TWI452953B - Copper cladding for printed circuit boards and copper clad laminates for printed circuit boards - Google Patents
Copper cladding for printed circuit boards and copper clad laminates for printed circuit boards Download PDFInfo
- Publication number
- TWI452953B TWI452953B TW098118522A TW98118522A TWI452953B TW I452953 B TWI452953 B TW I452953B TW 098118522 A TW098118522 A TW 098118522A TW 98118522 A TW98118522 A TW 98118522A TW I452953 B TWI452953 B TW I452953B
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- copper foil
- nickel
- zinc
- printed circuit
- layer
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/38—Improvement of the adhesion between the insulating substrate and the metal
- H05K3/382—Improvement of the adhesion between the insulating substrate and the metal by special treatment of the metal
- H05K3/384—Improvement of the adhesion between the insulating substrate and the metal by special treatment of the metal by plating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/321—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
- C23C28/3455—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer with a refractory ceramic layer, e.g. refractory metal oxide, ZrO2, rare earth oxides or a thermal barrier system comprising at least one refractory oxide layer
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/565—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of zinc
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0614—Strips or foils
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
- H05K2201/0203—Fillers and particles
- H05K2201/0206—Materials
- H05K2201/0239—Coupling agent for particles
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/03—Conductive materials
- H05K2201/0332—Structure of the conductor
- H05K2201/0335—Layered conductors or foils
- H05K2201/0355—Metal foils
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/07—Treatments involving liquids, e.g. plating, rinsing
- H05K2203/0703—Plating
