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TW201319320A - 銅或銅合金用蝕刻液 - Google Patents

銅或銅合金用蝕刻液 Download PDF

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Publication number
TW201319320A
TW201319320A TW101135853A TW101135853A TW201319320A TW 201319320 A TW201319320 A TW 201319320A TW 101135853 A TW101135853 A TW 101135853A TW 101135853 A TW101135853 A TW 101135853A TW 201319320 A TW201319320 A TW 201319320A
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TW
Taiwan
Prior art keywords
copper
group
etching
acid
copper alloy
Prior art date
Application number
TW101135853A
Other languages
English (en)
Other versions
TWI565835B (zh
Inventor
小嶋努
小路祐吉
Original Assignee
尖端科技材料公司
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Filing date
Publication date
Application filed by 尖端科技材料公司 filed Critical 尖端科技材料公司
Publication of TW201319320A publication Critical patent/TW201319320A/zh
Application granted granted Critical
Publication of TWI565835B publication Critical patent/TWI565835B/zh

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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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/18—Acidic compositions for etching copper or alloys thereof
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/32—Alkaline compositions
    • C23F1/34—Alkaline compositions for etching copper or alloys thereof
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/44—Compositions for etching metallic material from a metallic material substrate of different composition
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    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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Abstract

本發明目的在於提供：在從同時具有銅或銅合金、與鎳的電子基板，對銅或銅合金施行蝕刻之步驟中，使用時的起泡較少，能高選擇性執行銅或銅合金之蝕刻的蝕刻液。本發明所使用的銅或銅合金用蝕刻液，係從同時具有銅或銅合金、與鎳的電子基板，對銅或銅合金選擇性施行蝕刻的步驟用蝕刻液；以鏈狀烷醇胺(A)、分子內具有酸基的螯合劑(B)、及過氧化氫(C)為必要成分。

Description

銅或銅合金用蝕刻液
本發明係關於從電子基板對銅或銅合金施行蝕刻的蝕刻液，特別係關於從具有由銅或銅合金與鎳所構成之電極(凸塊)的電子基板，對銅或銅合金施行選擇性蝕刻的蝕刻液。
電子裝置係為了性能提升而朝元件的細微化、高密度化演進，特別係半導體裝置在細微化技術方面已接近極限。作為高密度化的技術，習知使用焊接搭線、覆晶或凸塊的三次元構造裝置雖已實用化，但仍期待更進一步之高密度化。所以，正進行著貫通矽而製成細介層洞，再填充銅等導電體而製成電極的技術(TSV技術)開發(非專利文獻1)。
一般而言，TSV技術中，當以銅為電極時，在矽基板中鑿設孔，並在孔的內壁中製成矽氧化膜、鈦等阻障金屬層之後，再利用有機金屬氣相沉積法或物理氣相沉積法製成銅的種子層(圖1)。接著，在形成電極的部位以外之銅種子層上，利用阻劑樹脂形成保護膜(圖2)。又，在未形成保護膜的部分處埋藏銅等金屬，並施行凸塊形成。但是，若維持銅狀態便會因表面氧化現象等而導致耦接可靠性變差，因而一般係分別積層鎳層、及由金、錫及銀的合金所構成之焊錫層(圖3)。之後，藉由去除阻劑樹脂而形成凸塊(圖4)。
但是，銅的種子層、與阻障金屬層係不僅形成於矽基板的 孔內部，於矽基板表面亦有形成，在去除阻劑後仍會殘留。因而，必需利用蝕刻液予以除去(圖5)。
其中，作為對銅的種子層施行濕式蝕刻之方法，係廣泛採用由硫酸與過氧化氫混合液等由酸與氧化劑構成的蝕刻液之方法(專利文獻1)。又，亦廣泛已知使用含有氯化銅、三氯化鐵的蝕刻液之方法(專利文獻2)。又，亦廣泛已知使用由硫酸與過氧化氫、屬於聚乙二醇衍生物之界面活性劑所構成之蝕刻液的方法(專利文獻3)。
然而，如專利文獻1~3的蝕刻方法，在對電子基板上所形成銅的種子層於凸塊形成後再施行蝕刻時，因為用於凸塊形成而使用的鎳亦被蝕刻，因而有凸塊發生變形的問題。
再者，目前的蝕刻裝置因為係利用感測器檢測藥液的緩衝槽之液面並進行管理，因而蝕刻液的氣泡產生會導致感測器出現錯誤動作。又，因為蝕刻液係利用泵進行循環，因而氣泡會造成泵咬入空氣，導致送液出現不良情況。所以，如專利文獻3的蝕刻方法中，有因氣泡生成而導致缺乏作業性的問題。
[先前技術文献] [非專利文獻]
[非專利文獻1]「三次元安裝用之TSV技術」(傳田精一著、2009年、工業調查會出版)第12~16頁
[專利文獻]
[專利文獻1]日本專利特開2000-286531號公報
[專利文獻2]日本專利特開2008-285720號公報
[專利文獻3]日本專利特開2009-120870號公報
本發明目的在於提供：在從同時具有銅或銅合金、與鎳的電子基板，對銅或銅合金施行蝕刻之步驟中，使用時的起泡較少，能高選擇性執行銅或銅合金之蝕刻的蝕刻液。
本發明者等為達成上述目的而經深入鑽研，結果遂完成本發明。
