JPH0738368B2 - Method for manufacturing aluminum electrode material for electrolytic capacitor - Google Patents
Method for manufacturing aluminum electrode material for electrolytic capacitorInfo
- Publication number
- JPH0738368B2 JPH0738368B2 JP9058287A JP9058287A JPH0738368B2 JP H0738368 B2 JPH0738368 B2 JP H0738368B2 JP 9058287 A JP9058287 A JP 9058287A JP 9058287 A JP9058287 A JP 9058287A JP H0738368 B2 JPH0738368 B2 JP H0738368B2
- Authority
- JP
- Japan
- Prior art keywords
- titanium
- aluminum foil
- vapor deposition
- electrode material
- film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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Description
【発明の詳細な説明】 産業上の利用分野 この発明は電解コンデンサ用アルミニウム電極材料の製
造方法に関する。TECHNICAL FIELD The present invention relates to a method for producing an aluminum electrode material for an electrolytic capacitor.
なおこの明細書において、アルミニウムの語はアルミニ
ウム合金を含む意味において用いる。In this specification, the term aluminum is used to include an aluminum alloy.
従来の技術 電解コンデンサの小型、高静電容量を達成するために
は、アルミニウム電極材料の静電容量を高める必要があ
る。そして電極材料の静電容量を増加させるには、電極
材の表面積を大きくする、高誘電率の皮膜を形成する、
誘電体の皮膜厚さを薄くする、などが必要である。2. Description of the Related Art In order to achieve small size and high capacitance of electrolytic capacitors, it is necessary to increase the capacitance of aluminum electrode material. And to increase the capacitance of the electrode material, increase the surface area of the electrode material, form a film of high dielectric constant,
It is necessary to reduce the thickness of the dielectric film.
そこでこれらを達成して静電容量を増大しうる電極材料
として、本出願人は先に、粗面化したアルミニウム箔の
表面に、蒸着法による所定膜厚のチタン皮膜を形成した
電極材料を提案した（特開昭61-180420号、特開昭61-21
4420号）。かかる電極材料によれば、アルミニウム箔表
面の凹凸効果がチタン皮膜に波及するとともに、これに
チタン皮膜自体の凹凸効果が相俟って皮膜表面を粗な状
態となしうる結果、チタン皮膜を形成しないアルミニウ
ム箔に較べて拡面率を向上しえ、ひいては静電容量の増
大化が可能となった。Therefore, as an electrode material capable of achieving these and increasing the electrostatic capacitance, the present applicant has previously proposed an electrode material in which a titanium film having a predetermined thickness is formed by a vapor deposition method on the surface of a roughened aluminum foil. (JP-A 61-180420, JP-A 61-21
No. 4420). According to such an electrode material, the unevenness effect on the surface of the aluminum foil spreads to the titanium film, and the unevenness effect of the titanium film itself can be combined with this to make the film surface rough, so that the titanium film is not formed. Compared with aluminum foil, the area expansion ratio can be improved, and the capacitance can be increased.
ところで、上記のように、アルミニウム箔にチタン蒸着
皮膜を形成する場合、アルミニウム箔をコイルに形成し
て、真空ベルジャー内で該コイルを巻き取りながら蒸着
処理を行う方法が、量産性が高いこと等の理由から採用
されている。By the way, as described above, when the titanium vapor deposition film is formed on the aluminum foil, the method of forming the aluminum foil on the coil and performing the vapor deposition treatment while winding the coil in the vacuum bell jar has high mass productivity, etc. It has been adopted for the reason.
而して、従来、かかる蒸着処理操作にあっては、皮膜と
アルミニウム箔との密着性の向上、処理の迅速性等の観
点から、所定膜厚、例えば１μｍ前後の膜厚のチタン皮
膜を一回の蒸着処理で一度に形成していたため、次のよ
うな欠点があった。Thus, conventionally, in such a vapor deposition treatment operation, a titanium film having a predetermined film thickness, for example, a film thickness of about 1 μm, is used in order to improve the adhesion between the film and the aluminum foil, the speed of the treatment, and the like. Since it was formed at one time by vapor deposition processing once, it had the following drawbacks.
