CN103658660A - Porous aluminum body, aluminum electrolytic capacitor, and manufacturing method of porous aluminum body - Google Patents
Porous aluminum body, aluminum electrolytic capacitor, and manufacturing method of porous aluminum body Download PDFInfo
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Abstract
The invention provides a porous aluminum body with an anode oxide film with sufficient bending strength, relatively low current leakage and high quality, an aluminum electrolytic capacitor using the porous aluminum body and a manufacturing method of the porous aluminum body. The porous aluminum body (10) comprises an aluminum foil (20) and an aluminum porous layer (30) stacked on at least one surface of the aluminum foil (20). The aluminum foil (20) is 10-50 microns thick, the iron content is less than 1000 weight ppm, and the silicon content is 500-5000 weight ppm. The aluminum porous layer (30) is formed by sintering aluminum powder bodies with the iron content less than 1000 weight ppm and the silicon content being 50-3000 weight ppm.
Description
Technical field
The present invention relates to possess at least one face of aluminium foil aluminium porous layer porous aluminium body, use the manufacture method of aluminium electrolutic capacitor and this porous aluminium body of this porous aluminium body.
Background technology
As the purposes of aluminium foil, the electrode of aluminium electrolutic capacitor has been proposed, by carrier of the catalyst of contaminated atmospheric cleaning etc.After aluminium foil expands surface area by the etching in the etching solutions such as hydrochloric acid, because anodic oxidation is formed with oxide-film on surface.
In patent documentation 1, sintered aluminium powder on aluminium foil has been proposed and lamination has the porous aluminium body of the structure of aluminium porous layer.This porous aluminium body has advantages of the etch processes that does not need to use hydrochloric acid etc.
In patent documentation 2, having proposed by using silicone content is the aluminium powder body formation porous aluminium body of 100～3000 ppm by weight, improves the technology of the bending strength of porous aluminium body.
Patent documentation 1: Japanese kokai publication hei 2-267916 communique
Patent documentation 2: TOHKEMY 2011-52291 communique
Summary of the invention
When manufacture possesses the aluminium electrolutic capacitor of porous aluminium body, there is the operations such as coiling porous aluminium.So, need to make porous aluminium body for the above bending strength of regulation.Yet the technology of only recording with patent documentation 2, can not obtain the Porous aluminium body that possesses the bending strength needing sometimes.In addition, there is the situation that its leakage current value is larger in the porous aluminium body that patent documentation 1,2 is recorded.
Problem of the present invention is to provide a kind of porous aluminium body that can form the second best in quality anode oxide film that has sufficient bending strength and show lower leakage current value, uses the manufacture method of aluminium electrolutic capacitor and this porous aluminium body of this porous aluminium body.
In order to solve above-mentioned problem, the invention provides a kind of porous aluminium body, it has aluminium foil and is stacked in the aluminium porous layer at least one face of this aluminium foil, above-mentioned porous aluminium body is characterised in that: the thickness of above-mentioned aluminium foil is that 10～50 μ m, iron content less than 1000 ppm by weight and silicone content are 500～5000 ppm by weight, above-mentioned aluminium porous layer is the layer that aluminium powder sintering is formed, and iron content less than 1000 ppm by weight and the silicone content of above-mentioned aluminium powder body are 50～3000 ppm by weight.
In addition, the manufacture method of porous aluminium body of the present invention, it is characterized in that, comprise: the first operation, at thickness, be that 10～50 μ m, iron content less than 1000 ppm by weight and silicone content are to form the film consist of the constituent that comprises aluminium powder body at least one side of aluminium foil of 500～5000 ppm by weight, wherein, iron content less than 1000 ppm by weight of above-mentioned aluminium powder body and silicone content are 50～3000 ppm by weight; The second operation, by above-mentioned film sintering at the more than 560 ℃ temperature below 660 ℃, forms aluminium porous layer.
Porous aluminium body of the present invention is used specific aluminium foil and the aluminium powder body forming, so leakage current value is lower, the agglutinating property between aluminium foil and aluminium powder body improves, and bending strength is higher.
