TWI778944B - 沉積方法 - Google Patents

沉積方法 Download PDF

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TWI778944B
TWI778944B TW105132593A TW105132593A TWI778944B TW I778944 B TWI778944 B TW I778944B TW 105132593 A TW105132593 A TW 105132593A TW 105132593 A TW105132593 A TW 105132593A TW I778944 B TWI778944 B TW I778944B
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layer
additive
aluminum nitride
piezoelectric device
film
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史帝芬Ｒ 柏吉斯
隆達 辛德曼
阿密特 瑞斯托吉
史考特 海摩爾
康斯坦尼 法拉果斯
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英商Ｓｐｔｓ科技公司
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Abstract

依據本發明，提供一種藉由脈衝直流反應性濺鍍沉積含有至少一選自Sc、Y、Ti、Cr、Mg及Hf之添加元素的一含添加劑之氮化鋁膜之方法，此方法包含步驟：藉由脈衝直流反應性濺鍍，以一偏壓電力施用於一膜撐體，使此含添加劑之氮化鋁膜之一第一層沉積於此膜層體上；以及藉由脈衝直流反應性濺鍍，無偏壓電力供應至此膜撐體，或以低於在濺鍍沉積第一層期間施用之偏壓電力之一偏壓電力施用於此膜撐體，使此含添加劑的氮化鋁膜之一第二層沉積於第一層上，第二層具有與第一層相同之組成物。

Description

沉積方法
本發明係有關於一種藉由脈衝直流反應性濺鍍一含添加劑的氮化鋁膜之沉積方法。本發明亦係有關於此等膜本身及包含此等膜之壓電裝置。
對生產AlN薄膜有興趣，特別係因為其等之壓電性質。一可能之重要應用係於體聲波(BAW)頻率共振裝置。BAW裝置係由被夾於二電極間之一共振壓電層(通常係氮化鋁)所組成。此係行動通訊產業之一科技推動者，因為其等可被用以製造具高高抑制、低損耗，及極低溫度漂移之小且便宜之精密濾波器。經濺鍍之氮化鋁係廣泛用於製造BAW濾波器，主要係因為其相對較高之壓電常數，其於一般四面積鍵結二元半導體間係最高。但是，缺點係氮化鋁膜固有地具有相當低的電機耦合係數，此限制含氮化鋁之濾波器可達成之頻帶寬度。
為了改良氮化鋁薄膜的壓電性質，已建議併入諸如Sc、Y、Ti、Cr、Mg及Hf之金屬添加劑。例如，鈧可於犧牲鋁之情況下併入合金中。因為Sc-N鍵係比1.9A之Al-N鍵長度長0.35A，由於此鍵長度差異，於此膜產生一應力。因為此多變鍵長度，合金材料燮得更軟。但是，藉由較大單位晶胞，於電機耦合係數具顯著改良。此可於圖1看出，其係以與鈍氮化鋁膜相比之Al93.9Sc6.1N的應力百分率顯示 電機耦合係數。於0膜應力，與純氮化鋁膜之6.2%的耦合係數相比，Al93.9Sc6.1N膜展現約8%之耦合係數。此表示於耦合係數約30%之相對改良。需瞭解當組成物以Al100-xScxN型式表示時，數值100-x及x係以百分率表示，且以百分率表示之x以化學計量化學術語可等同於0.0x。