発明が解決しようとする問題点 即ち、１μｍ前後のチタン皮膜を一度に形成する場合、
蒸着粒子の凝縮潜熱、蒸発源からの輻射熱によりアルミ
ニウム箔の温度は上昇する。もっとも、チタン皮膜形成
中は冷却ドラムでアルミニウム箔を冷却してはいるもの
の、それでもなお、通常200℃以上の達するもとなる。
かかるアルミニウム箔温度の上昇により、蒸着皮膜はチ
タン粒子が融合したような状態となり易く、こうなると
皮膜表面が平滑化してその凹凸効果が失われる効果、所
期する静電容量を得ることができないというような欠点
があることが判明した。Problems to be Solved by the Invention That is, when a titanium film of about 1 μm is formed at one time,
The temperature of the aluminum foil rises due to latent heat of condensation of vapor deposition particles and radiant heat from an evaporation source. However, while the aluminum foil is being cooled by the cooling drum during the titanium film formation, it is still usually 200 ° C or higher.
Due to the increase in the temperature of the aluminum foil, the vapor deposition film is likely to be in a state in which titanium particles are fused, and in this case, the effect that the film surface is smoothed and the unevenness effect is lost, and the desired capacitance cannot be obtained. It turned out that there are such drawbacks.
この発明は、かかる事情のもとになされたものであっ
て、チタン皮膜表面を凹凸状となしえて拡面率の高い即
ち静電容量の大きな電解コンデンサを確実に提供するこ
とを目的とするものである。The present invention has been made under such circumstances, and an object of the present invention is to reliably provide an electrolytic capacitor having a high surface area ratio, that is, a large electrostatic capacity, by making the surface of the titanium film uneven. Is.
問題点を解決するための手段 上記目的において、この発明は、粒子の融合状態による
チタン表面の平滑化が、前述のように、蒸着処理中にお
けるアルミニウム箔の温度上昇に起因していることに鑑
み、アルミニウム箔の温度上昇を来たすことなく所定膜
厚のチタン皮膜を被覆形成せんとするものであり、この
ために、一回の蒸着処理によって一気に所定膜厚を達成
するのではなく、アルミニウム箔の温度上昇にさほど影
響を与えない程度の少量の蒸着処理を間欠的に繰り返す
ことによって、チタン薄膜層を順次的に堆積せしめ、も
って所期する膜厚のチタン皮膜を形成せんとするもので
ある。Means for Solving the Problems In the above object, the present invention is based on the fact that the smoothing of the titanium surface due to the fused state of the particles is caused by the temperature rise of the aluminum foil during the vapor deposition process as described above. In order to form a titanium film having a predetermined film thickness without causing the temperature of the aluminum foil to rise, for this reason, it is not possible to achieve the predetermined film thickness at once by a single vapor deposition process. By intermittently repeating a small amount of vapor deposition treatment that does not significantly affect the temperature rise, titanium thin film layers are sequentially deposited to form a titanium film having a desired thickness.
即ちこの発明は、粗面化されたアルミニウム箔の表面
に、チタン蒸着処理の少量実施を間欠的に繰り返すこと
によってチタン薄膜層を順次的に堆積せしめ、もって所
定膜厚のチタン皮膜を形成することを特徴とする電解コ
ンデンサ用アルミニウム電極材料の製造方法を要旨とす
るものである。That is, according to the present invention, a titanium thin film layer is sequentially deposited on a surface of a roughened aluminum foil by intermittently repeating a small amount of titanium vapor deposition treatment to form a titanium film having a predetermined thickness. The gist is a method for producing an aluminum electrode material for an electrolytic capacitor, which is characterized in that.
上記アルミニウム箔の組成は特に限定されるものではな
く、電解コンデンサ用として用いられるものであれば良
い。The composition of the aluminum foil is not particularly limited as long as it is used for an electrolytic capacitor.
