TWI762587B - 表面處理鋁材及其製備方法、以及該表面處理鋁材與樹脂等被接合部件形成的表面處理鋁材/被接合部件的接合體及其製備方法 - Google Patents
表面處理鋁材及其製備方法、以及該表面處理鋁材與樹脂等被接合部件形成的表面處理鋁材/被接合部件的接合體及其製備方法 Download PDFInfo
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- TWI762587B TWI762587B TW107106022A TW107106022A TWI762587B TW I762587 B TWI762587 B TW I762587B TW 107106022 A TW107106022 A TW 107106022A TW 107106022 A TW107106022 A TW 107106022A TW I762587 B TWI762587 B TW I762587B
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- Prior art keywords
- oxide film
- treated aluminum
- aluminum material
- joined
- resin
- Prior art date
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Classifications
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Abstract
本發明提供一種表面處理鋁材及其製備方法,該表面處理鋁材包括鋁基材、以及形成於其表面之至少一部分上之鹼交流電解氧化膜,該鹼交流電解氧化膜包括形成於表面側之多孔型鋁氧化膜層、以及形成於基底側之阻隔型鋁氧化膜層,且形成有與塑性加工方向垂直之複數個加工槽;以及該表面處理鋁材與樹脂等被接合部件形成的表面處理鋁材/被接合部件的接合體及其製備方法。
Description
本發明係關於一種實施表面處理之純鋁材或鋁合金材(以下,單獨略記為「鋁材」)及其製備方法,詳細而言,關於如下表面處理鋁材及其製備方法:藉由對實施形成樹脂密接性優異之鹼交流電解氧化膜之表面處理之鋁材實施塑性加工,同時於該鹼交流電解氧化膜上導入微細之加工槽,從而形成優異於樹脂密接後之耐久性、以及鹼交流電解氧化膜與鋁基底間之耐久性兩之鹼交流電解氧化膜。進而,本發明係關於一種包含該表面處理鋁材及樹脂等被接合部件,且具備優異之密接耐久性及加工配合度的表面處理鋁材/被接合部件之接合體及其製備方法。
鋁材由於輕量,且具有適度之機械特性,另外,具有美感、導電性、散熱性、耐蝕性、回收再利用性優異之特徵,故使用於多種結構部件、熱交換器部件、容器類、包裝類、電子設備類、機械類等。另外,藉由對該等鋁材之一部分或全部實施表面處理,而賦予或提高該等鋁材之耐蝕性、絕緣性、密接性、抗菌性、耐磨耗性等性質後使用之情形亦多。
另外,近年來,以汽車產業為中心,省資源化或省能量化推進,將鋁材應用於結構部件中時,為了實現進一步之輕量化而提出有將鋁材之一部分或全部與樹脂接合之結構部件。該等結構部件由於用於運輸用設備,故而要求在大氣環境或腐蝕環境中之高密接耐久性。另外,會有對該等結構部件實施彎曲加工或壓力加工等之情形,亦會有實施塑性加工後與樹脂接合之情形。
於製造如上所述之將鋁材與樹脂接合之部件或塗裝部件等之情形時,亦為了提高鋁材之樹脂密接性而需要表面處理。例如,提出有如專利文獻1之鹼交流電解法。即,將液溫為35~85℃且丙烯酸化合物聚合物濃度為0.1~10重量%之鹼性水溶液用於電解液,以電流密度為4~50A/dm2、頻率為20~100Hz、電解時間為5~60秒進行交流電解處理。藉此,獲得於表面具備形成有大小為5~50nm之小孔之氧化膜的鋁材。
另外,於使鋁材與樹脂等密接後,進行彎曲加工等之情形時,為了提高加工配合度,例如提出有如專利文獻2之方法。即,將pH值為9~13且液溫為30~90℃之鹼性水溶液作為電解液,使用電解結束時之陽極峰值電壓為25~200V之波形而進行交流電解處理。藉此,獲得多孔型鋁氧化膜層表面之小孔面積佔有率係為5~50%之鋁材。
於該等先前技術文獻中,係關於對鋁材實施表面處理後,立即將樹脂密接之方法。然而,於鋁材上形成氧化膜後,亦會有採用如下步驟之情形:於接合樹脂之前對鋁材施加壓力加工、彎曲加 工、拉伸加工等塑性加工,然後於加工部上接合樹脂。
然而,若對如專利文獻1所記載之表面處理鋁材實施塑性加工,則於接合樹脂之前會有氧化膜自鋁基底上剝離之情況,其結果係為會有無法與樹脂接合之問題。
於專利文獻2中記載之表面處理中,若係為使鋁材與樹脂等密接之後,則可進行彎曲加工,但若於進行表面處理後且進行樹脂接合之前實施塑性加工,則不論加工方向如何,均於多孔型鋁氧化膜層之整個面上傳播龜裂,會有無法獲得所需之接合強度之問題。