即，本發明的銅或銅合金用蝕刻液，係從同時具有銅或銅合金、與鎳的電子基板，對銅或銅合金選擇性地施行蝕刻之步驟用的蝕刻液；其以鏈狀烷醇胺(A)、分子內具有酸基的螯合劑(B)、及過氧化氫(C)為必要成分。本發明的電子基板之製造方法，係包括有使用該蝕刻液，從同時具有銅或銅合金與鎳的電子基板選擇性施行銅或銅合金蝕刻的步驟。
本發明係從同時具有銅或銅合金與鎳的電子基板，施行銅或銅合金蝕刻的步驟，能高選擇性施行銅或銅合金的蝕刻。
本發明的銅或銅合金用蝕刻液係使用時的起泡較少，從同 時具有銅或銅合金、與鎳的電子基板，對銅或銅合金選擇性地施行蝕刻的步驟用蝕刻液，係以鏈狀烷醇胺(A)、分子內具有酸基的螯合劑(B)、及過氧化氫(C)為必要成分。
本發明中，被蝕刻之同時具有銅或銅合金與鎳的電子基板，可舉例如半導體、平面顯示器所使用者，作為銅可舉例如利用化學氣相沉積法(CVD法)、物理氣相沉積法(PVD法)、原子層沉積法(ALD法)、鍍敷等所形成者等等。又，作為鎳亦可舉例如依上述方法形成者等。
本發明之銅或銅合金用蝕刻液的第1必要成分之鏈狀烷醇胺(A)，係含有羥基與1個或2個以上的氮原子，且未含有脂環或雜環的脂肪族烷醇胺，具體可舉例如下述一般式(1)所示之鏈狀烷醇單胺(A1)或下述一般式(2)所示之鏈狀烷醇多元胺(A2)等。
[式(1)中，R1~R3係表示各自獨立的氫原子、或其中一部分亦可被羥基所取代的烷基。但，R1~R3中至少1者係被羥基所取代的烷基。]
[化2] [式(2)中，R4~R8係表示各自獨立的氫原子、或其中一部分亦可被羥基所取代的烷基。但，R4~R8中至少1者係被羥基所取代的烷基。Y1與Y2係表示各自獨立的碳數1~4個的伸烷基。n係表示0或1~4的整數。]
一般式(1)所示之鏈狀烷醇單胺(monoamine)(A1)中，R1~R3係氫原子、烷基、其中一部分被羥基所取代的烷基，各自可為相同亦可為不同，R1~R3中至少1者必需為被羥基所取代的烷基。
烷基可舉例如碳數1~5的直鏈狀或分支狀者。具體可舉例如：甲基、乙基、正丙基、異丙基、正丁基、異丁基、第二丁基、第三丁基、正戊基、異戊基、第三戊基等。
其中一部分被羥基所取代的烷基可舉例如碳數1~5的直鏈狀或分支狀者。
此種其中一部分被羥基所取代的烷基可舉例如：羥甲基、1-羥乙基、2-羥乙基、1-羥丙基、2-羥丙基、3-羥丙基、1-羥異丙基、2-羥異丙基、二羥甲基、1,1-二羥乙基、1,2-二羥乙基、2,3-二羥丙基、1,2,3-三羥丙基等。
一般式(2)所示之鏈狀多元胺(A2)中，R4~R8係氫原子、烷基、其中一部分被羥基所取代的烷基，各自可為相同亦可為 不同，R4~R8中至少1者必需為被羥基所取代的烷基。
烷基及其中一部分被羥基所取代的烷基係與前述R1~R3所示烷基、及其中一部分被羥基所取代的烷基相同。
一般式(2)中的Y1及Y2所示之伸烷基，可舉例如碳數1~4的直鏈狀或分支狀伸烷基。
具體可舉例如：亞甲基、伸乙基、伸丙基、四亞甲基、伸丁基、2,2-二甲基伸丙基、2-乙基伸丙基等。
Y1及Y2所示之伸烷基的碳數，係從抑制蝕刻液起泡等觀點而言，較佳係1~4、更佳係1~3、特佳係2。
一般式(2)中的n係0或1~4的整數、較佳係0或1~2。n個[-Y1-N(-R8)-]係可為相同亦可為不同。
一般式(1)及(2)所示之鏈狀烷醇胺(A)係從抑制蝕刻液起泡等觀點而言，較佳係HLB為12~45者。
此處所謂「HLB」係指親水性與親油性間之平衡的指標，已知有例如「界面活性劑入門」[2007年三洋化成工業股份有限公司出版、藤本武彥著]第212頁所記載，依照小田法獲得的計算值，並非依照格里芬(Griffin)法獲得的計算值。