That is iron content less than 1000 ppm by weight of the aluminium powder body that, the iron content of aluminium foil and aluminium porous layer are used.When aluminium porous layer is carried out to anodic oxidation, can form the second best in quality anode oxide film that shows lower leakage current value.
In addition, the silicone content of aluminium foil is 500～5000 ppm by weight, and the silicone content of the aluminium powder body that aluminium porous layer is used is 50～3000 ppm by weight.When to silicone content when the aluminium foil of above-mentioned scope and aluminium powder body carry out sintering, can obtain the higher bond strength (sintering strength) of aluminium foil and aluminium porous layer (aluminium powder body).Thus, porous aluminium body possesses higher bending strength.
On the other hand, the thickness of aluminium foil is 10～50 μ m, so can obtain the porous aluminium body of suitable intensity.Even if the thickness of aluminium foil surpasses 50 μ m, surface area and intensity can not improve yet, and thickness increases redundantly.When the thickness less than 10 μ m of aluminium foil, the intensity of porous aluminium body is lower.
In the present invention, the average grain diameter of preferred above-mentioned aluminium powder body is 1～10 μ m.Thus, can effectively expand the surface area of porous aluminium body.When the average grain diameter less than 1 μ m of aluminium powder body, the gap between aluminium powder body is narrow, and the invalid part not playing a role as electrode etc. increases.When the average grain diameter of aluminium powder body surpasses 10 μ m, the gap between aluminium powder body is wide, and the expansion of surface area is insufficient.
In the present invention, also can form above-mentioned aluminium porous layer at two faces of above-mentioned aluminium foil.
In the present invention, also can form anode oxide film at above-mentioned aluminium porous layer.This porous aluminium body is used as the anode of aluminium electrolutic capacitor etc.In this situation, after above-mentioned the second operation, comprise above-mentioned aluminium porous layer is carried out to anodised the 3rd operation.
Porous aluminium body of the present invention possesses: iron content less than 1000 ppm by weight and silicone content are the aluminium foil of 500～5000 ppm by weight; With iron content less than 1000 ppm by weight and silicone content be the aluminium porous layer of 50～3000 ppm by weight.Therefore, can form the second best in quality anode oxide film that can obtain higher bending strength and show lower leakage current value.In addition,, because the thickness of aluminium foil is 10～50 μ m, can obtain suitable intensity.
Accompanying drawing explanation
Fig. 1 means the key diagram of the cross section structure of having applied porous aluminium body of the present invention.
Fig. 2 means the key diagram of the surface texture of having applied porous aluminium body of the present invention.
Description of reference numerals
10 ... porous aluminium body
20 ... aluminium foil
30 ... aluminium porous layer
The specific embodiment
(structure of porous aluminium body)
Fig. 1 means the key diagram of the cross section structure of having applied porous aluminium body of the present invention, is to utilize electron microscope the cross section of porous aluminium body to be amplified to the photo of 600 times of shootings.Fig. 2 means the key diagram of the surface texture of having applied porous aluminium body of the present invention, is the photo that utilizes electron microscope to take the surface of porous aluminium body.Wherein, in Fig. 2, represented the surface of porous aluminium body amplify the photo of 1000 times and amplify the photo of 3000 times.
The thickness of aluminium foil 20 can be 10～50 μ m, in Fig. 1, represents that used thickness is the porous aluminium body 10 of the aluminium foil 20 of approximately 30 μ m.In addition,, in Fig. 1, represent to be formed with the porous aluminium body 10 that thickness is the aluminium porous layer 30 of approximately 50 μ m.
Herein, iron content less than 1000 ppm by weight of aluminium foil 20 and silicone content are 500～5000 ppm by weight.This is that bending strength reduces because during silicone content less than 500 ppm by weight of aluminium foil 20, and while surpassing 5000 ppm by weight, leakage current value raises.And then, when the silicone content of aluminium foil 20 is 500～3000 ppm by weight, can obtain higher electrostatic capacitance, so further preferred.