圖1中亦可看出一較高耦合係數係以一更可拉伸之膜達成。但是，受高應力之膜係不適於大規模之BAW製造，因為其等易破裂及剝離。此會造成其後於製造方法上有關於可靠度之問題。比約300mm更厚之AlScN膜觀察到的另外問題係其等隨著增加之鈧含量，其等易遭受建構品質降級。由於形成自膜表面突起之不定向顆粒，其係以表面粗糙表現。於三元氮化物Al100-xScxN，具有數個競爭性之穩定相。但是，纖綠礦Al100-xScxN型式係一非平衡態。因此，於應力或鈧濃度大量改變，例如，於顆粒邊界，會於一另外結晶位向相對輕易地成核。例如，於圖2，吾等呈現使用相同PVD沉積參數沉積之典型(a)1.5微米氮化鋁膜及(b)1.5微米Al94Sc6N膜之SEM影像。圖2(a)顯示之氮化鋁膜係平滑、無缺陷且相對無特徵，而圖2(b)顯示之自三元鈧合金形成之膜具有高密度之嵌入膜內之錐體狀結晶。此等缺陷用以降低此等膜之耦合係數及品質因數。此外，此等缺陷對進一步之下游加工，諸如，膜微影術/蝕刻及其後之層沉積於此膜頂面上，造成問題。雖然明顯缺陷量，AlScN膜展現良好之c-軸定向，且少於1.50之測得的XRD(0002)FWHM(半峰全寬)係可與純氮化鋁膜之結果相比擬。此確認一濺鍍AlScN膜可為用於製造高性能BAW濾波器之一優異候選者，只要能發現一種降低缺陷量之方法。為了考量大量商業化之BAW生產，每100平方微米少於20之缺陷量係需要的。最終商業化之進一步條件可為此方法係以一經濟上可行之方式進行。
本發明於其至少一些實施例係解決上述問題之一或多者。
依據本發明之一方面，提供一種藉由脈衝直流反應性 濺鍍沉積含有至少一選自Sc、Y、Ti、Cr、Mg及Hf之添加元素的一含添加劑之氮化鋁膜之方法，此方法包含步驟：藉由脈衝直流反應性濺鍍，以一偏壓電力施用於一膜撐體，使此含添加劑之氮化鋁膜之一第一層沉積於此膜層體上；以及藉由脈衝直流反應性濺鍍，無偏壓電力供應至此膜撐體，或以低於在濺鍍沉積第一層期間施用之偏壓電力之一偏壓電力施用於此膜撐體，使此含添加劑的氮化鋁膜之一第二層沉積於第一層上，第二層具有與第一層相同之組成物。
以此方式，具有相對較低缺陷量之改良膜可被獲得。
此至少一添加元素可以0.5原子%至40原子%之範圍，較佳係2原子%至15原子%之範圍，且最佳係3原子%至10原子%之範圍的量存在。於此等濃度，此化合物可被認為係不同於一摻雜式AlN的一合金。
含添加劑之氮化鋁膜可含有選自Sc、Y、Ti、Cr、Mg及Hf之一添加元素。於此等實施例，含添加劑之氮化鋁膜可為一二元合金。較佳地，含添加劑之氮化鋁膜係Al1-xScxN。
第一層可使用大於70W之偏壓電力沉積。第一層可使用少於250之偏壓電力沉積。第一層可使用75至200W之範圍的偏壓電力沉積。
第二層可使用少於125W之偏壓電力沉積。
施用至膜撐體之偏壓電力可為一射頻電源(RF power)。
反應性濺鍍可使用一磁控管實施。
反應性濺鍍可使用單一標靶實施。一般，此標靶會係由鋁及至少一添加元素形成之一複合標靶。使用複數個標靶係可能，但可能較不具經濟吸引力。
反應性濺鍍可於一包含氮之氣體氛圍中實施。此氣體氛圍可包含氮及諸如氬之惰性氣體的混合物。
一般，第一層係比第二層更不可拉伸。雖不欲受任何 特別理論或推測所限制，但相信於沉積第一層期間使用一較高偏壓電力造成第一層係比第二層更不可拉伸。再次地雖不欲受任何特別理論或推測所限制，但相信第一層助於調準第二層之生長，此會造成具有相對較低缺陷量之一膜。
第一層可具有少於250nm之厚度。第一層可具有20至150nm之範圍的厚度。
含添加劑之氮化鋁膜可具有0.3微米或更大之厚度。較佳地，含添加劑之氮化鋁膜具有0.6微米或更大之厚度。更佳地，含添加劑之氮化鋁膜具有1.0微米或更大之厚度。含添加劑之氮化鋁膜可具有2.0微米或更少之厚度。但是，更厚之膜係於本發明範圍內。
於某些實施例，無進一步之含有氮化鋁的層被沉積於第二層上。換言之，含添加劑之氮化鋁膜係基本上由第一層及第二層所組成。
於其它實施例，濺鍍沉積第一層及第二層之步驟係循環地實施，使得含添加劑之氮化鋁膜包含四或更多層。例如，該等步驟可循環地實施兩次產生包含四層的一含添加劑之氮化鋁膜，或此等步驟可循環地實施三次，使得含添加劑之氮化鋁膜包含六層。其它變化係於本發明範圍內。