HLB值可從有機化合物的有機性值與無機性值之比率進行計算。
HLB≒10×無機性/有機性
關於用於導出HLB的有機性值及無機性值，可使用前述「界面活性劑入門」第213頁所記載表的值進行計算。
鏈狀烷醇單胺(A1)可舉例如：單乙醇胺、2-(甲基胺基)乙醇、2-(乙基胺基)乙醇、2-(異丙基胺基)乙醇、2-胺基-2-甲基-1-丙醇、2-(二甲基胺基)乙醇、2-(二乙基胺基)乙醇、二乙醇胺、三乙醇胺、3-胺基-1-丙醇、1-胺基-2-丙醇、二異丙醇胺、三異丙醇胺、及3-(二乙基胺基)-1-丙醇等。
鏈狀烷醇多元胺(A2)可舉例如：2-[(2-胺乙基)胺基]乙醇、2-[甲基[2-(二甲基胺基)乙基]胺基]乙醇、2,2'-(伸乙基雙亞胺基)雙乙醇、N-(2-羥乙基)-N'-(2-胺乙基)乙二胺、N-(3-羥丙基)乙二胺、2,2'-(2-胺乙基亞胺基)二乙醇、N-(2-羥乙基)-N'-(2-胺乙基)乙二胺、2-[雙(2-胺乙基)胺基]乙醇、1-[2-[(2-胺乙基)胺基]乙基]胺基-2-丙醇、3,3',3",3'"-[3-羥丙基亞胺基雙(伸乙基次氨基)]肆(1-丙醇)、N,N,N',N'-四(2-羥乙基)乙二胺、N,N,N',N',N"-伍(2-羥丙基)二乙三胺、N,N,N',N'-肆(2-羥乙基)三甲二胺、N,N-雙(羥乙基)二乙三胺、N1,N4-雙(羥乙基)二乙三胺、N,N,N',N',N"-伍(2-羥丙基)二乙三胺、N1-(2-羥丙基)三乙四胺、N4-(2-羥丙基)三乙四胺、N-(2-羥丙基)三乙四胺等。
本發明的蝕刻劑係視需要亦可經水稀釋後才使用，而鏈狀烷醇胺(A)的含有量係從銅或銅合金與鎳的蝕刻速度比之觀點而言，根據使用時的蝕刻液合計重量，較佳係0.05~6重量%、更佳係0.1~3重量%、特佳係0.2~1.5重量%。
本發明第2必要成分的分子內具有酸基之螯合劑(B)，係 具有提高銅或銅合金之蝕刻速度的作用。
本發明的分子內具有酸基之螯合劑(B)，係含有2個以上為使具有螯合效果的官能基，其中若1個以上係酸基，則其餘官能基亦可為醇性羥基、酚性羥基、腈基、硫醇基、胺基等。
本發明的螯合劑(B)中，酸基可舉例如：羧基、膦基、磺酸基、磷酸基、硫酸基、硝酸基、硼酸基等。
另外，螯合劑(B)亦可在蝕刻液中依鹽的形式含有。
本發明的螯合劑(B)或其鹽可舉例如：酸基係含有羧基2個以上的有機酸或其鹽(B1)、酸基係含有膦酸基2個以上的有機酸或其鹽(B2)、酸基係含有磺酸基2個以上的有機酸或其鹽(B3)、酸基係含有羧基與膦酸基各1個以上的有機酸或其鹽(B4)等。
再者，分子內具有酸基的螯合劑(B)係在分子內具有呈螯合效果之羥基的前提下，酸基亦可為羧基、膦酸基或磺酸基僅含1個的螯合劑(B5)。
酸基係含有羧基2個以上的有機酸或其鹽(B1)，可舉例如：乙二胺四醋酸(鹽)、二乙三胺五醋酸(鹽)、三乙四胺六醋酸(鹽)、羥乙基乙二胺三醋酸(鹽)、二羥乙基乙二胺四醋酸(鹽)、硝化酸醋酸(鹽)、羥乙基亞胺基雙醋酸(鹽)、β-丙胺酸雙醋酸(鹽)、天冬胺酸雙醋酸(鹽)、甲基甘胺酸雙醋酸(鹽)、亞胺基二琥珀酸(鹽)、絲胺酸雙醋酸(鹽)、羥基亞胺 基二琥珀酸(鹽)、酒石酸(鹽)、檸檬酸(鹽)、均苯四甲酸(鹽)、苯并多元羧酸(鹽)、環戊烷四羧酸(鹽)等。
酸基係含有膦酸基2個以上的有機酸或其鹽(B2)，可舉例如：甲基二膦酸(鹽)、胺基三(亞甲基膦酸)(鹽)、1-羥基亞乙基-1,1-二膦酸(鹽)、乙二胺四(亞甲基膦酸)(鹽)、六亞甲基二胺四(亞甲基膦酸)(鹽)、丙二胺四(亞甲基膦酸)(鹽)、二乙三胺五(亞甲基膦酸)(鹽)、三乙四胺六(亞甲基膦酸)(鹽)、三胺基三乙基胺六(亞甲基膦酸)(鹽)、反-1,2-環己二胺四(亞甲基膦酸)(鹽)、乙二醇醚二胺四(亞甲基膦酸)(鹽)、四乙五胺七(亞甲基膦酸)(鹽)等。
