TWI460074B - 供可黏合的晶圓表面用之應力減低的Ｎｉ－Ｐ／Ｐｄ堆疊 - Google Patents

供可黏合的晶圓表面用之應力減低的Ｎｉ－Ｐ／Ｐｄ堆疊 Download PDF

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TWI460074B
TWI460074B TW098133728A TW98133728A TWI460074B TW I460074 B TWI460074 B TW I460074B TW 098133728 A TW098133728 A TW 098133728A TW 98133728 A TW98133728 A TW 98133728A TW I460074 B TWI460074 B TW I460074B
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Taiwan
Prior art keywords
layer
substrate
thickness
wafer
stress
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TW098133728A
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English (en)
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TW201029842A (en
Inventor
Albrecht Uhlig
Josef Gaida
Christof Suchentrunk
Mike Boyle
Brian Washo
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Atotech Deutschland Gmbh
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Publication of TW201029842A publication Critical patent/TW201029842A/zh
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Description

供可黏合的晶圓表面用之應力減低的Ni-P/Pd堆疊
本發明係關於一種具有可黏合的金屬塗層之基板，其在Al或Cu表面上包含Ni-P層和Pd層，該層具有特定厚度和減低的應力。此外，本發明係關於該基板之製法。
用於導線接合和倒裝晶片接合的無電鎳鈀金法為此技藝已知者並述於，例如，歐洲專利申請案EP 0 701 281 A2。類似的方法述於美國專利案第6,445,069號和歐洲專利申請案EP 1 126 519 A2。底部凸塊金屬化(under bump metallisation,UBM)係因應各種技術方法而發展，例如，晶圓高度縮小化、電力訊號完整和金屬堆疊可靠性。晶圓越來越薄並，因此，任何施用的金屬堆疊會造成所不欲的晶圓翹曲。
根據以前技藝，Cu或Al層先塗覆在晶圓表面上，然後將Ni-P和Pd(和任意的Au)鍍在晶圓表面的個別部件(“墊”)上。以前技藝的層堆疊之澱積內應力會造成晶圓翹曲。
因此，本發明之目的係提供供可黏合的晶圓表面用的Ni-P/Pd堆疊，其應力減低並藉此而儘量減低或防止晶圓翹曲。
 [發明總論]
本發明的目的係藉一種具有可黏合的金屬塗層之基板而達到，該基板的Al或Cu表面上依序包含：(a)Ni-P層，(b)Pd層，和任意地，(c)Au層，其中該Ni-Pd層(a)的厚度是0.2至10微米，該Pd層(b)的厚度是0.05至10微米，而該任意的Au層(c)的厚度是0.01至0.5微米，且其中該Ni-P層(a)的P含量為10.5至14重量%。所得Ni-P/P堆疊(層(a)和(b))的(抗拉)澱積內應力通常不高於34.48MPa(5,000psi)。
[發明之詳細說明]