依據本發明之第二方面，提供藉由依據本發明第一方面之方法製造之一種含添加劑之氮化鋁膜。
依據本發明之第三方面，提供一種含添加劑之氮化鋁膜，其含有至少一選自Sc、Y、Ti、Cr、Mg及Hf之添加元素，此膜包含具相同組成物之第一層及第二層，其中，第一層及第二層每一者具有一相關聯應力，且第一層之應力係比第二層之應力有更小之正值。
依據本發明第四方面，提供一種壓電裝置，其包含依據本發明第二或第三方面之一含添加劑之氮化鋁膜。壓電裝置可為一BAW裝置。一般，BAW裝置包含一第一電極及一第二電極，且含添加劑之氮化鋁膜係沉積於第一電極與第二電極之間。
雖然本發明已於上作說明，但其係擴散至上述特徵或於下列說明、圖式，或申請專利範圍中之任何發明組合。例如，與本發明之一方面有關所述之任何特徵係被認為亦與本發明之另外方面有關作揭露。
依據本發明之膜、裝置，及方法之實施例現將參考所附圖式作說明，其中：圖1顯示Al93.9Sc6.1N及純AlN膜之為膜應力的函數之耦合係數；圖2顯示於相同製程條件下沉積之典型1.3微米厚之(a)AlN膜及(b)Al94Sc6N膜之表面的SEM影像；圖3顯示連續沉積及二步驟沉積的Al94Sc6N膜之為平板射頻偏壓的函數之缺陷密度及膜應力；圖4顯示以一高偏壓起始步驟之一AlScN膜的表面於此膜之(a)中央及(b)邊緣之SEM影像；圖5顯示使用連續沉積而沉積之一AlScN膜的表面於此膜之(a)中央及(b)邊緣之SEM影像；圖6顯示使用連續沉積及使用具有各種第一沉積膜厚度之二步驟沉積而製造之1200nmAl94Sc6N膜的缺陷密度；以及圖7顯示(a)單一習知技藝連續沉積，(b)使用三個循環之具有高及低射頻偏壓之沉積，及(c)使用具有高射頻偏壓第一層之第一步驟的二步驟沉積而沉積之AlScN膜的缺陷量。
發明人已發現用於濺鍍沉積一含添加劑之氮化鋁膜之一有利方法。含添加劑之氮化鋁膜含有至少一選自Sc、Y、Ti、Cr、Mg及Hf之添加元素。結果係於下有關於其中x=6之Al100-xScxN膜作呈現。但是，此方法係可普遍地施用於於上探討之其它添加元素及此膜內之其它添加濃度。含添加劑之氮化鋁膜係使用反應性脈衝直流濺鍍沉積自一Al100-x Xx標靶產生，其中，X表示添加元素。於第一步驟， 含添加劑之氮化鋁膜之第一層係濺鍍沉積於一膜撐體上，諸如，一平板上。射頻偏壓電力係於沉積第一層期間施用於平板。然後，含添加劑之氮化鋁膜之第二層係沉積於第一層上。於沉積第二層期間，少於在沉積第一層期間施用之射頻偏壓電力的一射頻偏壓電力施用於平板。另外，第二層可於無施用於平板之射頻偏壓電力下沉積。
膜係藉由脈衝直流反應性濺鍍而沉積。一複合式鋁鈧標靶可用於在氬及氮氛圍中之濺鍍。有關於可被使用或可適於用本發明之裝置的一般細節係熟習此項藝之讀者所熟知，諸如，於申請人之歐洲專利申請案EP2871259中所述之裝置，此案之全部內容在此被併入以供參考。
已發現可使用本發明大量降低單一出平面結晶缺陷的生長。此能使膜以一平滑表面及足夠低之缺陷量沉積，而能成功地大量製造含添加劑之氮化鋁合金膜。此亦為成功地大量製造諸如BAW濾波器之相關壓電裝置鋪路。相對較厚的含添加劑之氮化鋁膜可以此方式沉積，例如，具有1-2微米範圍之厚度的膜。但是，具有較小或較大厚度之膜亦可被沉積。一般，第一層之厚度係相對較小。第一層之代表性但非限制性的厚度範圍係約20-100nm。
1200nmAl0.94Sc0.06N膜係使用此方法使用單一標靶濺鍍沉積。此等膜包含於平板上使用一高射頻偏壓產生之一90nm第一層，及於平板上使用一低射頻偏壓沉積之一1110nm第二層。具有此組成物之膜亦使用習知技藝所知型式之一連續單濺鍍沉積而沉積。於150mm晶圓上進行之實驗的典型沉積參數係顯示於表1中。典型製程壓力係於4至12毫托耳。超過60nm/min之沉積速率使用此等條件達成。
Figure 105132593-A0305-02-0009-1