In addition, aluminium porous layer 30 is layers that the aluminium powder sintering that is 50～3000 ppm by weight by iron content less than 1000 ppm by weight and silicone content forms.Aluminium powder body is sintering when mutually maintaining space.This is that bending strength reduces because during silicone content less than 50 ppm by weight of aluminium porous layer 30, and while surpassing 3000 ppm by weight, leakage current value raises.And then, when the silicone content of aluminium porous layer 30 is 50～1000 ppm by weight, can obtain higher electrostatic capacitance, so further preferred.
The shape of aluminium powder body without particular limitation of, roughly spherical, indefinite shape, flakey, fibrous etc. all can suitably use.Particularly in order to maintain the space between aluminium powder body, preferably by powder that roughly spherical particle forms.Preferably the average grain diameter of aluminium powder body is 1～10 μ m.
This porous aluminium body 10, can obtain or its above electrostatic capacitance equal with existing etched foil.Particularly, the porous aluminium body 10 of present embodiment, can replace the etched foil with thicker erosion trace of the capacitor that mesohigh uses to use.
In situation by porous aluminium body 10 as the anode of aluminium electrolutic capacitor, on aluminium porous layer 30, form anode oxide film.At this moment, on aluminium foil 20, have the situation of the part of exposing from aluminium porous layer 30, on aluminium foil 20, also form anode oxide film.
(manufacture method)
The manufacture method of having applied porous aluminium body 10 of the present invention is, first, in the first operation, at thickness, be that 10～50 μ m, iron content less than 1000 ppm by weight and silicone content are at least one side of aluminium foil 20 of 500～5000 ppm by weight, to form the film that the constituent by the aluminium powder body comprising forms, wherein iron content less than 1000 ppm by weight of above-mentioned aluminium powder body and silicone content are 50～3000 ppm by weight.Preferably the average grain diameter of aluminium powder body is 1～10 μ m.Aluminium foil 20 and aluminium powder body also can contain one or more in the elements such as copper (Cu), manganese (Mn), magnesium (Mg), chromium (Cr), zinc (Zn), titanium (Ti), vanadium (V), gallium (Ga), nickel (Ni), boron (B), zirconium (Zr).In this situation, preferably the amount of these elements is respectively below 100 ppm by weight, particularly below 50 ppm by weight.
Aluminium powder body is by atomization, melt rotation method, rotating disk method, rotary electrode method, other the manufactures such as emergency cooling solidification method.In these methods, industrial production preferred atomization, particularly gas atomization.In atomization, by making motlten metal atomization obtain powder.
Above-mentioned constituent also can comprise resin binder, solvent, sintering aid, surfactant etc. as required.These all can use known or commercially available.Preferably contain at least one in resin binder or solvent and use as paste constituent.Thus, can form efficiently epithelium.As resin binder, can suitably use the natural resins such as synthetic resin such as carboxy-modified vistanex, vinyl acetate resin, vinyl chloride resin, vinyl chloride-vinyl acetate copolymer resin, vinyl alcohol resin, butyral resin, fluoroethylene resin, acrylic resin, mylar, polyurethane resin, epoxy resin, urea resin, phenolic resins, acrylonitrile resin, nitrocellulose resin, paraffin, Tissuemat E or wax, tar, glue, paint, rosin, beeswax, or wax.These adhesives have separately because of the kind of molecular weight, resin etc. when the heating volatilization and together residual because of its residue of pyrolysis and aluminium powder, can require to distinguish use according to static characteristic etc.
While modulating above-mentioned constituent, also can add solvent.As solvent, can be used alone or as a mixture water, ethanol, toluene, ketone, ester class etc.
In addition, the formation of above-mentioned epithelium, can suitably select known method according to the character of constituent and state etc.For example, in the situation that constituent is powder (solid), on base material, form (or thermo-compressed) its pressed compact.In this situation, can make pressed compact pass through sintering curing, and aluminium powder is fixed on aluminium foil 20.In addition, be in the situation of aqueous (paste), the enough roller coat of energy, brushing, spraying, impregnating coating method form epithelium, in addition, also can enough known printing processes form epithelium.In addition, can as required, make at the temperature of film in the more than 20 ℃ scope below 300 ℃ dry.