- H05K2203/0723—Electroplating, e.g. finish plating
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12431—Foil or filament smaller than 6 mils
- Y10T428/12438—Composite
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
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- Mechanical Engineering (AREA)
- Electrochemistry (AREA)
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- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Parts Printed On Printed Circuit Boards (AREA)
- Manufacturing Of Printed Wiring (AREA)
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- Electroplating Methods And Accessories (AREA)
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- Other Surface Treatments For Metallic Materials (AREA)
Description
本發明,係關於一種耐藥品性及接著性優異之印刷電路基板用銅箔及印刷電路基板用覆銅積層板,特別是關於一種在銅箔之至少與樹脂的接著面,具有含有鎳與鋅或此等化合物之層(以下,稱為「鎳鋅層」。),並在該層上具有鉻酸鹽被膜層、及進一步視需要所設之矽烷偶合劑層的印刷電路基板用銅箔及使用該銅箔所製成之印刷電路基板用覆銅積層板。
半導體封裝基板為印刷電路基板之一種,係用於構裝半導體IC晶片、其他半導體元件之印刷電路基板。形成於半導體封裝基板之電路由於較通常之印刷電路基板微細,因此基板材料係使用與一般印刷電路基板不同之樹脂基材。
半導體封裝基板,通常藉由下列步驟來製作。首先,在高溫高壓下將銅箔積層接著於合成樹脂等之基材。將此稱為覆銅積層板或僅稱為積層板。接著,為了將作為目標之導電性電路形成於積層板上,係藉由耐蝕刻性樹脂等材料,將與電路相同之圖案印刷於銅箔上。然後,藉由蝕刻處理將所露出之銅箔的不要部分加以去除。
蝕刻後,去除印刷部而在基板上形成導電性電路。最後將規定之元件焊接於所形成之導電性電路,而形成電子元件用之各種印刷電路基板。最後,與抗蝕劑或增層(buildup)樹脂基板接合。
一般,對印刷電路基板用銅箔之品質要求,在與樹脂基材接著之接著面(所謂粗化面)及非接著面(所謂光澤面)並不相同,必須同時滿足兩者。
對光澤面之要求,係要求(1)外觀良好及保存時沒有氧化變色現象,(2)焊料潤濕性良好,(3)高溫加熱時沒有氧化變色現象,(4)與抗蝕劑之密合性良好等。
而另一方面,對於粗化面,主要可舉出(1)在保存時沒有氧化變色現象,(2)即使在經過高溫加熱、濕式處理、焊接、藥品處理等後,與基材之剝離強度仍高,(3)在經過與基材之積層、蝕刻後,沒有生成所謂積層污點等。
又,近年來隨著電路印刷圖案的微細化,亦要求銅箔表面的低粗度化。
並且,於電腦或行動通訊等電子機器中,隨著通訊之高速化、大容量化,電氣訊號朝高頻化邁進,故要求可因應上述需求之印刷電路基板及銅箔。若電氣訊號之頻率在1GHz以上時,則電流流過導體表面之集膚效應(skin effect)的影響變得顯著,而無法忽視表面之凹凸導致電流傳遞路徑產生變化、阻抗(Impedance)變大之影響。考量此點,亦希望銅箔之表面粗糙度小。
為了因應此要求,而提出了許多對印刷電路基板用銅箔之表面處理方法。
壓延銅箔與電解銅箔的表面處理方法有所不同,電解銅箔之表面處理方法之一例如下所述。
亦即,首先,為了提高銅與樹脂基材之接著力(剝離強度),一般係將銅與氧化銅所構成之微粒附著於銅箔表面(粗化處理),然後為了使銅箔具有耐熱特性,而形成黃銅或鋅等耐熱層(障壁層)。
又,最後為了防止在運送時或保存時發生表面氧化等現象,係施以藉由浸漬或電解所進行之鉻酸鹽處理或電解鋅鉻酸鹽處理等防鏽處理,藉此製成製品。
其中,尤以形成耐熱層之表面處理方法為決定銅箔表面性狀之重要關鍵。因此,形成耐熱層之金屬或合金可舉出如Zn、Cu-Ni合金、Cu-Co合金及Cu-Zn合金等,而形成有Zn、Cu-Ni合金、Cu-Co合金及Cu-Zn合金等之被覆層之大部分的銅箔已實用化(例如,參照專利文獻1)。
