CN102426922B - Preparation method of pre-composite high dielectric constant medium film aluminum electrode foil - Google Patents
Preparation method of pre-composite high dielectric constant medium film aluminum electrode foil Download PDFInfo
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- CN102426922B CN102426922B CN 201110227433 CN201110227433A CN102426922B CN 102426922 B CN102426922 B CN 102426922B CN 201110227433 CN201110227433 CN 201110227433 CN 201110227433 A CN201110227433 A CN 201110227433A CN 102426922 B CN102426922 B CN 102426922B
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Abstract
A preparation method of a pre-composite high dielectric constant medium film aluminum electrode foil belongs to the electronic material technology field. In the invention, a high dielectric property of a SBA material and an Al2O3 skeleton structure are used and composite processing are performed in advance to the SBA material, the Al2O3 skeleton structure and BT so as to form a SBA (containing beta-Al2O3)/BT pre-composite structure. Then, through traditional anodic oxidation, by using a conduction effect of the Al2O3 skeleton structure in the pre-composite structure to Al and O irons, the BT material can exist in the high dielectric constant composite medium film as a 0-3 type composite form so that purposes of controlling a medium phase ingredient and a micro existence state can be reached. A technology is simple and is easy to be controlled. The method can be combined with aluminum electrode foil corrosion and a forming technology production line so as to realize the linkage production. Compared to the traditional technology, by using the technology of the invention, an aluminum forming foil specific volume in a low pressure stage has increased by 40%.
Description
Technical field
The invention belongs to technical field of electronic materials, relate to electrolytic capacitor with the technology of preparing of aluminum electric pole foil, especially have the preparation method of high-k composite dielectric film aluminum electric pole foil.
Background technology
The high speed development of microelectronic industry has been accelerated the process that the Circuits System integrated level improves, aluminium electrolytic capacitor as in the electronic circuit must but be difficult to integrated a kind of discrete electronic device, the size of its volume has become the huge obstacle of restriction complete electronic set system miniaturization.The core component of aluminium electrolytic capacitor is aluminum electric pole foil, its volume dwindle the raising that depends on aluminum electric pole foil specific volume level.Along with updating of aluminum electric pole foil corrosion technology, the expansion face multiplying power of aluminium etched foil is near theoretical limit, and the specific volume that improves aluminum electric pole foil by the method is very difficult.Therefore, by the dielectric constant of Composite Preparation technology raising aluminum electric pole foil deielectric-coating, becoming the important technology approach of the high specific volume aluminum electric pole foil of present acquisition, is the focus of studying in recent years and paying close attention to.
The conventional aluminum electrolytic capacitor is lower with the relative dielectric constant of anodic alumina films, be generally 7～10, and the relative dielectric constant of valve metal (Ti, Ta, Nb, Zr etc.) oxide is than aluminum oxide height, and the relative dielectric constant of ferroelectric material barium titanate, strontium titanates etc. more can reach hundreds of even several ten thousand.These high dielectric constant materials are incorporated in the alumilite process deielectric-coating, form the high-k composite dielectric film, can improve the aluminum electric pole foil specific volume from this technical thought, thereby improve the capacity of aluminium electrolytic capacitor, dwindle its volume.Existing patent (spy opens flat 3-131014, EP350108, the spy opens clear 55-69291, CN100463086C, CN1272815C, CN100365167C) has prepared the high-k composite dielectric film by physics or chemical method, thereby has improved the specific capacitance of aluminium electrolytic capacitor effectively.Above-mentioned technology part has obtained promotion and application in mesohigh section aluminum electric pole foil, but improves effect and not obvious at the capacity of low pressure stage, and its capacity increase rate also differs greatly apart from the compound theoretical capacity of high dielectric.
In fact, the microcosmic component of composite dielectric film and growth conditions are the key factors that determines the performance of composite dielectric film dielectric property.Existing compound capacity increasing technique all is by directly depositing the single phase material of high-k at aluminium foil surface, and anodic oxidation forms aluminium electrolytic capacitor high dielectric constant film then, and this high-k composite dielectric film generally is layer growth.Theoretical calculating shows that this stratiform composite mode is unfavorable for the raising of the whole effective dielectric constant of deielectric-coating, and is all the more so during especially for low pressure stage deielectric-coating thinner thickness.