アルミニウム箔の粗面化は、その凹凸効果をチタン皮膜
表面に波及せしめて、チタン皮膜表面の拡面率向上を助
長するために施されるものである。この粗面化は、一般
的には、電気化学的あるいは化学的な湿式エッチングに
より行われるが、機械加工により行うものとしても良
い。粗面化の状態や程度は特に限定されないが、好まし
い粗面化状態として、第１図に示すように、アルミニウ
ム箔（１）の表面を海綿状組織層（２）に形成した場合
を挙げうる。この海綿状組織層（２）とは、同図に示す
ように、三次元方向においては連続気泡状態に複雑に連
通した空隙部（2a）を有する組織層をいう。The roughening of the aluminum foil is carried out in order to spread the unevenness effect on the surface of the titanium film and promote the improvement of the surface expansion rate of the surface of the titanium film. This roughening is generally performed by electrochemical or chemical wet etching, but it may be performed by machining. The state and degree of roughening are not particularly limited, but a preferable roughening state may be a case where the surface of the aluminum foil (1) is formed into a spongy tissue layer (2) as shown in FIG. . The spongy tissue layer (2) refers to a tissue layer having voids (2a) that are intricately connected to each other in an open-cell state in the three-dimensional direction, as shown in FIG.
アルミニウム箔表面へのチタン皮膜の形成は、この発明
では次のようにして行う。即ち、まずチタン蒸着処理を
少量実施することにより、第２図に示すように、アルミ
ニウム箔（１）表面へ最下層のチタン薄膜層（3a）を被
覆形成する。この蒸着処理は少量実施であるから、該処
理によってアルミニウム箔が大幅な温度上昇を来たす虞
れはない。その後アルミニウム箔の冷却時間をおいたの
ち、前記と同様に蒸着処理の少量実施を行って次層のチ
タン薄膜層（3b）を堆積状態に形成する。以後同様の蒸
着処理を行い、チタン薄膜層（3c）（3d）…を順次的に
堆積せしめ、もって所期する膜厚のチタン皮膜（３）を
形成する。このように、蒸着処理の少量実施を間欠的に
繰り返してチタン薄膜層を順次的に堆積せしめることに
より、アルミニウム箔の温度上昇を来たす虞れはなくな
り、低温度に保持した状態のままチタン皮膜（３）を形
成することができる。その結果、チタン粒子の融合によ
りチタン皮膜表面が平滑化する不都合がなくなる。In the present invention, the titanium film is formed on the surface of the aluminum foil as follows. That is, first, by performing a small amount of titanium vapor deposition treatment, as shown in FIG. 2, the lowermost titanium thin film layer (3a) is coated on the surface of the aluminum foil (1). Since this vapor deposition process is carried out in a small amount, there is no possibility that the temperature of the aluminum foil will rise significantly due to the process. Then, after cooling the aluminum foil, a small amount of vapor deposition is carried out in the same manner as described above to form a titanium thin film layer (3b) as a next layer in a deposited state. Thereafter, the same vapor deposition process is performed to sequentially deposit the titanium thin film layers (3c) (3d) ..., thereby forming the titanium film (3) having a desired film thickness. As described above, by intermittently repeating a small amount of the vapor deposition process to sequentially deposit the titanium thin film layers, there is no fear that the temperature of the aluminum foil will rise, and the titanium film ( 3) can be formed. As a result, the inconvenience of smoothing the surface of the titanium coating due to the fusion of the titanium particles is eliminated.
