CN101093751B - Preparation method of high specific volume cathode foil - Google Patents
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Abstract
一种高比容阴极箔的制备方法，其特征在于：选择光箔作为基材，先在其表面采用化成处理，使之在铝箔表面形成一层致密的、均匀的、具有单向导电性的氧化铝层，然后再采用磁控溅射方法在其表面形成一层钛金属膜。铝箔表面经过蒸镀处理后，还可再进行高温处理，使钛金属表面形成一层钝化膜。本发明由于提前对铝表面进行阳极氧化，与蒸镀金属直接接触的就是在氧化气氛下稳定的氧化铝层，对蒸镀金属的附着力无影响。在空气中进行高温炭化时，不会影响产品的阻抗和容量，大大简化了高比容固体电容的制备难度。另外，在磁控溅射过程中，通过连续地调节氮气浓度，可使铝箔表面金属钛成分呈梯度下降，氮化钛成分呈梯度增长，进一步提高了溅射层的稳定性。A method for preparing a high specific volume cathode foil, which is characterized in that: a light foil is selected as a base material, and a chemical conversion treatment is performed on its surface to form a layer of dense, uniform, and unidirectionally conductive on the surface of the aluminum foil. Aluminum oxide layer, and then use magnetron sputtering method to form a layer of titanium metal film on its surface. After the surface of the aluminum foil is vapor-deposited, it can be subjected to high-temperature treatment to form a passivation film on the surface of the titanium metal. In the present invention, since the aluminum surface is anodized in advance, the aluminum oxide layer that is in direct contact with the evaporated metal is the stable aluminum oxide layer in an oxidizing atmosphere, and has no influence on the adhesion of the evaporated metal. When high-temperature carbonization is carried out in air, the impedance and capacity of the product will not be affected, which greatly simplifies the difficulty of preparing high specific volume solid capacitors. In addition, during the magnetron sputtering process, by continuously adjusting the nitrogen concentration, the metal titanium composition on the surface of the aluminum foil can be gradiently decreased, and the titanium nitride composition can be gradiently increased, which further improves the stability of the sputtered layer.
Description
[technical field]
The present invention relates to a kind of aluminium electrolytic capacitor, relate in particular to a kind of cathode with high specific volume manufacturing aluminum foil that can be applicable to solid electrolyte capacitor.
[background technology]
Aluminium electrolytic capacitor becomes a kind of important foundation components and parts that are widely used in all kinds of electronic system products, high speed development along with information industry, complete electronic set is swift and violent to thin, light, little direction growth momentum, as in circuit, acting on the aluminium electrolytic capacitor of still not replacing, its volume limiting factor that become bigger than normal, demand exploring new technical cue urgently and increase substantially the ratio electric capacity of capacitor and other every electrical property, to adapt to the requirement of electronic device long lifetime.In general, be formed on anode oxide film on the aluminum electric pole foil by anodic oxidation, as the dielectric layer of aluminium electrolytic capacitor, its physics and chemical property have determined the performance of aluminium electrolytic capacitor.In the prior art, the dielectric layer of aluminum electrolysis capacitor anode foil obtains by chemical synthesis technology, described chemical synthesis technology is utilized electrochemical principle exactly, aluminium foil is carried out anodized, oxygen atom in the solution is combined with the aluminium atom, form the oxide film dielectric layer that one deck has certain dielectric constant and ability specific voltage at aluminium foil surface.
Raising aluminium electrolytic capacitor aluminium foil than the approach of electric capacity is: the long-pending S of real surface that 1. increases aluminium foil; 2. improve the relative dielectric constant ε r of dielectric layer; 3. reduce the thickness d of dielectric layer.Adopting chemistry or electrochemical etching method to enlarge aluminium foil surface long-pending is to improve the effective way of aluminium foil than electric capacity, at present in the technology, the etch factor of aluminium foil promptly expands face multiplying power G (forming the effective area of capacity and the ratio of geometric area), the target paper tinsel can reach 200, low blocking is 100, high blocking is 30, though its technology is still in continuous development, but demonstrated sign near the limit, this is because will enlarge G again, the hole that has only further refinement corrosion to form, and this will cause Working electrolyte to enter the hole difficulty, with deielectric-coating surface loose contact, loss, impedance, deteriorations such as frequency characteristic.Because under specific withstand voltage, the thickness d of dielectric layer and relative dielectric constant ε r are that the structure of matter by dielectric layer is determined, therefore might improve by the structure of matter that changes dielectric layer and compare electric capacity.At present, by changing the structure of matter of dielectric layer, form the complex oxide film of high-k, the ratio electric capacity that improves aluminium foil has become a focus of capacitor material research.