In recent years, conducting particles is distributed to constitutes compound system in the dielectric base body, can reach the purpose that significantly improves the dielectric film dielectric constant and the concern that enjoys the researcher.People such as Bhola N have prepared high dielectric Sodium Beta-alumina (SBA) system material (Bhola N.Pal by low temperature liquid polymerization process, Bal Mukund Dhar, Kevin C.See and Howard E.Katz.Nature Materials, 2009,8:898～903), this material has special two-dimension netted microstructure, and its skeleton structure is β-Al
2O
3, the Na ion is at Al
2O
3Have good two-dimentional conductibility between insulating barrier lattice dot matrix, under outer field action, the dielectric constant of this material can reach 170.
Technology contents
The invention provides a kind of preparation method of pre-composite high-dielectric constant dielectric film aluminum electrode foil electrode foil.This method is utilized high dielectric property and the Al of SBA material
2O
3Skeleton structure is carried out Combined Processing in advance with ferroelectric barium titanate (BT) material, forms SBA and (contains β-Al
2O
3The pre-composite construction of)/BT; Then by conventional anodization, by Al in the pre-composite construction
2O
3Skeleton structure makes the BT material be present in the high-k composite dielectric film with 0-3 type complex form to the conduction of Al, O ion, reaches the purpose of control medium phase component and microcosmic existence.Compare with existing high-k composite dielectric film aluminum electric pole foil preparation method, this method can realize the control to complex media phase micro Distribution state, and have characteristics with low cost, simple to operate, can expand the face production line with present electrochemical corrosion and change into production line and realize interlock production.
The technology of the present invention implementation is as follows:
A kind of preparation method of pre-composite high-dielectric constant dielectric film aluminum electrode foil electrode foil may further comprise the steps:
Step 1: aluminum nitrate and sodium hydrogensulfite are dissolved in the EGME simultaneously, stir under the room temperature and obtain solution 1, control solution 1 concentration is between 0.1～0.5mol/L, and wherein the mol ratio of aluminum nitrate and sodium hydrogensulfite is between 1: 1～40: 1.
Step 2: barium acetate is dissolved in the glacial acetic acid, obtains solution 2, control solution 2 concentration are between 0.1～1mol/L.
Step 3: butyl titanate is dissolved in the lactic acid, and 60～80 ℃ of following stirrings obtain solution 3, and control solution 3 concentration are between 0.1～1mol/L.
Step 4: step 3 gained solution 3 is slowly added in the step 2 gained solution 2, obtain solution 4, the mol ratio of control butyl titanate and barium acetate is 1: 1, adds glacial acetic acid simultaneously and adjusts the pH value of solution 4 between 1～2.
Step 5: the solution 1 of step 1 gained is added in the solution 4 of step 4 gained, obtain solution 5, the mol ratio of control aluminum nitrate and barium acetate is between 1: 5～1: 50; Handle solution 5 ageings more than 20 hours then.
Step 6: in the solution 5 after the aluminium etched foil be impregnated in the ageing of step 5 gained and handle 1～10 minute, take out then, with washed with de-ionized water and oven dry.
Step 7: will heat-treat through the aluminium etched foil that step 6 was handled, heat treatment temperature is controlled between 300～550 ℃, and heat treatment time is 2～30 minutes.Heat treatment process can directly realize in air atmosphere.In general, the control heat treatment temperature is 450～550 ℃, and heat treatment time is to be best between 10～30 minutes.
Step 8: will carry out anodized through the aluminium etched foil that step 7 was handled, and finally obtain the aluminum electric pole foil of pre-composite high-dielectric constant deielectric-coating.
The present invention adds equally with the SBA material of organic system as the solvent preparation in the high dielectric barium titanate material organic system that adopts the sol-gel process preparation, and exist for barium-titanate material and the SBA material of organic system provide good combinational environment.The aluminium etched foil through impregnation process, and forms SBA on its surface and (contains β-Al in this composite system after heat treatment process
2O
3The pre-composite construction of)/BT, the organic principle in the system is removed through pyrolysis.
Al in the SBA material
2O
3Skeleton structure and barium-titanate material compound in advance can effectively change the existence of composite dielectric film after anodic oxidation.Al
2O
3Skeleton structure can be the pathway that follow-up anode oxidation process provides Al, O ion, promotes newly-generated Al
2O
3Medium separates the BT particulate, forms the high-k composite dielectric film with body phase composite construction at aluminium etched foil spatial induction.Simultaneously, the SBA material has certain crystalline structure, is conducive to induce in anode oxidation process the generation of crystal formation pellumina, and the crystal formation pellumina has promoted the raising of composite dielectric film dielectric constant to a certain extent.The aluminium anodes that utilizes the present invention to prepare changes into paper tinsel and compares with the paper tinsel of handling without the present invention that changes into, and specific volume can improve about 40% at low pressure stage; And changing into paper tinsel with respect to only carrying out the single aluminium anodes of handling mutually of high dielectric barium titanate, specific volume has 10% raising approximately at low pressure stage.