The thickness of film without particular limitation of, be generally below the above 1000 μ m of 20 μ m, be particularly preferably below the above 200 μ m of 20 μ m.The in the situation that of thickness less than 20 μ m, sometimes can not obtain the electrostatic capacitance of requirement.In addition,, in the situation that thickness is greater than 1000 μ m, sometimes there is adaptation with paper tinsel bad or chap in rear operation.
In addition,, for aluminium foil 20, also can, before forming epithelium, make the operation of the surface roughening of aluminium foil 20.The method of this roughening can be used known technology such as cleaning, etching, sandblast.
Then, in the second operation, by film sintering at the more than 560 ℃ temperature below 660 ℃.Sintering time is according to differences such as sintering temperatures, but conventionally can in 5～24 hours extent and scopes, suitably determine.Sintering atmosphere especially restriction, can be such as vacuum atmosphere, inertness gas atmosphere, oxidizing gas atmosphere (atmosphere), reducing atmosphere etc. any.Be particularly preferably vacuum atmosphere or reducing atmosphere.In addition about pressure conditions, can be also any in normal pressure, decompression or pressurization.Wherein, in the situation that in constituent, (in epithelium) contains the organic principles such as resin binder, preferably after the first operation, before the second operation, more than 100 ℃ to carrying out the retention time in the temperature range below 600 ℃, be more than 5 hours heat treated (ungrease treatment) in advance.Heat treated atmosphere now without particular limitation of, can be any in vacuum atmosphere, inertness gas atmosphere or oxidizing gas atmosphere for example.In addition, pressure conditions can be also any in normal pressure, decompression or pressurization.
In addition,, in the situation by porous aluminium body 10 as the anode of aluminium electrolutic capacitor, in the 3rd operation after the first operation and the second operation, on aluminium porous layer 30, form anode oxide film.Now, on aluminium foil 20, in the part of exposing from aluminium porous layer 30, also form anode oxide film.
In order to use this anodised porous aluminium body 10 manufacture aluminium electrolutic capacitors, first, make to reel and form capacitor element across dividing plate by anode foils and Cathode Foil that anodised porous aluminium body 10 forms.Then, capacitor element is impregnated in electrolyte.Afterwards, the capacitor element that comprises electrolyte is accommodated in shell, utilizes seal body that shell is sealed.
(the main effect of present embodiment)
As mentioned above, in the present embodiment, the silicone content of aluminium foil 20 is 500～5000 ppm by weight, and the silicone content of the aluminium powder body that aluminium porous layer 30 is used is 50～3000 ppm by weight.Therefore, when sintering, can obtain aluminium foil 20 and aluminium porous layer 30(aluminium powder body) higher bond strength (sintering strength), porous aluminium body 10 possesses higher bending strength.Therefore, when manufacturing porous aluminium body 10, when porous aluminium body 10 is carried out to anodic oxidation and use when anodised porous aluminium body 10 has been manufactured aluminium electrolutic capacitor, can suppress the bad generations such as porous aluminium body 10 bendings.
In addition, because iron content less than 1000 ppm by weight of the aluminium powder body that the iron content of aluminium foil 20 and aluminium porous layer 30 are used, so when aluminium porous layer 30 has been carried out to anodic oxidation, can form the second best in quality anode oxide film.That is, iron content is 1000 ppm by weight when above, take that to residue in compound between the thick Al-Fe metalloid in anode oxide film be starting point, and leakage current increases, but when iron content less than 1000 ppm by weight, the increase of this leakage current value does not occur.
And then, because the thickness of aluminium foil 20 is 10～50 μ m, can obtain suitable intensity.Even if the thickness of aluminium foil 20 surpasses 50 μ m, surface area and intensity can not improve yet, so as aluminium foil 20 thickening redundantly.In addition,, when the thickness less than 10 μ m of aluminium foil 20, the intensity of porous aluminium body 10 is lower.
