TWI222961B - Low dielectric constant material and method of processing by CVD - Google Patents

Low dielectric constant material and method of processing by CVD Download PDF

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TWI222961B
TWI222961B TW92134625A TW92134625A TWI222961B TW I222961 B TWI222961 B TW I222961B TW 92134625 A TW92134625 A TW 92134625A TW 92134625 A TW92134625 A TW 92134625A TW I222961 B TWI222961 B TW I222961B
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TW92134625A
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TW200409738A (en
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Mark Leonard O'neill
Aaron Scott Lukas
Mark Daniel Bitner
Jean Louise Vincent
Raymond Nicholas Vrtis
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Air Prod & Chem
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  • Other Resins Obtained By Reactions Not Involving Carbon-To-Carbon Unsaturated Bonds (AREA)

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1222961 還沒有相關的資料來證明膜的這種性能。根據所給出的矽 派度2.2克/立方釐米，其值相當於6·6χ1〇22原子/立方 釐米，可以估算F和C的濃度，ρ大概是6 —丨5原子％，◦ 大概是0· 05- 1. 5原子％。 美國專利案第6, 41〇, 463號中，Matsuki給出了一種 製造膜的方法，這種膜的介電常數很小，該膜把反應氣在 反應器中的停留時間提高到至少100msec。Matsuki沒有給 出在膜製造過程中提供氧的氣體（例如，〇2)的使用。 儘管有上述發展，在現有技術中還沒有任何方案可以 2功的結合預期的機械、電導、熱和氧化穩定性等各個性 吨，這些性能對積體電路中産生低k值介電材料極爲重要。 本文中所有引用參考文獻的全文以引用的方式併入 文中。 + 發明内容
^本發明提供一種摻雜碳的氟化矽玻璃膜（也就是，CFsg j〇FSG之一有機氟化矽玻璃），該膜含有有機物質和無機 氣’其中不包括相當多的碳氟化合物。 +發明的一個具體實 來表示的一種膜，其中，v+w+x+y+z=1〇〇%，V衫 到35原子％，w & 1〇到65原子％1從1〇到5〇原子 ^從2到30原子％，2從〇·ι到15原子％，而且其 貝上；又有氣石炭鍵合。 本發明的另一個具體實施例，提供的可用> 12 1222961 z = 1〇〇 y從ίο