先前技術文獻
專利文獻
專利文獻1:日本專利特開2009-228064號公報
專利文獻2:日本專利特開2016-148079號公報
本發明等人為了解決上述問題而反覆研究,結果完成本發明。已發現,藉由以既定之應變速度對多孔性鋁氧化膜層實施塑性加工,不會於氧化膜整個面上產生龜裂,可僅在與加工方向垂直之方向上微細地導入加工槽。而且,藉由以既定之寬度及間隔設置該加工槽,不僅可抑制鹼交流電解氧化膜自鋁基底上剝離,而且可於小孔部與加工槽部之兩中流入作為被接合部件之樹脂等。其結果係為發現,藉由表面處理鋁材與被接合部件之機械性接合效果 提高,而獲得與例如易接著性樹脂及難接著性樹脂等被接合部件之密接性更進一步優異之鹼交流電解氧化膜結構。
另外發現,藉由以既定之應變速度實施塑性加工,可在與加工方向垂直之方向上微細地導入加工槽,尤其藉由於表面處理前預先調整鋁基材之強度,進而調整自交流電解處理後直至塑性加工為止之表面處理鋁材之溫度,可控制於塑性加工時所導入之複數個加工槽之間隔。其結果為,可更進一步抑制鹼交流電解氧化膜自鋁基底上剝離。
即,本發明於請求項1中提供一種表面處理鋁材,其中:包括鋁基材、以及形成於其表面之至少一部分上之鹼交流電解氧化膜,且於該鹼交流電解氧化膜上形成有與塑性加工方向垂直之複數個加工槽。
本發明於請求項2中提供如下,其係於請求項1中,該鹼交流電解氧化膜包括:形成於表面側之厚度為20~1000nm之多孔型鋁氧化膜層、以及形成於基底側之厚度為3~30nm之阻隔型鋁氧化膜層。
本發明於請求項3中提供如下,其係於請求項1或2中,於該多孔型鋁氧化膜層上形成有平均最大徑5~120nm之小孔。
本發明於請求項4中提供如下,其係於請求項1~3之任一項中,該加工槽之寬度係為5~5000nm。
本發明於請求項5中提供如下,其係於請求項1~4之 任一項中,該加工槽之間隔係為5~5000nm。
本發明於請求項6中提供如下,其係於請求項1~5之任一項中,相對於該多孔型鋁氧化膜層表面積,全部小孔面積佔有率係為5~50%。
本發明於請求項7中提供如下,其係於請求項1~6之任一項中,該多孔型鋁氧化膜層中之小孔之平均最大徑係為5~120nm。
本發明於請求項8中提供一種表面處理鋁材之製備方法,其係如請求項1~7之任一項所述之表面處理鋁材之製備方法,其中:使用經表面處理之鋁基材之電極及對電極,將鹼性水溶液作為電解液而進行交流電解處理後,以應變速度為1.0×10-3~1.0×103/s對經交流電解處理之鋁基材進行塑性加工。
本發明於請求項9中提供如下,其係於請求項8中,該鹼性水溶液之電解液之溫度係為30~90℃。
本發明於請求項10中提供如下,其係於請求項8或9中,該鹼性水溶液之電解液之pH值係為9~13。
本發明於請求項11中提供如下,其係於請求項8~10之任一項中,該交流電解處理之電解處理時間係為5~600秒。
本發明於請求項12中提供如下,其係於請求項8~11之任一項中,該交流電解處理之電流密度係為4~50A/dm2。
本發明於請求項13中提供如下,其係於請求項8~12之任一項中,該交流電解處理之頻率係為10~100Hz。
本發明於請求項14中提供如下,其係於請求項8~13之任一項中,電極中所使用之該鋁基材之拉伸強度係為30~450MPa。
本發明於請求項15中提供如下,其係於請求項8~14之任一項中,將該鋁基材保持於0~300℃,直至對該經交流電解處理之鋁基材進行塑性加工為止。
本發明於請求項16中提供一種表面處理鋁材/被接合部件之接合體,其包括:如請求項1~7之任一項所述之表面處理鋁材、以及其鹼交流電解氧化膜側之被接合部件。
本發明於請求項17中提供如下,其係於請求項16中,該被接合部件為樹脂。
本發明於請求項18中提供一種表面處理鋁材/被接合部件之接合體之製備方法,其係如請求項17所述之表面處理鋁材/被接合部件之接合體之製備方法,其中:將成為該被接合部件之樹脂加熱而成為流動狀態,接觸‧滲透於該多孔性鋁氧化膜層中,藉此使該流動狀態之樹脂流入至該小孔及該加工槽中,將流動狀態之樹脂冷卻固化或硬化。
依據本發明,獲得特徵在於形成有具備與樹脂等被接合部件之優異密接耐久性,及加工配合度之鹼交流電解氧化膜的表面處理鋁材、以及可以短時間且以簡便之步驟形成該鹼交流電解氧化膜之製備方法。進而依據本發明,獲得包括該表面處理鋁材及 樹脂等被接合部件、且具備優異之密接耐久性及加工配合度之表面處理鋁材/被接合部件之接合體及其製備方法。
1‧‧‧多孔型鋁氧化膜層
2‧‧‧阻隔型鋁氧化膜層
3‧‧‧鋁基材(之基底)
4‧‧‧小孔
5‧‧‧加工槽
6‧‧‧表面處理鋁材
7‧‧‧樹脂等被接合部件
8‧‧‧表面處理鋁材/被接合部件之接合體
9‧‧‧對電極板
10‧‧‧對電極板
11‧‧‧鋁基板
12‧‧‧交流電源
13‧‧‧電解液
14‧‧‧對電極板連接開關
