JP7093607B2 - 表面処理アルミニウム材及びその製造方法、ならびに、当該表面処理アルミニウム材と樹脂等の被接合部材とからなる表面処理アルミニウム材/被接合部材の接合体及びその製造方法 - Google Patents
表面処理アルミニウム材及びその製造方法、ならびに、当該表面処理アルミニウム材と樹脂等の被接合部材とからなる表面処理アルミニウム材/被接合部材の接合体及びその製造方法 Download PDFInfo
- Publication number
- JP7093607B2 JP7093607B2 JP2018022589A JP2018022589A JP7093607B2 JP 7093607 B2 JP7093607 B2 JP 7093607B2 JP 2018022589 A JP2018022589 A JP 2018022589A JP 2018022589 A JP2018022589 A JP 2018022589A JP 7093607 B2 JP7093607 B2 JP 7093607B2
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- Prior art keywords
- oxide film
- aluminum material
- treated aluminum
- electrolytic
- alkaline
- 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.)
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Images
Classifications
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Description
前記アルカリ交流電解酸化皮膜が、表面側に形成された厚さ20~1000nmのポーラス型アルミニウム酸化皮膜層と、素地側に形成された厚さ3~30nmのバリア型アルミニウム酸化皮膜層とから成り、前記ポーラス型アルミニウム酸化皮膜層には、平均最大径5~120nmの小孔が形成されており、前記ポーラス型アルミニウム酸化皮膜層の表面積に対する全小孔の面積占有率が5~50%であり、
前記複数の加工溝が、小孔の壁面を縫って繋ぐようにして塑性加工方向と垂直方向に沿って形成されていることを特徴とする表面処理アルミニウム材とした。
A.アルミニウム基材
本発明に係る表面処理アルミニウム材に用いるアルミニウム基材としては、純アルミニウム又はアルミニウム合金が用いられる。アルミニウム合金の成分は特に限定されるものではなく、JISに規定される合金を始めとする各種合金を使用することができる。形状も特に限定されるものではなく、平板状、任意の断面形状の棒状、円筒状などの形状のものを用いることができる。なお、安定してアルカリ交流電解酸化皮膜を形成できることか
ら、平板状のものが好適に用いられる。
図1(a)に示すように、本発明に係る表面処理アルミニウム材6は、アルミニウム基材3の表面の少なくとも一部に、アルカリ交流電解酸化皮膜が形成されている。なお、図(a)の例では、アルミニウム基材3の一方の表面にアルカリ交流電解酸化皮膜が形成されている。このアルカリ交流電解酸化皮膜は、表面側に形成されたポーラス型アルミニウム酸化皮膜層1と、アルミニウム基材である素地側に形成されたバリア型アルミニウム酸化皮膜層2とから成り、材料に対する塑性加工方向と垂直な加工溝5を有する。なお、図中4は、ポーラス型アルミニウム酸化皮膜層1に形成された小孔を示す。
本発明では、アルカリ交流電解酸化皮膜において、被接合体である樹脂等との接合性を向上させるために材料の塑性加工方向と垂直な複数の加工溝が形成されていることを特徴とする。このような加工溝は、小孔の壁面を縫って繋ぐようにして塑性加工方向と垂直方向に沿って発生する。塑性加工が引張成形、圧延成形、押出成形等のように材料加工方向が一方向の場合には、互いに加工方向にほぼ垂直で、かつ、ほぼ直線状の複数の加工溝が形成される。一方、プレス成形、張り出し成形等のように材料加工方向が複数方向ある場合には、直線状にはならないが、互いに加工方向にほぼ垂直な加工溝が形成される。
図1(a)、(b)に示すように、ポーラス型アルミニウム酸化皮膜層1には、表面から内部に延びる小孔4が形成されている。ポーラス型アルミニウム酸化皮膜層1の表面において、凹凸を考慮しない(縦×横で算出される)表面積に対して、存在する全ての小孔4の開口面積の総和が占める割合を小孔の面積占有率として、この小孔の面積占有率を5~50%とするのが好ましく、10~45%とするのがより好ましい。この小孔の面積占有率が5%未満では、被接合部材である樹脂等との接合における小孔が示すアンカー効果が不足する。その結果、アルカリ交流電解酸化皮膜による密着耐久性が低下する場合がある。一方、この面積占有率が50%を超えると、初期には大きな上記アンカー効果が得られるものの、面積占有率が大き過ぎるために上記アンカー効果の経時的な低下が大きくなって、アルカリ交流電解酸化皮膜による密着耐久性が却って低下する場合がある。