Siv〇wCxHyFz來表示的一種膜，其中，v+w+x+y + %，v從10到3 5原子％，w從1 〇到6 5原子％， 子％，Μ足〇· ;l到15原子 而且其中實質上沒有氟碳鍵 到50原子％ ’ X從1到30原 %，其限制條件爲x/z〉〇. 25， 合0 个赞明的另 、•八… J⑺公式
Siv〇wCxHyFz 來表示的一種膜，其中，v+w+x+y+z=1〇〇 %，V從10到35原子％，w從10到65原子％，y從切 到50原子％，又從i到3〇原子％，z從〇1到π原子 %，其中〇·5原子％或者更少的破氟鍵、结合，其中可防止 膜的性能隨環境條件的變化而變化。 本發明的另一個具體實施例，提供的可用公式 Siv〇wCxHyFz 來表示的一種膜，其中，Hw+x+y+z=1〇〇 %，V從10到35原子％，％從1〇到65原子％，y從 到50原子％，x & i到3〇原子％，z從〇1到π原子 ::其限制條件爲χ/ζ>〇·25,其中〇·5原子％或者更少的 山#鍵、"β 其中可防止膜的性能在微電子處理的過程中 變化。 實施方式 本發明一 膜材料相對於 能、熱穩性、 果是由於膜中 個較佳具體實施例提供一種薄膜材料，該薄 SG材料具有低介電常數、改良的機械性 化學抗性（對氧氣，水環境，等）。這種結 添加了碳（可以是碳化矽，但是其較佳地主 13 1222961 於猜a和/或奈米屢痕硬度大於[順。通過對比，介 電常數爲2. 8到3.2之間的參考〇SG膜，具有低於觀a 的彈性模數和低於i.SGPa的奈米屢痕硬度（參見上圖2, 相對應的例子1、2、4和5) 。 ^ 本發明的膜適合防止膜性能隨環境條件變化而變化。 本發明的膜具有熱穩定性和較好的化 …一條件下，該膜平均質量損失 和/或在空氣中425r等溫條件下，該膜平均質量損 失低於 l.〇wt%/hr。 、 環境條件對膜性能影響極大，微電子處理過程就是一 個典型例子。如此處理過程（例如，加溫退火，電介質腐 敍和後腐姓灰化）可以頻繁地進行化學和/或熱氧化。和傳 統的〇SG膜相比’本發明的膜可以更有效的防止膜性能隨 核境條件變化而變化。例如，本發明的膜在整個典型的微 =子處理過程中實質上保持其介電常數不變。較好地，其 介電常數的增加小於1〇%和/或〇」。其介電常數的增加數 值小於參4 0SG膜由環境條件增加的參考介電常數的數 =在某些具體實施例中’該膜介電常數的增加數值相對 =參考〇SG膜由於環境條件而增加的介電常數數值的 或更少’較好的増加2〇%或更少，更好的增加ι〇%或更少。 、在佳具體實施例中’膜中的氟分佈或者氟遷移到一 ^或多個相鄰層的趨勢是另一個膜性能，其用於抵 的變化。 在較佳具體實施例中，同樣，碳濃度也是一個膜性能， 16 1222961 在某些具體實施例中，本發明包括一個改良過程，丈 用於通過化學蒸發沈積法析出〇SG，該過程之中至少一 ς 分析出的OSG材料用於産 " 生貝貝上爲自由基的有機氟的 膜，而一個無機氟源則伴隨 〜仟I思無機齓一併析出。因此， 明可以用來改良以前的、 ^現在的和未來的過程，包括美國 專利案第6, 〇54, 379、6 秸吳国 ，147,〇〇9 和 6, 159,871 99/41423中報導的。和 h、 和相應的傳統加工過程生産的産 比，通過改良的加工過程生產 ;生旧座σ口擁有改良的性能。 佳地，膜的至少一錄嫌ρ α 機械性犯乓加，最少爲10% ;其埶稃 定性增加；化學穩定槌秘上i / 、…德 ^ θ加和/或環境穩定性增加。 生産低介電常數膜的過程包括·卩 τ匕栝.（a)在真空腔體内提 i、一個基板，（b )直*脉辦士 〃二I體中引入氣相反應物，其包括提 供氟的氣體，提 ^ ，仏乳的乳體和至少一種包含有機石夕和有機 矽虱烷的丽驅氣體；和（c) 裎π A㈢π π β 门飞異二腔體内的氣相反應物 袄供此Ϊ促使其反應而在基板上成臈。 基板最好是半導體材料。 有機碎燒和有機石夕童ρ θ 俄矽虱烷疋較好的前驅氣體。