TWI680194B - 焊接材料、焊料接頭及焊接材料的檢查方法 - Google Patents
焊接材料、焊料接頭及焊接材料的檢查方法 Download PDFInfo
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- TWI680194B TWI680194B TW105120278A TW105120278A TWI680194B TW I680194 B TWI680194 B TW I680194B TW 105120278 A TW105120278 A TW 105120278A TW 105120278 A TW105120278 A TW 105120278A TW I680194 B TWI680194 B TW I680194B
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- core
- aforementioned
- ball
- oxide film
- welding material
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- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0227—Rods, wires
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
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- B23K35/0233—Sheets, foils
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- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
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- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/262—Sn as the principal constituent
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- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
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- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/302—Cu as the principal constituent
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- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3033—Ni as the principal constituent
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- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3046—Co as the principal constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3601—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with inorganic compounds as principal constituents
- B23K35/3602—Carbonates, basic oxides or hydroxides
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- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/365—Selection of non-metallic compositions of coating materials either alone or conjoint with selection of soldering or welding materials
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- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- H05K3/32—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
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Abstract
其目的係正確地辨別不容易氧化之焊接材料。
Cu核心球1係包括:具有規定之大小而在半導體封裝和印刷電路基板之間來確保間隔之Cu球2以及被覆Cu球2之焊接層3。Cu核心球1係在溫度25℃、濕度40%之室內之150℃恆溫槽之72小時之燃燒試驗後之L*a*b*表色系之亮度為62.5以上,燃燒試驗前之焊接材料之L*a*b*表色系之亮度為65以上,並且,L*a*b*表色系之黃色度為7.0以下。
Description
本發明係關於一種焊接材料、焊料接頭及焊接材料的檢查方法。
在近年來,由於小型資訊機器之發達而在搭載之電子零件,進行急速之小型化。在電子零件,為了應付由於小型化之要求而造成之連接端子之窄小化或構裝面積之縮小化,因此,適用在背面來設置電極之球閘陣列(在以下,稱為「BGA」。)。
在適用BGA之電子零件,有例如半導體封裝。半導體封裝係例如具有電極之半導體晶片,透過焊接凸塊而接合在印刷電路基板之導電性接端面墊,藉由以樹脂來密封這些而構成半導體封裝。在近年來,為了應付更加高之高密度構裝之要求,因此,開發半導體封裝來堆積於高度。
作為焊接凸塊係開發例如Cu核心球。在專利文獻1,記載:包括成為芯部之Cu球以及被覆Cu球表面之焊接層的Cu核心球。使用Cu核心球而構成之焊接凸塊係在電子零件構裝於印刷電路基板之際,即使是半導體封裝之重量來施加於焊接凸塊,也可以在焊接之熔點,藉由無熔融之Cu球而支持半導體封裝。可以藉此而防止由於半導體封裝之本身重量來破壞焊接凸塊。
但是,有在Cu核心球之焊接表面來形成氧化膜之狀態發生。由於該氧化膜之影響而在焊接和電極之間,發生潤濕之不良,結果,有所謂發生Cu核心球之構裝不良而大幅度地降低半導體封裝之生產性或良品率之問題發生。因此,在Cu核心球,要求耐氧化性。