此等之中,形成有Cu-Zn合金(黃銅)所構成之耐熱層的銅箔使用在由環氧樹脂等所構成之印刷電路基板時,由於具有樹脂層無污點,且經高溫保持印刷電路基板後之銅箔的剝離強度劣化少等優異特性,因此在工業上廣為使用。關於形成由此黃銅所構成之耐熱層的方法,詳述於專利文獻2。
近年來,於印刷電路基板,特別是封裝基板之製造步驟中,為了提高抗蝕劑或增層樹脂基板與為電路面之銅箔之光澤面的密合性,係使用以硫酸、過氧化氫混合液進行軟蝕刻(soft etching)來將銅箔光澤面加以粗面化之處理。
然而,若以上述硫酸、過氧化氫混合液來對印刷電路基板(係使用形成有由黃銅所構成之耐熱層的銅箔)之銅箔電路光澤面進行軟蝕刻,則會發生先前所形成之電路圖案兩側端部(邊緣部)之侵蝕(電路侵蝕)現象,而產生與樹脂基材之剝離強度劣化的問題。
此電路侵蝕現象,係指銅箔電路與樹脂基材之接著邊界層,亦即露出由黃銅所構成之耐熱層的電路側面被上述硫酸、過氧化氫混合液所侵蝕,而因此導致通常應呈現黃色(由黃銅所構成之故)之電路的端部附近的粗化面側呈現紅色,此部分之銅箔的剝離強度顯著劣化的現象。又,若整個電路圖案均發生此現象時,電路圖案將會自基材剝離,而成為嚴重之問題。
專利文獻1:日本特公昭51-35711號公報
專利文獻2:日本特公昭54-6701號公報
本發明之課題,在於開發一種在不會使其他諸特性劣化下,可提高將銅箔與樹脂基材加以積層所製成之印刷電路基板之銅箔的常態剝離強度、及以高溫將印刷電路板保持規定時間後的剝離強度(以下,稱為耐熱剝離強度),且適用作為上述電路侵蝕現象經減少之半導體封裝基板用的銅箔。特別是在於當將銅箔積層於樹脂基材,大幅提升耐熱剝離強度,且使用硫酸、過氧化氫系蝕刻液對電路進行軟蝕刻時,確立可有效防止電路侵蝕現象之銅箔的表面處理技術。
為了解決上述課題,本發明人對在銅箔上進行表面處理之條件等經過潛心研究的結果,發現在進行以下之銅箔的耐熱剝離強度提升及耐硫酸、過氧化氫性,亦即以硫酸、過氧化氫混合液所進行之銅箔光澤面的軟蝕刻時,對銅箔反側之粗化面的耐侵蝕性(耐電路侵蝕性)有效。
由以上,本發明提供:1)一種印刷電路基板用銅箔,係在銅箔之粗化面,具備含有鎳與鋅或此等化合物之層(以下,稱為「鎳鋅層」),以及在該層上,具備鉻酸鹽被膜層,其特徵在於,該鎳鋅層之銅箔每單位面積的鋅附著重量在180μg/dm2
以上、3500μg/dm2
以下,鍍敷被膜中之鎳重量比率{鎳附著重量/(鎳附著重量+鋅附著重量)}在0.38以上、0.7以下。
2)如1)所記載之印刷電路基板用銅箔,其中,該{鎳附著重量/(鎳附著重量+鋅附著重量)}在0.4以上、0.55以下。
3)如1)或2)之任一項所記載之印刷電路基板用銅箔,其中,該鉻酸鹽被膜層之銅箔每單位面積的鉻附著重量在30μg/dm2
以上、100μg/dm2
以下。
4)如1)至3)中任一項所記載之印刷電路基板用銅箔,其中,該鎳鋅層所含有之全部鋅中,以鋅氧化物或鋅氫氧化物之形態存在之鋅佔有45~90%。
5)如1)至3)中任一項所記載之印刷電路基板用銅箔,其中,該鎳鋅層所含有之全部鎳中,以鎳氧化物或鎳氫氧化物之形態存在之鎳佔有60~80%。
6)如1)至5)中任一項所記載之印刷電路基板用銅箔,其中,在該鉻酸鹽層上,進一步具備矽烷偶合劑層。
7)如1)至6)中任一項所記載之印刷電路基板用銅箔,其中,銅箔為電解銅箔,粗化面為電鍍時之粗面、或是對此粗面進一步施以粗化處理之面、或是對電解銅箔之光澤面施以粗化處理之面。
8)如1)至6)中任一項所記載之印刷電路基板用銅箔,其中,銅箔為壓延銅箔,粗化面為對該壓延銅箔施以粗化處理之面。
9)一種印刷電路基板用覆銅積層板,係將1)至8)中任一項所記載之印刷電路基板用銅箔與印刷電路基板用樹脂基材加以貼合而製成。
如以上所示,本發明之印刷電路基板用銅箔,為了不使印刷電路基板經高溫保持後之銅箔的剝離強度發生劣化,係使用鎳鋅層,而並不使用被認為是以往所需要件之由黃銅所構成的耐熱層。
藉此,可大幅地提升銅箔之耐熱剝離強度。且,藉此可得到能夠有效防止因藥品所造成之電路侵蝕現象,特別是能夠提升耐硫酸、過氧化氫性之新穎的特性,作為印刷電路基板用銅箔(特別是半導體封裝基板用銅箔)、以及將銅箔與樹脂基材加以貼合所製成之覆銅積層板(特別是半導體封裝基板用覆銅積層板)極為有效。當然,亦可使用作為一般之印刷電路基板用銅箔。
接著,為了容易理解本發明,係具體且詳細地對本發明進行說明。
本發明之銅箔,雖然電解銅箔及壓延銅箔皆可使用,但是在電解銅箔之情形時,可適用在電鍍時之粗面。又,並且可對此粗面進一步施以粗化處理。例如,為了提升樹脂基材與積層後之銅箔的剝離(peel)強度,係在脫脂後之銅箔表面施以粗化處理(例如銅之「瘤」狀電沉積)的電解銅箔,並可直接使用之。
