A CN2009100600688 A CN 2009100600688A CN 200910060068 A CN200910060068 A CN 200910060068A CN 101651046 B CN101651046 B CN 101651046B
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CN101651046A (en
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冯哲圣
梁孜
陈金菊
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SICHUAN LIYE ELECTRONICS CO Ltd
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University of Electronic Science and Technology of China
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Abstract

The invention relates to a preparation method of an Al2O3/TiO2 compound dielectric film aluminum electrode foil, belonging to the technical field of electronic materials. The invention adopts a cathode electrochemical deposition technology and comprises the following steps: depositing TiO3(H2O)x on the surface of an aluminum etching foil through an inert metal anode and a soluble titanium salt solution system; then decomposing the TiO3(H2O)x through temperature control heat treatment to obtain an anatase TiO2 nanometer high dielectric oxidation film; and finally, through a conventional barrier type aluminum anode oxidation technology, preparing an Al2O3/TiO2 compound dielectric film with a high dielectric constant so as to obtain the Al2O3/TiO2 compound dielectric film aluminum electrode foil. Under the condition that the thickness of the compound dielectric film on the surface of the aluminum electrode foil is the same as that of a conventional dielectric film, the aluminum electrode foil of the invention has higher dielectric constant and can effectively improve the capacitance level.

Description

A kind of Al 2O 3/ TiO 2The preparation method of composite dielectric film aluminum electric pole foil
Technical field
The invention belongs to technical field of electronic materials, relate to a kind of preparation method of composite dielectric film aluminum electric pole foil, the aluminum electric pole foil that utilizes the present invention to prepare is mainly used in the aluminium electrolytic capacitor.
Background technology
Aluminium electrolytic capacitor plays indispensable effect with its unit volume rate capabilities height, characteristics with low cost in the electronic devices and components field.The core component of aluminium electrolytic capacitor is an aluminum electric pole foil, adopts anode oxidation process to handle the alumina deielectric-coating that the back obtains at surface of aluminum electrode foil, is the critical material that aluminium electrolytic capacitor forms capacitance characteristic.Miniaturization, high performance, long lifetime are the aluminium electrolytic capacitor main directions of development at present.
Aluminium electrolytic capacitor realizes that the key of miniaturization is the preparation of height ratio capacity (abbreviation specific volume) aluminum electric pole foil.According to plate condenser static capacity fundamental formular: C ∝ ε 0ε rS/d can improve the technology of aluminum electric pole foil specific volume by following three kinds of approach: the thickness d that the first, reduces the surface of aluminum electrode foil deielectric-coating; The second, increase aluminum electric pole foil specific area S; Three, improve the DIELECTRIC CONSTANT of surface of aluminum electrode foil deielectric-coating rIn fact, voltage-resistent characteristic also is an important indicator weighing aluminum electric pole foil, the thickness and the proof voltage of alumina deielectric-coating are closely related, at present under identical proof voltage, the technological means that can reduce deielectric-coating thickness significantly still lacks, and therefore the difficulty that increases substantially by technological approaches one realization aluminum electric pole foil specific volume level is very big.At present industrial extensive employing technological approaches two improves aluminum electric pole foil specific volume level, its technological means is by in mixed acid system aluminium foil being implemented chemistry and the processing of electrochemical corrosion expansion face, form microcosmic etch pit hole at surface of aluminum electrode foil, increase the aluminum electric pole foil specific area, thereby reach the purpose that improves the aluminum electric pole foil specific volume.For a long time, technological approaches two is the main method of industrial raising aluminum electric pole foil specific volume level always.Yet for guaranteeing the mechanical strength of aluminum electric pole foil necessity, electrochemical corrosion is expanded face and can not infinitely be carried out.Over past ten years, the electrochemical corrosion of industrial products is expanded the face multiplying power near theoretical multiplying power, improves specific volume difficulty day by day by enlarging the electrode foil method for specific area.On this technological approaches, the researcher is by adjusting aluminium foil surface texture, optimize the corrosive liquid system, adopt multiple means such as frequency conversion corrosion power supply and multistage etching process to make etched foil surface pit morphology Control more accurate, pit density further improves, the continuous refinement of pit, approximation theory expands the face multiplying power as far as possible.But meticulous micropore will cause working electrolyte to soak into difficulty, cause that aluminium electrolytic capacitor loss rising, impedance operator and frequency characteristic descend.Therefore realize that by technological approaches two aluminum electric pole foil specific volume level has entered bottleneck stage.