該Cu核心球之氧化膜問題係有由於Cu核心球之製作後之保管環境之溫度或濕度而產生之狀態發生。即使是在形成氧化膜之Cu核心球來構裝於半導體封裝之電極上之後而進行重熔處理之狀態,也同樣地發生焊接之潤濕不良,構成Cu核心球之焊接係無法潤濕擴散至電極整體,成為露出電極之狀態,有所謂由於Cu核心球相對於電極之位置偏離等而發生Cu核心球之構裝不良之問題產生。因此,Cu核心球之製作後之氧化膜厚度之管理係也成為重要之問題。
於是,本申請人係著眼於黃色度和亮度之2個指標,來作為在焊接之熔融前而事前管理氧化膜厚度之指標,提議:藉由在黃色度和亮度,選定符合於預先設定之值之Cu核心球而正確地管理形成於Cu核心球表面之氧化膜厚度之方法。可以藉由使用以該Cu核心球之氧化膜厚度之管理方法來得到之Cu核心球,而良好地進行半導體晶片對於印刷電路基板之接合。
【先前技術文獻】
【專利文獻】
【專利文獻1】國際公開第95/24113號
但是,在Cu球來施行電鍍處理之後,一般係實施用以除去殘留於Cu核心球表面之電鍍液中之有機錯化劑、pH值調整劑、pH值緩衝劑、促進劑、安定劑、界面活性劑、光澤劑、半光澤劑、平滑劑等之電鍍液殘渣之洗淨處理。但是,即使是在製作後之黃色度和亮度來符合於預先設定之值之Cu核心球,也在洗淨處理呈不充分之狀態下,在Cu核心球之表面,殘留許多之電鍍液殘渣,即使是藉由適當之保管條件而進行保管,也有配合殘留之電鍍液殘渣量而在Cu核心球之長期間保管後,比起通常而還更加地促進Cu核心球表面之焊接之氧化之狀態發生。結果,即使是使用在製作後之黃色度和亮度來符合於預先設定之值之Cu核心球,也有在半導體晶片對於印刷電路基板之接合時,由於形成在Cu核心球表面之氧化膜而產生接合不良之狀態發生。
於是,本發明係有鑒於前述之課題而完成的,其目的係提供即使是在長期間之保管後也不容易氧化之焊接材料和焊料接頭。此外,本發明係提供可以正確地將即使是在長期間之保管後也不容易氧化之焊接材料予以辨別之焊接材料的檢查方法。
本發明人們係發現:在Cu核心球之洗淨處理後,在藉由以規定之溫度、大氣濕度條件下而進行加熱處理來刻意地促進氧化之Cu核心球,在滿足燃燒試驗後之L*a*b*表色系
之亮度(L*值)為62.5以上之條件之狀態下,得到電鍍液殘渣量少、也就是不容易氧化之Cu核心球。此外,在本發明,所謂燃燒試驗係為了在Cu核心球1之洗淨後,刻意地促進配合殘留之電鍍液量而形成之氧化膜成長之試驗,係指例如在溫度為25℃、濕度為40%之室內之150℃恆溫槽而對於製作後之Cu核心球來進行72小時之加熱保管之試驗。在製作後之Cu核心球,也包含例如進行加速試驗等。
(1):一種焊接材料,係包括由在接合物和被接合物之間來確保間隔之核心以及被覆前述核心之Sn或者是以Sn來作為主成分之焊接合金而構成之被覆層的焊接材料,其特徵為:在溫度25℃、濕度40%之室內之150℃恆溫槽之72小時之燃燒試驗後之L*a*b*表色系之亮度為62.5以上,前述之燃燒試驗前之前述焊接材料之L*a*b*表色系之亮度為65以上,並且,L*a*b*表色系之黃色度為7.0以下。
(2):在前述(1)之焊接材料,其特徵為:藉著由Ni和Co來選擇之一種以上之元素而構成之層來被覆之前述之核心係藉由前述之被覆層而進行被覆。
(3):在前述(1)或(2)之焊接材料,其特徵為:在前述之焊接材料,前述燃燒試驗後之L*a*b*表色系之前述亮度係70.2以上。
(4):在前述(1)至(3)中任一項之焊接材料,其特徵為:前述之核心係藉著由球狀之Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg來組成之群組而選擇之至少一
種元素或樹脂材料來構成。
(5):在前述(1)至(3)中任一項之焊接材料,其特徵為:前述之核心係藉著由圓柱狀之Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg來組成之群組而選擇之至少一種元素或樹脂材料來構成。
(6):一種焊料接頭,係使用前述(1)至(5)中任一項之焊接材料。
(7):一種焊接材料,係包括由在接合物和被接合物之間來確保間隔之核心以及被覆前述核心之Sn或者是以Sn來作為主成分之焊接合金而構成之被覆層的焊接材料,其特徵為:在進行溫度25℃、濕度40%之室內之150℃恆溫槽之72小時加熱後之氧化膜厚度係4.9nm以下。
(8):在前述(7)之焊接材料,其特徵為:藉著由Ni和Co來選擇之一種以上之元素而構成之層來被覆之前述之核心係藉由前述之被覆層而進行被覆。
(9):在前述(7)或(8)之焊接材料,其特徵為:前述之燃燒試驗後之前述之氧化膜厚度係3.1nm以下。
(10):在前述(7)至(9)中任一項之焊接材料,其特徵為:前述之核心係藉著由球狀之Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg來組成之群組而選擇之至少一種元素或樹脂材料來構成。
(11):在前述(7)至(9)中任一項之焊接材
料,其特徵為:前述之核心係藉著由圓柱狀之Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg來組成之群組而選擇之至少一種元素或樹脂材料來構成。
(12):一種焊料接頭,係使用前述(7)至(11)中任一項之焊接材料。
(13):一種焊接材料的檢查方法,其特徵為具有:在溫度25℃、濕度40%之室內而設定成為150℃之恆溫槽,對於包括由在接合物和被接合物之間來確保間隔之核心以及被覆該核心之Sn或者是以Sn來作為主成分之焊接合金而構成之被覆層的焊接材料,進行72小時之加熱之製程;以及,將在加熱於前述製程之前述焊接材料之L*a*b*表色系之亮度成為62.5以上之焊接材料予以取得之製程。
如果是藉由本發明之焊接材料、焊料接頭及焊接材料的檢查方法的話,則能夠以正確且短時間,來區別在長期保管後而不容易氧化之Cu核心球。
1‧‧‧Cu核心球(焊接材料)
2‧‧‧Cu球(核心)
3‧‧‧焊接層(被覆層)
圖1係在本發明之某一實施形態來顯示Cu核心球之構成例之剖面圖。
圖2係顯示在燃燒試驗前之Cu核心球之黃色度和氧化膜厚度之間之關係之圖。
圖3係顯示在燃燒試驗前之Cu核心球之亮度和氧化膜厚
度之間之關係之圖。
圖4係顯示在燃燒試驗後之Cu核心球之黃色度和保管期間之間之關係之圖。
圖5係顯示在燃燒試驗後之Cu核心球之亮度和氧化膜厚度之間之關係之圖。
在以下,參照附件之圖式,同時,就本發明揭示之理想之實施形態而詳細地進行說明。此外,在以下之說明,全部之亮度及黃色度係指L*a*b*表色系。
[關於Cu核心球]
圖1係顯示本發明之Cu核心球1之構造之一例之剖面圖。正如圖1所示,本發明之Cu核心球1係包括:具有規定之大小且在半導體封裝(接合物)和印刷電路基板(被接合物)之間來確保間隔之Cu球(核心)2以及被覆Cu球2之焊接層(被覆層)3。
˙燃燒試驗前之Cu核心球1之亮度及黃色度
本發明之Cu核心球1係燃燒試驗前之L*a*b*表色系之亮度為65以上,並且,L*a*b*表色系之黃色度為7.0以下。可以藉由選定亮度及黃色度為前述範圍內之Cu核心球1而以一定值以下,來管理形成於焊接層3之表面之氧化膜厚度。
在本發明,在燃燒試驗前之Cu核心球1,無法僅藉由黃色度或亮度之一個指標而正確地管理氧化膜厚度,因此,藉由黃色度和亮度之二個指標而管理Cu核心球1之氧化膜厚度。在以下,首先就無法僅藉由黃色度而管理Cu核心球