適合的有 機矽和有機矽氧烷包括 r1 S，〇2 ^如· （a)烷基矽烷，其用公式 K nS 1 R 4_n來表示，复中 9 ^ ’、 疋1到3的整數；R1和V是相 互獨立的’其爲至少一 個支鏈或者直鏈Ci到&的烷基（例 如，甲基，乙基），一徊Γ n r r m 3到Cs取代的或未取代的環烷基 (例如，環丁基，璟 A ^ 基），一個匕到G。部分不飽和烷 基（例如，丙烯基，τ 一、膝、 ^ ^ ^ 烯），一個匕到C12取代的和未 取代的方香族（例如，苯基， f本基），一個相應的直鏈 18 1222961 式」支鏈式’環鏈式部分不飽和烧基或者芳香族，其包含 炫氧基（例如，甲氧基，乙氧基，苯氧基），而R2選擇物 件則爲氫化物（例如’甲基矽烷，二甲基矽烷，三甲基矽 貌，四甲基石夕炫，苯基石夕烧，甲基苯石夕貌，環己基石夕炫， ’、丁基石夕院’乙基石夕燒，二乙基石夕院，四乙氧基石夕炫，二 甲基-乙氧基石夕烧，二甲基二甲氧基石夕燒，二甲基乙氧基 、元甲基一乙氧基矽烷，三乙氧基矽烷，三甲基苯氧基 錢和苯氧基㈣）；（b)直鏈式有機錢燒，其用公式 R (以〇)加3來表示’ #中，n是1到1〇的整數，或者 環鏈式有㈣氧烧，其用公式（RlR2siG) 10的整數，^丨和R2如上定義f存丨知1 疋2到 戈上疋義（例如，1，3，5，7-四甲義 ，4，5，6 —六苯基己矽烷，工，2 —二甲基—工 矽烷和1，2 -二苯基乙矽烷）。 在某些具體實施例中，有機石夕烧和有機石夕氧燒是 環鏈式烷基矽烷，一種環鏈式矽氧烷，或者包含在一隹 原子之間至少一個烷氧基或烷基的橋，例如， _矽 z —石夕乙 環四石夕氧烷，八甲基環四石夕氧烧，六甲基環三石夕氧烷，= 甲基二矽氧烷，1，1，2，2~四甲基二矽氧烷，和八甲基‘ 石夕氧燒），和（c )直鏈式有機碎燒低聚體，其用公 R2(SiRV)„R2來表示，其中，qua的整數，或者二 鏈式有機較，其用公式（siR1R2) n來表示，其中 3到10的整數，R1和R2如上定義（例如，i，2_二甲烏疋 矽烷，1，1，2 ’ 2-四甲基乙矽烷，i，2—二甲基一丄，工，土乙 二甲氧基乙六甲基乙料’八甲基丙钱，二’ 苯基乙 19 1222961 烷，1，3〜二矽丙烷，二甲基矽環丁烷，1，2〜二（三甲基 石夕氧烧)環丁燒，…—二甲基]，_2,6_二氧環己：二 1 一二曱基矽―2-氧環己烷，1，2一二（三曱基矽氧烷）乙 烷，1，4-二（二甲基甲矽烷基）苯，或者i，3—(二甲基 甲矽烷基）環丁烧。 在某些具體實施例中，有機矽烷/有機矽氧烷包含一個 活性側鏈基，這樣的側鏈基包含—個環氧化物，一個叛化 物’一個炔’―個二烯，苯基乙快基，一個應變環鏈式基，
和-個q Ci。基’它可以空間位阻或者應變有機石夕燒/有 機碎氧烧，例如，二田装々7 % ^如一甲基石夕乙炔，1-(三甲基甲矽烷基） 3 丁一烯，二甲基甲矽烷基環戊二烯，三甲基甲矽烷 基乙酸酯，和二-叔—丁氧基二乙酸基矽。 ☆較佳的提供氟的氣體應不含有F_c鍵（也就是，氟和 反鍵口），其不應出現在膜中。因此，較佳的提供氟的氣 體包括，例如，SIF4、肌、p2、HF、SFe、d队、队、
F2Cl Μα3、F2SlH2、F3SiH、有機氟化矽烷和它們的混合 物/、要有機氟化矽不包括F— C鍵就可以。另外較佳的提 七、氟的亂體包括上述烧基石夕烧，烧氧基石夕燒，直鍵式和環 鏈式有機矽氧烷，直鏈式和環鏈式有機矽低聚體，環鏈式 或者橋式有機矽，和有活性側鏈基的有機矽，如果一個氟 ’、取代至少一個矽取代基，在此則至少有一個s丨—F 鍵。更特殊的，合適的提供氟的氣體包括，例如，敦化三 甲基矽烷’二氟二甲基矽烷，甲基三氟化矽，1化三乙氧 夕烷，1，2-二氟-1，1，2，2 —四甲基乙矽烷，或者二 20 1222961 無摻氟的有機石夕烧（用於提供碳）。 