15‧‧‧密接耐久性試驗供試材
16‧‧‧密接耐久性試驗供試材
17‧‧‧一液型環氧樹脂系接著劑
18‧‧‧PPS樹脂
圖1係本發明之表面處理鋁材之示意圖。
圖2係表示本發明之表面處理鋁材之製備方法中所使用之電解裝置之正面圖。
圖3係本發明之表面處理鋁材之密接耐久性試驗用試料之正面圖。
圖4係使用本發明之表面處理鋁材之剪切試驗片狀之接合體之正面圖。
以下,依序對本發明之詳情進行說明。
A.鋁基材
本發明之表面處理鋁材中所使用之鋁基材係使用純鋁或鋁合金。鋁合金之成分並無特別限定,可使用以JIS中所規定之合金為代表之各種合金。形狀亦無特別限定,可使用平板狀、任意剖面形狀之棒狀、圓筒狀等形狀。此外,就可以穩定地形成鹼交流電解氧化膜之方面而言,適合使用平板狀。
此外,於鋁基材為平板狀之情形時,可於平板之任一表面上形成鹼交流電解氧化膜,或亦可於兩個表面上形成鹼交流電解氧化膜。另外,於鋁基材為任意剖面形狀之棒狀之情形時,可遍 及表面整體而形成鹼交流電解氧化膜,或亦可於表面之一部分上形成鹼交流電解氧化膜。進而,於鋁基材為圓筒狀之情形時,可於圓筒之外表面及內表面之至少任一面上,遍及表面整體而形成鹼交流電解氧化膜,或亦可於表面之一部分上形成鹼交流電解氧化膜。
B.鹼交流電解氧化膜
如圖1(a)所示,本發明之表面處理鋁材6係於鋁基材3之表面之至少一部分上形成有鹼交流電解氧化膜。此外,圖(a)之例中,於鋁基材3之其中一個表面形成有鹼交流電解氧化膜。該鹼交流電解氧化膜包括:形成於表面側之多孔型鋁氧化膜層1、以及形成於作為鋁基材之基底側之阻隔型鋁氧化膜層2,且具有與對材料之塑性加工方向垂直之加工槽5。此外,圖中4示出形成於多孔型鋁氧化膜層1上之小孔。
此處,鹼交流電解氧化膜之厚度可採取後述多孔型鋁氧化膜層與阻隔型鋁氧化膜層之厚度之和,即23~1030nm之範圍,較佳為30~1000nm,更佳為50~500nm。若該厚度小於23nm,則會有由鹼交流電解氧化膜帶來之密接耐久性下降之情形,若超過1030nm,則多孔型鋁氧化膜層之表層部會溶解一部分,另外會有由鹼交流電解氧化膜帶來之密接耐久性下降之情形。
此外,圖1(a)之表面處理鋁材6係藉由對鋁基材3實施鹼交流電解處理,於其表面設置鹼交流電解氧化膜後,對材料實施塑性加工而形成加工槽5之狀態。此處,係藉由鹼交流電解處 理,於鋁基材3之表面之至少一部分,即遍及表面整體或於表面之一部分上形成有鹼交流電解氧化膜。
繼而,圖1(b)係表示於圖1(a)之狀態之表面處理鋁材6中,於其鹼交流電解氧化膜側接合有樹脂等被接合部件7之表面處理鋁材/被接合部件之接合體8,即包括表面處理鋁材6、以及其鹼交流電解氧化膜側之樹脂等被接合部件7的表面處理鋁材/被接合部件之接合體8。另外,被接合部件7由於流入至小孔4及加工槽5之兩中而與該等接合,故而經由鹼交流電解氧化膜而獲得鋁基材3與被接合部件7之更牢固之接合體8。
B-1.加工槽
本發明中特徵在於,於鹼交流電解氧化膜中,為了提高與作為被接合體之樹脂等之接合性而形成有與材料之塑性加工方向垂直之複數個加工槽。此種加工槽係將小孔之壁面縫合而相連,沿著與塑性加工方向垂直之方向而產生。於塑性加工如拉伸成形、壓延成形、擠出成形等般,材料加工方向為一個方向之情形時,形成相互間與加工方向大致垂直、且大致直線狀之複數個加工槽。另一方面,於如衝壓成形、拉伸成形等般,材料加工方向有複數個方向之情形時,雖不成為直線狀,但形成相互間與加工方向大致垂直之加工槽。
如圖1(b)所示,藉由向如上所述之加工槽5中流入樹脂等被接合部件7,則所流入之被接合部件7與鹼交流電解氧化膜接合而發揮增黏效果,而且亦與鋁基材3之加工槽部接合而發揮 增黏效果,因此可抑制鹼交流電解氧化膜(1+2)自鋁基材3之基底上剝離。
加工槽係在與塑性加工方向垂直之方向之長度方向上延伸之槽,將與該長度方向正交之長度作為加工槽之寬度。該加工槽之寬度較佳為5~5000nm,更佳為10~2000nm。於加工槽之寬度小於5nm之情形時,使樹脂等被接合部件密接時,有會有加工槽未有流入接合部件之情形。由如上所述之加工槽未有流入被接合部件所引起之空隙部,使接合強度下降。另一方面,於加工槽之寬度超過5000nm之情形時,接合部中小孔所占之部分減少,會有由小孔帶來之增黏效果降低而使接合強度下降之情形。
另外,鄰接之加工槽之間隔較佳為5~5000nm,更佳為10~2000nm。於該加工槽之間隔小於5nm之情形時,加工槽之密度極度變大。其結果為,接合部中與鋁基材接觸之鹼交流電解氧化膜減少,會有鋁基材自基底上剝離之顧慮。另一方面,於加工槽之間隔超過5000nm之情形時,接合部中加工槽所占之部分減少,會有由加工槽中所會有被接合部件帶來鋁基材之增黏效果降低,其結果為無法獲得樹脂等被接合部件與鋁基材之所需接合強度之情形。
B-2.多孔型鋁氧化膜層