一般,於鼓式電解銅箔製造裝置,一側(鼓側)為光澤面,相反側則為粗面。而於壓延銅箔,則為任一側皆具有光澤之壓延面。於本發明中,雖然電解銅箔具有粗面與光澤面,但為粗面時,則可直接加以使用。而電解銅箔之光澤面,為了進一步提高剝離強度,係施以粗化處理,形成粗化面。
於壓延銅箔,亦同樣地施以粗化處理。粗化處理,無論是何種情形,皆可使用業已公知之粗化處理,並無特別限制。
本發明之粗化面,係指電解銅箔之電鍍時的粗面,及施有粗化處理之電解銅箔或壓延銅箔的粗化處理面,可適用於所有之銅箔。
首先,對半導體封裝基板用銅箔,並不設置以往即被認為是必須之黃銅被覆層。以往,若無黃銅被覆層,雖會擔心印刷電路基板在高溫下保持一定時間後其銅箔之剝離強度(耐熱剝離強度)會發生下降等之特性下降,但形成鎳鋅層來代替黃銅被覆層,以提升耐熱剝離強度。因此,於本發明中,不在以往被認為是常識之銅箔上形成黃銅被覆層,係重要特徵之一。
鎳鋅層,並非均勻之鎳-鋅合金,而是包含鎳及鋅之一部份為氧化物或氫氧化物者,例如,包含含有表面氧化膜或氫氧化膜之鎳鋅層者。
如上述,本發明之半導體封裝基板用銅箔,係由形成在銅箔之粗化面(為與樹脂之接著面)的鎳鋅層、鉻酸鹽被膜層及視需要所設之矽烷偶合劑層所構成。銅箔,可使用上述之壓延銅箔或電解銅箔。又鉻酸鹽被膜層,可使用電解鉻酸鹽被膜層或浸漬鉻酸鹽被膜層。
本發明,如上述,例如係在銅箔之粗化面,形成含有鎳與鋅或此等化合物之層(以下,稱為「鎳鋅層」。),惟必須使上述鎳鋅層之銅箔每單位面積的鋅附著重量在180μg/dm2
以上、3500μg/dm2
以下。若鋅附著重量未達180μg/dm2
,則高溫加熱後之剝離強度的劣化將會加劇。又,若鋅附著重量在3500μg/dm2
以上時,則硫酸、過氧化氫系蝕刻液所造成之電路端部的侵蝕將會變得顯著。
必須使{鎳附著重量/(鎳附著重量+鋅附著重量)}在0.38以上、0.7以下。若未達0.38,則無法有效防止電路侵蝕現象。又,若在0.7以上,則耐熱剝離強度將會降低。
鎳鋅層,通常係以下述條件來形成。然而,只要是可達成鎳鋅層之每單位面積的鋅附著重量在180μg/dm2
以上、3500μg/dm2
以下,{鎳附著重量/(鎳附著重量+鋅附著重量)}在0.38以上、0.7以下之電鍍條件的話,則並無特別限制,亦可使用其他的電鍍條件。
使Ni:10g/L~30g/L,Zn:1g/L~15g/L,硫酸(H2
SO4
):1g/L~12g/L為基本鍍浴。
並視需要,添加氯化物離子:1g/L~5g/L。
接著,此鉻酸鹽被膜層之製作,鉻酸鹽處理可適用電解鉻酸鹽處理、浸漬鉻酸鹽處理、及鉻酸鹽鍍浴中含有鋅之鋅鉻酸鹽處理。
無論是在任何一種情形,若鉻附著重量未達30μg/dm2
,則由於增加耐酸性與耐熱性之效果少,因此使鉻附著重量在30μg/dm2
以上。又,若鉻附著重量超過100μg/dm2
時,則鉻酸鹽處理之效果將會飽和,鉻附著重量無法再增加。若總結此等,則鉻酸鹽處理層中每單位面積之鉻附著重量較佳為30~100μg/dm2
。
用以形成上述鉻酸鹽被膜層之條件之例記載如下。然而,如上述,並不必受到此條件之限制,業已公知之鉻酸鹽處理皆可使用。
一般,浸漬鉻酸鹽處理之情形,可達成每單位面積之鉻附著重量30~40μg/dm2
。又,電解鉻酸鹽處理之情形,則可達成每單位面積之鉻附著重量30~100μg/dm2
。
此防銹處理,係會對銅箔之耐酸性與耐熱性造成影響的因素之一,藉由鉻酸鹽處理,由於可更加提升銅箔之耐藥品性與耐熱性,因此為有效。
CrO3
或K2
Cr2
O7
:1~12g/L,Zn(OH)2
或ZnSO4
.7H2
O:0~10g/L,Na2
SO4
:0~20g/L,pH 2.5~12.5,溫度:20~60℃,時間:0.5~20秒
CrO3
或K2
Cr2
O7
:1~12g/L,Zn(OH)2
或ZnSO4
.7H2
O:0~10g/L,Na2
SO4
:0~20g/L,pH 2.5~12.5,溫度:20~60℃,電流密度0.5~5A/dm2
,時間:0.5~20秒
本發明之印刷電路基板用銅箔所使用之矽烷偶合劑,較佳為,至少含有四烷氧矽烷、與具備有具有與樹脂之反應性之官能基的烷氧矽烷之1種以上。此矽烷偶合劑之選擇亦為任意,但較佳為考慮與樹脂之接著性來加以選擇。
並且,本發明,提供一種上述1)~8)之任一項所記載之印刷電路基板用銅箔,及9)所記載之將印刷電路基板用銅箔與樹脂基材加以貼合所製成之覆銅積層板。
接著,於此防銹層上,施以矽烷偶合劑處理(塗布後,乾燥)。
矽烷偶合劑處理之條件如下述。