除了提供氟的氣體、提供氧的氣體和有機矽烷/有機矽 . 氧烷外，額外的材料可以在沈積反應之前、之中和/或之後， 加入到真空腔體中。這些材料包括，例如，惰性氣體（例 如：，、Ar、N2、Kr、Xe、等等，其也許需要-種載氣做 爲V里的易揮發的前驅氣體，和/或其可以加速沈積材料的 退火，可以提供更穩定的最終膜）和活性物質，如氣相或 者液相有機物質，NH3、H2、c〇2或⑶。有機物質，例如， ch4、C2H6、C2H4、C2H2、C3H8、苯、萘、曱苯和苯乙烯，等 _ 等’爲本發明膜提供碳。 給氣相反應物施加能量誘發氣體反應使其在基板上形 成膜。該能量可以由此提供，例如，熱、電漿、脈衝電漿， 螺旋電漿，高密度電漿，感應耦合電漿和引控式電漿方法。 使用次頻源改善在基板表面的電漿性能。通過電漿辅助化 學蒸氣沈積法形成的膜較好。特別的，最好是在13. 56mhz 頻率下，生成電容耦合電漿。基於基板表面積，較好的電 漿能量在0· 02到7 watts/cm2之間，更好的在〇· 3到3 · watts/cm2 之間 〇 每種氣相反應物的流速範圍，每單一 2〇〇mm晶片，其 值較好的在10到500〇5(^111之間，更好的在2〇0到2〇〇〇%(：111 之間。個別速率的選定取決於提供期望的膜中氟、礙等的 含量和比值。所需的真實流速取決於晶片的大小、真空腔 體結構’和沒有任何限定到200匪的晶片或者單晶片腔體。 最好以至少50nm/min的沈積速率來析出膜。 22 1222961 沈積過程真空腔體的壓力較好的爲〇 〇1到600t〇rrt 間’更好的爲1到1 〇 t 〇 r r之間。 基於使用三甲基矽烷作爲有機矽烷前驅，在2〇〇mm矽 晶片基板，本發明較好的方法參看下表1。 表1 壓力（torr ) 4. 0 基板溫度（°C ) 350 空間距離（mil) 320 RF 能量（Watts ) 400 二甲基碎烧流量（seem) 540 〇2 流量（seem) 90 SiF4流量（seem) 250 較佳的，以咼産量的單一加工過程完成本發明。不希 望有其他理論的限定，我們認爲，本發明的加工過程提供 的膜在其完整的剖面圖的各處具有更爲均勻的無機氟分 佈，其如Uchida等人講授的，不像多步驟後處理氟化過 程。另外，本發明的膜中有機氟非實質（insubstantiai) 3里（其中非貫質〈^substantial〉，，用於此，其定義爲 小於氟總含量的5%，更好的是小於敦總含量的ι% )也比 較均勻的分佈在膜的完整的剖面圖的各處，其並不是中心 密集的。 k g在許夕貫例中單一加工過程較好，在本發明範圍 23 1222961 内’其過程也包括膜析出的後處理過程。該後處理過程包 括，例如，熱處理、電漿處理和化學處理中的至少其中一 種。 ’、 儘官析出膜的厚度隨要求而變化，豆 請以⑼微米之間。沈積在無圖案表面—上的平板 斤子的句勻f生’其厚度變化程度小於2 %，在合理排除邊 緣的基板上超過i的標準偏差，例如，在均勻性統計計算 中，基板的一條l〇mm最外層邊緣就不包括其中。 膜的孔隙率隨著容積密度相應的減少而增加，由此， 導致進一步降低材料的介電常數，而拓展了該材料的適用 範圍（例如，k<2· 5 )。 通過下面的實例更詳盡的闡述本發明，但是’應該瞭 解本發明不僅僅局限於此。 實施例 以應用材料精度—5000的系統，配有超能量2000高頻 發生器（an Advance Energy 2000 rf generator)的一個 200mm DxZ腔體，和不摻雜TE〇s加工工具爲條件進行所有 的實驗。其方法包括以下基本步驟：氣體流的初始組成和 穩定性’沈積析出，和在晶片脫除之前淨化/抽空腔體。隨 後在母個沈積過程之後利用C2 F6 + 02就地清除腔體， 之後再乾燥腔體。 