本發明基於驚訝地發現到，藉由選擇個別堆疊的個別層厚度使其在前述範圍內及藉由選擇該Ni-P層的前述磷含量，所得Ni-P/Pd堆疊的澱積內應力將不高於34.48MPa(5,000psi)或甚至更低且經此堆疊塗覆的晶圓之翹曲可因此而微小化或完全避免。
根據本發明之堆疊中，該Ni-P層的厚度是0.2至10微米，以0.5至3.0微米為佳。
該Pd層的厚度在0.05至1.0微米的範圍內，以0.1至0.5微米為佳。
該任意的Au層的厚度是0.01至0.5微米，以0.01至0.3微米為佳。
該Ni-P層的P含量在10.5至14重量%的範圍內。下文中，有時將此層稱為“高磷Ni-P層”。
該高磷Ni-P層的澱積內應力通常變小(0至34.48MPa(0至5,000psi))。磷含量介於4重量%和約10.5重量%之間(“中磷”)的Ni-P層的應力有彈性，而高於10.5重量%(“高磷”)的高磷含量得到較小應力(請參考W.Riedel,“Electroless Nickel Plating”,Finishing Publications Ltd.,1991,p.111)。
Pd層的澱積內抗拉應力以不高於137.9MPa(20,000psi)為佳，不高於103.4MPa(15,000psi)更佳，且不高於68.96MPa(10,000psi)最佳。此處，注意到以前技藝的Ni-P/Pd堆疊(請參考如美國專利案第4,424,241號)之Pd層的膜抗拉應力高至206.9至344.8MPa(30,000至50,000psi)。
個別層的澱積內應力值可藉在與製造堆疊的相同條件下將層單獨澱積在銅基板(測試條)上，及藉市售測定裝置測定個別層的應力而測得。
然後，更詳細地描述根據本發明之包含供可黏合的晶圓表面用之應力減低的Ni-P/Pd堆疊之基板之製備： 其包含所謂的“底部凸塊金屬化”(UBM)，其係就近來有關晶圓高度縮小化、電力訊號完整和金屬堆疊可靠性的需求而開發。
此UBM法通常可分成四個不同的部分。
第一部分包含前處理並包括Al/Al-合金和Cu墊的表面製備。對於Al和Al合金之前處理，可利用各種浸鋅處理，例如XenolyteTM cleaner ACATM 、XenolyteTM Etch MATM 、XenolyteTM CFATM 或XenolyteTM CF(皆可得自Atotech Deutschland GmbH)，其符合不含氰化物化學品的工業標準。
UBM法的第二部分包含無電鎳鍍覆。
在此無電鎳鍍覆的步驟中，可使用的水性無電鎳鍍覆溶液包含鎳鹽和次磷酸或其浸液可溶性鹽(選自次磷酸鈉、次磷酸鉀和次磷酸銨)。此溶液應不含添加的次磷酸鎳，且不含可形成不溶性正亞磷酸鹽的鹼金屬或鹼土金屬離子。
在該無電鎳溶液中，使用的操作鎳離子濃度通常由約1至約18克/升，以約3至約9克/升為佳。以不同方式陳述，鎳離子濃度將在0.02至約0.3莫耳/升的範圍內，或較佳地在約0.05至約0.15莫耳/升的範圍內。
該鎳鍍覆溶液亦含有衍生自自次磷酸或其浸液可溶性鹽(如，次磷酸鈉、次磷酸鉀和次磷酸銨)的次磷酸鹽離子作為還原劑。
鍍覆浸液中的還原劑用量係至少足以符合化學計量還原無電鎳反應中的鎳陽離子以釋出鎳金屬，且此濃度通常在約0.05至約1.0莫耳/升的範圍內。以不同方式陳述，引入此次磷酸鹽還原性離子以使得次磷酸鹽離子濃度約2至約60克/升，或由約12至50克/升，或甚至由約20至約45克/升。慣用實施方式中，在反應期間內重新補充此還原劑。
本發明之含有鎳和磷還原劑(如，次磷酸鹽或其鈉、鉀或銨鹽)的鍍覆溶液在基板上連續澱積鎳－磷合金塗層。通常約10.5重量%至約14重量%的高磷含量(“高磷”)係藉由在pH介於約3至約6(以pH由約4至5.6為佳)進行鍍覆操作以提供具有高磷含量的合金澱積而得到。
可含括於鎳鍍覆溶液中的其他材料是例如緩衝劑、螯合或錯合劑、潤濕劑、加速劑、抑制劑、亮光劑...等。這些材料為此技藝已知者。
因此，一體系中，錯合劑或錯合劑混合物可含括於鍍覆溶液中。在此技藝中亦將此錯合劑稱為螯合劑。此錯合劑在此鍍覆溶液中的含量必須足以錯合存在於溶液中的鎳離子及進一步使鍍覆法期間內形成的次磷酸鹽分解產物安定。通常，此錯合劑的用量高至約200克/升，更常是約15至約75克/升。另一體系中，此錯合劑的存在量由約20至約60克/升。