The present invention has the following advantages and effect:
1. the pre-composite high-dielectric constant dielectric film aluminum electrode foil electrode foil of the present invention preparation, its specific volume becomes paper tinsel to improve 10% at low pressure stage than the calorize of only handling through barium titanate, and becomes paper tinsel to improve about 40% than the calorize without any processing.
2. high dielectric barium titanate material and SBA material is compound in advance, is conducive to form the high-k composite dielectric film with body phase composite construction at surface of aluminum electrode foil after anodic oxidation.
3. the present invention is simple and convenient, is easy to realize interlock production with existing aluminum electric pole foil industrial production line.
Embodiment
Embodiment 1:
A kind of preparation method of pre-composite high-dielectric constant dielectric film aluminum electrode foil electrode foil may further comprise the steps:
Step 1: aluminum nitrate and sodium hydrogensulfite are dissolved in the EGME simultaneously, stir under the room temperature and obtain solution 1, control solution 1 concentration is between 0.1～0.5mol/L, and wherein the mol ratio of aluminum nitrate and sodium hydrogensulfite is between 1: 1～40: 1;
Step 2: barium acetate is dissolved in the glacial acetic acid, obtains solution 2, control solution 2 concentration are between 0.1～1mol/L;
Step 3: butyl titanate is dissolved in the lactic acid, and 60～80 ℃ of following stirrings obtain solution 3, and control solution 3 concentration are between 0.1～1mol/L;
Step 4: step 3 gained solution 3 is slowly added in the step 2 gained solution 2, obtain solution 4, the mol ratio of control butyl titanate and barium acetate is 1: 1, adds glacial acetic acid simultaneously and adjusts the pH value of solution 4 between 1～2;
Step 5: the solution 1 of step 1 gained is added in the solution 4 of step 4 gained, obtain solution 5, the mol ratio of control aluminum nitrate and barium acetate is 1: 10; Handle solution 5 ageings more than 20 hours then;
Step 6: in the solution 5 after the aluminium etched foil be impregnated in the ageing of step 5 gained and handle 5 minutes, take out then, with washed with de-ionized water and oven dry;
Step 7: will place the Muffle furnace of air atmosphere to heat-treat through the aluminium etched foil that step 6 was handled, heat treatment temperature be 550 ℃, and the time is 10 minutes;
Step 8: will carry out anodized through the aluminium etched foil that step 7 was handled, and finally obtain the aluminum electric pole foil of pre-composite high-dielectric constant deielectric-coating.Concrete anode oxidation process is: anodic oxidation electrolyte employing mass fraction is 15% ammonium adipate solution, and electrolyte temperature is controlled between 75 ± 2 ℃, and oxidation current density is 50mA/cm
2, arrive the 20V constant voltage anodic oxidation again 10 minutes of energizing behind the voltage; Through 550 ℃ of heat treatment 2min of Muffle furnace, place above-mentioned ammonium adipate solution more then, anodic oxidation is 2 minutes under identical voltage.
Adopt and obtain calorize behind the above-mentioned processing step and become paper tinsel, test changes into the paper tinsel specific volume as can be known: through the paper tinsel that changes into of PROCESS FOR TREATMENT of the present invention, its specific volume is handled than single phase barium titanate and has been improved 9.2%, and becomes the paper tinsel specific volume to improve 38% with respect to the calorize without any Processing of Preparation.