[summary of the invention]
For solving the problems of the technologies described above, the invention provides a kind of cathode with high specific volume manufacturing aluminum foil that can be applicable to solid electrolyte capacitor, it can introduce one deck high-k, high-specific surface area plated film at aluminium foil surface, makes it have very high specific capacity and chemical substance and air are at high temperature had good stable.
For achieving the above object, technical scheme proposed by the invention is:
A kind of preparation method of foil of cathode with high specific volume, it is characterized in that: select aluminium foil as base material, adopt on its surface earlier and change into processing, make it to form one deck densification, uniform, as to have unilateral conduction alumina layer, and then adopt magnetically controlled sputter method to form one deck titanium metal film, titanium nitride film, nitrogen calorize titanium film or titanium carbonitride film on its surface at aluminium foil surface; The described time 5min～30min that changes into processing, 50 ℃～80 ℃ of temperature, voltage is between 1.0～3.0 volts.
Described aluminium foil surface carries out high-temperature process after handling through magnetron sputtering again, makes surface of metal titanium form one deck passivating film;
In the described magnetron sputtering step, adopt the concentration style that improves nitrogen continuously, the composition of Titanium is descended in gradient, the composition of titanium nitride increases in gradient;
The thicknesses of layers of described titanium metal film, titanium nitride film, nitrogen calorize titanium film or titanium carbonitride film is between 1～3 μ m;
Described aluminium foil adopts mechanical means to brush out ditch earlier on its surface earlier and returns before changing into treatment step;
Perhaps, described aluminium foil adopts chemistry or electrochemical method that aluminium foil surface is slightly corroded earlier before changing into treatment step, and its corrosion multiplying power is 1～10.
The temperature that described magnetron sputtering is handled the back high-temperature process of doing is 300～500 ℃, and the time is 20～60 minutes.
The invention has the beneficial effects as follows: by before the aluminium foil evaporation, forming one deck densification, uniform, as to have unilateral conduction alumina layer on its surface, can carry out anodic oxidation to the aluminium surface in advance, air is directly contacted with alumina layer, thereby improved the adhesive force of titanium film to evaporation metal, even if in air, carry out high temperature carbonization, also can not influence the impedance and the capacity of product, simplify the preparation difficulty of high specific volume solid electric capacity greatly.In addition, aluminium foil behind the evaporation is carried out high-temperature process again, make surface of metal titanium form one deck passivating film, can make its capacity stable, and because the iris action of passivating film, can avoid changing into liquid and highly acid electrolyte corrosiveness, improve the stability of final products solid electrolyte capacitors titanium.
[embodiment]
At present, in the aluminium electrolytic capacitor field, the specific volume of aluminum electric pole foil is proportional to the relative dielectric constant of oxide-film.Aluminium anode oxide film Al
20
3Dielectric constant be generally 8～10, and Detitanium-ore-type TiO
2Dielectric constant be 48, rutile TiO
2Dielectric constant be 110～117.In the prior art field, will have ceramic oxide such as high-k valve metal oxides and be incorporated into through the method on the aluminium foil of expansion face and can adopt physical method or chemical method.
Physical method normally will have high-k valve metal or its oxide, adopt the way of magnetron sputtering, electron beam heating equal vacuum evaporation, make it form the coating of micron thickness at aluminium foil surface; Chemical method then is that the aluminium foil that will be coated with metal alkoxide carries out elevated temperature heat and decomposes or hydrolysis, prepares ultra micro (nanoscale) metal oxide powder and is deposited on method on the aluminium foil.Two kinds of methods are compared, and adopt the aluminium foil specific capacity of vacuum deposition method gained higher, and impedance is lower.
For the conductive solid polymer electrochemical capacitor, its capacity is closely related with tightness degree and the contact area that aluminium foil contacts with solid electrolyte with impedance, and solid electrolyte adheres to tight more on Cathode Foil and anode foils, and contact area is big more, it is big more that it draws capacity, and impedance is more little.Compare with liquid electrolytic electric capacity, because solid electrolyte and the contacted area of aluminium foil and level of intimate can not show a candle to the exposure level of liquid electrolyte and aluminium foil after all in the solid electrolytic capacitor, so in wet-electrolytic capacitor, show and the problem of inapparent capacity extraction rate, it is most important just to seem in solid electrolytic capacitor.For the fuse of same size, solid electric capacity will seek out the capacity close with liquid electrolytic electric capacity, is a very thing of difficulty.