かかるチタン蒸着処理の少量実施を間欠的に行わしめる
ための具体的処理方法の好ましい例として、連続的巻き
取り蒸着法を挙げうる。即ちこの方法は、第３図に示す
ように、図示しない真空ベツジャー内において、コイル
（８）に巻かれた粗面化アルミニウム箔（１）を、回転
する冷却ロール（４）の下部周面に沿わせて搬送しつつ
巻き取りコイル（９）に巻き取る一方で、冷却ロール
（４）の下方に電子ビーム蒸発源（５）を配設し、冷却
ロール（４）の周面に沿って移動中のアルミニウム箔
（１）に前記蒸発源（５）からチタンを蒸着せしめて付
着させ、まずアルミニウム箔（１）の長さ方向全域に最
下層のチタン薄膜層（3a）を連続的に形成する。こうし
て巻き取りコイル（９）に巻き取ったのち、今度は元の
コイル（８）にアルミニウム箔を巻き戻しながら、次層
のチタン薄膜層（3b）を同じくアルミニウム箔の長さ方
向全域に連続的に形成する。そしてその後所期する膜厚
に達するまでコイルの巻き取りと巻き戻しを繰り返して
同様の蒸着処理を行い、チタン薄膜層を順次的に堆積せ
しめるものである。なお、第３図において、（６）はガ
イドロール、（７）はアルミニウム箔（１）への蒸着範
囲を規制する規制板である。このような方法の採用によ
って、例えばコイルの巻き取り、巻き戻し速度を変える
ことなどでチタン薄膜層の形成条件の設定が容易となる
とともに、効率良く蒸着処理を行うことができる。また
この方法によれば、冷却ロール（４）に沿ってアルミニ
ウム箔が移動することから、該箔の位置によって蒸発源
（５）からのチタン粒子の該箔に対する入射角が変化す
ることとなる。この入射角の変化が効果的にチタン皮膜
表面をより粗な状態とし、容量増加に対して好ましい影
響を与えうるという効果もある。As a preferable example of a specific treatment method for intermittently performing such a small amount of titanium vapor deposition treatment, a continuous winding vapor deposition method can be cited. That is, as shown in FIG. 3, in this method, a roughened aluminum foil (1) wound around a coil (8) is applied to the lower peripheral surface of a rotating cooling roll (4) in a vacuum betger (not shown). The electron beam evaporation source (5) is arranged below the cooling roll (4) while being wound along the winding coil (9) while being conveyed along, and moved along the peripheral surface of the cooling roll (4). Titanium is vapor-deposited from the evaporation source (5) and attached to the aluminum foil (1) therein, and first, the titanium thin film layer (3a) as the lowermost layer is continuously formed over the entire length of the aluminum foil (1). . After being wound on the winding coil (9) in this way, this time the aluminum foil is rewound on the original coil (8), and the titanium thin film layer (3b) of the next layer is continuously spread over the entire length of the aluminum foil. To form. Then, winding and unwinding of the coil are repeated until the desired film thickness is reached, and the same vapor deposition process is performed to sequentially deposit the titanium thin film layers. In FIG. 3, (6) is a guide roll, and (7) is a regulating plate for regulating the vapor deposition range on the aluminum foil (1). By adopting such a method, it becomes easy to set the conditions for forming the titanium thin film layer by changing, for example, the winding and rewinding speed of the coil, and the vapor deposition process can be performed efficiently. Further, according to this method, since the aluminum foil moves along the cooling roll (4), the incident angle of the titanium particles from the evaporation source (5) to the foil changes depending on the position of the foil. This change in the incident angle also effectively brings the surface of the titanium film into a rougher state, and has a positive effect on the increase in capacity.
ここで、前記チタン皮膜（３）の最終膜厚は0.1〜３μ
ｍ（皮膜量換算0.045〜1.35mg/cm2）に設定するのが望
ましい。0.1μｍ未満では、皮膜表面が平滑なものとな
ってしまい、ひいては静電容量が小さいものとなってし
まう虞れがあるからであり、逆に３μｍを超えても使用
チタン材料の増大、コスト上昇にみあうだけの効果が得
られない虞れがあるからである。また、蒸着処理の間欠
的実施回数、還元すればチタン薄膜層の層数は２〜10の
範囲とするのが良い。10回を超えて蒸着処理を繰り返し
ても、効果が飽和するのみならず、却って生産性が悪化
し処理コストが高くつくからである。蒸着速度は、所期
するチタン皮膜厚さと蒸着処理回数との関係を考慮して
適宜決定されるべきものであるが、望ましくは、100〜5
000Å/sec（付着量換算4.5×10-3〜0.225mg/cm2sec）に
設定するのが良い。5000Å/secを超える蒸着速度では雰
囲気圧の影響がなくなり、静電容量が低下するなどの欠
点を派生する虞れがあるからであり、逆に100Å/sec未
満の蒸着速度では生産性が悪く処理コストが高くつくか
らである。また蒸着処理雰囲気はAr等の不活性ガス雰囲
気とするのが、チタン皮膜表面をより粗面化できること
から好ましい。雰囲気圧は５×10-5〜５×10-3Torrとす
るのが良い。５×10-5Torr未満では皮膜の微細粗面化効
果が減少して静電容量の小さいものとなる虞れがあるか
らであり、逆に５×10-3Torrを超える圧力に設定する
と、チタンが蒸発しにくくなるうえ、アルミニウム箔と
の密着性が悪くなる虞れがあるからである。量産性を考
えた場合、好適には１×10-3Torr程度の圧力に設定する
のが良い。蒸発距離は150〜400mmとするのが良い。400m
mを超えるとチタンの付着効率（チタン皮膜の形成量／
チタンの蒸発量）が悪くなる虞れがあるからであり、逆
に150mm未満では、付着効率は良くなるが蒸発源からの
輻射熱でアルミニウム箔表面の温度上昇をきたすととも
に、ガス圧の影響が少なくなり静電容量が低下する虞れ
があるからである。Here, the final film thickness of the titanium film (3) is 0.1 to 3 μm.