1之氧化膜厚度之理由,來進行說明。
圖2係顯示在Cu核心球1和焊接球之黃色度(b*值)和氧化膜厚度之間之關係之圖。縱軸係表示黃色度,橫軸係表示氧化膜厚度。正如圖2所示,在焊接球,隨著表面之氧化膜厚度變厚而也提高黃色度,氧化膜厚度和黃色度係成為概略比例關係。因此,如果是焊接球的話,則可以藉由黃色度而管理氧化膜厚度,至一定之膜厚為止。
相對於此,在Cu核心球1,比起焊接球,還更加提早地進行氧化,隨著這個而也提高黃色度,然後,無關於氧化膜厚度之增加,降低黃色度,氧化膜厚度和黃色度係無成為比例關係。例如在氧化膜厚度為4nm之狀態下,黃色度成為7.2,但是,在氧化膜厚度為8.7nm之狀態下,黃色度成為2.9,在氧化膜厚度和黃色度之間,並無成立相聯關係。認為這個係被覆Cu球表面之焊料電鍍中之不純物,成為要因。因此,在僅藉由黃色度而造成之管理,有所謂無法正確地管理氧化膜厚度之問題發生。
接著,就無法僅藉由亮度而管理Cu核心球1之氧化膜厚度之理由,來進行說明。圖3係顯示Cu核心球1及焊接球之氧化膜厚度和亮度之間之關係之圖形。縱軸係表示亮度,橫軸係表示氧化膜厚度。正如圖3所示,Cu核心球1之氧化膜厚度和亮度係有所謂隨著氧化膜越加變厚而亮度越低之相聯關係。求出此時之氧化膜厚度和亮度之相關係數R。相關係數R係求出於-1至1之範圍。接著,算出之相關係數係進行二次方而求出貢獻率R2。貢獻率R2係求出於0至1之範圍,表示越加接近於1而在亮度和氧化膜厚度,有存在相聯關係。
Cu核心球1之氧化膜厚度和亮度之貢獻率R2係成為=0.8229,成為比較小於1之值。相對於此,在僅使用圖2所示之黃色度呈降低前之值而藉由前述之方法來求出氧化膜厚度和黃色度之貢獻率之時,藉由黃色度而造成之管理係貢獻率R2=0.9523而成為比較接近於1之值。因此,在僅藉由亮度而造成之管理,有所謂在測定值之偏差變多而無法呈高精度地管理氧化膜厚度之問題發生。因此,在本發明,使用亮度和黃色度之二個指標而進行在燃燒試驗前之Cu核心球1之氧化膜厚度之正確管理。
˙燃燒試驗後之Cu核心球1之亮度及黃色度
本發明之Cu核心球1係燃燒試驗後之L*a*b*表色系之亮度為62.5以上。在150℃之大氣濕度下而加熱72小時之Cu核心球1之理由係因為即使是無進行經過長期間、例如1個月之保管試驗,也能夠配合殘留於Cu核心球1之洗淨後之電鍍液殘渣量,以短時間,將形成之氧化膜予以形成之緣故。此外,Cu核心球1之亮度為62.5以上之理由係為了正確地辨別及管理由於燃燒試驗而使得氧化膜超過規定之膜厚(4.9nm)之Cu核心球1之緣故。此外,Cu核心球1之L*a*b*表色系之亮度係更加理想是70.2以上。在該狀態下,可以更加嚴格地管理氧化膜厚度。可以藉由滿足前述之2個條件而減少在Cu核心球1之洗淨後之電鍍液殘渣量,呈簡易且容易地辨別在長期間保管後而不容易氧化之Cu核心球1。
接著,關於管理在燃燒試驗後之Cu核心球1之氧化膜厚度之指標而進行說明。在燃燒試驗後之Cu核心球1,
因為可以僅藉由亮度之1個指標而進行氧化膜厚度之正確管理,所以,僅藉由亮度而管理Cu核心球1之氧化膜厚度。首先,在黃色度之指標,就無法管理Cu核心球1之氧化膜厚度之理由而進行說明。
圖4係顯示在Cu核心球1之黃色度和保管期間之間之關係之圖。縱軸係表示黃色度,橫軸係表示保管期間。在Cu核心球1,比起一般之焊接球,還更加提早地進行氧化,隨著這個而也提高黃色度,然後,無論保管期間是否變長,也降低黃色度,在黃色度和保管期間,無成為比例關係。在此,保管期間為1日以後之Cu核心球1之保管天數和黃色度之貢獻率R2係=0.589而成為離開於1之值。因此,在藉由黃色度而造成之管理,在測定值,有許多之偏差,有所謂無法呈高精度地管理氧化膜厚度之問題發生。
接著,就可以僅藉由亮度之指標而管理Cu核心球1之氧化膜厚度之理由,來進行說明。圖5係顯示Cu核心球1之氧化膜厚度和亮度之間之關係之圖形。縱軸係表示亮度,橫軸係表示氧化膜厚度。Cu核心球1之氧化膜厚度和亮度係有所謂氧化膜越加厚而越加降低亮度之相聯關係。Cu核心球1之氧化膜厚度和亮度之貢獻率R2係成為=0.9332而成為接近於1之值。因此,如果是藉由以亮度而造成之管理的話,則在測定值,偏差變少,可以呈高精度地管理氧化膜厚度。
相對於燃燒試驗前,在僅藉由亮度而造成之管理,在測定值之偏差變多,無法呈高精度地管理Cu核心球1之氧化膜厚度,相對地,在燃燒試驗後,在僅藉由亮度而造成
之管理,可以呈高精度地管理Cu核心球1之氧化膜厚度,其理由係認為正如下列之敘述。在進行於燃燒試驗前之試驗,詳細地敘述於後面,但是,改變溫度˙濕度˙加熱時間等之各種條件,假定各種形式之氧化舉動,即使是在其任何一種氧化舉動之狀態下,如果是可以在製造之即刻後而進行構裝的話,則以製造可以抑制氧化膜厚度之形成之Cu核心球,來作為目的。
相對地,在本發明之燃燒試驗,假定可以抑制「在長期間保管後」之氧化膜厚度之成長之Cu核心球,因此,無必要假定各種之氧化舉動而正如進行於燃燒試驗前之試驗,僅注目於藉由高溫保管而造成之氧化舉動。於是,詳細之細節係敘述於後面,本發明之燃燒試驗係藉由決定加熱之溫度在150℃以上之某一定值,僅改變加熱時間,統一這個以外之條件,進行實驗,而僅觀察在高溫保管時之氧化舉動。所謂假定之氧化舉動是僅在高溫保管時係所謂也類似氧化膜厚度之成長舉動。接著,所謂類似氧化膜厚度之成長舉動係判明所謂也類似亮度之變化,亮度和氧化膜厚度之相聯關係變佳。因此,在本發明,使用亮度,來作為一個指標而進行在燃燒試驗後之Cu核心球1之氧化膜厚度之正確管理。
[關於Cu球2]
接著,關於構成本發明之Cu核心球1之Cu球2而詳細地進行說明。此外,Cu球2之構造等係共通於燃燒試驗前後,因此,整理於以下而進行說明。Cu球2係在Cu核心球1使用於焊接凸塊之際,無熔融於焊接之溫度,因此,具有抑制焊料接頭之高度偏差之機能。所以,Cu球2係最好是真圓度比較
高而直徑之偏差比較小。
˙Cu球2之組成
Cu球2係可以藉由Cu單體之組成而構成,並且,也可以藉由以Cu來作為主成分之合金組成而構成。在藉由合金而構成Cu球2之狀態下,Cu含有量係50質量%以上。此外,作為成為核心之球係也除了Cu以外,還可以藉由Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg之金屬單體和合金、金屬氧化物或金屬混合氧化物而構成。
˙Cu球2之純度
Cu球2之純度係並無特別限定,由抑制因為純度之降低而造成之Cu球2之電傳導度和熱傳導率之惡化並且配合需要而抑制α射線量之觀點來看的話,則成為99.9%以上。作為包含於Cu球2之不純物元素係列舉Sn、Sb、Bi、Ni、Zn、Fe、Al、As、Ag、In、Gd、Pb、Au、P、S、Co等。
˙Cu球2之真圓度
由控制面間隔高度之觀點來看的話,則Cu球2之真圓度係0.95以上。在Cu球2之真圓度未滿0.95之時,Cu球2係成為不定形狀,因此,在形成凸塊時,形成高度不均勻之凸塊,提高發生接合不良之可能性。此外,在Cu核心球1搭載於電極而進行重熔之際,Cu核心球1係引起位置偏離,也惡化自行對準定位性。真圓度係更加理想是0.990以上。在本發明,所謂真圓度係表示來自真圓之偏差。真圓度係藉由例如最小二次方中心法(LSC法)、最小區域中心法(MZC法)、最大