一體系中，羧酸、多元胺或磺酸或它們的混合物可以作為鎳錯合或螯合劑。有用的羧酸包括單－、二－、三－或四－羧酸。此羧酸可經各式各樣的取代基(如，羥基或胺基)取代且此酸可以它們的鈉、鉀或銨鹽形式引至鍍覆溶液中。一些錯合劑(如，醋酸)亦可作為緩衝劑，且考慮它們的雙重官能性，此添加劑組份的適當濃度可經最適化而用於任何鍍覆溶液。
可作為本發明之溶液中之鎳錯合或螯合劑的羧酸的例子包括：單羧酸，如，醋酸、羥基乙酸(乙醇酸)、胺基乙酸(甘胺酸)、2-胺基丙酸(丙胺酸)、2-羥基丙酸(乳酸)；二羧酸，如，丁二酸、胺基丁二酸(天冬胺酸)、羥基丁二酸(蘋果酸)、丙二酸、酒石酸；三羧酸，如，2-羥基-1,2,3-丙三酸(檸檬酸)；和四羧酸，如，乙二胺四醋酸(EDTA)。一體系中，前述錯合/螯合劑中的2或多者之混合物用於鎳鍍覆溶液。
本發明之水性無電鎳鍍覆浸液可在前述pH範圍內操作。由於鍍覆溶液在操作期間內，有因為形成氫離子而變得較具酸性的趨勢，所以可以於浸液中定期或連續添加可溶性和浸液可相容的鹼性物質(如，鈉、鉀或銨的氫氧化物、碳酸鹽和碳酸氫鹽)而調整pH。可藉添加用量至多約30克/升且通常由約2至約10克/升之各式各樣的緩衝化合物(如，醋酸、丙酸、硼酸之類)以改良鍍覆溶液之操作pH的安定性。如前述者，一些緩衝用化合物(如，醋酸和丙酸)亦可作為錯合劑。
無電鎳鍍覆溶液亦可包括此技藝目前知道的類型之有機和/或無機安定劑，包括鉛離子、鎘離子、錫離子、鉍離子、銻離子和鋅離子，其可便利地以浸液可溶和可相容的鹽形式(如，醋酸鹽...等)引入。可用於無電鍍覆溶液的有機安定劑包括含硫化合物，例如，硫脲、硫醇、磺酸鹽、硫氰酸鹽...等。此安定劑可以小量使用，如，溶液的0.05至約5ppm，更常是約0.1至2或3ppm。
此鎳鍍覆溶液可任意地使用目前已知之可溶於並可與其他浸液成份相容的各種類型中之任何類型的一或多種潤濕劑。一體系中，使用此潤濕劑防止或阻礙鎳合金澱積物表面腐蝕，且此潤濕劑用量可高達約1克/升。
待鍍覆的基板與鍍覆溶液於至少約40℃至溶液的沸點之溫度接觸。一體系中，於溫度約70℃至約95℃，更常是溫度約80℃至約90℃，使用酸性類型的無電鎳鍍覆溶液。鹼性類型的無電鎳鍍覆溶液通常在寬操作範圍內操作，但通常於比酸性無電鍍覆溶液為低的溫度操作。
無電鎳溶液與待鍍覆的基板的接觸時間取決於鎳－磷合金的所欲厚度。通常，此接觸時間可由1至30分鐘。
鎳合金的鍍覆期間內，通常施以溫和攪動，且此攪動可為溫和空氣攪動、機械攪動、浸液藉抽吸循環、滾筒鍍覆之旋轉...等。此鍍覆溶液亦可經定期或連續過濾處理以降低其中的污染物含量。一些體系中，亦可定期或連續重新補充浸液的構份，以維持構份濃度，且特別地，維持鎳離子和次磷酸離子的濃度，並使pH在所欲限制內。
此UBM法的第三個步驟包含自無電鈀鍍覆浸液鍍覆。
此無電鈀浸液述於EP 0 698 130 B1且本發明以添加的安定劑加以修飾。令人感興趣地，其可以未經先前活化處理而用以將Pd層鍍覆在高磷Ni-P層上。但是，特別是用於在較低溫度的Pd鍍覆，可任意地在無電Pd鍍覆步驟之前進行活化高磷Ni-P層的步驟。
用於無電Pd鍍覆的較佳浸液參數如下：
pH：　5至6.5為佳，5.6至6.0更佳
浸液溫度：70至90℃為佳，82至87℃更佳
浸泡時間：　3至20分鐘為佳，5至10分鐘更佳
外加的安定劑：10至500毫克/升為佳，100至300毫克/升更佳
如果在無電Pd鍍覆步驟之前進行活化步驟，則Pd鍍覆浸液溫度可低至約40℃(且至高約95℃)。此活化處理可以，例如，藉所謂的可離子化的Pd活化劑而達成，該活化劑通常為酸性，含有Pd2+ 來源，如，PdCl2 或PdSO4 ，並在Ni-P層上澱積元素Pd的晶種層。此活化劑為嫻熟者已知者且以溶液形式販售(商標名Xenolyte Activator ACU1TM ，Atotech Deutschland GmbH的產品)。所謂的膠態酸性活化劑(其中Pd籠被Sn所環繞)亦為已知者且可使用。