如圖1(a)、(b)所示,於多孔型鋁氧化膜層1上形成有自表面向內部延伸之小孔4。於多孔型鋁氧化膜層1之表面中,將相對於不考慮凹凸(以縱×橫而算出)之表面積,所會有之全部小孔4 之開口面積之總和所占之比例設為小孔之面積佔有率,將該小孔之面積佔有率設較佳為5~50%,更佳為設為10~45%。若該小孔之面積佔有率小於5%,則與作為被接合部件之樹脂等之接合中的小孔所顯示之增黏效果不足。其結果為,會有由鹼交流電解氧化膜帶來之密接耐久性下降之情形。另一方面,若該面積佔有率超過50%,則雖於初期獲得大的上述增黏效果,但由於面積佔有率過大,故而上述增黏效果之經時性下降變大,會有由鹼交流電解氧化膜帶來之密接耐久性反而下降之情形。
多孔型鋁氧化膜層1之表面之小孔4之開口當自上方觀察時,其形狀為圓形、橢圓形、矩形、多角形等多種。作為此種開口之徑,將最大長度設為最大徑。例如,於開口之形狀為圓形之情形時,該徑為直徑,完全相同,最大徑係以直徑來規定。取而代之,於開口之形狀為橢圓形之情形時,該徑由短徑變化為長徑,最大徑係以長徑來規定。矩形或多角形等之情形亦同樣,將開口中測定之徑中最大規定為最大徑。而且,於多孔型鋁氧化膜層1之表面中,將所會有之全部小孔之各最大徑之算術平均數規定為平均最大徑。
上述平均最大徑較佳為5~120nm,更佳為10~30nm。若該平均最大徑小於5nm,則與小孔之面積佔有率不足之情形同樣,與樹脂等之接合中之增黏效果不足,會有由鹼交流電解氧化膜帶來之密接耐久性下降之情形。另一方面,若平均最大徑超過120nm,則與小孔之面積佔有率變得過大之情形同樣,與樹脂等接合中之增黏效果經時性降低,會有由鹼交流電解氧化膜帶來之密接 耐久性下降之情形。進而,與小孔之面積佔有率變得過大之情形同樣,多孔型鋁氧化膜層中之除小孔以外之部分減少,增黏效果之經時性下降變大,會有由鹼交流電解氧化膜帶來之密接耐久性反而下降之情形。
多孔型鋁氧化膜層之厚度較佳為20~1000nm,更佳為30~500nm。若多孔型鋁氧化膜層之厚度小於20nm,則厚度變得不充分,故而難以形成小孔結構,難以形成加工槽。其結果為,與樹脂等之接合中之由小孔帶來之增黏效果不足,進而,於加工槽中產生樹脂無法流入之空隙部分,會有由鹼交流電解氧化膜帶來之接合強度下降之情形。另一方面,若多孔型鋁氧化膜層之厚度超過1000nm,則多孔型鋁氧化膜層自身容易凝聚破壞,於加工槽形成時會有鹼交流電解氧化膜自鋁基材之基底上脫落之情形。
B-3.阻隔型鋁氧化膜層
多孔型鋁氧化膜層與鋁基材之基底之間之阻隔型鋁氧化膜層之厚度較佳為3~30nm,更佳為5~25nm。若阻隔型鋁氧化膜層之厚度小於3nm,則介隔會有之阻隔型鋁氧化膜層會太薄,因此用以將多孔型鋁氧化膜層與鋁基材之基底結合之結合力會弱,會有加工槽之形成時會有多孔型鋁氧化膜層破壞之顧慮。另一方面,若阻隔型鋁氧化膜層之厚度超過30nm,則會有加工槽之形成時會有所形成之槽不均勻之顧慮。
C.表面處理鋁材之製備方法
以下,對本發明之表面處理鋁材之製備方法進行說明。
C-1.電極
作為用以製造表面具備滿足上述條件之鹼交流電解氧化膜之表面處理鋁材的一種方法,可列舉如下方法:將經表面處理之鋁基材作為其中一個電極,使用另一個對電極,於既定之條件下進行交流電解處理而形成鹼交流電解氧化膜。
本發明中,經交流電解處理之鋁基材之電極之拉伸強度較佳為30~450MPa,更佳為50~400MPa。若該拉伸強度小於30MPa,則會有加工槽之寬度減小之情形,於使樹脂等被接合部件密接時,有時會有未流入被接合部件之加工槽。會有由如上所述之加工槽未有流入接合部件所引起之空隙部使接合強度下降之情形。另一方面,若該拉伸強度超過450MPa,則會有難以導入加工槽之情形,有時由加工槽帶來之對鋁基材之增黏效果降低。
本發明中,經交流電解處理之鋁基材與對電極之形狀並無特別限定,為了使鋁基材與對電極之距離均勻,穩定地形成經交流電解處理之鹼交流電解氧化膜,鋁基材與對電極為使用板狀較佳。
如圖2所示,準備已接線之對電極板9、10,於該等2片對電極板之間,以使經表面處理之鋁基板11之兩個表面分別與對電極板9、10之表面平行之方式設置。鋁基板11係經由交流電源12而與對電極板9、10連接。該等鋁基板11、對電極板9、10設置於加入有鹼性水溶液之電解液13之電解層中。對向之鋁基板11與對電極面彼此之尺寸設為大致相同,將兩電極於靜止狀態下 進行電解操作為較佳。另外,於僅對經表面處理之鋁基板11之其中一個表面進行處理之情形時,亦可藉由關閉對電極板連接開關14而僅對鋁基板11之其中一個表面(鋁基材電極之圖中之左側之表面)進行處理。
交流電解處理中所使用之一對電極中之其中一個電極係應藉由電解處理而進行表面處理之鋁基材。另一對電極可使用例如黑鉛、鋁、鈦電極等公知之電極,不會因為電解液之鹼成分或溫度而劣化,導電性優異,進而其自身不產生電化學反應之材質。就上述方面而言,對電極為使用黑鉛電極較佳。其原因在於:除了黑鉛電極之化學性質穩定,且價廉而容易獲取之外,藉由黑鉛電極中所會有之大量氣孔之作用,而於交流電解步驟中電力線適度擴散,因此多孔型鋁氧化膜層及阻隔型鋁氧化膜層皆容易變得更均勻。