酸基係含有磺酸基2個以上的有機酸或其鹽(B3)，可舉例如：甲二磺酸(鹽)、乙二磺酸(鹽)、酚二磺酸(鹽)、萘二磺酸(鹽)、哌-1,4-雙(2-乙烷磺酸)(鹽)等。
酸基係含有羧基與膦酸基各1個以上的有機酸或其鹽(B4)，可舉例如：磷酸醋酸(鹽)、2-羥基-2-磷酸醋酸(鹽)、羧膦酸(鹽)、3-膦醯基丙酸(鹽)、4-(3-膦醯基丙基)-2-哌羧酸(鹽)等。
羥基與酸基為羧基、膦酸基或磺酸基僅含1個的螯合劑(B5)，可舉例如：乳酸(鹽)、水楊酸(鹽)、沒食子酸(鹽)、2-羥乙基膦酸(鹽)、2-羥基乙烷磺酸(鹽)等。
本發明的螯合劑(B)中，從銅或銅合金的蝕刻速度觀點而言，較佳係上述(B1)、(B2)、(B3)，更佳係(B2)。
分子內具有酸基的螯合劑(B)可單獨使用、或同時併用2以上。
分子內具有酸基的螯合劑(B)之含有量，從銅或銅合金的蝕刻速度觀點而言，根據使用時的蝕刻液合計重量，較佳係0.1~50重量%、更佳係0.5~30重量%、特佳係1~20重量%。
本發明第3必要成分的過氧化氫(C)係具有提高蝕刻速度的作用。過氧化氫(C)可使用過氧化氫的水溶液。
過氧化氫(C)含有量係從蝕刻速度的觀點而言，根據使用時的蝕刻液合計重量，依純分換算計較佳係0.05~20重量%、更佳係0.1~10重量%、特佳係0.2~5重量%。
本發明的鏈狀烷醇胺(A)、與分子內具有酸基的螯合劑(B)之重量比(B)/(A)，從銅或銅合金與鎳的蝕刻速度比、及起泡的觀點而言，通常係1~100、較佳係2~50、更佳係5~30。
本發明分子內具有酸基的螯合劑(B)、與過氧化氫(C)的重量比(B)/(C)，從銅或銅合金的蝕刻速度觀點而言，通常係1~30、較佳係2~20、更佳係3~10。
本發明的蝕刻液最好係由(A)、(B)、(C)、及視需要的溶劑相混合使用。該溶劑可舉例如：水、醇、乙二醇醚、醚、酯、酮、碳酸酯、醯胺等。
蝕刻液的溶劑係從容易處置的觀點而言，較佳為水。
本發明的蝕刻液係在保護佈線金屬之目的下，視需要可添加三唑類、咪唑類、硫醇化合物、糖醇類等抗腐蝕劑。
本發明的蝕刻液係在保護佈線金屬之目的下，視需要可添加抗氧化劑。
抗氧化劑可舉例如：兒茶素、生育酚、鄰苯二酚、甲基鄰苯二酚、乙基鄰苯二酚、第三丁基鄰苯二酚、沒食子酸、沒食子酸甲酯、沒食子酸丙酯等酚類；3-羥基黃素酮、抗壞血酸(ascorbic acid)等。
本發明的蝕刻液中，在pH調整之目的下，可添加鹼性化合物或酸性化合物。
在此目的下添加的鹼性化合物係有如：氨、胺或氫氧化四烷基銨、含氮雜環式化合物。胺可舉例如脂肪族胺、伸烷二胺、聚伸烷多元胺、芳香族胺、脂環式胺、胍等。
再者，在此目的下添加的酸性化合物，係有如：硫酸、鹽酸、硝酸、氫氟酸等無機酸；醋酸等有機酸。
再者，在使蝕刻速度安定化之目的下，無機酸或其鹽的添加係屬有效。此種無機酸較佳係硫酸、鹽酸、硝酸、氫氟酸等。
本發明的蝕刻液係在保護佈線金屬之目的下，視需要可添加消泡劑。
消泡劑可舉例如：聚矽氧消泡劑、長鏈醇消泡劑、脂肪酸酯消泡劑及金屬皂消泡劑等。環氧乙烷-環氧丙烷共聚合體亦可使用為消泡劑。
使用本發明的蝕刻液，經由從同時具有銅或銅合金與鎳的 電子基板，選擇性對銅或銅合金施行蝕刻處理的步驟，便可製造電子基板。
本發明中，銅或銅合金的蝕刻處理方法可舉例如浸漬式蝕刻、單片式蝕刻等。
本發明的蝕刻液通常係依10~100℃範圍、較佳係20℃~80℃的溫度條件使用。從蝕刻速度的觀點而言，較佳係達10℃以上，從蝕刻速度不會發生平衡的觀點而言，較佳係100℃以下的溫度。