In addition, because the average grain diameter of aluminium powder body is 1～10 μ m, so enlarged surface is long-pending effectively.During the average grain diameter less than 1 μ m of aluminium powder body, the gap between aluminium powder body is narrow, and the invalid part not playing a role as electrode etc. increases.When the average grain diameter of aluminium powder body surpasses 10 μ m, the gap between aluminium powder body is wide, and the expansion of surface area is insufficient.That is, by anodic oxidation, form film withstand voltage while be more than 200V anode oxide film, space is buried, electrostatic capacitance reduction.On the other hand, when average grain diameter surpasses 10 μ m, it is excessive that space part becomes, and surface area reduces, and can not obtain the electrostatic capacitance of requirement.Wherein, the average grain diameter of aluminium powder body can be measured by enough laser diffraction formula particles distribution instruments.
(embodiment)
Then, embodiments of the invention are described.First, on two faces of the aluminium foil of thickness 30 μ m, width 500mm, form the different aluminium powder bodies such as average grain diameter, keeping space and with the aluminium porous layer of every part of thickness 40 μ m sintering, manufacturing porous aluminium body.More specifically, by aluminium powder body 60 weight portions and cellulose family adhesive 40 weight portion (solvents: toluene, 7 % by weight are resin parts) mix, obtain after the constituent of solid composition 60 % by weight, use unfilled corner wheel coating machine (Comma Coater) this composition to be coated to two faces of aluminium foil (JIS1N30-H18), form film (the first operation).
Then, after making film dry, by by aluminium foil in argon gas atmosphere 635 ℃ of sintering of temperature 7 hours, manufacture porous aluminium body (the second operation).The thickness of the porous aluminium body after sintering is approximately 130 μ m(aluminium foils: 30 μ m+ aluminium porous layers 30: each face 50 μ m).
Then, in boric acid class forming liquid, porous aluminium body is carried out to anodized (the 3rd operation).
In addition, the appropriate extraction property of porous aluminium body from anodic oxidation is measured the sampling of use, measures bending strength.Bending strength is carried out according to the automatic beam test method of MIT type (EIAJ RC-2364A) of EIAJ's regulation.
The automatic beam test device of MIT type is used the device of being stipulated by JIS P8115, bending number of times is the bending number of times of each electrode material fracture, by 90-degree bent be 1 time, to restore to the original state be 2 times, 90-degree bent is 3 times round about, to restore to the original state be to count for 4 times.And, the not enough stipulated number of the measurement result of bending strength be considered as bending strength " defective ", from anodised object, get rid of, for the measurement result of bending strength, be more than stipulated number, be considered as bending strength " good ", as anodised object.
In addition,, for the porous aluminium body after anodic oxidation, according to JEITA specification, carried out the withstand voltage mensuration of electrostatic capacitance and film.Wherein, the film of sampling is withstand voltage is before and after 410V.In addition, in the boric acid class solution with synthetic liquid the same terms, apply the withstand voltage voltage of 0.9 times of film, measure current value after 10 minutes as leakage current value.In table 1, represent its result.Wherein, in table 1, " Al powder " represents aluminium powder body, and " particle diameter " represents average grain diameter." Fe amount " represents iron content (ppm by weight), and " Si amount " represents silicone content (ppm by weight).
[table 1]
As known from Table 1, the bending strength of the comparative example 5 of the comparative example 1 of silicone content less than 500 ppm by weight of aluminium foil and silicone content less than 50 ppm by weight of aluminium powder body is lower.In addition, the silicone content of aluminium foil surpasses the comparative example 2 of 5000 ppm by weight, the iron content of aluminium powder body surpasses the comparative example 3 of 1000 ppm by weight and the iron content of aluminium foil is significantly higher over the leakage current value of the comparative example 4 of 1000 ppm by weight.
On the other hand, using iron content less than 1000 ppm by weight and silicone content is that the aluminium foil of 500～5000 ppm by weight and iron content less than 1000 ppm by weight and silicone content are that the bending strength of embodiment 1～7 of aluminium powder body of 50～3000 ppm by weight is all large and leakage current value is all lower.
Wherein, among embodiment 1～7, the embodiment 6 that the embodiment 5 of average grain diameter less than 1 μ m of aluminium powder body and the average grain diameter of aluminium powder body surpass 10 μ m compares with embodiment 1～4, and electrostatic capacitance is lower, so preferably the average grain diameter of aluminium powder body is 1～10 μ m.