矛J用在低電阻係數P_型晶片（〈0 · Q 2 〇hm-Cm )上的 Hg探測技術來測定介電常數，利用MTS奈米硬度計測定機 24 1222961 械性能，利用一台熱ΤΑ儀器2〇5〇TGA耦合一台MIDAC紅外 光譜儀（TGA-IR)進行熱解重量分析來測定熱穩定性和廢 氣産品。用一台Bruker ASX-200來獲取"C-NMR資料，用 物理電子器件（Physical Electronics) 5000LS 進行 射線電光子分光光譜（XPS )分析獲取成分組成資料。 基於美國專利案6, 1 59, 871和6, 054, 379和和 99/41123所述’建立相比較的1 ~ 6實例，並將其列於下 表2中。
25 1222961 表2 從三甲基矽烷和氧中〇SG沈積析出資料 相比較的實例號Ν〇· 1 2 3 4 5 6 基板溫度（°c) 350 350 350 350 350 350 厚度（nm) 668 633 661 669 1324 643 均勻度（+/—） 8 6 7 12 5 折射率 1. 442 1. 439 1. 444 1. 441 1. 431 1.4445 均勻度（+/—） 0.0073 0.0070 0.0090 0.0073 0.0047 平均 Cap./Hg (pF) 38 39. 1 37. 5 20. 9 介電常數 3. 03 2. 97 2. 99 3. 02 結合強度(Tape Pull) 100% 100% 100% 100% 100% 100% 楊氏模數（GPa) 8. 7 9. 0 8. 4 7. 6 7. 1 8. 2 NI 硬度（GPa) 1. 4 1. 4 1. 3 1. 1 1. 1 1. 3 元素（XPS) %c 22. 2 23. 3 23. 5 23. 5 22. 4 %Si 32. 7 35. 2 35 35. 1 35. 3 %〇 44. 3 41. 1 41. 2 41. 4 42. 3 %F 0 0 0 0 0 注：表2中沒有用xps測定的原子％ Η的數值。 基於本發明生成的幾種不同種類的膜的物理研究，其 結果列於下表3中（注：表3中沒有用XPS測定的原子％ η 的數值）。 26 1222961
ocsl6T-00T-hr s St ncol· 31- U Οιo)00Γ9 S 寸CoCN1r-爹辑« 842 700 260 5.50 § I O CO o T- O 701 400 o (M o cd 250 540 200 540 CD CO 寸 400 to CO CVI o LO o LO CM 540 S o o 1213 1000 s CO o CO jo 〇 〇 540 O s o T- 05 C\J 400 s CO o s 350 o S g s CVJ 615 600 o CD OJ o 寸· 8 o LO CO o s 8 o lO CVI 寸 o s o CO OJ q 寸· 350 540 S 250 in 600 o CD CVI q 350 540 S 250 T- CVJ CO 400 〇 o CD § o to CO o s S o ir> 00 CD 600 200 〇 S 350 o s s o T~ 619 600 o CD 寸_ JO § o s 8 s CM CO CO 00 1000 CO 〇 穿 350 540 § s Csl s CVJ T- 1000 260 〇 in § o LO s s CM s ¢0 600 o CO CVJ o 350 540 s T- 250 CO LO ⑦ 1000 260 o Tj- JO 350 540 § S CM CO CO 寸 400 o CO CVJ § CO o o CO s s CM LO 00 700 200 LO CM