Usually, the total capacity of capacitor is closely related by the actual capacity of drawing of its Cathode Foil and anode foils, has following relation.
C＝Ca×Cc/(Ca+Cc)
Wherein: C is the capacitor total capacity, and Ca is the anode foils specific volume, and Cc is the Cathode Foil specific volume.
By above-mentioned formula as can be seen, improve the specific volume of Cathode Foil, can make high the drawing of trying one's best of the capacity of anode foils.As want to draw the capacity of anode foils 80%, and the capacity that then needs Cathode Foil is 4 times of anode foils, wants to draw the capacity of anode foils 90%, the capacity that then needs Cathode Foil is 9 times of anode foils.For low pressure large bulk capacitance series, usually adopt the aluminium foil of low pressure high power capacity as anode foils, the high capacity of drawing anode foils of trying one's best, thereby the size of reduction capacitor, need adopt the very Cathode Foil of high power capacity, yet be difficult to reach so high capacity by the prepared conventional cathode paper tinsel of electrochemical corrosion.
At corrosive aluminum foil or light paper tinsel surperficial mode evaporation one deck titanium, titanium nitride or nitrogen titanium aluminide, titanium carbonitride by magnetron sputtering or other vacuum evaporations, greatly improved the specific area of aluminium foil, to compare with former paper tinsel surface, its specific capacity is several times and increases.With its negative electrode, can improve the capacity extraction rate greatly, and reduce the impedance and the DF value of electric capacity as solid electric capacity.
Because capacitor core before the impregnation polymerization generates solid electrolyte, need be handled through high temperature carbonization after a while usually, this just requires through the foil of cathode with high specific volume of special processing at high temperature in the air atmosphere, advantages of higher stability is arranged.On light paper tinsel or etched foil surface, the method by magnetron sputtering plates one deck titanium or titanium nitride, can make the very big raising of capacity of aluminium foil, uses it for the negative paper tinsel of coiling type solid electric capacity, can obtain desirable capacity extraction rate.But the applicant finds that high-temperature process will be found the big high attenuation of its capacity after a period of time in air, and impedance also improves a lot, for the Cathode Foil of using it for solid electric capacity has caused very big difficulty.If the high temperature carbonization process is carried out under nitrogen protection; these problems can be avoided; capacity and impedance nearly all do not have any change; but because high temperature processing step needs nitrogen protection; for production brings very big inconvenience; and under nitrogen atmosphere, obtain sufficient charing, need the long time.
By the Cathode Foil surface of the high specific volume of this class is analyzed, find at high temperature, above-mentioned defective mainly is that airborne oxygen can be to the binding site generation oxidation of aluminium and titanium, make the surface oxidation of aluminium, generate oxide layer, cause the script close attachment to descend to some extent, thereby cause its capacity and impedance operator acute exacerbation in the Titanium on aluminium surface and the combination degree between the base material.
Selective light paper tinsel of the present invention is as base material, earlier carry out anodized on its surface, its formation voltage is between 1.0～3.0 volts, change into 50 ℃～80 ℃ of temperature, change into time 5min～30min, make it form one deck densification, uniform, as to have unilateral conduction alumina layer, and then the mode of employing magnetron sputtering is at its surperficial evaporation one deck titanium, titanium nitride, nitrogen titanium aluminide or titanium carbonitride at aluminium foil surface, to improve the specific area of its aluminium foil, increase specific capacity.Owing in advance anodic oxidation is carried out on the aluminium surface, what directly contact with evaporation metal during magnetron sputtering is exactly alumina layer, and aluminium oxide is highly stable under oxidizing atmosphere, can not change, thus to the adhesive force of evaporation metal less than influencing.Thereby, even if in air, carry out high temperature carbonization, the final impedance and the capacity that also can not influence product, simplified the preparation difficulty of high specific volume solid electric capacity greatly, when simultaneously also having solved high-temperature process, airborne oxygen causes the problem of its capacity and impedance operator acute exacerbation to the binding site generation oxidation of aluminium and titanium.
Light paper tinsel as base material, can adopt the means of mechanical expansion face, adopting metallic brush to brush out ditch earlier on its surface returns, to increase its surface area, also can adopt chemistry or electrochemical means,, its surface slightly be corroded as adopting hydrochloric acid and sulfuric acid as corrosive liquid, suitably increase the surface, its corrosion multiplying power is defined as 1～10.This is because when Cathode Foil corrosion multiplying power is too high, can cause the impedance of Cathode Foil to increase.