In addition, among embodiment 1～7, the silicone content of aluminium powder body is that the silicone content of 1500 ppm by weight and aluminium foil is the embodiment 7 of 3500 ppm by weight, to compare electrostatic capacitance also lower with embodiment 1～4, so preferably the silicone content of aluminium powder body is 50～1000 ppm by weight, preferably the silicone content of aluminium foil is 500～3000 ppm by weight.
(other embodiment)
In the above-described embodiment, so that porous aluminium body is illustrated as centered by the anode of aluminium electrolutic capacitor.About porous aluminium body or be formed with the porous aluminium body of anode oxide film, can be used as catalyst carrier.For example, in situation for the resolution process of deodorizing or VOC, vehicle exhaust etc., porous aluminium body, as carried catalyst, carries palladium, platinum, ruthenium, rhodium, iridium, nickel, cobalt, iron, copper, zinc, gold, silver, rhenium, manganese, tin, their alloy or mixture.
Claims (9)
1. a porous aluminium body, it has aluminium foil and is stacked in the aluminium porous layer at least one face of this aluminium foil, and described porous aluminium body is characterised in that:
The thickness of described aluminium foil is that 10～50 μ m, iron content less than 1000 ppm by weight and silicone content are 500～5000 ppm by weight,
Described aluminium porous layer is the layer that aluminium powder sintering is formed,
Iron content less than 1000 ppm by weight and the silicone content of described aluminium powder body are 50～3000 ppm by weight.
2. porous aluminium body as claimed in claim 1, is characterized in that:
The average grain diameter of described aluminium powder body is 1～10 μ m.
3. porous aluminium body as claimed in claim 1, is characterized in that:
Described aluminium porous layer is stacked on two faces of described aluminium foil.
4. porous aluminium body as claimed in claim 1, is characterized in that:
The average grain diameter of described aluminium powder body is 1～10 μ m,
Described aluminium porous layer is stacked on two faces of described aluminium foil.
5. the porous aluminium body as described in any one in claim 1～4, is characterized in that:
On described aluminium porous layer, be formed with anode oxide film.
6. an aluminium electrolutic capacitor, is characterized in that:
There is in claim 1～5 the porous aluminium body described in any one as anode.
7. a manufacture method for porous aluminium body, is characterized in that, comprising:
The first operation, at thickness, be that 10～50 μ m, iron content less than 1000 ppm by weight and silicone content are to form the film consisting of the constituent that comprises aluminium powder body at least one faces of aluminium foil of 500～5000 ppm by weight, wherein, iron content less than 1000 ppm by weight of above-mentioned aluminium powder body and silicone content are 50～3000 ppm by weight; With
The second operation, by described film sintering at the more than 560 ℃ temperature below 660 ℃, forms aluminium porous layer.
8. the manufacture method of porous aluminium body as claimed in claim 7, is characterized in that:
The average grain diameter of described aluminium powder body is 1～10 μ m.
9. the manufacture method of porous aluminium body as claimed in claim 7 or 8, is characterized in that:
After being included in described the second operation, described aluminium porous layer is carried out to anodised the 3rd operation.
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| JP2012211476A JP6001977B2 (en) | 2012-09-25 | 2012-09-25 | Porous aluminum body, aluminum electrolytic capacitor, and method for producing porous aluminum body |
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| CN110648849A (en) * | 2019-09-26 | 2020-01-03 | 宇启材料科技南通有限公司 | Valve metal porous body coating electrode foil, manufacturing method and electrolytic capacitor |
| CN110648849B (en) * | 2019-09-26 | 2021-12-14 | 宇启材料科技南通有限公司 | Valve metal porous body coating electrode foil, manufacturing method and electrolytic capacitor |
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| CN111804920A (en) * | 2020-07-01 | 2020-10-23 | 益阳艾华富贤电子有限公司 | Preparation method of anode foil of aluminum electrolytic capacitor based on laser sintering |
| CN112053849A (en) * | 2020-07-23 | 2020-12-08 | 新疆众和股份有限公司 | Preparation method of electrode foil |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103658660B (en) | 2017-08-15 |
| JP2014065940A (en) | 2014-04-17 |
| JP6001977B2 (en) | 2016-10-05 |
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