As the main direction of aluminum current electrode foil capacity increasing technique, utilize clad aluminum deielectric-coating technology of preparing to improve the method for dielectric constant, that is technological approaches three become the key that realizes the aluminium electrolytic capacitor miniaturization, be subjected to extensive concern.
Usually the aluminum electric pole foil deielectric-coating of preparing traditionally is Al 2O 3, its dielectric constant is incorporated in the aluminium anode oxide film if can will have the metal oxide (high dielectric phase) of high dielectric property about 8～10, can form the high-k composite dielectric film, can effectively improve the aluminum electric pole foil specific volume.Effectively compound for realizing in the aluminium etched foil being carried out anodic oxidation (industrial being called changes into) process, common high dielectric is chosen as the oxide of valve metal system mutually, as Ta 2O 5(dielectric constant is 28), Nb 2O 5(dielectric constant is 41), TiO 2(dielectric constant is 48) etc.
Realize high dielectric phase and Al at present 2O 3Compound technological means mainly contains alloyage process, physical vapour deposition (PVD) (PVD method), sol-gal process, hydrolysis sedimentation etc.The existing flat 4-42519 of open patent prepares the high-k composite dielectric film by physical method depositing Ti metal alkoxide, but above technology film forming dielectric loss is excessive, and at low pressure stage (≤50V) effect and not obvious.Patent ZL03114518.3 has realized ferroelectric material composite dielectric film growing technology by sol-gal process.The prepared ferroelectric material composite dielectric film of sol-gal process, because the ferroelectric material sintering temperature is higher, aluminum electric pole foil burns easily in preparation process, and the whole sol-gel process cycle is longer.
Summary of the invention
The invention provides a kind of Al 2O 3/ TiO 2The preparation method of composite dielectric film aluminum electric pole foil, the cathodic electrochemical deposition technology that routine is applied to photocatalysis and field of nano material preparation is incorporated in the aluminum electric pole foil deielectric-coating technology of preparing, by selecting inert metal anode and soluble titanium salting liquid system, be implemented in the high dielectric phase of surface of aluminum electrode foil pre-deposition nano thickness, by conventional barrier type anode oxidation technology, prepare the high-k composite dielectric film then at aluminium foil surface.The aluminum electric pole foil that this method is prepared, its surface recombination deielectric-coating has higher dielectric constant under the thickness situation identical with the traditional sucrose film thickness, can effectively improve the electric capacity level of aluminum electric pole foil.
Technical solution of the present invention is as follows:
A kind of Al 2O 3/ TiO 2The preparation method of composite dielectric film aluminum electric pole foil as shown in Figure 1, may further comprise the steps:
Step 1: preparation TiCl 4And H 2O 2Mixed electrolytic solution.At first with TiCl 4Be dissolved in the mixed solvent of alcohol organic solvent and deionized water, drip H then 2O 2The aqueous solution is until obtaining color gamut at orange-yellow solution between brownish red.
Concrete course of reaction in the step 1 is as follows:
Ti 4++ H 2O 2+ (n-2) H 2O → [Ti (O 2) (OH) N-2] (4-n)++ nH +, contain [Ti (O because the mixed solution system reaction generates 2) (OH) N-2] (4-n)+Complex ion, wherein n equals 2,3 or 4, makes whole mixed solution system present certain color, works as TiCl 4And H 2O 2Ratio content and concentration when changing continuously within the specific limits, the color of whole mixed solution system orange-yellow to changing continuously between the brownish red.