將含有0.2體積%之環氧矽烷(epoxysilane)與0.4體積%之TEOS(四乙氧矽烷)的水溶液調整成pH5,進行塗布,然後加以乾燥。
使用將上述方式所製成之銅箔與下述之樹脂基材加以積層接著而成的印刷電路基板,實施各試驗,進行銅箔與樹脂基材之密合性的評價、與每單位面積之鎳及鋅的鍍敷附著重量的測定。又,藉由XPS(X射線光電子光譜法)來測定鎳鋅層中所含有之鎳及鋅之價數為0的金屬狀態與價數為2的氧化狀態的存在比。
與銅箔積層之樹脂基材,係使用以下之2種類。
BT樹脂(三氮雜苯一雙馬來亞醯胺系樹脂,商標名:三菱瓦斯化學股份有限公司製GHPL-802)另,BT樹脂,耐熱性高,係半導體封裝用印刷電路基板所使用之材料。
對將銅箔形成有鎳鋅層之面與FR-4樹脂基材加以積層所製成的積層板上的銅箔進行蝕刻,在積層板上形成10mm寬的銅箔電路。將此電路加以剝離,測定常態剝離強度。接著,測定將上述形成有10mm寬之銅箔電路的積層板於大氣中以180℃加熱2天後之剝離強度(以下稱為耐熱剝離強度)、以及與該常態剝離強度相較之相對劣化率(損耗%)。FR-4基板若與BT基板相比較,則耐熱性顯得較差。因此,當使用FR-4基板時,若具有良好的耐熱剝離強度與低劣化率,則使用BT基板時,亦會具有充分的耐熱剝離強度與劣化率。
對將銅箔形成有鎳鋅層之面與BT樹脂基材加以積層所製成的積層板上的銅箔進行蝕刻,在積層板上形成0.4mm寬的銅箔電路。將此電路加以剝離,測定常態剝離強度。接著,使用上述形成有0.4mm寬之銅箔電路的積層板,進行耐硫酸、過氧化氫性試驗。
此試驗,係將積層板上之銅箔電路浸漬於含有硫酸100~400g/L、過氧化氫10~60g/L的蝕刻液,將銅箔電路厚度蝕刻掉2μm後,測定剝離強度以及與該常態剝離強度相較之相對劣化率(損耗%)。
此時之剝離強度的測定,可說是在過份嚴酷的環境下,當使用FR-4基板時,係較一般所進行之耐藥品性的評價更加過份嚴酷的條件。因此,當使用BT基板時,若具有良好的耐硫酸、過氧化氫性,則FR-4基板亦會具有充分的耐藥品性(特別是耐硫酸、過氧化氫性)。
使銅箔形成有鎳鋅層之面以露出於表面的方式與FR-4樹脂基材積層,製作積層板。接著,以鹽酸或硝酸將露出於積層板表面之鎳鋅層與其母層之銅加以溶解,藉由進行溶解液中之鎳及鋅濃度的化學分析,來測定每單位面積之鎳及鋅的附著重量。
使用XPS(X射線光電子光譜法),來測定鎳鋅層中所含有之鎳及鋅之價數為0的金屬狀態與價數為2的氧化狀態的存在比。測定,係一邊藉由氬離子濺鍍對銅箔厚度進行蝕刻,一邊從最表面至銅層(為鎳鋅層之基底)為止間歇地進行,在自最表面起之深度,將各深度所得之氧化狀態之鎳及鋅的存在比加以積分,藉此計算出氧化鎳及氧化鋅(皆包含氫氧化物)在鎳鋅層全體的平均存在比。
測定所使用之機器為KRATOS公司製造之AXIS-HS,氬離子濺鍍的輸出為52.5W。於此條件下,銅箔厚度會在1分鐘被蝕刻掉約20。濺鍍時間係以15~100分鐘之條件進行。
接著,說明實施例及比較例。其結果示於以下各表。另,本實施例僅為表示較佳之一例者,本發明並不限定於此等之實施例。因此,包含於本發明之技術思想的變形、其他之實施例或態樣,全部包含於本發明。
另,為了與本發明進行比對,係揭露有比較例。
使用厚度12μm之電解銅箔,以下述所表示之條件,藉由電鍍將鎳鋅層形成在此銅箔的粗化面(表面平均粗糙度:3.8μm)。每單位面積之鎳及鋅的鍍敷附著重量與鍍敷被膜中的鎳重量比率示於表1。
(電鍍液組成)Ni:13g/L,Zn:5g/L,硫酸(H2
SO4
):8.5g/L
(電流密度)20A/dm2
(鍍敷時間)0.5~10秒
並且,在此鎳鋅層上,進行鉻酸鹽處理,形成防銹層。
以下表示處理條件。
CrO3
:4.0g/L,ZnSO4
.7H2
O:2.0g/L,Na2
SO4
:15g/L,pH:4.2,溫度:45℃,電流密度3.0A/dm2
,時間:1.5秒
由於電流密度固定(20A/dm2
),因此鍍敷附著重量係隨著鍍敷時間而變化。鍍敷時間係在0.5~10秒之範圍來進行處理。每單位面積之鋅的附著重量為194~3381μg/dm2
,鍍敷被膜中之鎳重量比率為37~52重量%。此等之條件,皆在本發明之範圍。
於FR-4基板之常態剝離強度為1.53~1.68kN/m,耐熱剝離強度為1.45~1.65kN/m,劣化率在5%以下之範圍,皆顯示出良好的常態剝離強度與耐熱剝離強度。另一方面,於BT基板之常態剝離強度為1.04~1.24kN/m之範圍。以硫酸、過氧化氫混合液處理後的剝離強度為0.91~1.09kN/m,劣化率為10~13%,顯示出良好之性質。
然而,於比較例1中,鋅之每單位面積的附著重量為159μg/dm2
,並不符合本發明。於此比較例1中,於FR-4基板之常態剝離強度為1.51kN/m,耐熱剝離強度為0.69kN/m,劣化率為54%,耐熱剝離強度大幅下降。