C-2.交流電解處理條件
交流電解處理係使用上述鋁基材之電極及對電極,將鹼性水溶液作為電解液。
本發明中,用作電解液之鹼水溶液可使用包含:磷酸鈉、磷酸氫鈉、焦磷酸鈉、焦磷酸鉀及偏磷酸鈉等磷酸鹽;氫氧化鈉及氫氧化鉀等鹼金屬氫氧化物;碳酸鈉、碳酸氫鈉、碳酸鉀等碳酸鹽;氫氧化銨;或該等之混合物的水溶液。如後所述,需要將電解液之pH值保持於特定之範圍內,因此使用含有可期待緩衝效果之磷酸鹽系物質之鹼性水溶液為較佳。如上所述之鹼性水溶液中所含之 鹼成分之濃度係以電解液之pH值成為所需值之方式適當調整,通常為1×10-4~1莫耳/升,較佳為1×10-3~0.8莫耳/升。此外,該等鹼性水溶液中,亦可為了提高鋁材表面之清潔度而添加界面活性劑或螯合劑等。
本發明中使用之電解液之pH值較佳為9~13,更佳為9.5~12.5。若pH值小於9,則電解液之鹼蝕刻力不足,因此多孔型鋁氧化膜層之小孔變小,會有由鹼交流電解氧化膜帶來之密接性下降之情形。另一方面,若pH值超過13,則鹼蝕刻力變得過剩,因此會有多孔型鋁氧化膜層溶解之情形,另外會有由鹼交流電解氧化膜帶來之密接性下降之情形。
本發明中使用之電解液之溫度較佳為30~90℃,更佳為35~85℃。若電解液溫度小於30℃,則鹼蝕刻力不足,因此多孔型鋁氧化膜層之小孔變小,會有由鹼交流電解氧化膜帶來之密接性下降之情形。另一方面,若超過90℃,則鹼蝕刻力變得過剩,因此會有多孔型鋁氧化膜層溶解之情形,另外會有由鹼交流電解氧化膜帶來之密接性下降之情形。
於本發明中之交流電解處理中,電流密度較佳為4~50A/dm2,更佳為5~40A/dm2。若電流密度小於4A/dm2,則在鹼交流電解氧化膜中,僅優先形成阻隔型鋁氧化膜層,因此會有無法獲得多孔型鋁氧化膜層之情形。另一方面,若超過50A/dm2,則電流變得過大,故而多孔型鋁氧化膜層之厚度控制變困難,容易產生處理不均,於導入加工槽之情形時,會有如下情形:於鹼交流電解 氧化膜極其厚之部分,多孔型鋁氧化膜層會自鋁基底上脫落。
作為本發明中之交流電解處理條件,交流頻率及電解時間較佳為如下所述。
電解時間較佳為5~600秒,更佳為10~500秒。若為小於5秒之處理時間,則會有多孔型鋁氧化膜層之形成不足之情形。其結果係為,會有由鹼交流電解氧化膜帶來之密接性變得不充分之情形。另一方面,若超過600秒,則會有多孔型鋁氧化膜層變得過厚,或多孔型鋁氧化膜層再溶解之顧慮。在這種場合,於加工槽導入時,會有如下情形:於鹼交流電解氧化膜極其厚之部分,多孔型鋁氧化膜層會自鋁基材之基底上脫落。
交流頻率較佳為10~100Hz、更佳為20~80Hz。若小於10Hz,則作為電性分解之直流性要素提高之結果係為,多孔型鋁氧化膜層之形成會被抑制。其結果為,當導入加工槽時,有時槽寬度變得過小,會有樹脂等被接合部件無法流入至加工槽內部之顧慮。另一方面,若超過100Hz,則陽極與陰極之反轉過快,因此鹼交流電解氧化膜整體之形成變得極其緩慢,為了獲得多孔型鋁氧化膜層之既定厚度而需要極其長之時間。此外,關於交流電解處理中之電解波形,可使用正弦波、矩形波、梯形波、三角波等波形。
本發明中之加工槽之寬度及間隔之測定中,使用藉由場發射型電子顯微鏡(FE-SEM)之表面觀察為較佳。具體而言,可從以加速電壓2kV、觀察視野10μm×7μm拍攝複數個部位之二 次電子像中,測量所觀察之任意加工槽之寬度。另外,加工槽之間隔亦同樣可測量任意之鄰接之2個加工槽之距離。此外,將一個觀察視野中之複數個部位之測定值之算術平均數作為該等加工槽之寬度及間隔。
本發明中之多孔型鋁氧化膜層之小孔之平均最大徑及面積佔有率之測定中,使用藉由場發射型電子顯微鏡(FE-SEM)之表面觀察以及藉由圖像分析軟體A像ㄑ (旭化成工程公司製造之2.50版)之粒子分析為較佳。具體而言,將以加速電壓2kV、觀察視野1μm×0.7μm拍攝複數個部位之二次電子像,輸入圖像分析軟體中,實施將於多孔型鋁氧化膜層之表面中觀察到之小孔部分視為粒子之各部位之粒子分析。
藉此,於各部位中,可測定多孔型鋁氧化膜層之表面之全部小孔之最大徑及開口面積。根據以上述方式獲得之各複數個部位中之小孔之最大徑之算術平均數,而求出平均最大徑。另外,於各部位中,根據全部小孔之開口面積之總和相對於不考慮凹凸之總面積之比,而獲得各部位之小孔之面積佔有率,根據以上述方式獲得之各複數個部位之算術平均數而求出小孔之面積佔有率。此外,關於小孔之最大徑、平均最大徑及面積佔有率,係如上述所規定。
本發明中之多孔型鋁氧化膜層及阻隔型鋁氧化膜層之厚度之測定中,使用藉由穿透型電子顯微鏡(TEM)之剖面觀察為較佳。具體而言,藉由利用超薄切片機等將各氧化膜層部分加工為 薄片,進行TEM觀察而測定。此外,將一個觀察視野中之複數個部位之測定值之算術平均數作為該等各氧化膜層之厚度。