Step 2: inert metal and aluminium etched foil be impregnated in the electrolyte of step 1 gained, are anodal with the inert metal, and the aluminium etched foil is a negative pole, carries out cathodic electrochemical deposition, obtains TiO at aluminium etched foil surface deposition 3(H 2O) x
Concrete course of reaction in the step 2 is as follows:
2H 2O+2e -→H 2+2OH -
[Ti(O 2)(OH) n-2] (4-n)++(4-n)OH -+(x-1)H 2O→TiO 3(H 2O) x
Step 3: adopt the surface deposition of washed with de-ionized water step 2 gained that TiO is arranged 3(H 2O) xThe aluminium etched foil.
Step 4: the surface deposition after step 3 cleaning is had TiO 3(H 2O) xThe aluminium etched foil carry out temperature control heat treatment, make the TiO that is deposited on aluminium etched foil surface 3(H 2O) xAnnealed dehydration obtains TiO 2Thereby, obtain TiO on aluminium etched foil surface 2Nano oxidized film.
Concrete course of reaction in the step 4 is as follows:
2TiO 3(H 2O) x→2TiO 2+O 2+2xH 2O
Step 5: the surface to step 4 gained has TiO 2The aluminium etched foil of nano oxidized film carries out anodic oxidation, obtains having Al 2O 3/ TiO 2The aluminum electric pole foil of composite dielectric film.
What technique scheme need further specify is:
1, prepares TiCl in the step 1 4And H 2O 2Mixed electrolytic solution the time, described H 2O 2Consumption should surpass TiCl 4Consumption.Because TiCl 4And H 2O 2Mixed electrolytic solution in have following reaction: Ti 4++ H 2O 2+ (n-2) H 2O → [Ti (O 2) (OH) N-2] (4-n)++ nH +Only at H 2O 2Under the excessive situation, Ti 4+Fully reaction generates [Ti (O 2) (OH) N-2] (4-n)+, otherwise part Ti 4+May with OH -Reaction generates Ti (OH) 4Precipitation so just is unfavorable for Ti 4+Make full use of.
2, prepare TiCl in the step 1 4And H 2O 2Mixed electrolytic solution the time, the volume ratio of described deionized water and alcohol organic solvent is 3: 1.Described alcohol organic solvent can be methyl alcohol, ethanol or propyl alcohol.
3, TiCl 4And H 2O 2Mixed electrolytic solution in, solute TiCl 4And H 2O 2Concentration can influence the effect of step 2 cathodic electrochemical deposition, if TiCl 4And H 2O 2Concentration excessive, can make TiO 3(H 2O) xInhomogeneous at aluminium etched foil surface deposition.During practical operation, should control TiCl in the mixed electrolytic solution 4And H 2O 2Concentration between 0.001～0.1mol/L.
When 4, step 2 was carried out cathodic electrochemical deposition, the concrete weighing apparatus stream DC power supply that adopts was carried out cathode electrodeposition, and electric current is 0.001～1A, and voltage is 5～50V, and electrodeposition temperature is 0～30 ℃, and electrodeposition time is 1～20 minute.
5, the surface deposition of step 3 pair step 2 gained has TiO 3(H 2O) xThe aluminium etched foil adopt washed with de-ionized water, its objective is the electrolyte that washes aluminium etched foil remained on surface, Cl especially wherein -Ion is in order to avoid Cl -Ion pair aluminium etched foil produces the burn into destruction.
6, the surface deposition after the step 4 pair cleaning has TiO 3(H 2O) xAluminium etched foil when carrying out temperature control heat treatment, concrete steps are as follows:
Step 4-1: the surface deposition after cleaning is had TiO 3(H 2O) xThe aluminium etched foil carry out Low Temperature Heat Treatment, to remove surface deposition TiO is arranged 3(H 2O) xThe moisture and the alcohol organic solvent on aluminium etched foil surface.Actual temp is controlled between 60～100 ℃, and the processing time is 5～10 minutes;
Step 4-2: the surface deposition after Low Temperature Heat Treatment is had TiO 3(H 2O) xThe aluminium etched foil carries out high-temperature heat treatment, makes the TiO that is deposited on aluminium etched foil surface 3(H 2O) xAnnealed dehydration obtains TiO 2Actual temp is controlled between 400～700 ℃, and the processing time is 1～10 minute.