CO § 400 540 8 100 197 o § o CO CM 〇 寸· S 350 540 § s CM 343 o o 〇 q ― t- S CO 540 s CVI 278 400 320 q tj- 180 g CO o s § 〇 LO CVJ 沉積速率（nm/min) I _ DU 4ΠΠ 黟 j獅 ipr 空間距離（mil) " P體壓力（t〇rr) 福間（sec) 基板酿（〇C) 1 :c iS m J )^ H ss i11 1 a is SiF4 ol9s OCVJIt ::断1«游 OH
soo.o §0.0 S5.0 §0.0 soo.o wos.o soo.o §0.0 soo.o soo.o soo.o soo.o §0.0 -.i.o510061寸CVJIoodl6C01QI001(丨/iMiplirl gg 丨L 9 §T001g M § FTcolg ^ —L § § ^ ^col— (1/+) sir ^F§~^~s~~Ζϋδ~~§ s~s~5 寸卜SI.~s~s~s~~0~1 ~^~1 ~989 glcollcol— (liaa)afltt 1 、 I； > 30.9 3.03 〇 T- o CO CO τ- 23.8 00 t σ> c5 in CO s OJ CO 系 o o 寸 CO τ- 00 cvi 00 00 TP- CO isi CO 46.8 卜 cd CVi 之 s oJ o T- Λ od CO T- 22.9 寸 in CO 寸 σ> CO CM S 3.29 0 1 T- CO s 寸 CO 00 LO T- CO IT) CO (D 寸 cvi K o CO o T- CO d 00 Τ 寸 UO 1- 卜 LO CO (D CO cJ CO oi CVJ N r- co_ o Ύ- 00 T- T- Ο cvi t- c\i CO •r— N： CO 寸 CO CO σ> CVJ CO T- CO o T- 00 T~ T- o cvi CO cvi C\J LO CO 寸 od CO CO 卜 s CO r- CO 於 o o ⑦ cvi T- cvi CD 〇3 寸 l〇 CO oo od CO C\j ― 00 d s c\i 於 o o 00 CO I— CO T- LO σ> 努 l〇 5 LO cvi 卜 CD OJ CO T- co 洛 o T- 11.1 卜_ T— CO CO CVJ CO 00 岛 ― T- io LO 卜 1— CO o o in CO r- OJ 〇j 卜 T- T- CO CO CO « O) to 42.4 努 CO o o 卜 uo 寸 cvi CO CO CO CO (J) CO σ> 00 σ> CVJ cvi CO o o p 寸· 1— CO c\i 14.5 T- cvi CO CO ιό T- 47.8 o CO 於 o o CD 寸· CO cJ CVJ 〇ϋ .T- CO 寸 卜 39.3 CO CO 於 o o 18.0 CO cvi iq 卜 寸 cd CO CO o s ci o o 00 σ> CO CO 48.2 OJ CO CO o T- cvi cvi CM 寸 CO 00 s 3.08 於 o o 00 ui t™· i〇 cvi 37.7 o CO 於 o o 12.9 CM cvi 3.03 o T- q T- T- 05 T- 〇 55 〇 % F s ! u ! ) ) 1 thmi] ipr <s s 2 <ύ l R M Id 'S _ \ UjJ ;tt • iniJ -|g XA « 1R ΖΊ 1222961 用一台SCI Filmtek2000反射儀5點平均法來測量厚度和 折射率。