內接中心法(MIC法)、最小外接中心法(MCC法)等之各種方法而求出。詳細地說,所謂真圓度係例如在500個之各個Cu球2之直徑除以長徑之際而算出之算術平均值,表示值越加接近成為上限之1.00而越加接近於真圓。在本發明之所謂長徑之長度和直徑之長度係指藉由mitutoyo公司製之超快速影像、ULTRA QV350-PRO測定裝置而測定之長度。
˙Cu球2之直徑
Cu球2之直徑係1~1000μm。在Cu球2之直徑位處於該範圍之時,可以穩定地製造球狀之Cu球2,並且,可以抑制在端子間為窄間距之狀態下之連接短路。
在此,例如在本發明之Cu核心球1之直徑為1~300μm程度之狀態下,「Cu核心球」之集合體係可以稱為「Cu核心粉末」。在此,「Cu核心粉末」係各個之Cu核心球1包括前述特性之許多之Cu核心球1之集合體。例如所謂練合成為焊接糊膏中之粉末等之單一之Cu核心球1係區別於使用形態。同樣地,也在使用於焊接凸塊之形成之狀態下,通常處理成為集合體,因此,使用於此種形態之「Cu核心粉末」係區別於單一之Cu核心球1。
[關於焊接層3]
接著,就構成本發明之Cu核心球1之焊接層3而詳細地進行說明。此外,焊接層3之構造等係共通於燃燒試驗前後,因此,整理於以下而進行說明。焊接層3係在Cu核心球1使用於焊接凸塊之際,藉由重熔時之溫度而進行熔融,發揮作為呈電氣地接合半導體封裝之電極和印刷電路基板之電極之接
合構件之機能。
˙焊接層3之組成
焊接層3係也可以成為Sn單體之組成,並且,也可以成為以Sn作為主成分之無鉛焊接合金之合金組成,並且,也可以成為Sn-Pb焊接合金之組成。在藉由合金而構成焊接層3之狀態下,Sn之含有量係40質量%以上。作為無鉛焊接組成之一例係列舉例如Sn、Sn-Ag合金、Sn-Cu合金、Sn-Bi合金、Sn-Ag-Cu合金、Sn-In合金以及在這些來添加規定之合金元素者。作為添加之合金元素係列舉例如Ag、Cu、In、Ni、Co、Sb、P、Fe等。關於添加之合金元素之添加量,最好是抑制成為無鉛焊接合金之黃色度和亮度幾乎相同於Sn單體之黃色度和亮度之幾乎相同程度之量。即使是在這些當中,由熱疲勞壽命之觀點來看的話,則焊接層3之合金組成係也最好是Sn-3Ag-0.5Cu合金。焊接層3之厚度係並無特別限制,但是,如果是100μm(單邊)以下的話,則變得充分。一般係可以是20~50μm。此外,本發明之以Sn作為主成分之無鉛焊接合金之Sn含有量係最好是Sn為80%以上,更加理想是Sn為90%以上。
此外,也可以在Cu球2之表面和焊接層3之間,設置由被覆Cu球2之Ni和Co來選擇之1種以上元素而構成之層、例如Ni電鍍層或Co電鍍層等。可以藉此而在對於電極之接合時,減低Cu擴散至焊接中之擴散,可以抑制Cu球2之Cu侵蝕。Ni電鍍層或Co電鍍層等之膜厚係例如單邊0.1~20μm。此外,可以在Cu核心球1之表面,被覆助熔劑。
[Cu核心球1之製造方法]
接著,說明本發明之Cu核心球1之製造方法之一例。首先,準備例如陶瓷之耐熱性板且在底部來設置形成半球狀之許多之圓形溝之耐熱板。溝之直徑或深度係配合Cu球2之粒徑而適度地設定,例如直徑為0.8mm,深度為0.88mm。接著,將藉由切斷成為材料之Cu細線而得到之晶片形狀之Cu材料(在以下,稱為「晶片材料」。),分別每一個地投入至耐熱板之溝內。
接著,在填充還原性氣體、例如氨分解氣體之爐內,將在溝內來投入晶片材料之耐熱板,升溫至1100~1300℃,進行30~60分鐘之加熱處理。此時,在爐內溫度成為Cu之熔點以上時,晶片材料係進行熔融而成為球狀。然後,藉由冷卻爐內而在耐熱板之溝內,成形Cu球2。在冷卻後,在成為未滿Cu熔點之溫度之800~1000℃,對於成形之Cu球2,再度進行加熱處理。
此外,作為其他之方法係有:由設置於坩堝底部之篩孔開始,滴下熔融Cu,冷卻該液滴,造粒Cu球2之霧化法;以及,藉由熱電漿而加熱Cu切斷金屬至1000℃以上,進行造粒之方法。像這樣造粒之Cu球2係可以分別在800~1000℃之溫度,施行30~60分鐘之再加熱處理。此外,可以在造粒Cu球2之前,於800~1000℃,對於成為Cu球2原料之Cu材料,進行加熱處理。
作為成為Cu球2原料之Cu材料係可以使用例如顆粒、線材、條柱等。Cu材料之純度係由無過度降低Cu球2之純度之觀點來看的話,則可以是99.9~99.99%。
此外,在使用高純度之Cu材料之狀態下,無進行前述之加熱處理,可以相同於習知而降低熔融Cu之保持溫度至1000℃程度。可以像這樣而使得前述之加熱處理,配合Cu材料之純度,適度地進行省略或變更。
作為流動正如前面之敘述來製作之Cu球2或電鍍液而在Cu球2來形成焊接層3之方法係有:習知之滾筒電鍍等之電解電鍍法、連接於電鍍槽之幫浦係在電鍍槽中之電鍍液來產生高速度亂流而以電鍍液之亂流在Cu球2來形成焊接層3之方法、藉由在電鍍槽來設置振動板而以規定之頻率來進行振動而對於電鍍液來進行高速度亂流攪拌並且藉由電鍍液之亂流而在Cu球2來形成焊接層3之方法等。
接著,在直徑100μm之Cu球2來被覆膜厚(單邊)2μm之Ni電鍍之後,形成膜厚(單邊)18μm之Sn-Ag-Cu之焊接層3,製作直徑大約140μm之Cu核心球1。
本發明之某一實施形態之含Sn-Ag-Cu電鍍液係在以水作為主體之媒體,含有磺酸類以及作為金屬成分之Sn、Ag和Cu,來成為必要成分。
金屬成分係在電鍍液中,存在成為Sn離子(Sn2+及/或Sn4+)、Ag離子(Ag+)和Cu離子(Cu+及/或Cu2+)。電鍍液係藉著混合主要由水和磺酸類之所組成之電鍍母液以及金屬化合物而得到,由於金屬離子之安定性,因此,最好是包含有機錯化劑。
作為電鍍液中之金屬化合物係可以例舉例如以下者。作為Sn化合物之具體例係列舉甲烷磺酸、乙烷磺酸、2-
丙醇磺酸、p-苯酚磺酸等之有機磺酸之錫鹽、硫酸錫、氧化錫、硝酸錫、氯化錫、溴化錫、碘化錫、磷酸錫、焦磷酸錫、乙酸錫、甲酸錫、檸檬酸錫、葡糖酸錫、酒石酸錫、乳酸錫、琥珀酸錫、氨基磺酸錫、硼氟化錫、矽氟化錫等之一代Sn化合物。這些Sn化合物係可以單獨一種或者是混合二種以上而使用。
作為Cu化合物係列舉前述之有機磺酸之銅鹽、硫酸銅、氧化銅、硝酸銅、氯化銅、溴化銅、碘化銅、磷酸銅、焦磷酸銅、乙酸銅、甲酸銅、檸檬酸銅、葡糖酸銅、酒石酸銅、乳酸銅、琥珀酸銅、氨基磺酸銅、硼氟化銅、矽氟化銅等。這些Cu化合物係可以單獨一種或者是混合二種以上而使用。
作為Ag化合物係列舉前述之有機磺酸之銀鹽、硫酸銀、氧化銀、氯化銀、硝酸銀、溴化銀、碘化銀、磷酸銀、焦磷酸銀、乙酸銀、甲酸銀、檸檬酸銀、葡糖酸銀、酒石酸銀、乳酸銀、琥珀酸銀、氨基磺酸銀、硼氟化銀、矽氟化銀等。這些Ag化合物係可以單獨一種或者是混合二種以上而使用。
此外,在直徑100μm之Cu球2來形成膜厚(單邊)20μm之Sn-Ag-Cu之焊接層3之狀態下,需要大約0.0108庫侖之電量。