In the magnetron sputtering process, by improving the concentration of nitrogen continuously, from aluminium foil surface, the composition of Titanium descends in gradient with acquisition, and the composition of titanium nitride increases in gradient.Because titanium nitride is at high temperature more stable to air than titanium, thereby further improve the stability of sputtering layer.Thickness of coating is lower than 1 μ m between 1～3 μ m, or is higher than 3 μ m, and the aluminium foil capacity is all not enough.
Behind the aluminium foil surface process magnetron sputtering layer of metal titanium, again 300～500 ℃ of following high-temperature process 20～60 minutes, (it is identical to carry out high temperature carbonization in high-temperature process herein and the air, be in high temperature furnace, to handle) make surface of metal titanium form one deck passivating film, can make capacity stable, and because the iris action of passivating film, can avoid changing into liquid and highly acid electrolyte corrosiveness, thereby improve the stability of final products solid electrolyte capacitor titanium.
Embodiment below by contrast illustrates characteristics of the present invention.
Contrast test one:
(1) Comparative Examples:
At pressure is 7 * 10
-3In the vacuum chamber of Pa, be provided with and put paper tinsel, receive two beaming rollers of paper tinsel, the thick smooth paper tinsel of 50 μ m, through the means of mechanical expansion face, adopt the hard metal brush to brush out ditch and return on its surface, the degree of depth is about 1 μ m, to increase the processing on its surface, can pass through a cylindric drum cooler by continuous reeling.Then with Titanium as the target source, adopt the mode of magnetron sputtering, adding man-hour its evaporation rate is 0.5 μ m/min, continuous evaporating-plating 3 minutes, the thick 1.5 μ m of coating.Recording than electric capacity is 2100 μ F/cm
2, then aluminium foil is placed air, 300 ℃ were heated 1 hour down, and recording its capacity is 520 μ F/cm
2
(2) test example:
Do base material with the thick smooth paper tinsel of 50 μ m, handle by the identical processing mode in early stage of Comparative Examples earlier, and then change into processing, wherein with 15% ammonium adipate solution as changing into liquid, formation voltage is 1.8 volts, the time of changing into is half an hour, changes into 80 ℃ of temperature, does vacuum evaporation then and handles, during evaporation with Titanium as the target source, adopt the mode of magnetron sputtering, adding man-hour its evaporation rate is 0.5 μ m/min, continuous evaporating-plating 3 minutes, the thick 1.5 μ m of coating, and in evaporate process, increase continuously the concentration of nitrogen, make that the composition of titanium nitride increases in gradient in the plated film.Recording than electric capacity is 2000 μ F/cm
2, again aluminium foil is placed air, 300 ℃ were heated 1 hour down, and recording its capacity is 1780 μ F/cm
2
Contrast test two:
(1) Comparative Examples:
Not pass through the thick smooth paper tinsel of 50 μ m that changes into processing, other are identical with embodiment one Comparative Examples, and thickness of coating is 3 μ m.Recording than electric capacity is 1900 μ F/cm
2, aluminium foil places air, and 500 ℃ were heated 30 minutes down, and recording its capacity is 480 μ F/cm
2
(2) test example:
Do base material with the thick smooth paper tinsel of 50 μ m, handle earlier, and then change into processing by the identical processing mode in early stage of Comparative Examples, wherein with ammonium adipate solution as changing into liquid, formation voltage is 2.5v, the time of changing into is 25min, and changing into temperature is 70 ℃, carries out vapor deposition treatment then, adding man-hour its evaporation rate is 1 μ m/min, continuous evaporating-plating 3 minutes, the thick 3 μ m of coating, the method and apparatus of its evaporation is identical with Comparative Examples.Recording than electric capacity is 2000 μ F/cm
2, again aluminium foil is placed air, 500 ℃ were heated 30 minutes down, and recording its capacity is 1850 μ F/cm
2
Contrast test three:
(1) Comparative Examples:
With not through changing into the electrochemical corrosion aluminium foil instead of optical paper tinsel of processing, its corrosion multiplying power is 6, then with Titanium as the target source, adopt the mode of magnetron sputtering, adding man-hour its evaporation rate is 0.5 μ m/min, continuous evaporating-plating 4 minutes, thickness of coating is 2 μ m.Recording than electric capacity is 1200 μ F/cm