It is desirable to set m (0.045 to 1.35 mg / cm 2 in terms of coating amount). If it is less than 0.1 μm, the surface of the film will be smooth, which may result in a small electrostatic capacity. Conversely, if it exceeds 3 μm, the titanium material used will increase and the cost will increase. This is because there is a possibility that the effect of getting closer to each other may not be obtained. In addition, the number of titanium thin film layers is preferably in the range of 2 to 10 if the deposition process is performed intermittently or if it is reduced. Even if the vapor deposition treatment is repeated more than 10 times, not only the effect is saturated, but also the productivity is rather deteriorated and the treatment cost becomes high. The vapor deposition rate should be appropriately determined in consideration of the relationship between the desired titanium film thickness and the number of vapor deposition treatments, and is preferably 100 to 5
It is better to set it to 000Å / sec (4.5 x 10 -3 to 0.225 mg / cm 2 sec in terms of adhesion amount). At a deposition rate of more than 5000 Å / sec, the influence of the atmospheric pressure will disappear, which may lead to defects such as a decrease in electrostatic capacity. This is because the cost is high. Further, it is preferable that the atmosphere for the vapor deposition treatment is an atmosphere of an inert gas such as Ar, because the surface of the titanium film can be roughened more. The atmospheric pressure is preferably 5 × 10 -5 to 5 × 10 -3 Torr. This is because if it is less than 5 × 10 -5 Torr, the effect of finely roughening the coating may be reduced and the electrostatic capacity may be small. Conversely, if the pressure is set to exceed 5 × 10 -3 Torr, This is because it is difficult for titanium to evaporate, and the adhesion with the aluminum foil may deteriorate. Considering mass productivity, it is preferable to set the pressure to about 1 × 10 −3 Torr. The evaporation distance should be 150-400 mm. 400m
If it exceeds m, the adhesion efficiency of titanium (amount of titanium film formed /
On the contrary, if it is less than 150 mm, the adhesion efficiency will be improved, but the radiation heat from the evaporation source will raise the temperature of the aluminum foil surface and the effect of gas pressure will be small. This is because there is a risk that the electrostatic capacity will decrease.
チタン皮膜（３）を形成したアルミニウム箔は、これを
そのまま電解コンデンサ用陰極材料としても良く、ある
いはその後硼酸、硼酸アンモニウム、酒石酸、酒石酸ア
ンモニウム等の溶液あるいは水溶液中で陽極酸化処理
し、酸化皮膜を形成して陽極材料として使用しても良
い。The aluminum foil on which the titanium film (3) has been formed may be used as it is as a cathode material for an electrolytic capacitor, or thereafter, anodized in a solution or aqueous solution of boric acid, ammonium borate, tartaric acid, ammonium tartrate, etc. to form an oxide film. It may be formed and used as an anode material.
