2008年4月30日

半導體製程用濕式化學品的發展趨勢



伊默克化學科技 行銷暨海外事業部經理 廖伯佑
業務處處長 李盈壕
摘要
台灣的半導體產業經過近十餘年來產、官、學界的努力,已躍升成為全球第四大IC生產國,未來更有多座十二吋晶圓新廠將陸續投入,包括晶圓代工、記憶體、ASIC等不同半導體產品製造之領域。而因應半導體工業製造的需求,高精密濕式化學材料也伴隨之快速發展。本文將就化學材料中具關鍵代表性之高純度化學藥品在半導體製程應用及發展趨勢,分別作一介紹。


關鍵詞
濕式化學品 (wet chemicals)、濕式清洗 (wet cleaning)、濕式蝕刻 (wet etching)、黃光 (photolithography)、化學氣相沉積 (CVD)、化學機械研磨 (CMP)。


前言
近幾年來隨著我國積體電路及平面顯示器產業的持續蓬勃發展,不僅帶動了傳統化學、化工、機械、電機、建築等產業的相繼轉型投入;更重要的是這些傳統產業的升級,也相對地加速了我國半導體相關產業在產品品質及世界競爭力上的提升。以濕式化學品在半導體的應用上為例,雖然半導體生產所需化學品金額僅佔每單位晶圓生產成本的3~4%,但化學品的純度及品質卻直接影響到最終產品的良率和元件的品質暨可靠度。在0.13m製程以下製程平坦化的技術,以及銅製程的應用中,濕式化學品更將扮演著舉足輕重的角色。
半導體基本製程大略可分為薄膜、擴散、微影、蝕刻及化學機械研磨等模組,所使用之濕式化學品如下圖一所示。以下將針對各模組在其製程所需之化學品做剖析。

圖一、半導體生產流程圖


濕式潔淨技術與高純度化學品
在次微米晶圓製造過程中,無論是薄膜沈積、高溫爐管擴散、氧化或是蝕刻後晶圓表面處理,都需要經過許多高純度的化學品的清洗,再以超純水洗滌至最後以異丙醇除水乾燥的步驟。從60年代早期開始發展的RCA洗淨配方,一直被沿用至今日,雖然在各個模組中持續開發出不同的應用方式,也只限於在化學品的比例及清洗的順序上做了些微的調整。但是在目前閘極氧化層的厚度已小於100埃(Å),為達到閘極氧化層電性的要求及元件品質及可靠度,化學品的純度卻必須一直不停的被提升(如表二)。

Year 1986 1990 1993 1997 2001 2003
記憶體 (bit) 1M 4M 16M 64M 256M 1G
製程線寬 (m) 1.2 0.8 0.5 0.25 0.18 0.13
金屬不純物 規格 (ppt) 10,000 1,000 500 100 10 5
實測值 (ppt) 5,000 500 100 10 1 0.5
微粒子 規格 (m) 0.5 0.5 0.3 0.2 0.1 0.05
(pcs/ml) 50 50 200 100 100 100
實測值 (m) 0.5 0.5 0.3 0.2 0.1 0.05
(pcs/ml) 30 10 50 30 30 30
表二、高純度化學品規格演進(資料來源:伊默克化學, 2002)

洗淨的主要目的,是藉由高純度的化學品,來移除晶圓表面的細微污染,其中包含:微粒子、金屬不純物、有機污染物以及自然氧化層等。但製程上卻應盡量避免污染源的進入,並隨時保持人員、機台及材料的潔淨,才是真正克服晶圓污染的方法。以下將對各類污染源及化學品清洗的機制做討論。

晶片污染源
一般而言,矽晶片上可能的污染大約可分為微粒子、金屬、有機物、表面微粗糙度及自然生成氧化層等五大類,其可能來源及對製程的影響如表三。


污染源 污染來源 可能影響
微粒子 化學品、氣體
儀器設備
環境
操作人員 閘極氧化層崩潰電壓下降
生產量率降低
金屬不純物 儀器設備
離子佈植
乾蝕刻製程
化學品及金屬容器 接合介面漏電流
氧化層崩潰電壓下降
元件可靠度降低
有機污染物 光阻
環境
塑膠容器
操作人員 蝕刻不完全
降低氧化層品質
表面微粗糙 化學藥品
晶圓材料
洗淨方程式 閘極氧化層崩潰電壓下降
低載子遷移率
自然生成氧化層 空氣中濕氣
純水中溶氧
化學品 接觸窗電阻上升
氧化層品質劣化
不良金屬矽化物
表三、晶圓污染源及影響