圖3顯示連續單一沉積及本發明之二步驟方法二者之膜的缺陷密度(以每100平方微米之缺陷數)及應力(MPa)。數據係以平板上之施用射頻偏壓(80W，100W，120W)的函數顯示。於圖3，以陰影線長條顯示之缺陷度數據係有關於藉由連續單一沉積產生之膜。可看到增加射頻偏壓改良缺陷度，即使缺陷密度保持高於20個缺陷/100平方微米。但是，亦可看出於高射頻偏壓之改良缺陷度造成一壓縮膜(連續單一沉積膜之應力數數係以黑色方塊顯示)。相反地，本發明之二步驟濺鍍沉積方法造成對所有射頻偏壓電力(無陰影線之長條)係少於20個缺陷/100平方微米之優異缺陷度值。藉由此二步驟方法產生之膜的整體應力係可變的，可看到範圍係從相當強的拉伸值至相當強的壓縮值(空白方塊)。此能讓使用者選擇沉積膜之壓力同時獲得優異缺陷度值。
膜品質之改良可於圖4及5中清楚看到。圖4顯示使用本發明之二步驟方法沉積之Al0.94Sc0.06N膜於中央及邊緣處之SEM影像。圖5顯示使用連續濺鍍沉積而沉積之拉伸Al0.94Sc0.06N膜之中央及邊緣處之SEM影像。圖3顯示之缺陷密度數據係於此等膜之中央處測得。缺陷度於此等膜之中央與邊緣之間會相當大量地變化。此可能與於藉由磁控管濺鍍系統沉積之膜各處固有發生之從中央至邊緣之應力 變化有關。此可被歸因於藉由DC磁控管造成之膜各處之電漿密度變化及平板各處之任何從中央至邊緣之溫度變化。表2顯示藉由單一連續沉積及藉由本發明之二步驟方法產生的膜之從中央至邊緣的缺陷密度變化。表2顯示缺陷密度對於二步驟方法於膜之整個區域係維持低於20個缺陷/100平方微米。再者，此等膜之應力係可從高壓縮至高拉伸作調整。事實上，最低缺陷密度係於產生之最具拉伸性的膜觀察到。此膜可能亦展現最高耦合係數。此外，所有此等膜展現具有FWHM<1.5°之優異c-軸位向。此滿足於大量製造環境生產BAW之進一步要求。表2亦顯示於藉由單一連續沉積生產之膜各處觀察到之缺陷密度係比使用本發明之二步驟方法生產之所有膜更差。
Figure 105132593-A0305-02-0010-2
亦實施實驗研究第一層之厚度對使用二步驟方法產生之膜的缺陷密度之作用。一般製程條件被用以生產適度拉伸(約200MPa)之Al0.94Sc0.06N膜，其中，第一層之厚度係從25nm至90nm變化。圖6亦顯示使用連續單一沉積技術沉積之具有相同組成物及厚度之膜上測得之缺陷密度。被研究之所有厚的厚度係1200nm。使用本發明之二步驟方法生產之所有膜對於所有第一層度於膜品質係顯示顯著改良。與使用單一連續濺鍍沉積技術產生之膜相比，缺陷密度係以約10：1 降低。優異數據係於第一層(其係藉由於平板上之高射頻偏壓產生)係僅25nm厚時獲得。進一步增加第一層之厚度似乎未於缺陷密度造成統計上之顯著改良。
上述實驗係有關於由二層的含添加劑之氮化鋁膜構成之膜，其中，第一層係使用相對較高射頻電力施用於平板而濺鍍沉積，其後，使用較低射頻偏壓電力濺鍍沉積第二層。亦於本發明範圍內係沉積含添加劑之氮化鋁膜之另外層。特別地，可以一循環方式實施第一及第二層之濺鍍沉積。
實施實驗研究膜缺陷密度是否能利用使用一相對較高射頻偏壓及一較低射頻偏壓之交替式步驟而改良。AlScN膜係以藉由具有於200W之射頻偏壓電力之一第一步驟及於80W之射頻偏壓電力之一第二步驟的三個連續循環產生之堆疊物而沉積。高射頻偏壓電力步驟被實施產生一50nm厚之層，且較低射頻偏壓電力步驟被實施產生一400nm厚之層。此等循環被實施，使得此膜包含六層，其中之三層係使用高射頻偏壓產生之相對較薄的層，且三層係使用較低射頻偏壓產生之相對較厚的層。缺陷密度係於此等膜之中央、中間部份，及邊緣處測量，且結果係顯示於圖7(b)。作為比較，圖7(a)顯示自使用單一連續沉積獲得之具有相同組成物及相似厚度的膜獲得之缺陷密度數據。圖7(c)顯示使用本發明之二步驟方法產生之具有相同組成物及相似厚度之膜獲得之缺陷密度數據，其中，一50nm厚之第一層係使用150W之射頻偏壓電力沉積。以缺陷密度而言，最佳結果係使用二步驟方法獲得。但是，六層堆疊物觀察到之缺陷密度亦優異，且表現出對於藉由單一連續沉積而獲得之膜相當大改良。認為循環式方法可特別用於生產相對較厚的含添加劑之氮化鋁膜，例如，具有大於1.5微米總厚度之膜。