ポーラス型アルミニウム酸化皮膜層とアルミニウム基材の素地との間のバリア型アルミニウム酸化皮膜層の厚さは、好ましくは3~30nm、より好ましくは5~25nmである。バリア型アルミニウム酸化皮膜層の厚さが3nm未満では、介在するバリア型アルミニウム酸化皮膜層が薄いためポーラス型アルミニウム酸化皮膜層とアルミニウム基材の素地とを結合するための結合力が弱く、加工溝の形成時においてポーラス型アルミニウム酸化皮膜層が破壊する虞がある。一方、バリア型アルミニウム酸化皮膜層の厚さが30nmを超えると、加工溝の形成時において形成される溝が不均一になる虞がある。
以下に、本発明に係る表面処理アルミニウム材の製造方法について説明する。
上述の条件を満たすアルカリ交流電解酸化皮膜を表面に備えた表面処理アルミニウム材を製造するための一つの方法として、表面処理されるアルミニウム基材を一方の電極とし、他方の対電極を用いて所定の条件下で交流電解処理することにより、アルカリ交流電解酸化皮膜を形成する方法を挙げることができる。
の一方の表面(アルミニウム基材電極の図中における左側の表面)のみを処理することも
できる。
交流電解処理は、上記アルミニウム基材の電極と対電極とを用い、アルカリ性水溶液を電解液とするものである。
なお、上記保持温度は、保持中において必ずしも一定温度である必要はなく、0~300℃の範囲内で変化してもよい。
図1(b)に示すように、本発明に係る表面処理アルミニウム材に樹脂等の被接合部材を接合して、表面処理アルミニウム材/被接合部材の接合体8が得られる。上述のように、このような接合体では、樹脂等の被接合部材7は、アルカリ交流電解酸化皮膜(1+2)及びアルミニウム基材3の素地の両方に接合しており、また、被接合部材7は、小孔4と加工溝5の両方に流入してアンカー効果を発揮するので、アルカリ交流電解酸化皮膜(1+2)を介したアルミニウム基材3と被接合部材7の接合をより強固なものとできる。
電解処理されるアルミニウム基材として、縦600mm×横800mm×厚さ2.0mmを有するJIS5052-Oのアルミニウム合金の平板を使用した。このアルミニウム合金板の25℃における引張強度は195MPaであった。
以上のようにして作製した表面処理アルミニウム材試料に対し、FE-SEMによる表面観察(観察視野:0.7μm×1μm)により、ポーラス型アルミニウム酸化皮膜層の小孔の平均最大径を測定した。結果を表1に示す。なお、表1に示す小孔の平均最大径については、100箇所の小孔の測定結果の算術平均値とした。
以上のようにして作製した表面処理アルミニウム材試料に対し、FE-SEMによる表面観察(観察視野:10μm×7μm)により、アルカリ交流電解酸化皮膜の加工溝幅及び加工溝間隔を測定した。結果を表1に示す。なお、表に示す加工溝幅及び加工溝間隔については、100箇所の測定結果の算術平均値とした。
上記のようにして作製した表面処理アルミニウム材試料に対し、TEMによりアルカリ交流電解酸化皮膜の縦方向に沿った断面観察を実施した。具体的には、ポーラス型アルミニウム酸化皮膜層及びバリア型アルミニウム酸化皮膜層のそれぞれの厚さを測定した。これらの酸化皮膜層の厚さを測定するために、ウルトラミクロトームを用いて供試材から断面観察用薄片試料を作製した。次に、この薄片試料において観察視野(1μm×1μm)中の任意の100箇所を選択してTEM断面観察により、それぞれの酸化皮膜層の厚さを測定した。結果を表1に示す。なお、これらの酸化皮膜層の厚さについては、100箇所の測定結果の算術平均値とした。
上記のように作製した表面処理アルミニウム材試料(JIS 1A号試験片)から縦50mm×横25mmにそれぞれ平行に切り取った供試材を20枚用意した。なお、試料と供試材の縦横は同じである。密着耐久性試験は、まず、2枚の供試材15、16を図3に示すように、縦方向の重なり長さが10mmとなるように重ね合わせて(接着面積10mm×25mm=250mm2)、直径200μmのガラスビーズを添加した1液型エポキシ樹脂系接着剤17を用いて接着し、このような接合体を10組作製した。次いで、接着した接合体を、加熱炉中において170℃で20分間加熱処理して接着剤を硬化させて密着耐久試験用の試験片とした。
◎:凝集破壊率が95%以上のもの
○:凝集破壊率が85%以上95%未満のもの
△:凝集破壊率が75%以上85%未満のもの
×:凝集破壊率が75%未満のもの
結果を表2に示す。同表には、10組の供試材のうちの上記◎、○、△、×の個数をそれぞれ示すが、全てが◎と○から構成される場合を合格、それ以外の場合を不合格と判定した。
上記のように作製した表面処理アルミニウム材試料から縦50mm×横10mmに切断した供試材を10枚用意し、ガラス繊維含有PPS樹脂(DIC社製)を用い、アルミニウム合金板のインサート成形による接合試験片を作製した。射出成形金型に表面処理アルミニウム材試料をインサートし、金型を閉め金型を加熱することで、150℃まで接合試験片を加熱後、PPS樹脂を射出温度320℃で射出することで、図4に示すせん断試験片状の接合体を得た。接合部は、表面処理アルミニウム材試料端部の縦5mm×横10mm部分とした