電鍍液中之各金屬之練合量係作為Sn2+而成為0.21~2mol/L,最好是0.25~1mol/L,作為Ag+而成為0.01~0.1mol/L,最好是0.02~0.05mol/L,作為Cu2+而成為0.002~0.02mol/L,最好是0.003~0.01mol/L。在此,關係到電鍍者係Sn2+,在本發明,可以調整Sn2+量。
此外,Ag離子濃度相對於Cu離子濃度(Ag/Cu
莫爾數比)係最好是4.5~5.58之範圍。如果是該範圍的話,則可以形成例如Sn-3Ag-0.5Cu合金之低熔點Sn-Ag-Cu焊接層3。此外,藉由法拉第電分解法則,以下列之公式(1)而估計要求之焊料電鍍之析出量,算出電量,在電鍍液來導通電流而成為算出之電量,流動Cu球2和電鍍液,同時,進行電鍍處理。電鍍槽之容量係可以配合Cu球2和電鍍液之總投入量而決定。
w(g)=(I×t×M)/(Z×F)˙˙˙公式(1)
在公式(1)中,w係表示電解析出量(g),I係表示電流(A),t係表示通電時間(秒),M係表示析出之元素之原子量(在Sn之狀態下,成為118.71。),Z係表示原子價(在Sn之狀態下,成為2價。),F係表示法拉第常數(96500庫倫),電量Q(A˙秒)係表示(I×t)。
在本發明,流動Cu球2和電鍍液,同時,進行電鍍,但是,關於流動之方法,並無特別限定。例如滾筒電解電鍍法,可以藉由滾筒之旋轉而流動Cu球2和電鍍液。
可以在電鍍處理後,藉由乾燥於大氣中或N2氛圍中而得到本發明之Cu核心球1。
在此,正如前面之敘述,在Cu球2來進行焊料電鍍之狀態下,有電鍍液之殘渣來殘留於Cu核心球1表面之狀態發生。因此,為了除去殘留於Cu核心球1表面之電鍍液殘渣,所以,一般係實施洗淨處理。作為洗淨液係可以使用例如純水、異丙醇等之醇或酮(丙酮)等之有機溶劑、磷酸三鈉等之酸性洗淨液、鹼性洗淨液等。洗淨液係能夠以單體來使用,
並且,也可以組合複數種之洗淨液而使用。
作為洗淨方法係可以採用例如浸漬洗淨、超音波洗淨、噴灑洗淨、噴淋洗淨、噴射洗淨、真空洗淨、脫氣洗淨、滾筒洗淨、搖動刷擦洗淨、噴流泡沫洗淨、微型泡沫洗淨等。洗淨方法係可以配合要求之洗淨效果而採用單一之洗淨方法,並且,也可以組合複數種之洗淨方法。配合洗淨方法或洗淨液、洗淨時間而在洗淨後,使得殘留於Cu核心球1表面之電鍍殘渣也不同,保管時之氧化程度也不同,因此,可以藉由充分地實施洗淨處理而得到在長期間保管後也不容易氧化之Cu核心球1。
[接材料之其他之構成例(其1)]
此外,構成本發明之Cu核心球1之核心係也可以藉由樹脂球而構成。作為樹脂材料係列舉例如由胺基樹脂、丙烯樹脂、乙烯-乙酸乙烯基樹脂、苯乙烯-丁二烯嵌段共聚物、聚酯樹脂、三聚氰胺樹脂、苯酚樹脂、醇酸樹脂、聚醯亞胺樹脂、胺基甲酸乙酯樹脂、環氧樹脂、交聯樹脂等而組成者。即使是在其中,也最好是使用聚乙炔、聚吡咯、聚噻吩、聚苯胺等之導電性塑膠等。可以在核心成為樹脂材料之狀態下,藉由樹脂球以及被覆樹脂球表面之Sn-Ag-Cu系之焊料電鍍層(被覆層)而構成Cu核心球。此外,前述之被覆層之種類和層積構造係並非限定於前述之例子。
[焊接材料之其他之構成例(其2)]
在前述之實施形態,就藉由亮度和黃色度而管理Cu核心球1之氧化程度之例子,來進行說明,但是,並非限定於此。可以藉由例如直接地管理形成於Cu核心球表面之氧化膜之膜
厚而管理在洗淨後之Cu核心球之氧化程度。本發明之其他之Cu核心球係包括:在半導體封裝和印刷電路基板之間來確保間隔之Cu球以及被覆Cu球之焊接層;在150度之大氣濕度下而進行72小時之燃燒試驗後之氧化膜厚度係4.9nm以下。可以藉由管理在燃燒試驗後之Cu核心球之氧化膜厚度在4.9nm以下,而充分地實施洗淨,辨別及取得不容易氧化(氧化膜變薄)之Cu核心球。Cu核心球之氧化膜厚度係更加理想是3.1nm以下。此外,關於呈實質地相同於前述之Cu核心球1之相同構造機能而言,為了方便起見,省略說明。
[焊接材料之其他之構成例(其3)]
在前述之實施形態,就焊接材料之形狀為球形之狀態而進行說明,在焊接材料之形狀為柱形之狀態,也可以適用本發明。在焊接材料成為柱形狀之狀態,焊接材料係由形成圓柱狀之柱和被覆柱表面之焊接層而構成。該焊接材料係在150℃之大氣濕度下而進行72小時之燃燒試驗後之L*a*b*表色系之亮度為62.5以上,燃燒試驗前之焊接材料之L*a*b*表色系之亮度為65以上,並且,L*a*b*表色系之黃色度為7.0以下。
作為柱材料係可以使用Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg之金屬單體、合金、金屬氧化物或金屬混合氧化物、或者是樹脂材料。焊接層係也可以成為Sn單體之組成,並且,也可以成為以Sn作為主成分之無鉛焊接合金之合金組成,並且,也可以成為Sn-Pb焊接合金之組成。在藉由合金而構成焊接層之狀態下,Sn含有量係40質量%以上。作
為無鉛焊接組成之一例係列舉例如Sn、Sn-Ag合金、Sn-Cu合金、Sn-Bi合金、Sn-Ag-Cu合金、Sn-In合金以及在這些金屬˙合金來添加規定之合金元素者。作為添加之合金元素係列舉例如Ag、Cu、In、Ni、Co、Sb、P、Fe等。此外,前述之所謂Cu核心球1係如果是除去形狀(真圓度)的話,則在實質上,成為相同之構造機能,因此,為了方便起見,省略說明。
此外,本發明之Cu核心球1係可以使用在電子零件之焊料接頭。在本例子,所謂焊料接頭係指例如焊接凸塊來構裝於印刷電路基板之電極上之構造。此外,所謂焊接凸塊係指例如在半導體晶片之電極上來構裝Cu核心球1之構造。
在以下,就本發明之實施例而進行說明,但是,本發明係並非限定於這些。
˙Cu球之製作
準備純度99.995%以下之Cu線。在將準備之各個Cu線來投入至坩堝中之後,使得坩堝之溫度來升溫至1200℃,進行45分鐘之加熱處理。接著,由設置於坩堝底部之篩孔開始,滴下熔融Cu之液滴,冷卻滴下之液滴,製造平均粒徑100μm之Cu球。
˙真圓度
製作之Cu球之真圓度係使用CNC圖像測定系統而進行測定。具體地說,使用mitutoyo公司製之超快速影像、ULTRA QV350-PRO測定裝置。在本實施例,藉由前述之測定裝置而測定Cu球之長徑之長度和直徑之長度,算出以500個之各Cu球之直徑來除以長徑之值之算術平均值,求出真圓度。表示值
越加接近成為上限之1.00而越加接近真圓。
˙燃燒試驗前之Cu核心球之氧化膜厚度、亮度及黃色度
接著,在製作之直徑100μm之Cu核心球之表面,形成膜厚(單邊)2μm之電鍍Ni層,製作直徑104μm之電鍍Ni之Cu球,並且,在電鍍Ni層之表面,形成膜厚18μm之焊接層而製作直徑140μm之Cu核心球。在焊接層,使用Sn-3Ag-0.5Cu合金。接著,將製作之Cu核心球,來投入至加入純水之燒杯中,藉由攪拌機而進行10分鐘之攪拌洗淨。接著,藉由下列之各實施例和比較例之所顯示之條件而分別測定Cu核心球之氧化膜厚度、亮度及黃色度。