用膝拉拔钻貼測試法（t a p e p u 11 t e s t )來、、貝ij 量粘附力。在一台MTS奈米壓痕硬度儀來測定揚氏模數和 奈米壓痕硬度。利用XPS法在30秒Ar濺射後進行元素分 析。列表中不包括氫的原子％值。 圖la和圖lb所示爲氮氣條件下，繼後爲空氣條件下， 425 C ’ 5個小時的等溫TGAs圖。這些資料表明在惰性氣 體（氮氣氣氛）條件下，本發明膜的熱穩定性（實施例Μ) 比〇SG型材料猶微好一些。然而，在環境氣氛轉到空氣時， 對於〇SG材料來說，其重量損失顯著且急n本發 料的膜則表現的相當穩定。 f到刪。CTGA的掃描資料。這些資料表明本發明膜 a所示的實施例16)和咖（圖2b所示 到100(TC的熱穩定性。當 工風中本 吐 田在虱乳_以10°c/min進行我
時，0SG材料在約彻Γ開始心t ^ 明膜在較長的時間内保持較緩的重量損失，L在：: 以10°C/min進行掃描日车，甘去 工且在工瑕 ^ Q 、八重量損失在約47(TC才開始 圖所示爲在空氣中，425i〇 膜和0SG的& 專kir'件下，實例16 〜丄κ 口丨j面圖。這此咨 僅損失队和水，_心=本發明膜（虛線） ⑶2’水和⑽。這裏沒有迹象丄:)抽失相當大部分 氟有機材料，如果材料中 樣品中釋放出任何的 所期望的。 壬何摻氟物質，該樣品則 28 1222961 圖4所示爲實施例16中膜的13c NMR光譜，其中沒有 有機氟的可見信號，而預期在約+9〇ppm出現-CH2F信號’ 到約+150ppm出現-CF3信號。該技術僅僅發現一種形式的 石厌即和砍結合的碳’其對應中心約在〇ppm。 因此，本發明提供膜和製造此類膜的加工過程，該膜 中’貫質上或者完全爲自由基的C—F鍵。和0SG材料相比’ 其具有低介電常數、改善的機械性能、熱穩定性、和化學 抗性（對氧氣、水氣氛，等等）等性能。 實施例21 一個本發明預期實施例，其基於使用1，3，5，7 —四 甲基環丁石夕氧烧（TMCTS )作爲有機石夕烧前驅，一個200mm 石夕晶片基板，具體資料列於下表4中。 表 4 壓力（torr ) 4. 0 基板溫度（°c ) 350 間距（mil ) 250 RF 能量(Watts) 300 TMCTS ( g/min ) 1.0 〇2 流量（seem ) 50 SiF4 流量（seem ) 150 ' —----- 其期望k值在2. 8到3.0之間’揚氏模數約爲ι5(}ρ& 29 1222961 奈米壓痕硬度約爲2GPa。 一個本發明預期實施例，其基於使用二甲基二甲氧基 石夕燒（DMDMOS )作爲有機石夕烧前驅，一個2〇〇inm矽晶片基 才反’具體資料列於下表5中。 表5 壓力（torr ) 4. 0 基板溫度（°C ) 350 間距（m i 1 ) 250 RF 能量（Watts) 500 DMDMOS ( g/min ) 1. 0 〇2 流量（sccm ) 100 〜 SiF4流量（seem) 200 其期望k值在2. 8到3· 0之間，揚氏模數約爲15GPa， 奈米壓痕硬度約爲2GPa。 _ 一個本發明預期實施例，其基於使用二乙氧基曱基矽 、元（DEMS )作爲有機矽烷前驅，一個矽晶片基板， 具體資料列於下表6中。 30 表6 壓力（torr ) 4. 0 ~~ 基板溫度（°C ) 350 間距（m i 1 ) 250 ' RF 能量(Watts) 300 ~~ DEMS ( g/min) 1. 0 〇 2 流量（s c c m ) 100 S i F 4 流量（s c c m ) 200 1222961 其期望k值在2· 8到3· 0之間，揚氏模數約爲15Gpa， 奈米壓痕硬度約爲2GPa。 