◎:凝集破壊率が95%以上のもの
○:凝集破壊率が85%以上95%未満のもの
△:凝集破壊率が75%以上85%未満のもの
×:凝集破壊率が75%未満のもの
結果を表2に示す。同表には、10組のせん断試験片状の接合体のうちの上記◎、○、△、×の個数をそれぞれ示すが、全てが◎又は○からなる場合を合格、それ以外を不合格と判定した。
上記アルカリ交流電解酸化皮膜の密着耐久性評価及び熱可塑性樹脂の接合性評価の両方が合格であったものを総合評価が合格とし、これら各評価の少なくともいずれか一つが不
合格のものを総合評価が不合格とした。
2‥‥‥バリア型アルミニウム酸化皮膜層
3‥‥‥アルミニウム基材(の素地)
4‥‥‥小孔
5‥‥‥加工溝
6‥‥‥表面処理アルミニウム材
7‥‥‥樹脂等の被接合部材
8‥‥‥表面処理アルミニウム材/被接合部材の接合体
9‥‥‥対電極板
10‥‥‥対電極板
11‥‥‥アルミニウム基板
12‥‥‥交流電源
13‥‥‥電解液
14‥‥‥対電極板接続スイッチ
15‥‥‥密着耐久性試験供試材
16‥‥‥密着耐久性試験供試材
17‥‥‥1液型エポキシ樹脂系接着剤
18‥‥‥PPS樹脂
Claims (16)
- アルミニウム基材と、その表面の少なくとも一部に形成されたアルカリ交流電解酸化皮膜とを含み、当該アルカリ交流電解酸化皮膜には、塑性加工方向と垂直な複数の加工溝が形成されている表面処理アルミニウム材において、
前記アルカリ交流電解酸化皮膜が、表面側に形成された厚さ20~1000nmのポーラス型アルミニウム酸化皮膜層と、素地側に形成された厚さ3~30nmのバリア型アルミニウム酸化皮膜層とから成り、前記ポーラス型アルミニウム酸化皮膜層には、平均最大径5~120nmの小孔が形成されており、前記ポーラス型アルミニウム酸化皮膜層の表面積に対する全小孔の面積占有率が5~50%であり、
前記複数の加工溝が、小孔の壁面を縫って繋ぐようにして塑性加工方向と垂直方向に沿って形成されていることを特徴とする表面処理アルミニウム材。 - 前記塑性加工方向が一方向である、請求項1に記載の表面処理アルミニウム材。
- 前記ポーラス型アルミニウム酸化皮膜層における小孔の平均最大径が10~30nmである、請求項1又は2に記載の表面処理アルミニウム材。
- 前記加工溝の幅が5~5000nmである、請求項1~3のいずれか一項に記載の表面処理アルミニウム材。
- 前記加工溝の間隔が5~5000nmである、請求項1~4のいずれか一項に記載の表面処理アルミニウム材。
- 請求項1~5のいずれか一項に記載の表面処理アルミニウム材の製造方法であって、表面処理されるアルミニウム基材の電極と対電極とを用い、アルカリ性水溶液を電解液として交流電解処理後に、交流電解処理したアルミニウム基材にひずみ速度1.0×10-3~1.0×103/sで塑性加工を施すことを特徴とする表面処理アルミニウム材の製造方法。
- 前記アルカリ性水溶液の電解液の温度が30~90℃である、請求項6に記載の表面処理アルミニウム材の製造方法。
- 前記アルカリ性水溶液の電解液のpHが9~13である、請求項6又は7に記載の表面処理アルミニウム材の製造方法。
- 前記交流電解処理の電解処理時間が5~600秒である、請求項6~8のいずれか一項に記載の表面処理アルミニウム材の製造方法。
- 前記交流電解処理の電流密度が4~50A/dm2である、請求項6~9のいずれか一項に記載の表面処理アルミニウム材の製造方法。
- 前記交流電解処理の周波数が10~100Hzである、請求項6~10のいずれか一項に記載の表面処理アルミニウム材の製造方法。
- 電極に用いる前記アルミニウム基材の引張強度が30~450MPaである、請求項6~11のいずれか一項に記載の表面処理アルミニウム材の製造方法。
- 前記交流電解処理したアルミニウム基材を塑性加工するまでにおいて、当該アルミニウム基材を0~300℃で保持する、請求項6~12のいずれか一項に記載の表面処理アルミニウム材の製造方法。
- 請求項1~5のいずれか一項に記載の表面処理アルミニウム材と、そのアルカリ交流電解酸化皮膜側の被接合部材とを含む表面処理アルミニウム材/被接合部材の接合体。
- 前記被接合部材が樹脂である、請求項14に記載の表面処理アルミニウム材/被接合部材の接合体。
- 請求項15に記載の表面処理アルミニウム材/被接合部材の接合体の製造方法であって、請求項6~13のいずれか一項に記載の表面処理アルミニウム材の製造方法によって表面処理アルミニウム材を製造し、当該表面処理アルミニウム材に被接合部材を接合する表面処理アルミニウム材/被接合部材の接合体の製造方法において、前記被接合部材となる樹脂を加熱して流動状態として前記ポーラス型アルミニウム酸化皮膜層に接触・浸透させることにより、当該流動状態の樹脂を前記小孔と加工溝に流入させ、流動状態の樹脂を冷却固化又は硬化することを特徴とする表面処理アルミニウム材/被接合部材の接合体の製造方法。
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