另一方面,於比較例2中,鋅的附著量為3909μg/dm2
,並不符合本發明。於此比較例2中,於BT基板(過份嚴酷之環境下)之常態剝離強度為1.10kN/m,以硫酸、過氧化氫混合液處理後的剝離強度為0.93kN/m,劣化率為16%,具有必要充分之特性。然而,由於Ni之附著重量變多,故在形成銅箔電路時,Ni未受到蝕刻而殘留下來,成為電路不良的原因。因此,作為印刷電路基板用銅箔之表面處理並不適當,比較例2並不符合本發明。
由以上,於本實施例1~7中,FR-4基板具有良好的剝離強度與耐熱剝離強度,BT基板之耐硫酸、過氧化氫性試驗顯示出良好的耐藥品性。因此,於本實施例中,高溫加熱後之剝離強度的劣化少,且可理解保有可大幅改善電路侵蝕現象之有效特性。
特別是在將樹脂基材與銅箔加以積層,並使用硫酸、過氧化氫系蝕刻液對電路進行軟蝕刻時,可得到能夠有效防止電路侵蝕現象的銅箔表面處理技術。
以下述所示之條件,改變電流密度,形成鎳鋅層。每單位面積之鎳及鋅的鍍敷附著重量、與鍍敷被膜中之鎳重量比率示於表2。
(電流密度)3~40A/dm2
(鍍敷時間)0.5~10秒
上述電流密度以外之製造條件,係與實施例1~7相同。基板之種類及剝離強度之測定亦為與實施例1~7相同的條件。此結果同樣地示於表2。
鍍敷附著重量如表2所示,每單位面積之鋅的附著重量為330~724μg/dm2
,鍍敷被膜中之鎳重量比率為43~52重量%。此等之條件,皆在本發明之範圍。
若電流密度低於3A/dm2
,則由於不會生成鎳鋅層,故作為本案之鎳鋅層的鍍敷條件並不適當。又,若電流密度超過40A/dm2
,則由於在陰極(銅箔)會產生大量的氫,電流效率會變得極低,故作為鎳鋅層的處理條件並不適當。因此,形成本案之鎳鋅層時的電流密度,較佳為3~40A/dm2
。
於FR-4基板之常態剝離強度為1.48~1.56kN/m,耐熱剝離強度為1.40~1.52kN/m,劣化率在7%以下的範圍,皆顯示出良好的常態剝離強度與耐熱剝離強度。
另一方面,於BT基板之常態剝離強度為0.92~1.04kN/m,以硫酸、過氧化氫混合液處理後的剝離強度為0.88~0.98kN/m,劣化率為3~11%,顯示出良好的性質。
由以上,於本實施例8~13中,FR-4基板具有良好的剝離強度與耐熱剝離強度,BT基板則顯示出良好的耐硫酸、過氧化氫性。因此,於本實施例中,高溫加熱後之剝離強度的劣化少,可理解保有可大幅改善電路侵蝕現象之有效特性。
接著,說明鍍敷被膜中之Ni重量比率的範圍。作為一例,實施例1、7、14及比較例3、4示於表3。又,每單位面積之鎳及鋅的鍍敷附著重量與鍍敷被膜中的鎳重量比率示於表3。
上述以外之製造條件,係與實施例1~13相同。基板之種類及剝離強度之測定亦為與實施例1~13相同的條件。此結果同樣地示於表3。鍍敷被膜中的Ni重量比率為0.38~0.54。
於FR-4基板之常態剝離強度為1.54~1.64kN/m,耐熱剝離強度為1.42~1.65kN/m,劣化率在8%以下的範圍,皆顯示出良好的常態剝離強度與耐熱剝離強度。
另一方面,於BT基板之常態剝離強度為1.04~1.20kN/m,以硫酸、過氧化氫混合液處理後的剝離強度為0.91~1.08kN/m,劣化率為13~15%,顯示出良好的性質。
然而,於比較例3中,Ni重量比率為0.37,並不符合本發明。於此比較例3中,於FR-4基板之常態剝離強度為1.39kN/m,耐熱剝離強度為0.97kN/m,劣化率為30%,耐熱剝離強度大幅下降。
另一方面,於比較例4中,Ni重量比率為0.76,並不符合本發明。於此比較例4中,於FR-4基板之常態剝離強度為1.50kN/m,耐熱剝離強度為1.02kN/m,劣化率為32%,與比較例3同樣地,耐熱剝離強度大幅下降。
因此,鍍敷被膜中的Ni重量比率的範圍,較佳為0.38~0.70,更佳為0.40~0.54。
以下述所示之條件,改變鍍敷浴組成,形成鎳鋅層。每單位面積之鎳及鋅的鍍敷附著重量與鍍敷被膜中的鎳重量比率示於表4。在此,與實施例1~14不同之處在於改變鍍敷浴之成分組成。
實施例15~19之鍍敷浴的成分組成表示如下。
(實施例15之鍍敷液組成)Ni:10g/L,Zn:1g/L,硫酸(H2
SO4
):8.5g/L。
(實施例16之鍍敷液組成)Ni:20g/L,Zn:8g/L,硫酸(H2
SO4
):1g/L。
(實施例17之鍍敷液組成)Ni:25g/L,Zn:12g/L,硫酸(H2
SO4
):12g/L。
(實施例18之鍍敷液組成)Ni:30g/L,Zn:15g/L,硫酸(H2
SO4
):8.5g/L。
(實施例19之鍍敷液組成)Ni:10g/L,Zn:1g/L,硫酸(H2
SO4