雖不受任何特別理論或推測所限制，但相信於沉積第一層期間使用較高偏壓電力能造成第一層係比第二層更不可拉伸。再次地雖不欲受任何特別理論或推測所限制，但相信第一層於第二層之 濺鍍沉積製程期間助於調準膜生長。此等層之製程條件可由使用者作改變，以便使此膜之一或多種性質最佳化，例如，膜應力或電機耦合係數。本發明之含添加劑之氮化鋁膜可用於廣泛範圍之最終應用，其中，BAW裝置係一例子。

Claims (17)

  1. 一種形成一壓電裝置(piezoelectric device)之一含添加劑之氮化鋁膜之濺鍍方法，此方法包含：藉由施加脈衝直流電流(pulsed DC electrical current)至包含鋁及至少一添加元素之一單一目標並以一偏壓電力(electrical bias power)施用於該壓電裝置之一膜撐體而沉積含有該至少一添加元素之氮化鋁至該壓電裝置之該膜撐體，從而自該目標濺鍍材料並形成該壓電裝置之該含添加劑之氮化鋁膜之一第一層；以及藉由施加脈衝直流電流至該目標並以無偏壓電力施加於該膜撐體或以低於形成該第一層期間所施加之該偏壓電力之一偏壓電力施加於該壓電裝置之該膜撐體而沉積含有該至少一添加元素之氮化鋁至該第一層上，從而自該目標濺鍍材料並在該第一層上形成該壓電裝置之該含添加劑之氮化鋁膜之一第二層，其中該至少一添加元素包含選自由Sc及Y所組成之群組之至少一元素，該第二層具有與該第一層相同之組成物，及在形成該第一層施加至該壓電裝置之該膜撐體之該偏壓電力係一射頻電源。
  2. 如請求項第1項之方法，其中該至少一添加元素係以0.5原子%至40原子%之範圍的量存在。
  3. 如請求項第1項之方法，其中該至少一添加元素係2原子%至15原子%之範圍的量存在。
  4. 如請求項第1項之方法，其中該至少一添加元素係以3原子%至10原子%之範圍的量存在。
  5. 如請求項第1項之方法，其中該壓電裝置之該含添加劑之氮 化鋁膜僅含有一添加元素，該添加元素為Sc或Y。
  6. 如請求項第1項之方法，其中形成該第一層係使用施加至該壓電裝置之該膜撐體之大於70W之一偏壓電力。
  7. 如請求項第4項之方法，其中形成該第一層係使用施加至該壓電裝置之該膜撐體之少於250W之一偏壓電力。
  8. 如請求項第1項之方法，其中形成該第二層係使用施加至該膜撐體之少於125W之一偏壓電力。
  9. 如請求項第1項之方法，其中該第一層係比該第二層更不可拉伸(tensile)。
  10. 如請求項第1項之方法，其中形成該第一層至20至150nm之範圍的厚度。
  11. 如請求項第1項之方法，其中形成該壓電裝置之該含添加劑之氮化鋁膜至0.3微米或更大之厚度。
  12. 如請求項第11項之方法，其中形成該壓電裝置之該含添加劑之氮化鋁膜至2.0微米或更少之厚度。
  13. 如請求項第1項之方法，其中形成該壓電裝置之該含添加劑之氮化鋁膜至0.6微米或更大之厚度。
  14. 如請求項第13項之方法，其中形成該壓電裝置之該含添加劑之氮化鋁膜至2.0微米或更少之厚度。
  15. 如請求項第1項之方法，其中無另外含添加劑之氮化鋁膜沉積於該第二層上。
  16. 如請求項第1項之方法，其中循環地實施形成該第一層及該第二層，使得該壓電裝置之該含添加劑之氮化鋁膜包含四或更多層。
  17. 如請求項第1項之方法，其中形成該第一層至20至150nm之範圍的厚度，且形成該壓電裝置之該含添加劑之氮化鋁膜至0.6微米或更大之厚度。
TW105132593A 2015-10-09 2016-10-07 沉積方法 TWI778944B (zh)

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