可以使用述於EP 0 698 130之無電鈀浸液的陳述中之外加的安定劑，無需使用任何額外的活化劑，將鈀澱積在高磷Ni-P層上。此外，此安定劑使得鈀的無電鍍覆於溫度介於70℃和90℃之間進行，此使得澱積的鈀層的內應力減低。已知的無電鈀浸液於如此高的浸液溫度之壽命短，此為工業應用無法接受者。外加的安定劑選自磺醯亞胺、多苯硫醚、嘧啶、多元醇和無機錯合劑(如，rhodanide)。較佳的磺醯亞胺係糖精，較佳的嘧啶是菸鹼醯胺、嘧啶-3-磺酸、菸鹼酸、2-羥基吡啶和菸鹼。較佳的多元醇是聚乙二醇、聚丙二醇、聚乙二醇－聚丙二醇共聚物和它們的衍生物。
最後，任意的金層可以鍍覆在Ni-P/Pd堆疊上。用於此目的，可以使用以前技藝已知的無電金鍍覆電解質。任意的金層在鈀層上方的厚度是0.01至0.5微米，以0.05至0.3微米為佳。任意的金層藉浸泡法澱積為最佳。此浸泡法述於，例如，H.Kaiser,Edelmetallschichten:Abscheidung,Eigenschaften,Anwendungen;E. Leuze Verlag,2002,p.43。適合用於無電金鍍覆的浸液為市售品，商標名為Aurotech SFplusTM (T=80至90℃；pH=4.5至6.0；浸泡時間=7至15分鐘；0.5至2克/升Au(K[Au(CN)2 ]形式))。
因此，如果使用經Al塗覆的晶圓作為本發明的起始基板，則此方法之步驟包含清潔、蝕刻、浸鋅(作為前處理步驟)，然後為鎳鍍覆，高磷Ni-Pd層的任意活化、鈀鍍覆和，任意地，金鍍覆。
因此，如果使用經Cu塗覆的晶圓作為本發明的起始基板，則前處理步驟包含清潔、任意地蝕刻、和Pd活化處理，然後再度為鎳鍍覆，高磷Ni-Pd層的任意活化、鈀鍍覆和，任意地，金鍍覆。
藉下列實例和比較例進一步說明本發明。
個別Pd或Ni-P層和Ni-P/Pd堆疊的內應力值係以“Deposit Stress Analyzer”(型號683；Speciality Testing ＆ Development Co.)測定。由相同公司得到之特別指定的試驗條經Ni-P、Pd和Ni-P/Pd層塗覆並根據設備供應商描述的程序試驗。
實例1(比較例)
自此技藝之包含1克/升Pd2+ 離子、27.6克/升甲酸和3克/升乙二胺之組成物的浸液(揭示於EP 0 698 130)於pH 5.5和溫度為55℃在中磷Ni-P層(XenolyteTM Ni MTM ，Atotech Deutschland GmbH)上鍍覆純Pd層。
經Ni-P鍍覆(1.3微米)的Cu基板在Pd浸液中的浸泡時間為5分鐘。所得的堆疊在抗拉方向的應力是103.4MPa(15,000psi)(用以計算應力，將Ni-P和Pd層厚度的和列入考慮；Pd層厚度是0.27微米)。
實例2(比較例)
自應力減低的Pd浸液(揭示於美國專利案第4,424,241號)將純Pd層鍍覆在覆在Cu基板上的中磷Ni-P層(XenolyteTM Ni MTM ，Atotech Deutschland GmbH)上。此Cu基板在XenolyteTM Ni MTM 浸液中浸泡5分鐘且於之後在鈀浸液中以去離子水沖洗5分鐘。
此Pd浸液含有：
Pd2+ 離子　1克/升
乙二胺　3克/升
甲酸鈉　40.8克/升
糖精鈉鹽水合物　0.2克/升(以無水物為基礎)
其pH為5.8且浸液溫度為85℃。
所得Ni-P/Pd堆疊的Ni-P層厚度為0.9微米且Pd層厚度為0.21微米。觀察到的總堆疊抗張應力是53.79MPa(7,800psi)。
實例3
測定在具有Ni-P層的Cu上之Ni-P/Pd堆疊(其得自高磷Ni-P浸液和自實例2中使用之應力減低的Pd浸液鍍覆的純Pd層)的膜應力。
此Pd浸液含有：
Ni2+ 離子　6克/升
次磷酸Na‧H2 O　30克/升
蘋果酸　10克/升
丁二酸　18克/升
乳酸　30克/升
Pb離子　0.2毫克/升
其pH為4.8且浸液溫度為85℃。
所得Ni-P層厚度為0.92微米且Pd層厚度為0.19微米。所得堆疊的應力值是21.38MPa(3,100psi)。
實例4
在Ni-P層以Xenolyte Activator ACU1(Atotech Deutschland GmbH的產品)進行額外的活化處理之後，得自實例1的Pd浸液之Pd層鍍覆在高磷Ni-P層(來自實例3中使用的高磷Ni-P浸液)上。