発明の効果 この発明は上述の次第で、粗面化されたアルミニウム箔
の表面に所定膜厚のチタン皮膜を形成するに際し、チタ
ン蒸着処理の少量実施を間欠的に繰り返すことによっ
て、チタン薄膜層を順次的に堆積せしめることにより、
所定膜厚を達成せんとするものである。従って従来の如
く、所定膜厚のチタン皮膜を一回の蒸着処理により一度
に形成する場合に較べて、アルミニウム箔の温度上昇を
抑制しえて低温度に保持した状態で所期するチタン皮膜
を形成することができるから、アルミニウム箔の温度上
昇に起因して生じていたチタン粒子の融合による皮膜表
面の平滑化を確実かつ有効に防止しえ、著しく粗な拡面
率の大きな皮膜表面を得ることができ、ひいては電極材
料の静電容量を増大することができる。しかもチタン薄
膜層表面の微細凹凸が、その上方に形成されるチタン薄
膜層に順次的に波及する結果、益々表面の粗なチタン薄
膜を得ることができ、高静電容量を達成することができ
る。さらにまた、アルミニウム箔の温度を低く保持しつ
つチタン皮膜の形成が可能であるから、連続的巻き取り
法により蒸着処理を行う場合には、巻き取りあるいは巻
き戻し時の材料変形（伸び）がなく、安定した静電容量
を得ることができるという効果をも奏する。EFFECTS OF THE INVENTION According to the present invention, when a titanium film having a predetermined thickness is formed on the surface of a roughened aluminum foil, a titanium thin film layer is formed by intermittently repeating a small amount of titanium vapor deposition treatment. By sequentially depositing,
It is intended to achieve a predetermined film thickness. Therefore, as compared with the conventional case where a titanium film having a predetermined thickness is formed at one time by a single vapor deposition process, the desired titanium film is formed while suppressing the temperature rise of the aluminum foil and keeping it at a low temperature. Therefore, it is possible to reliably and effectively prevent the smoothing of the coating surface due to the fusion of titanium particles caused by the temperature rise of the aluminum foil, and obtain a coating surface with a significantly large surface expansion ratio. It is possible to increase the capacitance of the electrode material. Moreover, as a result of the fine irregularities on the surface of the titanium thin film layer successively spreading to the titanium thin film layer formed thereabove, a titanium thin film having an increasingly rough surface can be obtained and a high capacitance can be achieved. . Furthermore, since the titanium film can be formed while keeping the temperature of the aluminum foil low, there is no material deformation (elongation) during winding or unwinding when the vapor deposition process is performed by the continuous winding method. Also, it has an effect that a stable capacitance can be obtained.
実施例 次にこの発明の実施例を比較例との対比において示す。Example Next, an example of the present invention will be shown in comparison with a comparative example.
［実施例１］ 塩酸を主成分とし、これに硝酸、リン酸、硫酸等を添加
して溶液中で交流電解エッチングを施し、表面を海綿状
組織層を有するものに粗面化したアルミニウム箔コイル
を用意した。なおアルミニウム箔は厚さ50μｍ、純度9
9.8％のものを用いた。[Example 1] An aluminum foil coil containing hydrochloric acid as a main component, to which nitric acid, phosphoric acid, sulfuric acid, etc. were added and subjected to AC electrolytic etching in a solution to roughen the surface to have a spongy tissue layer. Prepared. The aluminum foil has a thickness of 50 μm and a purity of 9
9.8% was used.
次に上記アルミニウム箔コイルを、１×10-3TorrのAr雰
囲気に保持した真空ベルジャー内において、第３図に示
す連続的巻き取り法により蒸着処理を施して、チタン皮
膜を形成した。皮膜の形成は以下の手順に従った。即
ち、まず前記アルミニウム箔コイルを巻き取りながら、
蒸着速度0.045mg/cm2secで皮膜量0.11mg/cm2のチタン薄
膜層をアルミニウム箔の長さ方向の全域にわたって連続
的に形成した。続いてコイルを巻き戻しながら、同様に
アルミニウム箔の長さ方向の全域に蒸着速度0.045mg/cm
2secで皮膜量0.11mg/cm2の二層目のチタン薄膜層を形成
し、もってチタン皮膜とした。該チタン皮膜の膜厚は0.
49μｍ（皮膜量換算0.22mg/cm2）であった。Next, the aluminum foil coil was vapor-deposited by a continuous winding method shown in FIG. 3 in a vacuum bell jar held in an Ar atmosphere of 1 × 10 −3 Torr to form a titanium film. The film formation was according to the following procedure. That is, first while winding the aluminum foil coil,
A titanium thin film layer having a coating amount of 0.11 mg / cm 2 was continuously formed at a deposition rate of 0.045 mg / cm 2 sec over the entire length of the aluminum foil. Then, while rewinding the coil, the vapor deposition rate is 0.045 mg / cm over the entire length of the aluminum foil in the same manner.