After high-temperature heat treatment, TiO 3(H 2O) xDecompose and obtain Detitanium-ore-type TiO 2, deposited film surface makes rete produce be full of cracks because the hydrone of sloughing causes volume contraction, this provides advantage for electrolyte in the follow-up anode oxidation process with contacting of aluminum substrate, the depositional coating surface as shown in Figure 2, while TiO 2Existence can effectively suppress Al in step 4 heat treatment process 2O 3The growth of heat oxide film.
7, step 5 pair step 4 gained surface has TiO 2The aluminium etched foil of nano oxidized film carries out anodic oxidation, because TiO in the step 4 2Rete has replaced Al 2O 3The existence of heat oxide film, anodic oxidation speed obviously improves, and this can be anodic oxidation and saves big volume and electricity.Anodised detailed process can adopt existing chemical synthesis technology.
Compared with prior art, the present invention has following characteristics: the first, adopt the cathodic electrochemical deposition method to deposit high dielectric phase medium film, by control solution composition, deposition current and sedimentation time, be may command high dielectric phase nucleation density and deposit thickness, realize the nanoscale control that high dielectric prepares mutually, help high dielectric phase and Al 2O 3Effectively compound; The second, the high dielectric of nanoscale deposits mutually after high temperature sintering, crystal formation can take place on the one hand to be transformed, further improve dielectric constant, can produce be full of cracks at the high dielectric phase surface of nanoscale on the other hand, electrolyte penetrating and contacting with aluminum substrate when helping follow-up anodic oxidation, promote the anodic oxidation process, improve high dielectric phase and Al 2O 3Combined efficiency; Three, compare with the conventional aluminium etched foil, obviously improve through the aluminum electric pole foil anodic oxidation speed of the high dielectric phase of cathode electrodeposition method pre-deposition, the oxidation current utilization ratio is higher, can reduce the industrial production energy consumption; Four, obvious through the aluminium etched foil compatibilization effect of the technology of the present invention processing.
Description of drawings
Fig. 1 is a schematic flow sheet of the present invention.
Fig. 2 is for to carry out electrochemical deposition gained Detitanium-ore-type TiO through this method 2The SEM photo of deposited film surface topography.
Fig. 3 is the SEM photo of the surface topography of the prepared composite dielectric film aluminum electric pole foil of the present invention.
Fig. 4 is the XRD analysis resolution chart of the prepared composite dielectric film aluminum electric pole foil of the present invention.
Embodiment
Execution mode 1:
Deionized water and methyl alcohol evenly mixed in 3: 1 ratio obtain methanol aqueous solution, adding TiCl 4And H 2O 2Solution, control TiCl 4Concentration is 0.005mol/L, H 2O 2Concentration is 0.02mol/L, and the control solution temperature is at 5 ℃; Be positive pole with inert metal platinum then, the aluminium etched foil is carried out cathode electrodeposition, electric current is 0.005A, and voltage is 8V, and sedimentation time is 20 minutes.
By low temperature and high-temperature heat treatment, wherein the temperature of Low Temperature Heat Treatment is 75 ℃, and the processing time is 5 minutes; The high-temperature heat treatment temperature is 550 ℃, and the processing time is 10 minutes.By above-mentioned temperature control heat treatment, at aluminium etched foil surface deposition Detitanium-ore-type TiO 2Nano oxidized film.
After adopting above-mentioned PROCESS FOR TREATMENT, etched foil changes into ammonium adipate under the 20V direct voltage, and test changes into the paper tinsel specific volume then, and it becomes paper tinsel specific volume growth rate to be about 11.7% with respect to handling prepared calorize without the method for the invention.