其中微粒子的污染一般來自製程用中所使用的超純水、氣體及化學品,以及機台、晶舟甚至是製程線上的人員。藉由靜電、凡得瓦爾力、毛細管現象或化學鍵而吸附於晶圓表面,或者陷入晶圓表面細微凹凸而生成的溝渠之中。金屬不純物主要來自於離子植入、乾式蝕刻及光阻灰化時,因離子撞擊機台內壁所造成;另外製程環境及化學品與化學品容器本身,也是可能的污染來源之一。有機污染物則多來自光阻的殘留物,另外牆壁的油漆、幫浦的機油、塑膠容器以及作業員的身體及衣物也都是可能的來源。自然生成氧化層肇因於晶圓表面暴露於空氣或水中的溶氧,而氧將晶圓表面的矽氫鍵(Si-H)氧化成為羥基(Si-OH),或是將矽氧化成為二氧化矽所生成,其中反應的速率與溶氧濃度即浸泡時間有關。最後,晶圓表面的微粗糙一般來自於潔淨製程中SC-1的製程,並與清洗溶液中氨水及雙氧水的混和比例、製程溫度及洗淨時間有直接的關聯。

濕式化學品清洗機制
(1) NH4OH/H2O2/H2O (SC-1, APM):
利用氨水的弱鹼性活化矽晶圓及微粒子表面,使晶圓表面與微粒子間相互排斥而達到洗淨的目的;雙氧水也可將矽晶圓表面氧化,藉由氨水對二氧化矽的微蝕刻達到去除微粒子的效果。另外氨水與部分過渡金屬離子易形成可溶性金屬錯合物,也可同時去除部分金屬不純物。一般的APM製程是以NH4OH:H2O2:H2O=0.05~1:1:5的體積比在70℃下進行,由於氨水的沸點較低且APM步驟容易造成表面微粗糙的現象,因此氨水與雙氧水濃度比例的控制在所有洗淨製程中最為困難,卻也是影響製程良率的關鍵。
(2) HCl/H2O2/H2O (SC-2, HPM):
HPM步驟在金屬雜質的去除上扮演重要的角色。由於一般的金屬氯鹽皆可輕易的溶於水中,因此HPM製程利用雙氧水氧化污染的金屬,再以鹽酸與金屬離子生成可溶性氯化物而溶解。製程中最常使用的是HCl:H2O2:H2O=1:1:6的體積比,在70℃下進行5~10分鐘的清洗。
(3) H2SO4/H2O2 (SPM, Piranha Clean, Caro Clean):
主要是在清除晶圓表面的有機物。利用硫酸及雙氧水生成的卡羅酸,其強氧化性及脫水性可破壞有機物的碳氫鍵結,而達到去除有機不純物的目的。在操作上常以H2SO4:H2O2=2~4:1的體積比,在130℃的高溫下進行10~15分鐘的浸泡。
(4) HF/H2O (DHF)或HF/NH4F/H2O (BHF):
應用於清除矽晶圓表面自然生成的氧化層,可使用稀釋後的氫氟酸(0.49%~2%)或是以氫氟酸與氟化銨所生成的緩衝溶液HF/NH4F=1:200~400,在室溫下進行15~30秒的反應。
為了防止水分中的溶氧再次與剛洗淨的矽表面反應,洗淨最後會再以異丙醇來做乾燥,並且可同時避免在晶圓表面留下水痕。
近幾年來,許多乾式的清洗的方程式被相繼的提出,包括日本東北大學Ohmi教授所提出之新式清潔流程,或是利用氣態的鹽酸及氫氟酸來取代濕式的製程;但目前都僅限於部份製程的應用,尤其乾式清洗對許多重金屬的清洗仍未能有效去除,因此濕式洗淨用的化學品在未來仍將扮演著重要的角色。