Embodiment 2:
A kind of preparation method of pre-composite high-dielectric constant dielectric film aluminum electrode foil electrode foil may further comprise the steps:
Step 1: aluminum nitrate and sodium hydrogensulfite are dissolved in the EGME simultaneously, stir under the room temperature and obtain solution 1, control solution 1 concentration is between 0.1～0.5mol/L, and wherein the mol ratio of aluminum nitrate and sodium hydrogensulfite is between 1: 1～40: 1;
Step 2: barium acetate is dissolved in the glacial acetic acid, obtains solution 2, control solution 2 concentration are between 0.1～1mol/L;
Step 3: butyl titanate is dissolved in the lactic acid, and 60～80 ℃ of following stirrings obtain solution 3, and control solution 3 concentration are between 0.1～1mol/L;
Step 4: step 3 gained solution 3 is slowly added in the step 2 gained solution 2, obtain solution 4, the mol ratio of control butyl titanate and barium acetate is 1: 1, adds glacial acetic acid simultaneously and adjusts the pH value of solution 4 between 1～2;
Step 5: the solution 1 of step 1 gained is added in the solution 4 of step 4 gained, obtain solution 5, the mol ratio of control aluminum nitrate and barium acetate is 1: 5; Handle solution 5 ageings more than 20 hours then;
Step 6: in the solution 5 after the aluminium etched foil be impregnated in the ageing of step 5 gained and handle 5 minutes, take out then, with washed with de-ionized water and oven dry;
Step 7: will place the Muffle furnace of air atmosphere to heat-treat through the aluminium etched foil that step 6 was handled, heat treatment temperature be 550 ℃, 10 minutes time;
Step 8: will carry out anodized through the aluminium etched foil that step 7 was handled, and finally obtain the aluminum electric pole foil of pre-composite high-dielectric constant deielectric-coating.Concrete anode oxidation process is: anodic oxidation electrolyte employing mass fraction is 15% ammonium adipate solution, and electrolyte temperature is controlled between 75 ± 2 ℃, and oxidation current density is 50mA/cm
2, arrive the 30V constant voltage anodic oxidation again 10 minutes of energizing behind the voltage; Through 550 ℃ of heat treatment 2min of Muffle furnace, place above-mentioned ammonium adipate solution more then, anodic oxidation is 2 minutes under identical voltage.
Obtain calorize after adopting above-mentioned processing step to handle and become paper tinsel, the specific volume test result that changes into paper tinsel shows: become paper tinsel with respect to the calorize of handling gained through single barium titanate mutually, the paper tinsel specific volume that changes into through PROCESS FOR TREATMENT gained of the present invention has improved 11.2%, and becomes the paper tinsel specific volume to improve 43% with respect to the calorize without any Processing of Preparation.
Embodiment 3:
A kind of preparation method of pre-composite high-dielectric constant dielectric film aluminum electrode foil electrode foil may further comprise the steps:
Step 1: aluminum nitrate and sodium hydrogensulfite are dissolved in the EGME simultaneously, stir under the room temperature and obtain solution 1, control solution 1 concentration is between 0.1～0.5mol/L, and wherein the mol ratio of aluminum nitrate and sodium hydrogensulfite is between 1: 1～40: 1;
Step 2: barium acetate is dissolved in the glacial acetic acid, obtains solution 2, control solution 2 concentration are between 0.1～1mol/L;
Step 3: butyl titanate is dissolved in the lactic acid, and 60～80 ℃ of following stirrings obtain solution 3, and control solution 3 concentration are between 0.1～1mol/L;
Step 4: step 3 gained solution 3 is slowly added in the step 2 gained solution 2, obtain solution 4, the mol ratio of control butyl titanate and barium acetate is 1: 1, adds glacial acetic acid simultaneously and adjusts the pH value of solution 4 between 1～2;
Step 5: the solution 1 of step 1 gained is added in the solution 4 of step 4 gained, obtain solution 5, the mol ratio of control aluminum nitrate and barium acetate is 1: 50; Handle solution 5 ageings more than 20 hours then;
Step 6: in the solution 5 after the aluminium etched foil be impregnated in the ageing of step 5 gained and handle 5 minutes, take out then, with washed with de-ionized water and oven dry;
Step 7: will place the Muffle furnace of air atmosphere to heat-treat through the aluminium etched foil that step 6 was handled, heat treatment temperature be 550 ℃, 10 minutes time;
Step 8: will carry out anodized through the aluminium etched foil that step 7 was handled, and finally obtain the aluminum electric pole foil of pre-composite high-dielectric constant deielectric-coating.Concrete anode oxidation process is: anodic oxidation electrolyte employing mass fraction is 15% ammonium adipate solution, and electrolyte temperature is controlled between 75 ± 2 ℃, and oxidation current density is 50mA/cm
2, arrive the 20V constant voltage anodic oxidation again 10 minutes of energizing behind the voltage; Through 550 ℃ of heat treatment 2min of Muffle furnace, place above-mentioned ammonium adipate solution more then, anodic oxidation is 2 minutes under identical voltage.
Adopt above-mentioned processing step to prepare calorize and become paper tinsel, the specific volume test result that changes into paper tinsel shows: the paper tinsel that changes into that adopts PROCESS FOR TREATMENT gained of the present invention, its specific volume more only changes into paper tinsel through barium titanate processing gained and has improved 8.1%, and has improved 36.8% with respect to the paper tinsel that changes into without any Processing of Preparation.