):6g/L,氯化物離子:5g/L。
(電流密度)20~25A/dm2
(鍍敷時間)1~8秒
上述以外之製造條件,係與實施例1~7相同。基板之種類及剝離強度之測定亦為與實施例1~7相同的條件。此結果同樣地示於表4。
每單位面積之鋅的附著重量為320~817μg/dm2
,鍍敷被膜中之鎳重量比率為44~50重量%。此等之條件,皆在本發明之範圍。
於FR-4基板之常態剝離強度為1.52~1.62kN/m,耐熱剝離強度為1.47~1.59kN/m,劣化率為7%以下之範圍,皆顯示出良好的剝離強度與耐熱剝離強度。
另一方面,於BT基板之常態剝離強度為0.98~1.09kN/m。以硫酸、過氧化氫混合液處理後的剝離強度為0.89~0.97kN/m,劣化率為8~17%,顯示出良好之性質。
由以上,於本實施例15~19中,FR-4基板具有良好的剝離強度與耐熱剝離強度,BT基板則顯示出良好的耐硫酸過氧化氫性。因此,於本實施例中,高溫加熱後之剝離強度的劣化少,可理解保有可大幅改善電路侵蝕現象之有效特性。
由以上,在製作本發明之鎳鋅層時的鍍敷浴的條件,較佳為鎳濃度10~30g/L,鋅濃度1~15g/L,硫酸濃度1~12g/L,氯化物離子0~5g/L。若不在此等之濃度範圍,鎳或鋅濃度變濃,則由於會對廢水處理造成影響,因此作為鍍敷浴之條件並不佳。又,若成分濃度偏低時,則除了會因鍍敷之濃度變化等的主要原因造成鍍敷浴的管理困難以外,而且電流效率會極度降低,因此作為鍍敷浴之條件並不佳。
在此,說明改變鉻酸鹽處理之方法時的實施例。
本實施例,係以與實施例1-7相同所示的條件,來形成鎳鋅層。為了進行比較,電流密度與鍍敷時間係為相同的條件(電流密度20A/dm2
,鍍敷時間1.8秒)。每單位面積之鎳及鋅的鍍敷附著重量與鍍敷被膜中之鎳及鋅的重量比率,同樣地示於表5。
在此,與實施例1~7不同之處,在於改變鉻酸鹽處理之條件。於實施例1~7中,進行有電解鋅鉻酸鹽處理。實施例20~22之鉻酸鹽處理的條件如下述。
(實施例20之鉻酸鹽處理)此係在鉻酸鹽浴中不含有鋅之電解鉻酸鹽處理。
CrO3
:6.0g/L,pH:10.0,溫度:25℃,電流密度:2A/dm2
,時間:2秒。
(實施例21之鉻酸鹽處理)此係電解鋅鉻酸鹽處理。
CrO3
:1.5g/L,ZnSO4
.7H2
O:1.0g/L,Na2
SO4
:10g/L,pH:4.5,溫度:50℃,電流密度:1.5A/dm2
,時間:2秒。
(實施例22之鉻酸鹽處理)此係浸漬鋅鉻酸鹽處理。
CrO3
:3.5g/L,ZnSO4
.7H2
O:2.4g/L,Na2
SO4
:15g/L,pH:4.2,溫度:40℃,時間:10秒。
基板之種類及剝離強度之測定為與實施例1~7相同的條件。此結果同樣地示於表5。
如表1所示,實施例20~22,鋅之附著量為347~552μg/dm2
,Ni比率為43~47重量%。此等之條件皆在本發明之範圍。於FR-4基板之常態剝離強度為1.48~1.54kN/m,耐熱剝離強度為1.43~1.50kN/m,劣化率為3%以下之範圍,皆顯示出良好的剝離強度。
另一方面,於BT基板之常態剝離強度為1.01~1.08kN/m,以硫酸、過氧化氫混合液處理後的剝離強度為0.83~0.98kN/m,劣化率為8~17%,顯示出良好的性質。
由以上,於本實施例20~22中,FR-4基板具有良好的剝離強度與耐熱性,BT基板顯示出良好的耐硫酸、過氧化氫性。因此,於本實施例,高溫加熱後之剝離強度的劣化少,可理解藉由選擇基板與蝕刻液,可保有可大幅改善電路侵蝕現象之有效特性。
從實施例20~22可知,本案之形成有鎳鋅層之銅箔的耐熱性與耐藥品性,由於不會受到鉻酸鹽處理之種類的影響,因此可適用各種鉻酸鹽處理作為防銹處理。
從以上之實施例及比較例可知,本發明幾乎不會發生因硫酸、過氧化氫液所造成之粗化面的侵蝕,高溫加熱後之剝離強度的劣化少等,在不會降低以往之由黃銅所構成之耐熱處理層的特性下,可大幅改善電路侵蝕現象。
接著,說明本案之鎳鋅層所含之鎳及鋅的化學狀態。
於一般合金鍍敷被膜,構成被膜之金屬元素為合金化,僅存在於最表層之極小部分的金屬元素因與大氣接觸而呈氧化狀態。
然而,若根據XPS之測定結果,本案之鎳鋅層並非鎳鋅合金本身,被膜中之鎳及鋅具有0價之金屬狀態與2價之氧化狀態(氧化物或氫氧化物)不僅共存於最表層且還共存於銅之基底的構造。例如於實施例14中,被膜中之全部鎳中,為氧化物或氫氧化物之化學形態者佔55%,被膜中之全部鋅中,呈2價之氧化狀態者佔72%。
本案之藉由表面處理所得之鎳鋅層,被膜中之全部鋅中,可確認為氧化物或氫氧化物之化學形態者的比率範圍為45~90%,同樣地被膜中之全部鎳中,為氧化物或氫氧化物之化學形態者的比率範圍為60~80%。如實施例所示,可確認於此種構成下,可發揮所欲之特性與效果。本發明,係包含此等之條件全部者。