[實施例]
以下，利用實施例及比較例針對本發明更進一步說明，惟本發明並不僅侷限於該等。以下，在無特別聲明之前提下，「%」係表示「重量%」，「份」係表示「重量份」。
<實施例1~7及比較例1~6>
將表1所記載的鏈狀烷醇胺(A)、分子內具有酸基的螯合劑(B)、過氧化氫(C)、及水，在聚丙烯製容器中施行混合，獲得本發明的蝕刻液與比較用的蝕刻液。
另外，表中的符號係表示以下化合物：
(A-1)：三乙醇胺
(A-2)：2-[(2-胺乙基)胺基]乙醇
(A-3)：1,2-雙[二(羥乙基)胺基]乙烷(三洋化成工業(股)製、商品名「SANNIX NE-240」)
(A'-1)：月桂醇之EO9莫耳加成物
(B-1)：檸檬酸
(B-2)：60%1-羥基亞乙基-1,1-二膦酸之水溶液
(B-3)：1,2-乙二磺酸二水合物
(B-4)：硝化三亞甲基膦酸
(B'-1)：乙二胺
(C-1)：35%過氧化氫水
性能評價係針對抑泡性、銅之蝕刻時間、及鎳之蝕刻性能(鎳/銅之蝕刻速率比)，依照以下方法實施。
<抑泡性>
抑泡性可根據Ross-Miles試驗[JIS K 3362(1998)]進行測定，經由使用該JIS所決定的裝置、且試驗液係使用經超純水施行調整過的蝕刻劑之試驗，在所有試驗液剛流出後，依目視測定氣泡高度(mm)，並依下述判定基準評價抑泡性。
○：未滿50mm
×：50mm以上
<銅之蝕刻時間>
銅之蝕刻時間係依照以下的操作方法，利用直到銅種子層的光澤消失為止之時間(分)進行評價。
(1)對矽基板施行加工製成圖4所示狀態的晶圓(銅種子層厚度1μm)，再將其裁剪為15mm四方正方形而製成測試片。
另外，利用掃描式電子顯微鏡(日立高科技公司製S-4800)觀察晶圓經裁剪為各1cm的測試片截面，結果凸塊寬度約30μm、凸塊高度約8μm。銅種子層的厚度係1μm。
(2)將蝕刻液裝入聚丙烯製容器中，在其中浸漬上述測試片並利用磁攪拌器施行攪拌。
(3)一邊攪拌，一邊依浸漬於液中的狀態目視觀察測試片的表面，測定直到銅種子層整面的銅光澤消失(圖5的3：能看到鈦層整面的狀態)之時間。
依該目的所使用的蝕刻液較佳係銅光澤消失時間為10分鐘以內。
另外，當60分鐘但光澤仍未消失者，便在60分鐘時中止浸漬，並在表1中記為「>60」。
<鎳之蝕刻量及鎳/銅之蝕刻速率比>
鎳之蝕刻量及鎳/銅之蝕刻速率比係依照以下的操作方法施行測定，並評價。
(1)對矽基板施行加工製成圖4所示狀態的晶圓(銅種子層厚度1μm)，再將其裁剪為15mm四方正方形而製成測試片。
(2)將蝕刻液裝入聚丙烯製容器中，在其中浸漬上述測試 片1分鐘，並利用磁攪拌器施行攪拌後再取出。
(3)利用掃描式電子顯微鏡(日立高科技公司製S-4800)施行可確認浸漬前測試片與浸漬後測試片的各自鎳層侵蝕程度及其寬度之側面照片拍攝。然後，從照片影像測定浸漬前測試片的鎳層(圖4之7)寬度A1(μm)、與浸漬後測試片的鎳層(圖5之7)寬度A2(μm)。
(4)鎳的蝕刻量係計算出依下述數式(1)所計算出的浸漬前後測試片之鎳層寬度變化(差)△ANi。
[數1]△ANi(μm)=(浸漬前測試片的鎳層寬度A1)-(浸漬後測試片的鎳層寬度A2) (1)
依下述判定基準施行評價。
○：未滿1μm
×：1μm以上
(5)讀取2個值及銅的蝕刻時間，代入下述數式(2)中並計算出鎳/銅的蝕刻速率比。
TCu：銅之蝕刻時間(分)
TNi：鎳之蝕刻時間、本評價法中為1分鐘
ACu：銅種子層之厚度、本評價法中為1μm
從依上述數式(2)所計算出的鎳/銅之蝕刻速率比，依下述判定基準施行評價。