濕式洗淨 溫度 乾式洗淨 溫度
1 SPM (H2SO4/H2O2) 120-150OC O3/H2O 室溫
2 UPW Rinse 室溫 FPM (HF/H2O2/H2O) 室溫
3 DHF (HF/H2O) 室溫 UPW Rinse 室溫
4 UPW Rinse 室溫 O3/H2O 室溫
5 SC-1 (NH4OH/H2O2/H2O) 70-90OC DHF 室溫
6 UPW Rinse 室溫 UPW Rinse 室溫
7 Hot UPW Rinse 70-90OC
8 UPW Rinse 室溫
9 SC-2 (HCl/H2O2/H2O) 70-90OC
10 UPW Rinse 室溫
11 DHF (HF/H2O) 室溫
12 UPW Rinse 室溫
表四、濕式及乾式清洗流程比較

微影用高純度化學品
微影製程的發展決定了積體電路代表性的指標—元件線寬大小,因此光阻材料成為IC製程中十分關鍵的材料。黃光步驟包含去水烘烤、黏著層塗佈、光阻塗佈、去邊、軟烤、曝光、烘烤、顯影及硬烤等步驟,其中所使用的關鍵材料如表五所示,包含有光阻、光阻稀釋液及顯影劑等。

製程機台 製程步驟 使用化學品
光阻塗佈機 去水烘烤
黏著處理 HMDS
光阻塗佈 光阻
晶緣殘餘光阻清洗 光阻稀釋液
軟烤
對準曝光設備 曝光
顯影設備 曝光後烘烤
顯影 顯影劑
硬烤
表五、黃光區微影製程使用之化學品

光阻
半導體製程所使用的光阻主要是由樹脂、感光劑及溶劑所組成,其中樹脂主要功能是做為蝕刻或離子植入時的阻障層;感光劑的部分則是照光後反應成易與顯影劑反應的化合物,以利顯影製程進行;溶劑用來使樹脂及感光劑均勻的分散,讓光阻塗佈製程得以順利進行。依光源的不同,光阻劑可分為G-line(436nm)、I-line(365nm)與深紫外線 Deep UV(193-248nm)三大類;深紫外線光阻劑與一般G-line、I-line的光阻劑最大差異在於,使用G-line、I-line光阻在曝光之後,即可直接進入顯影製程,而深紫外線光阻則必須再經過化學增幅法,才能進行顯影。

G-line光阻劑隨著機器之汰換而退出半導體製程,再加上I-line光阻劑的應用臨界在0.3μm線幅製程,而國內半導體業者已進入0.25μm線寬以下製程;因此近幾年我國半導體工業在光阻劑的使用,已經從G-line、I-line的光阻,進入到曝光波長更短的的深紫外線領域。如何在有限的晶圓上佈植更多電路圖案,惟有追求更細微的線寬,並朝向愈短曝光波長發展。未來進入0.13μm甚至0.09μm線寬製程,有賴於開發193nm深紫外線光阻劑。而隨著線寬朝向下一新世代發展,預估未來光阻材料將由157nm光阻劑接班。

光阻稀釋液
光阻乃是經由旋轉塗佈程序而在晶片上形成薄膜,但經常會在晶片邊緣形成珠狀殘餘物(Edge Bead).此晶圓殘餘光阻若不予以清除,將有可能會污染晶舟及其他晶圓表面,或甚至影響到曝光的效果;因此在顯影前必須使用光阻稀釋液,將晶圓殘餘光阻清洗乾淨。目前工業上較常使用之光阻稀釋液包括PO類的溶劑,例如VP-3, PGMEA, PGME;乳酸鹽類如Ethyl Lactate及酮類或酯類如Methyl Ethyl Ketone, n-Butyl Acetate等;其中以PGME及PGMEA混和的PO溶劑最被業界廣泛接受,然一般光阻稀釋液都有低燃點及高毒性的缺點,新一代開發的稀釋液如PGMEP等具有低毒性及較高閃點的優點,將可改善黃光區化學品對人體及環境安全的危害。

顯影劑
光阻材料在經過曝光過程之後,須再經由顯影過程將曝光的圖案顯現出來,而顯影製程之原理,是利用鹼性的顯影液與經曝光之光阻層部份進行酸鹼中和反應,使其與未經光阻層結構部份形成對比而達到顯像效果.在以往顯影劑為稀釋的氫氧化鈉、氫氧化鉀、碳酸鈉或碳酸鉀等水溶液,但由於鈉、鉀金屬離子可能會對元件造成污染,近年半導體製程來已逐漸改用稀釋的有機鹼溶液取代,如氫氧化四甲基銨(TMAH)溶液或氫氧化四乙基銨(TEAH)等,並在顯影劑中添加消泡劑及界面活性劑,以達到最好的潤濕及顯影效果.