2, aluminium foil places air, and 400 ℃ were heated 45 minutes down, and recording its capacity is 490 μ F/cm
2
(2) test example:
With electrochemical corrosion aluminium foil instead of optical paper tinsel, its corrosion multiplying power is 6, change into processing then, wherein with 15% ammonium adipate solution as changing into liquid, formation voltage is 2 volts, the time of changing into is 20 minutes, changes into 60 ℃ of temperature, carries out vacuum evaporation again and handles, during evaporation with Titanium as the target source, adopt the mode of magnetron sputtering, adding man-hour its evaporation rate is 0.5 μ m/min, continuous evaporating-plating 4 minutes, the thick 2 μ m of coating, and in evaporate process, increase continuously the concentration of nitrogen, make that the composition of titanium nitride increases in gradient in the plated film.Recording than electric capacity is 1300 μ F/cm
2, again aluminium foil is placed air, 400 ℃ were heated 45 minutes down, and recording its capacity is 900 μ F/cm
2
Contrast test four:
(1) Comparative Examples:
With not through changing into the electrochemical corrosion aluminium foil instead of optical paper tinsel of processing, its corrosion multiplying power is 2, then with Titanium as the target source, adopt the mode of magnetron sputtering, adding man-hour its evaporation rate is 0.5 μ m/min, continuous evaporating-plating 3 minutes, thickness of coating is 1 μ m.Recording than electric capacity is 1100 μ F/cm
2, aluminium foil places air, and 350 ℃ were heated 20 minutes down, and recording its capacity is 350 μ F/cm
2
(2) test example:
With electrochemical corrosion aluminium foil instead of optical paper tinsel, its corrosion multiplying power is 2, change into processing then, wherein with 15% ammonium adipate solution as changing into liquid, formation voltage is 1 volt, and the time of changing into is 10 minutes, changes into 50 ℃ of temperature, carrying out vacuum evaporation again handles, during evaporation with Titanium as the target source, adopt the mode of magnetron sputtering, adding man-hour its evaporation rate is 0.5 μ m/min, continuous evaporating-plating 3 minutes, the thick 1 μ m of coating, and in evaporate process, increase continuously the concentration of nitrogen, make that the composition of titanium nitride increases in gradient in the plated film, recording than electric capacity is 1150 μ F/cm
2, again aluminium foil is placed air, 350 ℃ were heated 20 minutes down, and recording its capacity is 860 μ F/cm
2
Contrast test five:
(1) Comparative Examples:
With not through changing into the electrochemical corrosion aluminium foil instead of optical paper tinsel of processing, its corrosion multiplying power is 10, then with Titanium as the target source, adopt the mode of magnetron sputtering, adding man-hour its evaporation rate is 0.5 μ m/min, continuous evaporating-plating 3 minutes, thickness of coating is 1.5 μ m.Recording than electric capacity is 1100 μ F/cm
2, aluminium foil places air, and 450 ℃ were heated 50 minutes down, and recording its capacity is 400 μ F/cm
2
(2) test example:
With electrochemical corrosion aluminium foil instead of optical paper tinsel, its corrosion multiplying power is 10, change into processing then, wherein with 15% ammonium adipate solution as changing into liquid, formation voltage is 3 volts, and the time of changing into is 15 minutes, changes into 80 ℃ of temperature, carrying out vacuum evaporation again handles, during evaporation with Titanium as the target source, adopt the mode of magnetron sputtering, adding man-hour its evaporation rate is 0.5 μ m/min, continuous evaporating-plating 3 minutes, the thick 1.5 μ m of coating, and in evaporate process, increase continuously the concentration of nitrogen, make that the composition of titanium nitride increases in gradient in the plated film, recording than electric capacity is 1170 μ F/cm
2, again aluminium foil is placed air, 450 ℃ were heated 50 minutes down, and recording its capacity is 920 μ F/cm
2
By above comparative example as can be known, the base material that changed into through low pressure has better high-temperature stability, and as base material, the light paper tinsel has bigger advantage than etched foil.
Claims (9)
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| CN102360955B (en) * | 2011-09-19 | 2013-05-08 | 常州大学 | Method for improving specific volume of an aluminum electrode foil by electrochemical deposition method |
| DE112016001993T5 (en) | 2015-04-28 | 2018-01-04 | Panasonic Intellectual Property Management Co., Ltd. | ELECTROLYTIC CAPACITOR |
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