本發明中之加工槽係藉由如下方式而形成:藉由上述交流電解處理而形成鹼交流電解氧化膜後,以既定之應變速度,使形成有鹼交流電解氧化膜之鋁基材進行塑性變形。
具體而言,藉由以應變速度1.0×10-3~1.0×103/s、較佳為5.0×10-3~1.0×102/s,對形成有鹼交流電解氧化膜之鋁基材進行塑性加工而形成。於該應變速度小於1.0×10-3/s之情形時,不論加工方向如何,均自多孔型鋁氧化膜層向整個面上傳播龜裂,鹼交流電解氧化膜自鋁基材之基底上脫離。其結果為,無法獲得由鹼交流電解氧化膜帶來之所需之接合強度。另一方面,於該應變速度超過1.0×103/s之情形時,不僅產生所需之加工槽,而且產生與加工方向平行之多餘的槽,導致鹼交流電解氧化膜自身之破壞。
另外,應變速度不必一直固定,只要變形中之應變速度處於上述範圍內即可。此外,形成加工槽之部分之應變速度可藉由使用伸長計而測定。於表面處理鋁材中,於接合樹脂等被接合部件之部分設置伸長計,可容易地測定加工時之應變速度。
本發明中,於自對鋁基材實施鹼交流電解處理之後,直至藉由塑性加工而形成加工槽為止之間,較佳為將形成有鹼交流電解氧化膜之鋁基材保持於較佳為0~300℃、更佳為5~280℃之溫度範圍內。於該保持溫度小於0℃之情形時,加工槽寬度會變得不均勻,會有由鹼交流電解氧化膜帶來之密接性部分性地下降之 情形。進而,亦會有加工槽之部分結露而產生局部之腐蝕的情形。另一方面,於該保持溫度超過300℃之情形時,會有與塑性加工之方向無關而產生由加熱引起之破裂的情形。其結果為,若於產生上述破裂之狀態下使加工槽成形,則會有鹼交流電解氧化膜自鋁基材之基底上部分性地脫落之情形。
此外,上述保持溫度於保持中不必為固定溫度,可於0~300℃之範圍內變化。
D.表面處理鋁材/被接合部件之接合體
如圖1(b)所示,於本發明之表面處理鋁材上接合樹脂等被接合部件,獲得表面處理鋁材/被接合部件之接合體8。如上所述,此種接合體中,樹脂等被接合部件7係與鹼交流電解氧化膜(1+2)以及鋁基材3之基底之兩者接合,另外,被接合部件7由於流入至小孔4與加工槽5之兩者中而發揮增黏效果,故而可使介隔有鹼交流電解氧化膜(1+2)之鋁基材3與被接合部件7之接合更牢固。
此種表面處理鋁材/被接合部件之接合體8可根據各種用途而使用。此處,被接合部件係使用樹脂、金屬、陶瓷等,就接合之容易性或可展開多種用途之方面而言,為使用樹脂較佳。樹脂可為熱硬化性樹脂,亦可為熱塑性樹脂,任一者均可使用,與本發明之表面處理鋁材中之形成於處理面上之特定之鹼交流電解氧化膜之特性相互結合,賦予多種效果。
例如,如上所述之接合體與鋁基材相比,通常樹脂之熱 膨脹率大,因此於接合界面中容易產生剝離或破裂。然而,於本發明之表面處理鋁材與樹脂之接合體中,本發明中之鹼交流電解氧化膜非常薄,且如上所述具有特定之形狀及結構,故而接合強度高,柔軟性優異,易於追隨樹脂之膨脹,難以產生剝離或破裂。本發明之表面處理鋁材與熱塑性樹脂之接合體可適合用作輕量、高剛性之複合材料。另外,本發明之表面處理鋁材與熱硬化性樹脂之接合體可適合用作印刷配線基板用途。
上述樹脂可使用各種熱塑性樹脂及熱硬化性樹脂。具體而言,於熱塑性樹脂中,使加熱而成為流動狀態之樹脂接觸‧滲透於多孔性鋁氧化膜層中,將其冷卻固化,藉此形成樹脂層。熱塑性樹脂例如可使用:聚烯烴(聚乙烯、聚丙烯等)、聚氯乙烯、聚酯(聚對苯二甲酸乙二酯、聚對苯二甲酸丁二酯等)、聚醯胺、聚苯硫醚、芳香族聚醚酮(聚醚醚酮、聚醚酮等)、聚苯乙烯、各種氟樹脂(聚四氟乙烯、聚氯三氟乙烯等)、丙烯酸樹脂(聚甲基丙烯酸甲酯等)、ABS樹脂(acrylonitrile butadiene styrene,丙烯腈丁二烯苯乙烯)樹脂、聚碳酸酯、熱塑性聚醯亞胺等。
另外,熱硬化性樹脂中,只要於硬化前之具有流動性之狀態下接觸‧滲透於多孔性鋁氧化膜層中,然後使其硬化即可。熱硬化性樹脂例如可使用:酚樹脂、環氧樹脂、三聚氰胺樹脂、脲樹脂、不飽和聚酯樹脂、醇酸樹脂、聚胺基甲酸酯、熱硬化性聚醯亞胺等。
此外,上述熱塑性樹脂與熱硬化性樹脂可分別單獨使用, 亦可作為將複數種之熱塑性樹脂或者複數種之熱硬化性樹脂混合而成之聚合物摻合物而使用。另外,亦可藉由添加各種填料,而改善樹脂之強度或熱膨脹率等物性。具體而言,可使用:玻璃纖維、碳纖維、聚芳醯胺纖維等各種纖維,或碳酸鈣、碳酸鎂、二氧化矽、滑石、玻璃、黏土等公知物質之填料。
實施例
以下,基於實施例及比較例,對本發明中之較佳實施形態進行詳細說明。
實施例1~2及比較例1~3
作為經電解處理之鋁基材,使用具有縱600mm×橫800mm×厚2.0mm之JIS5052-O之鋁合金之平板。該鋁合金板之25℃下之拉伸強度為195MPa。