蝕刻用濕式化學品
濕式蝕刻技術的優點在於其製程簡單、成本低廉、蝕刻選擇比高且產量速度快,而由於化學反應並無方向性乃是屬於一種等方向性蝕刻。濕式蝕刻的機制,一般是利用氧化劑將蝕刻材料氧化,再利用適當的酸將氧化後的材料溶解於水中。另外,為了讓蝕刻的速率穩定並延長化學品使用時間,常會在蝕刻液中加入介面活性劑及緩衝溶液來維持蝕刻溶液的穩定。一般而言,濕式蝕刻在半導體製程可用於下列幾個材料:

二氧化矽層蝕刻
以氫氟酸及氟化銨(HF/NH4F)所形成之緩衝溶液來蝕刻二氧化矽層,化學反應式如下:

SiO2 + 4HF+2NH4F  (NH4)2SiF6 + 2H2O

利用氫氟酸來蝕刻二氧化矽層的機制中,決定蝕刻速率的是[HF2-]的濃度,若HF濃度保持固定且緩衝溶液中NH4F能提供大量的之F-,蝕刻速率就可保持穩定。同時為了提高反應的均勻性以及對晶圓的潤濕性,一般在緩衝溶液中還會再加入少量的界面活性劑,來幫助化學品接觸疏水性的矽晶圓表面,同時也可改善蝕刻後晶圓表面的粗糙度。而影響蝕刻率之因素則包括:
SiO2層之型態:結構較鬆散(如:自然生成氧化層),蝕刻速率較快。
反應溫度:溫度升高,蝕刻率加快。
緩衝溶液之混合比例:其中HF比例愈高,蝕刻率愈快.

多晶矽層蝕刻
在目前製程上多使用硝酸(HNO3)、氫氟酸(HF)及醋酸(CH3COOH)三種成份之混合溶液來蝕刻多晶矽,其製程原理包含二道反應步驟:

Si + 4HNO3  SiO2 + 2H2O + 4NO2
SiO2 + 6HF  H2SiF6 + 2H2O

先利用HNO3之強氧化性將多晶矽氧化成為SiO2,再由HF與SiO2反應生成可溶性的矽氟酸,而其中CH3COOH則扮演類似緩衝溶液中H+提供者的角色,使蝕刻率能經常保持穩定。其中硝酸及氫氟酸的比例是影響蝕刻濃度的關鍵。

氮化矽層蝕刻
一般多使用85%的磷酸(H3PO4)在160~170℃之間做氮化矽層的蝕刻,化學反應式如下:

Si3N4 + 4H3PO4 + 10H2O  Si3O2(OH)8 + 4NH4H2PO4

值得一提的是,以熱磷酸對氮化矽及二氧化矽的蝕刻選擇比大於20:1,且於蝕刻率約為60埃/分鐘。

鋁導線蝕刻
鋁常在半導體製程中作為導電層材料,濕式鋁層蝕刻可使用多種無機酸鹼來進行,而已硝酸、磷酸及醋酸之混合溶液其蝕刻速率最為穩定,目前被廣泛運用在半導體製程中.主要之製程原理是利用硝酸氧化鋁金屬層之後,在與磷酸形成磷酸鋁溶於水中:

2Al + 6HNO3  Al2O3 + 3H2O + 6NO2
Al2O3 + 2H3PO4  2AlPO4 + 3H2O

其他金屬蝕刻
隨著半導體製程技術的不斷演進,許多金屬導線及阻障層都將被新的全新的金屬材料所取代。因此,濕式蝕刻的發展也必須跟著不斷地進步。下表六針對一些未來半導體製程可能使用的金屬蝕刻液作一整理。