A second titanium thin film layer having a coating amount of 0.11 mg / cm 2 was formed in 2 sec, and was used as a titanium coating. The thickness of the titanium film is 0.
It was 49 μm (0.22 mg / cm 2 in terms of coating amount).
［実施例２］ 実施例１と同じアルミニウム箔コイルを用い、該コイル
を１×10-4TorrのAr雰囲気に保持した真空ベルジャー内
において、実施例１と同様の方法により、まずコイルを
巻き取りながら0.068mg/cm2secの蒸着速度で皮膜量0.07
mg/cm2のチタン薄膜層をアルミニウム箔の長さ方向全域
に連続的に形成した。次にコイルを巻き戻しながら、巻
き取り時と同じ蒸着速度、皮膜量で二層目のチタン薄膜
層を被覆形成したのち、再度コイルを巻き取りながら同
一の蒸着処理を実施した三層目のチタン薄膜層を形成
し、もってチタン皮膜とした。このチタン皮膜の膜厚は
0.47μｍ（皮膜量換算0.21mg/cm2）であった。Example 2 The same aluminum foil coil as in Example 1 was used, and the coil was first wound in the same manner as in Example 1 in a vacuum bell jar holding the coil in an Ar atmosphere of 1 × 10 −4 Torr. However, the coating amount was 0.07 at the deposition rate of 0.068 mg / cm 2 sec.
A titanium thin film layer of mg / cm 2 was continuously formed over the entire length of the aluminum foil. Next, while rewinding the coil, a second titanium thin film layer was formed at the same vapor deposition rate and film amount as when winding, and then the same vapor deposition treatment was performed while winding the coil again. A thin film layer was formed and used as a titanium film. The thickness of this titanium film is
It was 0.47 μm (0.21 mg / cm 2 in terms of coating amount).
［比較例］ 実施例１と同じアルミニウム箔コイルを用い、該コイル
１×10-3TorrのAr雰囲気に保持した真空ベルジャー内に
おいて、実施例１と同様の方法により、該コイルを巻き
取りながら、蒸着速度0.045mg/cm2secで１回の蒸着処理
を行い、一度に膜厚0.49μｍ（皮膜量換算0.22mg/cm2）
のチタン皮膜を形成した。Comparative Example Using the same aluminum foil coil as in Example 1 and winding the coil in the same manner as in Example 1 in a vacuum bell jar held in an Ar atmosphere of 1 × 10 −3 Torr of the coil, The vapor deposition rate is 0.045mg / cm 2 sec, and the vapor deposition process is performed once, and the film thickness is 0.49μm at a time (coating amount conversion 0.22mg / cm 2 ).
A titanium film was formed.
上記により得られた３種類の電極材料につき、その静電
容量を30℃、10％硼酸アンモニウム溶液中で測定した。
また各材料のチタン皮膜の密着性を調べるため、同一条
件でセロテープによる剥離試験を実施し、皮膜の剥離の
有無を目視観察した。それらの結果を下記第１表に示
す。The capacitances of the three kinds of electrode materials obtained above were measured in a 10% ammonium borate solution at 30 ° C.
Further, in order to examine the adhesion of the titanium film of each material, a peeling test using a cellophane tape was carried out under the same conditions, and the presence or absence of film peeling was visually observed. The results are shown in Table 1 below.
上表の結果からわかるように、この発明に従って製造さ
れた電極材料は静電容量が大きく、またチタン皮膜の密
着性も問題ないことを確認しえた。 As can be seen from the results in the above table, it can be confirmed that the electrode material manufactured according to the present invention has a large electrostatic capacity and the titanium film has no problem in adhesion.
第１図はこの発明によって製造される電極材料の一例を
示す模式的断面図、第２図は第１図の一部拡大図、第３
図はこの発明を実施する蒸着処理法の一例としての連続
的巻き取り蒸着法の構成を示す説明的断面図である。 （１）……アルミニウム箔、（３）……チタン皮膜、
（3a）（3b）（3c）（3d）……チタン薄膜層。FIG. 1 is a schematic sectional view showing an example of an electrode material manufactured by the present invention, FIG. 2 is a partially enlarged view of FIG. 1, and FIG.