Execution mode 2:
Deionized water and methyl alcohol evenly mixed in 3: 1 ratio obtain methanol aqueous solution, adding TiCl 4And H 2O 2Solution, control TiCl 4Concentration is 0.01mol/L, H 2O 2Concentration is 0.03mol/L, and the control solution temperature is at 5 ℃; Be positive pole with inert metal platinum then, the aluminium etched foil is carried out cathode electrodeposition, electric current is 0.01A, and voltage is 15V, and sedimentation time is 10 minutes.
By low temperature and high-temperature heat treatment, wherein the temperature of Low Temperature Heat Treatment is 60 ℃, and the processing time is 5 minutes; The high-temperature heat treatment temperature is 450 ℃, and the processing time is 10 minutes.By above-mentioned temperature control heat treatment, at aluminium etched foil surface deposition Detitanium-ore-type TiO 2Nano oxidized film.
After adopting above-mentioned PROCESS FOR TREATMENT, etched foil changes into ammonium adipate under the 20V direct voltage, and test changes into the paper tinsel specific volume then, and it becomes paper tinsel specific volume growth rate to be about 15.3% with respect to handling prepared calorize without the method for the invention.
Execution mode 3:
Deionized water and methyl alcohol evenly mixed in 3: 1 ratio obtain methanol aqueous solution, adding TiCl 4And H 2O 2Solution, control TiCl 4Concentration is 0.1mol/L, H 2O 2Concentration is 0.2mol/L, and the control solution temperature is at 20 ℃; Be positive pole with inert metal platinum then, the aluminium etched foil is carried out cathode electrodeposition, electric current is 0.5A, and voltage is 50V, and sedimentation time is 1 minute.
By low temperature and high-temperature heat treatment, wherein the temperature of Low Temperature Heat Treatment is 100 ℃, and the processing time is 5 minutes; The high-temperature heat treatment temperature is 600 ℃, and the processing time is 2 minutes.By above-mentioned temperature control heat treatment, at aluminium etched foil surface deposition Detitanium-ore-type TiO 2Nano oxidized film.
After adopting above-mentioned PROCESS FOR TREATMENT, etched foil changes into ammonium adipate under the 35V direct voltage, and test changes into the paper tinsel specific volume then, and it becomes paper tinsel specific volume growth rate to be about 10.4% with respect to handling prepared calorize without the method for the invention.
According to the prepared composite dielectric film aluminum electric pole foil of above-mentioned real-time mode, the SEM photo of its surface topography as shown in Figure 3.The XRD analysis test is done in " ten " word symbol zone in Fig. 3, and the gained result can see TiO among Fig. 4 as shown in Figure 4 significantly 2Existence.

Claims (7)

1. Al 2O 3/ TiO 2The preparation method of composite dielectric film aluminum electric pole foil may further comprise the steps:
Step 1: preparation TiCl 4And H 2O 2Mixed electrolytic solution; At first with TiCl 4Be dissolved in the mixed solvent of alcohol organic solvent and deionized water, drip H then 2O 2The aqueous solution is until obtaining color gamut at orange-yellow solution between brownish red;
Step 2: inert metal and aluminium etched foil be impregnated in the electrolyte of step 1 gained, are anodal with the inert metal, and the aluminium etched foil is a negative pole, carries out cathodic electrochemical deposition, obtains TiO at aluminium etched foil surface deposition 3(H 2O) x
Step 3: adopt the surface deposition of washed with de-ionized water step 2 gained that TiO is arranged 3(H 2O) xThe aluminium etched foil;
Step 4: the surface deposition after step 3 cleaning is had TiO 3(H 2O) xThe aluminium etched foil carry out temperature control heat treatment, make the TiO that is deposited on aluminium etched foil surface 3(H 2O) xAnnealed dehydration obtains TiO 2Thereby, obtain TiO on aluminium etched foil surface 2Nano oxidized film;
Step 5: the surface to step 4 gained has TiO 2The aluminium etched foil of nano oxidized film carries out anodic oxidation, obtains having Al 2O 3/ TiO 2The aluminum electric pole foil of composite dielectric film.