在實施例1,使用在洗淨即刻後之Cu核心球。在實施例2,在常溫(曝露於大氣中)且濕度30~40%之狀態,保管攪拌洗淨之Cu核心球2日。在實施例3,在常溫且濕度30~40%之狀態,保管攪拌洗淨之Cu核心球5日。在實施例4,在常溫且濕度30~40%之狀態,保管攪拌洗淨之Cu核心球7日。在實施例5,在常溫且濕度30~40%之狀態,保管攪拌洗淨之Cu核心球10日。在實施例6,在常溫且濕度30~40%之狀態,保管攪拌洗淨之Cu核心球14日。在實施例7,在40℃且濕度90%之狀態,保管攪拌洗淨之Cu核心球1日。在實施例8,在常溫且濕度30~40%之狀態,保管攪拌洗淨之Cu核心球20日。在實施例9,在40℃且濕度90%之狀態,保管攪拌洗淨之Cu核心球2日。在實施例10,在200℃之狀態,保管攪拌洗淨之Cu核心球1小時。此外,常溫係20~30℃。
在比較例1,在40℃且濕度90%之狀態,保管攪拌洗淨之Cu核心球5日。在比較例2,在40℃且濕度90%之狀態,保管攪拌洗淨之Cu核心球7日。在比較例3,在40℃且濕度90%之狀態,保管攪拌洗淨之Cu核心球10日。在比較例4,在40℃且濕度90%之狀態,保管攪拌洗淨之Cu核心球14日。在比較例5,在200℃之狀態,保管攪拌洗淨之Cu核心球1日。在比較例6,在200℃之狀態,保管攪拌洗淨之Cu核心球2日。
接著,回收藉由前述之條件而保管之實施例1~10、比較例1~6之各Cu核心球,分別測定回收之各Cu核心球之亮度、黃色度及氧化膜厚度。Cu核心球之亮度及黃色度係使用konicaminolta公司製之CM-2600d型分光測色計而進行測定。Cu球之氧化膜厚度係使用ULVAC PHI700之FE-AES測定裝置而進行測定。測定裝置之加速電壓係10kV,照射電流係10nA。氧化膜厚度(深度)係由藉著離子(Ar)來削除試料表面之速度(蝕刻速度)而求出氧化膜厚度,使用成為來自於氧之Intensty之1/2波峰值之蝕刻深度,來作為氧化膜厚度近似值。蝕刻速度係藉由削除SiO2標準試料之速度而進行換算,成為SiO2換算值。將測定之各實施例1~10、比較例1~6之Cu核心球之亮度、黃色度及氧化膜厚度之間之關係,顯示於表1。在表1,氧化膜厚度之單位係(nm)。
正如表1之實施例1~10所示,在選定亮度為62.5以上且黃色度為7.0以下之Cu核心球之狀態下,氧化膜厚度係3.8nm以下。此外,正如表1之實施例1~5所示,在選定亮度為70以上且黃色度為5.1以下之Cu核心球之狀態下,氧化膜厚度係1.9nm以下,比起其他之實施例6~10,還得到氧化膜厚度更加薄之Cu核心球。
另一方面,正如比較例1~6所示,在Cu核心球之亮度未滿62.5或者黃色度超過7.0之狀態下,氧化膜厚度係
3.9nm以下,也更加厚於作為目標之氧化膜厚度。由以上而得知:可以藉由選定亮度為65以上且黃色度為7.0以下之Cu核心球而提供氧化膜厚度變薄之Cu核心球。
此外,即使是關於紅色度(a*值)而進行測定,但是,確認:和氧化膜厚度之間之相關係數以及貢獻率係小於1,無法在氧化膜厚度管理之指標來使用紅色度。
此外,測定各實施例1~10之Cu核心球之α射線量,結果,完全無顯示於前述之表1,但是,全部之Cu核心球之α射線量係0.0010cph/cm2以下,低於要求之0.0200cph/cm2。
˙燃燒試驗後之Cu核心球之氧化膜厚度、亮度及黃色度
接著,使用前述實施例1之燃燒試驗前之Cu核心球,對於該Cu核心球,實施用以在短期間來使得Cu核心球成為長期間保管之狀態之燃燒試驗。接著,分別測定在進行燃燒試驗後之Cu核心球之氧化膜厚度、亮度及黃色度。此外,使用之Cu核心球係正如前面之敘述,實施10分鐘之攪拌洗淨。
˙洗淨條件及燃燒試驗條件
首先,在溫度25℃(室溫)、濕度40%,設定恆溫槽來成為150℃,維持該狀態1小時以上。在實施例1A,在還藉由第1洗淨方法而將攪拌洗淨之Cu核心球予以洗淨之後,將洗淨之Cu核心球來放入至前述之恆溫槽而在150℃,保管3日。在實施例1B,在還藉由第2洗淨方法而將攪拌洗淨之Cu核心球予以洗淨之後,將洗淨之Cu核心球來放入至前述之恆溫槽而在150℃,保管3日。在實施例1C,在還藉由第3洗淨方法而將攪拌洗淨
之Cu核心球予以洗淨之後,將洗淨之Cu核心球來放入至前述之恆溫槽而在150℃,保管3日。在比較例1A,將前述之攪拌洗淨之Cu核心球來放入至前述之恆溫槽而在150℃,保管3日。
此外,在第1洗淨方法,在加入純水之燒杯中,投入製作之Cu核心球,將投入Cu核心球之燒杯來安裝於超音波洗淨機而進行10秒鐘之超音波洗淨。在第2洗淨方法,在加入純水之燒杯中,投入製作之Cu核心球,將投入Cu核心球之燒杯來安裝於超音波洗淨機而進行60秒鐘之超音波洗淨。在第3洗淨處理,在加入純水之燒杯中,投入製作之Cu核心球,將投入Cu核心球之燒杯來安裝於超音波洗淨機而進行180秒鐘之超音波洗淨。此外,在本實施例,將第1~第3洗淨方法,分類成為可以充分地除去電鍍液殘渣之高度洗淨效果之洗淨方法。此外,將僅攪拌洗淨之洗淨方法,分類成為無法充分地除去電鍍液殘渣之低洗淨效果之洗淨方法。
接著,將藉由前述之條件而進行洗淨及加熱保管之實施例1A、1B、1C、比較例1A之各Cu核心球予以回收。分別測定回收之各Cu核心球之亮度、黃色度及氧化膜厚度。Cu核心球之亮度及黃色度係使用konicaminolta公司製之CM-2600d型分光測色計而進行測定。Cu球之氧化膜厚度係使用ULVAC PHI700之FE-AES測定裝置而進行測定。測定裝置之加速電壓係10kV,照射電流係10nA。氧化膜厚度(深度)係由藉著離子(Ar)來削除試料表面之速度(蝕刻速度)而求出氧化膜厚度,使用成為來自於氧之Intensty之1/2波峰值之蝕刻深度,來作為氧化膜厚度近似值。蝕刻速度係藉由削除SiO2標準試料之速
度而進行換算,成為SiO2換算值。將測定之各實施例1A、1B、1C、比較例1A之Cu核心球之亮度、黃色度及氧化膜厚度之關係,顯示於表2。在表2,氧化膜厚度之單位係(nm)。
正如表2之實施例1A、1B、1C所示,在進行超音波洗淨而加入至攪拌洗淨來作為洗淨條件之狀態下,燃燒試驗後之亮度係62.5以上,Cu核心球之氧化膜厚度係4.9nm以下。藉此而得知:由於Cu核心球之氧化膜厚度和Cu核心球之洗淨條件係有相聯關係,因此,在選擇(取得)滿足於加熱保管後之亮度為62.5以上之條件之Cu核心球之狀態下,可以充分地實施洗淨,辨別在長期間之保管後也不容易氧化(氧化膜變薄)之Cu核心球而進行管理。
另一方面,正如表2之比較例1A所示,在僅進行攪拌洗淨來作為洗淨條件之狀態下,在燃燒試驗後之Cu核心球之亮度係未滿62.5,Cu核心球之氧化膜厚度係超過4.9nm。由以上而得知:在選定滿足於加熱保管後之亮度未滿62.5之條件之Cu核心球之狀態下,洗淨呈不充分,焊料電鍍液之殘渣量變多,結果,成為在長期間之保管後而容易氧化(氧化膜
變厚)之Cu核心球。
此外,在前述之燃燒試驗,就使用表1所示之實施例1之Cu核心球之例子而進行說明,但是,並非限定於此。得知:即使是使用表1所示之實施例2~10之Cu核心球之狀態,也並無顯示於表格,但是,得到相同於使用實施例1之Cu核心球之狀態之同樣結果。具體地說,燃燒試驗後之Cu核心球之亮度係62.5以上,Cu核心球之氧化膜厚度係4.9nm以下。
接著,將加熱˙保管處理前之Cu核心球之洗淨即刻後之Cu核心球之亮度、黃色度及氧化膜厚度之關係,顯示於表3。在表3,氧化膜厚度之單位係(nm)。