金屬 蝕刻溶液
TiN, Ti, W NH4OH/H2O2/H2O (1:1:5)
TaNx HF/H2O2 (1:2)
Cu HNO3/CH3COOH/H2O (1:20)
GaAs NH4OH/H2O, H3PO4/H2O2, Organic acids
Mo H3PO4/HNO3/ CH3COOH
Cr Ce(NH4)2(NO3)6/HNO3 or HclO4
Au KI/I2/H2O
ITO HNO3/HCl, HBr, Organic acids
Ni/V HNO3/CH3COOH
表六、金屬與相對蝕刻溶液

晶背蝕刻
當晶圓代工及記憶體製程進入12吋的單片製程(Single Wafer Process)的領域,晶背的污染不容易在蝕刻的同時被清洗乾淨,因此晶背蝕刻(Back-side Etching)就非常重要。由於晶背表層常包含了各類PVD、CVD、電鍍或光阻所殘餘的材料如二氧化矽、多晶矽、有機物、金屬、氮化矽等,因此濕式晶背蝕刻液必須由多種無機酸類組成,包括H3PO4, HNO3, H2SO4及HF等,如此才能有效的去除複雜之晶背表層的結構。

光阻剝離
無論乾式或濕式蝕刻之後,緊接著是必須做光阻剝離(Stripping)的製程,將圖案轉移(Patterning)用的光阻加以去除。在半導體製程中通常使用兩種去除光阻材料之方法,一為濕式去光阻法,另一則為乾式去光阻法。濕式去光阻法,是利用有機溶液將光阻材料溶解而達到去光阻之目的,所使用之有機溶劑如丙酮(Acetone), N-Methyl-Pyrolidinone(NMP), Dimethyl Sulfoxide(DMSO)或是Aminoethoxy ethanol等具有溶解大量光阻的特性;另一方法則可以使用無機溶液如硫酸和雙氧水的混和溶液(SPM),此方法雖然製程成本較低,但因容易造成金屬薄膜的腐蝕,目前僅有部份記憶體製程仍持續使用。乾式去光阻法則是使用氧氣或其電漿將光阻加以灰化(Ashing)。


化學氣相沉積製程用化學品
化學氣相沉積(Chemical Vapor Deposition, CVD) 是一種經由高溫氣化分解反應後將單種或多種氣相分子沉積於固相基板之半導體薄膜製程,而許多液相之先趨性化學品(Precursor)也廣泛地應用在下列兩種CVD製程中:

1. 介電材料CVD製程用先趨性化學品
最常見之介電材料CVD Precursor包括下列兩種:
(1) SiO2 CVD: TetraEthylOrthoSilicate (TEOS)
(2) BPSG CVD: TriMethylBorate (TMB)及TriMethylPhosphite (TMPI)
TEOS在低壓操作環境加熱至650-750℃集會產生下列分解反應,產生SiO2氣相分子
Si(C2H5O)4+12O2SiO2+8CO2+10H2O

若將TEOS及TMB、TMPI一起進行CVD反應,即會形成摻雜硼和磷成分之硼磷矽玻璃 (Boron Phosphate Silicate Glass, BPSG)介電材料之沉積,上述介電材料因降低了玻璃轉化溫度,因此再經由熱流處理後,可以得到相當好的平坦度及提供較佳之階梯覆蓋(Step Coverage)效果,因此廣泛的使用於半導體的製程中。

2. 金屬CVD製程用先趨性化學品
金屬薄膜製作在早期均是由物理氣相沉積(PVD)或濺鍍法(Sputtering)製作,然其階梯覆蓋能力不佳且無法準確地控制其組成,近年來已逐漸為CVD取代。而目前使用CVD法來製備金屬薄膜如鎢、鋁、鈦及銅之製程分別如下數式:
(1) W CVD:
2WF6(g)+3Si(s) 2W(s)+3SiF4(g)
WF6(g)+3H2(g) W(s)+6HF(g)
WF6(g)+SiH4(g) W(s)+SiF4(g)+2HF(g)+H2(g)
(2) Al CVD:
2Al(C4H9)3 2AlH(C4H9)2+C4H8 (150℃)
2Al+3H2+4C4H8 (250℃)
(3) Ti CVD:
TDMAT+NH3 TiN+…..
TDEAT+NH3 TiN+…
DMAT (Tetrakis Dimethyl Amino Titanium)及TDEAT (Tetrakis Diethyl Amino Titanium)
(4) Cu CVD:
Cu(II)L2+H2Cu(s)+2HL
Cu(II)bis(-diketonate)及Cu(II)bis(-ketoiminate)
L: Single charged ligand (-diketonate…)
使用CVD來製作金屬膜目以Cu及W最吸引人注意,因為銅金屬的導電度及抗電移性比鋁高,因此目前在0.13m以下的製程已經取代鋁成為高性能元件之主要金屬層。而鎢CVD製程因其擁有較佳之覆蓋能力、高純度(含氧量少)及高輸出量而深具發展潛力。