將該鋁合金板用於其中一個電極,且使用縱500mm×橫550mm×厚2.0mm之一對平板之黑鉛電極作為對電極。如圖2所示,準備已接線之黑鉛之對電極板9、10,於該等2片對電極板之間,以使經表面處理之鋁合金板之電極11之兩個表面分別與對電極板9、10之表面平行之方式設置。鋁合金板之電極11經由交流電源12而與對電極板9、10連接,該等電極11、對電極板9、10設置於加入有鹼性水溶液之電解液13之電解層中。使用如上所述之電解裝置,於將對電極板連接開關14接通之狀態下進行鹼交流電解處理。藉由該鹼交流電解處理,在與2片黑鉛之對電極板9、10分別對向之鋁合金板之電極11之兩面,形成包含表面側之多孔 型鋁氧化膜層以及基底側之阻隔型鋁氧化膜層之鹼交流電解氧化膜。此外,電解處理係對相同之3個鋁基材分別進行,表中所示之數值結果設為該等3個之算術平均數。
電解處理中所使用之電解液中,使用表1所示之pH值、溫度之以焦磷酸鈉作為主成分之鹼性水溶液。此外,以0.1莫耳/升之NaOH水溶液來適當調整pH值。另外,該鹼性水溶液之電解質濃度設為0.1莫耳/升。如圖2所示,於收納電解液之電解槽中配置鋁合金板之電極與兩個對電極,以表1所示之電解處理條件實施交流電解處理。此外,使鋁合金板之電極及黑鉛對電極之縱方向與電解槽之深度方向一致。
如以上所示,於鋁合金板電極之兩面形成鹼交流電解氧化膜。於電解處理後,將鋁合金板電極自電解槽中迅速取出,以室溫之純水進行水洗,於80℃之乾燥空氣中乾燥後,於室溫(25℃)之大氣中保持。
繼而,於以上述方式製備之於表面設置有鹼交流電解氧化膜之鋁合金板電極之鹼交流電解氧化膜上形成加工槽。具體而言,將於表面設置有鹼交流電解氧化膜之鋁合金板電極之試料,以JIS Z2241中記載之1A號試驗片形狀分別切割出30根,使用英斯特朗(Instron)製造之拉伸試驗機,以表1中記載之應變速度使各試料拉伸變形10%後,去除荷重,藉此製作表面處理鋁材試料。所製作之試料係於後述之密接耐久性評價試驗與熱塑性樹脂之接合性評價試驗中使用。
對於以上述方式製作之表面處理鋁材試料,進行以下之測定及評價。
[多孔型鋁氧化膜層之小孔之平均最大徑之測定]
對於以上述方式製作之表面處理鋁材試料,藉由利用FE-SEM之表面觀察(觀察視野:0.7μm×1μm),測定多孔型鋁氧化膜層之小孔之平均最大徑。將結果示於表1中。此外,關於表1所示之小孔之平均最大徑,設為100個部位之小孔之測定結果之算術平均數。
[加工槽寬度及加工槽間隔之測定]
對於以上述方式製作之表面處理鋁材試料,藉由利用FE- SEM之表面觀察(觀察視野:10μm×7μm),測定鹼交流電解氧化膜之加工槽寬度及加工槽間隔。將結果示於表1中。此外,關於表中所示之加工槽寬度及加工槽間隔,設為100個部位之測定結果之算術平均數。
[多孔型鋁氧化膜層及阻隔型鋁氧化膜層之厚度]
對於以上述方式製作之表面處理鋁材試料,藉由TEM而實施沿著鹼交流電解氧化膜之縱方向之剖面觀察。具體而言,測定多孔型鋁氧化膜層及阻隔型鋁氧化膜層之各自之厚度。為了測定該等氧化膜層之厚度,使用超薄切片機,由供試材來製作剖面觀察用薄片試料。繼而,於該薄片試料中選擇觀察視野(1μm×1μm)中之任意之100個部位,藉由TEM剖面觀察而測定各個氧化膜層之厚度。將結果示於表1中。此外,關於該等氧化膜層之厚度,設為100個部位之測定結果之算術平均數。
[鹼交流電解氧化膜之密接耐久性評價]
準備20片供試材,該供試材係從以上述方式製作之表面處理鋁材試料(JIS 1A號試驗片)上,分別平行地切取縱50mm×橫25mm而得。此外,試料與供試材之縱橫相同。密接耐久性試驗係首先如圖3所示,將2片供試材15、16以縱方向之重疊長度成為10mm之方式重合(接著面積10mm×25mm=250mm2),使用添加有直徑200μm之玻璃珠之一液型環氧樹脂系接著劑17而接著,製作10組如上所述之接合體。繼而,將接著之接合體於加熱爐中以170℃加熱處理20分鐘,使接著劑硬化而形成密接耐久試驗用 之試驗片。
對以上述方式製作之試驗片進行鹽水噴霧試驗方法(JIS Z 2371)中記載之中性鹽水噴霧試驗,1000小時後取出,利用拉伸試驗機以5mm/min之速度於長度方向上拉伸,測定接著部分之接著劑之凝聚破壞率,以下述基準進行評價。
◎:凝聚破壞率係為95%以上者
○:凝聚破壞率係為85%以上且小於95%者
△:凝聚破壞率係為75%以上且小於85%者
×:凝聚破壞率係為小於75%者
將結果示於表2中。該表中分別示出10組供試材中之上述◎、○、△、×之個數,將全部由◎及○所構成之情形判定為合格,且將其以外之情形判定為不合格。
[熱塑性樹脂之接合性評價]
準備10片供試材,該供試材係從以上述方式製作之表面處理鋁材試料上切斷為縱50mm×橫10mm而得,使用含玻璃纖維之 PPS樹脂(DIC公司製造),藉由鋁合金板之嵌入成形而製作接合試驗片。於射出成形模具中嵌入表面處理鋁材試料,將模具關閉,對模具加熱,藉此將接合試驗片加熱至150℃後,以射出溫度320℃射出PPS樹脂,藉此獲得圖4所示之剪切試驗片狀之接合體。接合部設為表面處理鋁材試料端部之縱5mm×橫10mm部分。