正如表3之參考例1~4所示,在進行燃燒試驗前之Cu核心球之洗淨即刻後之Cu核心球之亮度係71.2以上,氧化膜厚度係1.2nm以下。像這樣而確認:在洗淨即刻後而進行燃燒試驗前之狀態,無法促進由於電鍍液殘渣而造成之氧化膜之成長,因此,即使是洗淨條件呈不同之狀態,也無法像這樣,在氧化膜厚度來產生不同。
接著,將在溫度150℃來進行5日(120小時)之
燃燒試驗之狀態下之Cu核心球之亮度、黃色度及氧化膜厚度之關係,顯示於表4。在表4,氧化膜厚度之單位係(nm)。
正如表4之參考例5~7所示,在進行超音波洗淨而加入至攪拌洗淨來作為洗淨條件之狀態下,在燃燒試驗後之Cu核心球之亮度係57.1以上,Cu核心球之氧化膜厚度係8.1nm以下。另一方面,正如表4之參考例8所示,在僅進行攪拌洗淨來作為洗淨條件之狀態下,在燃燒試驗後之Cu核心球1之亮度係未滿57.1,Cu核心球之氧化膜厚度係超過8.1nm。
接著,將在溫度150℃來進行7日(168小時)之燃燒試驗之狀態下之Cu核心球之亮度、黃色度及氧化膜厚度之間之關係,顯示於表5。在表5,氧化膜厚度之單位係(nm)。
正如表5之參考例9~11所示,在進行超音波洗淨而加入至攪拌洗淨來作為洗淨條件之狀態下,在燃燒試驗後之Cu核心球之亮度係53.9以上,Cu核心球之氧化膜厚度係11.5nm以下。另一方面,正如表5之參考例12所示,在僅進行攪拌洗淨來作為洗淨條件之狀態下,在燃燒試驗後之Cu核心球1之亮度係未滿53.9,Cu核心球之氧化膜厚度係超過11.5nm。
在前述之本實施例和參考例,由相同批次處理之許多之Cu核心球中,抽出特定之Cu核心球而進行使用。因此,關於藉由本實施例和參考例之Cu核心球而得到之各個結果,也同樣適用於無進行燃燒試驗製程之相同批次處理之其他之Cu核心球。
此外,本發明係並非仍然僅限定於前述之實施形態,可以在實施階段,在無脫離其要旨之範圍內,改變構成要素而進行具體化。此外,可以藉由揭示於前述實施形態之複數個之構成要素之適當之組合而形成各種之發明。
Claims (17)
- 一種焊接材料,包括由在接合物和被接合物之間來確保間隔之核心以及被覆前述核心之Sn或者是以Sn來作為主成分之焊接合金而構成之被覆層,其特徵為:在溫度25℃、濕度40%之室內之150℃恆溫槽之72小時之燃燒試驗後之L*a*b*表色系之亮度為62.5以上,前述之燃燒試驗前之前述焊接材料之L*a*b*表色系之亮度為65以上,並且,L*a*b*表色系之黃色度為7.0以下。
- 如申請專利範圍第1項之焊接材料,其中,藉著由Ni和Co來選擇之一種以上之元素而構成之層來被覆之前述之核心係藉由前述之被覆層而進行被覆。
- 如申請專利範圍第1或2項之焊接材料,其中,在前述之焊接材料,前述燃燒試驗後之L*a*b*表色系之前述亮度係70.2以上。
- 如申請專利範圍第1或2項之焊接材料,其中,前述之核心係藉著由球狀之Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg來組成之群組而選擇之至少一種元素或樹脂材料來構成。
- 如申請專利範圍第3項之焊接材料,其中,前述之核心係藉著由球狀之Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg來組成之群組而選擇之至少一種元素或樹脂材料來構成。
- 如申請專利範圍第1或2項之焊接材料,其中,前述之核心係藉著由圓柱狀之Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg來組成之群組而選擇之至少一種元素或樹脂材料來構成。
- 如申請專利範圍第3項之焊接材料,其中,前述之核心係藉著由圓柱狀之Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg來組成之群組而選擇之至少一種元素或樹脂材料來構成。
- 一種焊料接頭,其特徵為:使用如申請專利範圍第1至7項中任一項所記載之焊接材料。
- 一種焊接材料,包括由在接合物和被接合物之間來確保間隔之核心以及被覆前述核心之Sn或者是以Sn來作為主成分之焊接合金而構成之被覆層,其特徵為:在溫度25℃、濕度40%之室內之150℃恆溫槽之72小時之燃燒試驗後之氧化膜厚度係4.9nm以下。
- 如申請專利範圍第9項之焊接材料,其中,藉著由Ni和Co來選擇之一種以上之元素而構成之層來被覆之前述之核心係藉由前述之被覆層而進行被覆。
- 如申請專利範圍第9或10項之焊接材料,其中,前述之燃燒試驗後之前述之氧化膜厚度係3.1nm以下。
- 如申請專利範圍第9或10項之焊接材料,其中,前述之核心係藉著由球狀之Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg來組成之群組而選擇之至少一種元素或樹脂材料來構成。
- 如申請專利範圍第11項之焊接材料,其中,前述之核心係藉著由球狀之Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg來組成之群組而選擇之至少一種元素或樹脂材料來構成。
- 如申請專利範圍第9或10項之焊接材料,其中,前述之核心係藉著由圓柱狀之Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg來組成之群組而選擇之至少一種元素或樹脂材料來構成。
- 如申請專利範圍第11項之焊接材料,其中,前述之核心係藉著由圓柱狀之Cu、Ni、Ag、Bi、Pb、Al、Sn、Fe、Zn、In、Ge、Sb、Co、Mn、Au、Si、Pt、Cr、La、Mo、Nb、Pd、Ti、Zr、Mg來組成之群組而選擇之至少一種元素或樹脂材料來構成。
- 一種焊料接頭,其特徵為:使用如申請專利範圍第9至15項中任一項所記載之焊接材料。
- 一種焊接材料的檢查方法,其特徵為具有:在溫度25℃、濕度40%之室內而設定成為150℃之恆溫槽,對於包括由在接合物和被接合物之間來確保間隔之核心以及被覆該核心之Sn或者是以Sn來作為主成分之焊接合金而構成之被覆層的焊接材料,進行72小時之加熱之製程;以及,將在加熱於前述製程之前述焊接材料之L*a*b*表色系之亮度成為62.5以上之焊接材料予以取得之製程。
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KR101904884B1 (ko) * | 2016-10-27 | 2018-10-10 | 덕산하이메탈(주) | 솔더볼 및 이를 이용한 반도체 패키지 |
KR101904891B1 (ko) * | 2016-11-14 | 2018-10-10 | 덕산하이메탈(주) | 솔더볼 및 이를 이용한 임베디드 칩 패키지 |
US10730150B2 (en) * | 2017-08-07 | 2020-08-04 | Honeywell International Inc. | Flowable brazing compositions and methods of brazing metal articles together using the same |
CN107793758B (zh) * | 2017-11-15 | 2020-08-07 | 江苏亚宝绝缘材料股份有限公司 | 一种碳纳米管复合聚酰亚胺树脂的聚合物及其制备与应用 |