Claims (3)
1. the preparation method of a pre-composite high-dielectric constant dielectric film aluminum electrode foil electrode foil may further comprise the steps:
Step 1: aluminum nitrate and sodium hydrogensulfite are dissolved in the EGME simultaneously, stir under the room temperature and obtain solution 1, control solution 1 concentration is between 0.1～0.5mol/L, and wherein the mol ratio of aluminum nitrate and sodium hydrogensulfite is between 1: 1～40: 1;
Step 2: barium acetate is dissolved in the glacial acetic acid, obtains solution 2, control solution 2 concentration are between 0.1～1mol/L;
Step 3: butyl titanate is dissolved in the lactic acid, and 60～80 ℃ of following stirrings obtain solution 3, and control solution 3 concentration are between 0.1～1mol/L;
Step 4: step 3 gained solution 3 is slowly added in the step 2 gained solution 2, obtain solution 4, the mol ratio of control butyl titanate and barium acetate is 1: 1, adds glacial acetic acid simultaneously and adjusts the pH value of solution 4 between 1～2;
Step 5: the solution 1 of step 1 gained is added in the step 4 gained solution 4, obtain solution 5, the mol ratio of control aluminum nitrate and barium acetate is between 1: 5～1: 50; Handle solution 5 ageings more than 20 hours then;
Step 6: in the solution 5 after the aluminium etched foil be impregnated in the ageing of step 5 gained and handle 1～10 minute, take out then, with washed with de-ionized water and oven dry;
Step 7: will heat-treat through the aluminium etched foil that step 6 was handled, heat treatment temperature is controlled between 300～550 ℃, and heat treatment time is 2～30 minutes;
Step 8: will carry out anodized through the aluminium etched foil that step 7 was handled, and finally obtain the aluminum electric pole foil of pre-composite high-dielectric constant deielectric-coating.
2. the preparation method of pre-composite high-dielectric constant dielectric film aluminum electrode foil electrode foil according to claim 1 is characterized in that, the step 7 pair equipment that adopts when the aluminium etched foil that step 6 was handled is heat-treated is the Muffle furnace under the air atmosphere.
3. the preparation method of pre-composite high-dielectric constant dielectric film aluminum electrode foil electrode foil according to claim 1, it is characterized in that, the technology of anodized described in the step 8 is: anodic oxidation electrolyte employing mass fraction is 15% ammonium adipate solution, electrolyte temperature control is between 75 ± 2 ℃, and oxidation current density is 50mA/cm
2, constant voltage anodic oxidation 10 minutes again behind the voltage of arrive setting of energizing.
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| CN102509626A (en) * | 2011-11-21 | 2012-06-20 | 电子科技大学 | Method for preparing aluminum electrode foil with high dielectric constant composite dielectric film |
| CN108807017A (en) * | 2018-06-22 | 2018-11-13 | 宇东箔材科技南通有限公司 | The preparation method of compound dielectric film aluminum electrode foil |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101093751A (en) * | 2006-11-17 | 2007-12-26 | 深圳清华大学研究院 | Method for preparing foil of cathode with high specific volume |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101093751A (en) * | 2006-11-17 | 2007-12-26 | 深圳清华大学研究院 | Method for preparing foil of cathode with high specific volume |
Non-Patent Citations (8)
| Title |
|---|
| Bhola N. Pal等.Solution-deposited sodium beta-alumina gate dielectrics for low-voltage and transparent field-effect transistors.《NATURE MATERIALS》.2009,第8卷 |
| Formation of Al2O3–BaTiO3 composite thin film to increase the specific capacitance of aluminum electrolytic capacitor;Xianfeng Du等;《Thin Solid Films》;20080418;第8436页第1段至8437页右栏第1段 * |
| Solution-deposited sodium beta-alumina gate dielectrics for low-voltage and transparent field-effect transistors;Bhola N. Pal等;《NATURE MATERIALS》;20091018;第8卷;899页左栏倒数第一段，902页左栏最后一段 * |
| Xianfeng Du等.Formation of Al2O3–BaTiO3 composite thin film to increase the specific capacitance of aluminum electrolytic capacitor.《Thin Solid Films》.2008, |
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| 阳极氧化温度对Al-Ti 复合氧化膜结构和电性能的影响;陈金菊等;《中国科学 E 辑 技术科学》;20061231;第36卷;252页第3-4段 * |
| 陈金菊等.阳极氧化温度对Al-Ti 复合氧化膜结构和电性能的影响.《中国科学 E 辑 技术科学》.2006,第36卷 |
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