如上所述,利用拉伸試驗機,將所製作之剪切試驗片狀接合體之10個以5mm/min.之速度進行拉伸,測定接著部分之接著劑即PPS樹脂18之凝聚破壞率,以下述基準進行評價。此外,圖4中,15為表面處理鋁材試料。
◎:凝聚破壞率係為95%以上者
○:凝聚破壞率係為85%以上且小於95%者
△:凝聚破壞率係為75%以上且小於85%者
×:凝聚破壞率係為小於75%者
將結果示於表2中。該表中分別示出10組剪切試驗片狀之接合體中之上述◎、○、△、×之個數,將全部包含◎或○之情形判定為合格,將其以外判定為不合格。
[綜合評價]
將上述鹼交流電解氧化膜之密接耐久性評價以及熱塑性樹脂之接合性評價之雙方合格者設為綜合評價合格,將該等各評價之至少任一不合格者設為綜合評價不合格。
如表2所示,實施例1~2中由於滿足本發明要件,故而鹼交流電解氧化膜之密接耐久性評價以及熱塑性樹脂之接合性 評價為合格,綜合評價亦為合格。
與此相對,比較例1~3中由於不滿足本發明要件,故而鹼交流電解氧化膜之密接耐久性評價以及熱塑性樹脂之接合性評價之任一者為不合格,綜合評價成為不合格。
具體而言,比較例1中,形成加工槽時之應變速度不足,產生與加工方向無關之龜裂。其結果為,密接耐久性評價成為不合格,綜合評價成為不合格。
比較例2中,形成加工槽時之應變速度變得過大,產生與加工方向平行之槽。其結果為,密接耐久性評價以及熱塑性樹脂之接合性評價成為不合格,綜合評價成為不合格。
比較例3中,代替交流電解處理而進行直流電解處理。其結果係為,未形成鹼交流電解氧化膜,密接耐久性評價以及熱塑性樹脂之接合性評價成為不合格,綜合評價成為不合格。
[產業上之可利用性]
依據本發明,可獲得與樹脂等被接合部件之密接耐久性優異、且加工配合度優異之表面處理鋁材。藉此,本發明之表面處理鋁材另外適合用於要求鋁基材與被接合部件之密接性以及加工配合度之本發明之強加工鋁/樹脂接合部件或樹脂塗裝鋁材。
1‧‧‧多孔型鋁氧化膜層
2‧‧‧阻隔型鋁氧化膜層
3‧‧‧鋁基材(之基底)
4‧‧‧小孔
5‧‧‧加工槽
6‧‧‧表面處理鋁材
7‧‧‧樹脂等被接合部件
8‧‧‧表面處理鋁材/被接合部件之接合體
Claims (18)
- 一種表面處理鋁材,包括鋁基材、以及形成於其表面之至少一部分上之鹼交流電解氧化膜,且於該鹼交流電解氧化膜上形成有與塑性加工方向垂直之複數個加工槽。
- 如請求項1之表面處理鋁材,其中該鹼交流電解氧化膜包括:形成於表面側之厚度20~1000nm之多孔型鋁氧化膜層、以及形成於基底側之厚度3~30nm之阻隔型鋁氧化膜層。
- 如請求項2之表面處理鋁材,其中於該多孔型鋁氧化膜層上,形成有平均最大徑5~120nm之小孔。
- 如請求項3之表面處理鋁材,其中相對於該多孔型鋁氧化膜層之表面積,全部該小孔之面積佔有率係為5~50%。
- 如請求項3之表面處理鋁材,其中該多孔型鋁氧化膜層中之該小孔之平均最大徑係為5~120nm。
- 如請求項1至5中任一項之表面處理鋁材,其中該加工槽之寬度係為5~5000nm。
- 如請求項1至5中任一項之表面處理鋁材,其中該加工槽之間隔係為5~5000nm。
- 一種表面處理鋁材之製備方法,其係如請求項1至7中任一項之表面處理鋁材之製備方法,其中:使用經表面處理之鋁基材之電極與對電極,將鹼性水溶液作為電解液而進行交流電解處理後,以應變速度1.0×10-3~1.0×103/s對經交流電解處理之鋁基材實施塑性加工。
- 如請求項8之表面處理鋁材之製備方法,其中該鹼性水溶液之電解液之溫度係為30~90℃。
- 如請求項8或9之表面處理鋁材之製備方法,其中該鹼性水溶液之電解液之pH值係為9~13。
- 如請求項8或9之表面處理鋁材之製備方法,其中該交流電解處理之電解處理時間係為5~600秒。
- 如請求項8或9之表面處理鋁材之製備方法,其中該交流電解處理之電流密度係為4~50A/dm2。
- 如請求項8或9之表面處理鋁材之製備方法,其中該交流電解處理之頻率係為10~100Hz。
- 如請求項8或9之表面處理鋁材之製備方法,其中電極中所使用之該鋁基材之拉伸強度係為30~450MPa。
- 如請求項8或9之表面處理鋁材之製備方法,其中將該鋁基材保持於0~300℃,直至對經該交流電解處理之鋁基材進行塑性加工為止。
- 一種表面處理鋁材/被接合部件之接合體,其包括:如請求項1至7中任一項之表面處理鋁材、以及其鹼交流電解氧化膜側之被接合部件。
- 如請求項16之表面處理鋁材/被接合部件之接合體,其中該被接合部件係為樹脂。
- 一種表面處理鋁材/被接合部件之接合體之製備方法,其係如請求項17之表面處理鋁材/被接合部件之接合體之製備方法,其 中:將成為該被接合部件之樹脂加熱而成為流動狀態,接觸‧滲透於多孔性鋁氧化膜層中,藉此使該流動狀態之樹脂流入至小孔及加工槽中,將流動狀態之樹脂冷卻固化或硬化。
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