化學機械研磨用濕式化學品
隨著半導體元件線寬縮減至0.25m以下,金屬導電層數超過三層以上,全面性平坦化製程已為不可忽略之關鍵製程。化學機械研磨(Chemical mechanical Polishing, CMP)是由IBM所開發出結合化學反應與機械研磨的製程,目前已經成為平坦化製程的主要技術。它不僅可以達成全面平坦化的目標,同時可增加元件設計的多樣性如新元件設計中的銅導線製程。在化學機械研磨的製程中所使用的化學品主要包括有研磨液(Slurry)及研磨後清洗液。

1. 研磨液
研磨漿溶液一般為含有磨損力之研磨顆粒與弱鹼或弱酸性的化學溶液。因應不同薄膜材料之研磨目的,其主成分可分為兩大類:
(1) 介電層平坦化研磨液:溶有矽土(Silica, SiO2)之KOH或TMAH溶液。
(2) 金屬層平坦化研磨液:溶有礬土(Al2O3)之Fe(NO3)3或H2O2溶液。
CMP製程的反應機制因牽涉到複雜之化學及機械之交互作用,在研磨的過程中,研磨液中所含之漿料(Abrasive)顆粒之粒徑分佈、研磨液之pH值及研磨速率等均對化學機械研磨製程有決定性的影響。

國內半導體業者所使用的化學研磨漿料幾乎全數仰賴美國CABOT、RODEL公司與日本FUJIMI進口。必須大費周章的以海運或空運來台,且化學機械研磨漿料在穩定的溫度控制下,其保存安定性僅有6-8個月;因此從國外進口不僅運費高、對化學品的安定性也會有影響。目前國內已有多家半導體製程化學品廠商投入鋁導線及銅製程研磨液的研發,相信在不久的將來,將可提供台灣半導體製造廠另一個成本低廉且品質穩定的研磨液選擇。

2. 研磨後清洗液

圖七、CMP研磨後清洗液的發展趨勢

由於研磨液是一種高黏度之化學品且含有大量的固體粉末,因此在進行CMP製程後必須立即進行清洗,否則將很容易在矽晶片表面上凝結成固態殘餘物。而一般清洗步驟可使用刷洗 (Brush Cleaning)、噴洗 (Spray Cleaning)及超音波清洗 (Ultrasonic Cleaning)等方式來進行,目前較普遍之清洗方式是使用稀釋之氨水以去除研磨後殘留之粒子污染物及稀釋之氫氟酸去除微量之金屬污染物;但是強酸及強鹼極易傷害銅導線及低介電材料,因此在銅製程中,一般會選用較溫和的有機酸或是有機鹼,輔以添加的介面活性劑及螯合劑,來去除研磨液的微粒子及金屬不純物。


結論
半導體製程用化學品不但與帶動了我國傳統化學工業的升級,在未來銅製程或12吋晶圓中的潔淨製程、微影技術、先進蝕刻及平坦技術的發展上,濕式化學品仍將扮演決定性的角色。化學材料業須不斷研發,才能促進國內半導體產業進入下一世代。雖然目前許多的關鍵性材料如光阻、研磨液及光阻剝離液等,仍大部份仰賴國外進口。未來必須仰賴政府、研究機構、化學品供應商及半導體製造廠之間的鼎力配合,才能真正提昇台灣製程用化學品的研發。


參考文獻
1. 莊達仁,VLSI製造技術,1995
2. 段定夫,電子月刊,1996, Vol.2, No.5
3. 張俊彥 教授,積體電路製造及設備技術手冊,1997
4. 2000、2001伊默克化學技術研討會,2001
5. 黃進修、鄭智和,化工技術月刊,2001, Vol.9, No.1
6. 周輝南,電子月刊,1996, Vol.2, No.5
7. 關東化學,300mm製程用高純度化學品評價

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