於上述中,雖對適用於電解銅箔之粗化面之情形進行說明,但是當然地亦同樣適用於光澤面經施以粗化處理之電解銅箔。並且經施以粗化處理之壓延銅箔亦相同。若使用電解銅箔及壓延銅箔之粗化面,雖然會因粗化處理之形狀、表面粗糙度的不同,使得常態剝離強度之絕對值產生不同,但是可降低耐熱剝離強度及硫酸、過氧化氫水處理後之剝離強度與常態剝離相較的相對劣化率。
於本發明之印刷電路基板用銅箔,特別是將選擇鎳鋅層之最佳條件作為發明之中心課題。藉此,以大幅提升銅箔之耐熱剝離強度,且有效防止電路侵蝕現象,使耐硫酸、過氧化氫性恆常穩定地發揮效力。
因此,應可容易理解電解銅箔及壓延銅箔之選擇或粗化面之選擇,可視目的來任意地加以選擇。
如以上所示,本發明之印刷電路基板用銅箔,為了不使高溫加熱後與樹脂之剝離強度劣化,故係使用鎳鋅層,而可大幅提升銅箔之耐熱剝離強度。又,藉此能夠賦予可有效防止電路侵蝕現象,可使耐硫酸、過氧化氫性恆常穩定地發揮效力之新穎特性,近年來印刷電路之微細圖案化及高頻化發展中,可適用作為印刷電路基板用銅箔(特別是半導體封裝基板用銅箔)及將銅箔與樹脂基材加以貼合所製成之印刷電路基板(特別是半導體封裝基板)用覆銅積層板。
Claims (9)
- 一種印刷電路基板用銅箔,係在銅箔之粗化面,具備含有鎳或鋅之氧化物或者鎳或鋅之氫氧化物之層(以下,稱為「鎳鋅層」),以及在該層上,具備鉻酸鹽被膜層,其特徵在於:該鎳鋅層之每單位面積的鋅附著重量在180μg/dm2 以上、3500μg/dm2 以下,鎳鋅層中之鎳重量比率{鎳附著重量/(鎳附著重量+鋅附著重量)}在0.38以上、0.7以下。
- 如申請專利範圍第1項之印刷電路基板用銅箔,其中,該{鎳附著重量/(鎳附著重量+鋅附著重量)}在0.4以上、0.55以下。
- 如申請專利範圍第1項之印刷電路基板用銅箔,其中,該鉻酸鹽被膜層之銅箔每單位面積的鉻附著重量在30μg/dm2 以上、100μg/dm2 以下。
- 如申請專利範圍第1至3項中任一項之印刷電路基板用銅箔,其中,該鎳鋅層所含有之全部鋅中,以鋅氧化物或鋅氫氧化物之形態存在之鋅佔有45~90%。
- 如申請專利範圍第1至3項中任一項之印刷電路基板用銅箔,其中,該鎳鋅層所含有之全部鎳中,以鎳氧化物或鎳氫氧化物之形態存在之鎳佔有60~80%。
- 如申請專利範圍第1至3項中任一項之印刷電路基板用銅箔,其中,在該鉻酸鹽層上,進一步具備矽烷偶合劑層。
- 如申請專利範圍第1至3項中任一項之印刷電路基板 用銅箔,其中,銅箔為電解銅箔,粗化面為電鍍時之粗面或是對此粗面進一步施以粗化處理之面、或是對電解銅箔之光澤面施以粗化處理之面。
- 如申請專利範圍第1至3項中任一項之印刷電路基板用銅箔,其中,銅箔為壓延銅箔,粗化面為對該壓延銅箔施以粗化處理之面。
- 一種印刷電路基板用覆銅積層板,係將申請專利範圍第1至8項中任一項之印刷電路基板用銅箔與印刷電路基板用樹脂基材加以貼合而製成。
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EP (1) | EP2290132A1 (zh) |
JP (1) | JP4938130B2 (zh) |
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MY (1) | MY151361A (zh) |
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EP2290132A1 (en) | 2011-03-02 |
WO2009154066A1 (ja) | 2009-12-23 |
KR101188147B1 (ko) | 2012-10-05 |
US20120148862A1 (en) | 2012-06-14 |
JPWO2009154066A1 (ja) | 2011-11-24 |
CN101981230A (zh) | 2011-02-23 |
US8142905B2 (en) | 2012-03-27 |
CN101981230B (zh) | 2013-01-16 |
TW201002165A (en) | 2010-01-01 |
US20100261033A1 (en) | 2010-10-14 |
JP4938130B2 (ja) | 2012-05-23 |
KR20100071098A (ko) | 2010-06-28 |
MY151361A (en) | 2014-05-15 |
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