2. Al according to claim 1 2O 3/ TiO 2The preparation method of composite dielectric film aluminum electric pole foil is characterized in that, prepares TiCl in the step 1 4And H 2O 2Mixed electrolytic solution the time, described H 2O 2Consumption surpass TiCl 4Consumption.
3. Al according to claim 1 2O 3/ TiO 2The preparation method of composite dielectric film aluminum electric pole foil is characterized in that, prepares TiCl in the step 1 4And H 2O 2Mixed electrolytic solution the time, the volume ratio of described deionized water and alcohol organic solvent is 3: 1.
4. Al according to claim 1 2O 3/ TiO 2The preparation method of composite dielectric film aluminum electric pole foil is characterized in that, alcohol organic solvent described in the step 1 is methyl alcohol, ethanol or propyl alcohol.
5. Al according to claim 1 2O 3/ TiO 2The preparation method of composite dielectric film aluminum electric pole foil is characterized in that, prepares TiCl in the step 1 4And H 2O 2Mixed electrolytic solution the time, control mixed electrolytic solution in TiCl 4And H 2O 2Concentration between 0.001～0.1mol/L.
6. Al according to claim 1 2O 3/ TiO 2The preparation method of composite dielectric film aluminum electric pole foil is characterized in that, when step 2 is carried out cathodic electrochemical deposition, the concrete weighing apparatus stream DC power supply that adopts is carried out cathode electrodeposition, and electric current is 0.001～1A, and voltage is 5～50V, electrodeposition temperature is 0～30 ℃, and electrodeposition time is 1～20 minute.
7. Al according to claim 1 2O 3/ TiO 2The preparation method of composite dielectric film aluminum electric pole foil is characterized in that, the surface deposition after the step 4 pair cleaning has TiO 3(H 2O) xAluminium etched foil when carrying out temperature control heat treatment, concrete steps are as follows:
Step 4-1: the surface deposition after cleaning is had TiO 3(H 2O) xThe aluminium etched foil carry out Low Temperature Heat Treatment, to remove surface deposition TiO is arranged 3(H 2O) xThe moisture and the alcohol organic solvent on aluminium etched foil surface; Actual temp is controlled between 60～100 ℃, and the processing time is 5～10 minutes;
Step 4-2: the surface deposition after Low Temperature Heat Treatment is had TiO 3(H 2O) xThe aluminium etched foil carries out high-temperature heat treatment, makes the TiO that is deposited on aluminium etched foil surface 3(H 2O) xAnnealed dehydration obtains TiO 2Actual temp is controlled between 400～700 ℃, and the processing time is 1～10 minute.
CN2009100600688A 2009-07-22 2009-07-22 Preparation method of Al2O3/TiO2 compound dielectric film aluminum electrode foil Active CN101651046B (en)

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CN102810400B (en) * 2011-05-31 2016-04-13 海洋王照明科技股份有限公司 A kind of composite solid electrolytic capacitor electrode plate and preparation method thereof
CN102605382B (en) * 2011-12-19 2014-10-29 浙江师范大学 Method for preparing high-purity nanometer titanium dioxide by electrolyzing titanium trichloride
CN104103428B (en) * 2013-04-01 2018-04-03 东莞东阳光科研发有限公司 A kind of manufacture method of aluminium electrolutic capacitor high pressure high-dielectric formed foil
CN103556197B (en) * 2013-10-31 2016-04-06 陕西师范大学 The method of monoatomic layer thicknesses of metal film prepared by flexible curling conductive substrates
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CN105702466B (en) * 2016-03-29 2018-03-09 扬州大学 A kind of preparation method of high-k formed aluminum foil
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CN112038098B (en) * 2020-08-17 2022-04-26 东莞东阳光科研发有限公司 Pretreatment method of electrode foil
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