○：未滿0.5
×：0.5以上
由表1中得知，實施例1~7毫無起泡的問題，銅種子層的蝕刻較快速，另一方面，未發現有鎳部分的蝕刻，可進行高選擇性的銅種子層蝕刻。
另一方面，未含過氧化氫水的比較例1、及未含分子內具有酸基之螯合劑的比較例2，銅種子層與鎳均未被蝕刻。
未含鏈狀烷醇胺的比較例3，雖銅種子層的蝕刻較快速，但鎳亦被蝕刻，無法高選擇性進行銅種子層蝕刻。取代鏈狀烷醇胺(A)改為使用月桂醇之EO9莫耳加成物(A'-1)的比較例4，雖高選擇性進行銅種子層蝕刻，但起泡頗多。
使用分子內未具有酸基之螯合劑(B'-1)的比較例5，亦是銅種子層的蝕刻較慢。
再者，取代螯合劑改為使用硫酸的比較例6，鎳被蝕刻。
(產業上之可利用性)
本發明的銅或銅合金用蝕刻液係對同時具有銅或銅合金與鎳的物品，由使用時的起泡較少、能高選擇性施行銅或銅合金蝕刻的觀點而言較為優異，因而能有效使用為印刷佈線基板、平面顯示器、MEMS、半導體裝置等電子基板製造時的步驟用藥劑。
1‧‧‧矽基板
2‧‧‧矽氧化膜
3‧‧‧鈦層
4‧‧‧銅種子層
5‧‧‧阻劑樹脂
6‧‧‧銅鍍敷層
7‧‧‧鎳鍍敷層
8‧‧‧金鍍敷層
9‧‧‧凸塊
圖1係在矽基板中鑿設孔，並在孔的內壁上積層著矽氧化膜、鈦層、銅種子層等各層的剖視圖。
圖2係在圖1的矽基板上塗佈阻劑樹脂而形成保護膜後的剖視圖。
圖3係在圖2的矽基板上更進一步積層鎳與金之金屬後的剖視圖。
圖4係從圖3的矽基板上去除了阻劑樹脂後的剖視圖。
圖5係從圖4的矽基板去除了銅種子層後的剖視圖。
圖6係從圖5的矽基板去除阻障金屬(鈦)層後的剖視圖。
1‧‧‧矽基板
2‧‧‧矽氧化膜
3‧‧‧鈦層
4‧‧‧銅種子層
6‧‧‧銅鍍敷層
7‧‧‧鎳鍍敷層
8‧‧‧金鍍敷層
9‧‧‧凸塊

Claims (8)

  1. 一種銅或銅合金用蝕刻液，係從同時具有銅或銅合金、與鎳的電子基板，對銅或銅合金選擇性地施行蝕刻的步驟用的蝕刻液；其以鏈狀烷醇胺(A)、分子內具有酸基的螯合劑(B)、及過氧化氫(C)為必要成分。
  2. 如申請專利範圍第1項之蝕刻液，其中，該鏈狀烷醇胺(A)係下述一般式(1)所示鏈狀烷醇單胺(A1)、或下述一般式(2)所示鏈狀烷醇多元胺(A2)： [式(1)中，R1~R3係表示各自獨立的氫原子、或其中一部分亦可被羥基所取代的烷基；其中，R1~R3中至少1者係被羥基所取代的烷基]； [式(2)中，R4~R8係表示各自獨立的氫原子、或其中一部分亦可被羥基所取代的烷基；其中，R4~R8中至少1者係被羥基所取代的烷基；Y1與Y2係表示各自獨立的碳數1~4個的伸烷基；n係表示0或1~4的整數]。
  3. 如申請專利範圍第1或2項之蝕刻液，其中，該鏈狀烷醇胺(A)的HLB係12~45。
  4. 如申請專利範圍第1至3項中任一項之蝕刻液，其中，該螯合劑(B)係分子內含有膦酸基及/或磺酸基合計2個以上的有機酸。
  5. 如申請專利範圍第1至3項中任一項之蝕刻液，其中，該螯合劑(B)係分子內含有羧基2個以上的有機酸。
  6. 如申請專利範圍第1至5項中任一項之蝕刻液，其中，該鏈狀烷醇胺(A)與該螯合劑(B)的重量比(B)/(A)係1~100。
  7. 如申請專利範圍第1至6項中任一項之蝕刻液，其中，該螯合劑(B)與過氧化氫(C)的重量比(B)/(C)係1~30。
  8. 一種電子基板之製造方法，係包括有：使用申請專利範圍第1至7項中任一項之銅或銅合金用蝕刻液，從同時具有銅或銅合金與鎳的電子基板，選擇性對銅或銅合金施行蝕刻的步驟。
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