FIG. 1 is an explanatory sectional view showing the structure of a continuous winding vapor deposition method as an example of the vapor deposition processing method for carrying out the present invention. (1) …… Aluminum foil, (3) …… Titanium film,
(3a) (3b) (3c) (3d) ... titanium thin film layer.
Claims (5)
タン蒸着処理の少量実施を間欠的に繰り返すことによっ
てチタン薄膜層を順次的に堆積せしめ、もって所定膜厚
のチタン皮膜を形成することを特徴とする電解コンデン
サ用アルミニウム電極材料の製造方法。1. A titanium thin film layer is sequentially deposited on a surface of a roughened aluminum foil by intermittently repeating a small amount of titanium vapor deposition treatment to form a titanium film having a predetermined thickness. A method for producing an aluminum electrode material for an electrolytic capacitor, comprising:
囲で行う特許請求の範囲第１項記載の電解コンデンサ用
アルミニウム電極材料の製造方法。2. The method for producing an aluminum electrode material for an electrolytic capacitor according to claim 1, wherein a small amount of titanium vapor deposition treatment is carried out within a range of 2 to 10 times.
タン蒸着処理の少量実施を行って、まずアルミニウム箔
に最下層のチタン薄膜層を連続的に形成したのち、コイ
ルを巻き戻して次層のチタン薄膜層を形成し、その後必
要に応じてコイルの巻き取りと巻き戻しを繰り返すこと
によりチタン薄膜層を順次的に堆積させる特許請求の範
囲第１項または第２項記載の電解コンデンサ用アルミニ
ウム電極材料の製造方法。3. A small amount of titanium vapor deposition treatment is carried out while winding an aluminum foil coil to first continuously form a lowermost titanium thin film layer on the aluminum foil, and then the coil is rewound to form a titanium thin film of the next layer. The aluminum electrode material for an electrolytic capacitor according to claim 1 or 2, wherein a titanium thin film layer is sequentially deposited by forming a layer and then repeating winding and unwinding of a coil as needed. Production method.
許請求の範囲第１項ないし第３項のいずれか１に記載の
電解コンデンサ用アルミニウム電極材料の製造方法。4. The method for producing an aluminum electrode material for electrolytic capacitors according to claim 1, wherein the titanium film has a thickness of 0.1 to 3 μm.
求の範囲第１項ないし第４項のいずれか１に記載の電解
コンデンサ用アルミニウム電極材料の製造方法。5. The method for producing an aluminum electrode material for an electrolytic capacitor according to any one of claims 1 to 4, wherein the vapor deposition rate is 100 to 5000 Å / sec.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9058287A JPH0738368B2 (en) | 1987-04-13 | 1987-04-13 | Method for manufacturing aluminum electrode material for electrolytic capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9058287A JPH0738368B2 (en) | 1987-04-13 | 1987-04-13 | Method for manufacturing aluminum electrode material for electrolytic capacitor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63255910A JPS63255910A (en) | 1988-10-24 |
| JPH0738368B2 true JPH0738368B2 (en) | 1995-04-26 |
Family
ID=14002435
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9058287A Expired - Lifetime JPH0738368B2 (en) | 1987-04-13 | 1987-04-13 | Method for manufacturing aluminum electrode material for electrolytic capacitor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0738368B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IL173121A (en) * | 2006-01-12 | 2011-07-31 | Dina Katsir | Electrodes, membranes, printing plate precursors and other articles including multi-strata porous coatings |
| JP2009164412A (en) | 2008-01-08 | 2009-07-23 | Kobe Steel Ltd | Porous metal thin film and manufacturing method thereof as well as capacitor |
| JP5181401B1 (en) * | 2012-07-12 | 2013-04-10 | 日本蓄電器工業株式会社 | Cathode foil for aluminum electrolytic capacitors |
-
1987
- 1987-04-13 JP JP9058287A patent/JPH0738368B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63255910A (en) | 1988-10-24 |
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