JP6439893B1 (ja) * | 2018-05-25 | 2018-12-19 | 千住金属工業株式会社 | ハンダボール、ハンダ継手および接合方法 |
JP6579253B1 (ja) * | 2018-11-09 | 2019-09-25 | 千住金属工業株式会社 | ハンダボール、ハンダ継手および接合方法 |
CN113303037B (zh) * | 2019-01-18 | 2024-03-12 | 三菱电机株式会社 | 焊料接合部的寿命预测部件及焊料接合部的寿命预测方法 |
CN110202295B (zh) * | 2019-05-24 | 2021-10-26 | 浙江强力控股有限公司 | 一种低温铝软钎焊锡膏及其制备方法 |
JP7381267B2 (ja) * | 2019-09-18 | 2023-11-15 | ナブテスコ株式会社 | 金属付加製造用粉粒体、その製造方法、その選別装置、その選別方法、粉体の純度判定装置、粉体の純度判定方法、粉体の保管方法、粉体の保管容器、金属造形物の製造方法、および、金属造形物の製造装置 |
CN111458328B (zh) * | 2020-04-26 | 2021-03-19 | 电子科技大学 | 一种检测印制电路板残留铜层分布的方法 |
CN111560530A (zh) * | 2020-06-12 | 2020-08-21 | 无锡隆达金属材料有限公司 | 一种白铜合金熔液熔炼工艺 |
CN111996413B (zh) * | 2020-08-21 | 2021-07-09 | 中国电子科技集团公司第三十八研究所 | 一种铅锡基焊料合金的制备方法及制得的焊料合金 |
JP6892621B1 (ja) * | 2020-09-10 | 2021-06-23 | 千住金属工業株式会社 | 核材料、電子部品及びバンプ電極の形成方法 |
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JP5590259B1 (ja) * | 2014-01-28 | 2014-09-17 | 千住金属工業株式会社 | Cu核ボール、はんだペーストおよびはんだ継手 |
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WO1995024113A1 (fr) | 1994-03-01 | 1995-09-08 | Sumitomo Special Metals Company Limited | Boule en cuivre et procede de production de cette derniere |
JP2007160401A (ja) * | 2005-11-15 | 2007-06-28 | Hitachi Metals Ltd | はんだ合金、はんだボールおよびそれを用いたはんだ接合部 |
JP4389112B2 (ja) * | 2008-01-17 | 2009-12-24 | ホライゾン技術研究所株式会社 | 半導体装置およびその製造方法 |
JP5071802B2 (ja) * | 2008-04-08 | 2012-11-14 | 日立金属株式会社 | はんだボール、はんだ層及びはんだバンプ |
JP5221231B2 (ja) * | 2008-07-18 | 2013-06-26 | 日立電線株式会社 | 太陽電池用リード線の製造方法 |
WO2010061795A1 (ja) * | 2008-11-27 | 2010-06-03 | 日立電線株式会社 | 太陽電池用リード線及びその製造方法、保管方法、並びに太陽電池 |
JP5418894B2 (ja) * | 2009-07-24 | 2014-02-19 | 日立金属株式会社 | 電子部品用複合ボールの製造方法 |
CN102166691A (zh) | 2010-02-25 | 2011-08-31 | 东莞市万丰纳米材料有限公司 | 一种微焊接材料 |
JP5606994B2 (ja) | 2010-09-30 | 2014-10-15 | 株式会社神戸製鋼所 | 肉盛溶接材料及び肉盛溶接金属が溶接された機械部品 |
WO2012118202A1 (ja) * | 2011-03-02 | 2012-09-07 | セントラル硝子株式会社 | 導電部付きガラス板用端子構造体及びこれを用いたガラス板物品 |
CN103831543B (zh) | 2012-11-23 | 2016-08-24 | 吴永恒 | 无铅焊接材料及其制备方法 |
CN107579007A (zh) | 2013-01-11 | 2018-01-12 | 千住金属工业株式会社 | 将铜球接合于电极的方法以及选择铜球的方法 |
JP5652560B1 (ja) * | 2014-02-04 | 2015-01-14 | 千住金属工業株式会社 | Cu核ボール、はんだペースト、フォームはんだ及びはんだ継手 |
US10137535B2 (en) * | 2014-02-04 | 2018-11-27 | Senju Metal Industry Co., Ltd. | Cu ball, Cu core ball, solder joint, solder paste, and solder foam |
CN107073656B (zh) * | 2014-11-05 | 2018-07-03 | 千住金属工业株式会社 | 软钎焊材料、焊膏、成形焊料、钎焊接头以及软钎焊材料的管理方法 |
JP6892568B2 (ja) * | 2015-12-21 | 2021-06-23 | ニホンハンダ株式会社 | 表面性に優れたSnを主成分とするはんだ合金の選別方法 |
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CN107735212A (zh) | 2018-02-23 |
CN107735212B (zh) | 2019-03-08 |
JP5850199B1 (ja) | 2016-02-03 |
US20180281118A1 (en) | 2018-10-04 |
US10888957B2 (en) | 2021-01-12 |
JP2017013080A (ja) | 2017-01-19 |
WO2017002704A1 (ja) | 2017-01-05 |
KR20180014217A (ko) | 2018-02-07 |
TW201715047A (zh) | 2017-05-01 |
EP3315245A4 (en) | 2018-11-21 |
KR101867796B1 (ko) | 2018-06-15 |
EP3315245A1 (en) | 2018-05-02 |
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