藉此得到的堆疊物之平均Ni-P層厚度是0.84微米，Pd層厚度是0.25微米且總抗拉應力值是27.58MPa(4,000psi)。在Pd鍍覆之前，Ni-P層之壓縮方向的應力是34.48MPa(5,000psi)。
實例5
得自Ni-P浸液(關於浸液組成，請參考實例3)的高磷Ni層在Cu上得到的壓縮應力自厚度為1微米(壓縮27.58MPa(4,000psi))至至少3微米(壓縮25.52MPa(3,700psi))略為降低。以組成述於實例2的浸液鍍覆0.3微米Pd層之後，1微米Ni-P的總堆疊物抗拉應力是20.69MPa(3,000psi)而3微米Ni-P的總堆疊物抗拉應力是21.38MPa(3,100psi)。
實例6(比較例)
具有實例1所述組成之先前技藝已知的浸液之Pd層於pH 5.5，溫度為55℃時直接澱積在以Xenolyte Activator ACU1(Atotech Deutschland GmbH的產品)進行過活化處理Cu上，其平均應力值是241.1MPa(35,000psi)。
實例7
來自實例2中使用之應力減低的浸液的Pd層於pH 5.8、溫度為85℃時直接澱積在以Xenolyte Activator ACU1(Atotech Deutschland GmbH的產品)進行過活化處理Cu基板上，得到平均應力值是89.65MPa(13,000psi)。此Pd浸液再於此溫度安定至少48小時，而在85℃3小時之後，實例1之先前技術已知的浸液有析出(plate out)情況。

Claims (8)

  1. 一種具有可黏合的金屬塗層之基板，其Al或Cu表面上依序包含：(a)Ni-P層，及(b)Pd層，其中該Ni-P層(a)的厚度是0.2至10微米，及該Pd層(b)的厚度是0.05至1.0微米，其中該Ni-P層(a)的P含量為10.5至14重量%，且其中由Ni-P層(a)和Pd層(b)所組成的堆疊之澱積內應力不高於34.48MPa(5,000psi)。
  2. 如申請專利範圍第1項之基板，其中該可黏合的金屬塗層於Al或Cu表面上依序包括(a)Ni-P層、(b)Pd層、和(c)Au層，而該Au層(c)的厚度是0.01至0.5微米。
  3. 如申請專利範圍第2項之基板，其中該Ni-P層(a)的厚度是0.5至3.0微米，該Pd層(b)的厚度是0.1至0.5微米，而該Au層(c)的厚度是0.01至0.3微米。
  4. 如申請專利範圍第1項之基板，其中該Pd層(b)的澱積內抗拉應力不大於137.9MPa(20,000psi)。
  5. 一種製造如申請專利範圍第1項之基板的方法，其包含下列步驟：(i)將具有Al或Cu表面的基板浸在包含鎳鹽和次磷酸或其浸液可溶性鹽(選自次磷酸鈉、次磷酸鉀和次磷酸銨)的Ni-P鍍液中，其中該溶液未添加次 磷酸鎳，且不含可形成不溶性正亞磷酸鹽的鹼金屬或鹼土金屬離子，在溫度由約70℃至約95℃且pH由約3至約6的情況下浸泡1至30分鐘，以在基板上得到Ni-P層，和(ii)將步驟(i)中得到之經Ni-P塗覆的基板浸在包含至少一種鈀離子來源、至少一種還原劑、至少一種錯合劑和10至500毫克/升的至少一種磺醯亞胺安定劑添加劑之Pd鍍液中，在pH5至6.5的Pd鍍液中浸泡3至20分鐘以在基板上得到Pd層，其中該Pd層係澱積在步驟(i)中所得的Ni-P層上，且在澱積Pd層之前，Ni-P層未經任何活化處理，且步驟(ii)係在由約70至約90℃的溫度進行，或其中該Pd層係在Ni-P層歷經活化處理之後澱積在步驟(i)中所得的Ni-P層上，且步驟(ii)係在由約40至約95℃的溫度進行。
  6. 如申請專利範圍第5項之方法，其中該基板是Al晶圓，且在鍍Ni-P層(步驟(i))之前，該晶圓表面經清潔和蝕刻或接著鋅化處理。
  7. 如申請專利範圍第5項之方法，其中該基板是Cu晶圓，且在鍍Ni-P層(步驟(i))之前，該晶圓表面經清潔，任意地，蝕刻，然後Pd活化處理。
  8. 如申請專利範圍第5至7項中任一項之方法，其中進一步包含：(iii)該經Ni-P層和Pd層塗覆的基板浸在Au 鍍液中的步驟。
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