實施例2 2 本發明的OFSG膜’其在壓力爲1— l6torr，電聚能量 爲 100 — lOOOWatts，電極間距爲 200 — 40〇〇milli-inches (5·08— 10.16mm)，溫度爲200 - 425Ό條件下，化合三 甲基矽烷（其流量流速爲1一 l〇〇〇sccm)，SiF4 (其流量流 速爲1 — lOOOsccm)，和〇2 (其流量流速爲1 — 2〇〇sccm) 沈積而成。相對應的0SG膜，在除了沒有SiF4以外相同沈 積條件下，其利用三曱基矽烷/〇2氣態混合沈積而成。 前驅氣體的結構和組成在很大程度上影響化學氣相沈 積法沈積析出的薄膜的結構和成分。利用SiF4作爲F源的 唯一來源，這保證了在前驅氣體混合物中不存在C _ F鍵。 由於C— F鍵沒有Si — F鍵的熱力學穩定性，故而很難形成 31 1222961 C—F鍵，所以在最終形成的膜 H 4出現的是Si 氟以SiF4的形式存在於前驅混合氣中，這樣可能也會. 影響沈積過程。可以很清楚的觀察到膜沈積速率的=化[ 與OSG的沈積過程相比，0FSG膜的沈積速率慢了 3〇—⑼ %。OFSG膜的前驅氣體中含有^匕，而〇SG膜的前驅氣體 中不含SiF4，其餘條件兩者相同。這可能是由於在電漿沈 積過程中形成的氟基表面退火而造成的。沈積過程中這種 變化最可能的結果就是從膜表面去除弱鍵物質。這使得 _ OFSG膜在同樣組成下更稠密，如下表7所示。
32 表7 OFSG OSG 折射率，η 1. 42 1. 44 介電常數，k 2. 86 + 0. 03 2. 90 + 0. 09 模數（GPa) 12·5±0·5 8. 0 zb 0. 5 硬度（Η，GPa) 1. 67 + 0. 20 1· 21±0. 25 密度（g/cm3) 1. 49 1. 35 沈積速率（nm/min) 330 + 80 890 + 140 粘合強度（MPa) 55 N/A 元素（XPS) %Si 36±1 36± 1 %0 42±3 41 ±3 %C 19±3 23±3 %H N/A N/A %F 3±1 n. d. 元素（RBS) %Si 22±1 18±1 %0 30±3 26±3 %C 18±3 21 ±3 %H 27±3 35±3 %F 3±1 n. d. 1222961 實施例23 根據實施例22中製備的膜，其熱穩定性研究的資料總 結在下表8中。比較OFSG和OSG膜性能，在空氣氣氛4個 小時425 °C條件下，退火之前和之後，其在熱穩定性方面 33 1222961 值，在氧化氣氛425 °C埶#、p作μ > …、退火條件下，來監控元素穩定性。 從OSG轉變到〇fsG的過葙由π々曰％、丨 中，很谷易觀測到除了氧以外的 其他7G素。參考圖5c’其表明碳在〇sG覆蓋層中並不穩定， 而在OFSG膜中則特別穩冬圖5e同樣表明在退火過程中， 並沒有從OFSG到OSG層問沾翁、垂必门，
1的亂遷移。因此，我們認爲〇FSG 組成中有氟的存在可以改善膜内碳的穩定性。 實施例25 根據實施例22中製備的〇SG和㈣膜，在氮氣和空 氣氣氛，425。(：條件下，其熱穩定性用重量損失來評價。對 二OFSG和0SG膜的資料繪製在圖仏和讣中。前者表明在 氮氣中重量損失爲每小時〇.〇5%，而在空 每小時對OSG的分析表明，其在氮氣中重量損^ 爲0.05%，但當其在425。。下暴露於空氣中，重量損失瞬 間達到2%。 實施例26 根據實施例22中製備的0SG和0FSG膜，其組成的熱 穩定性利用紅外（IR)光譜法來評價。對於〇pSG膜的沈積 條件爲：電漿能量400W ; 200mils間距；6t〇rr壓力；35(rc 溫度；54〇SCCm三甲基矽烷；90sccm氧氣；25〇sccm四氟 化矽；和200秒時間。對於0SG膜的沈積條件爲：電漿能 量 600W; 260mils 間距；4t〇rr 壓力；35(rc 溫度；54〇sccm 三曱基矽烷；9〇Sccm氧氣；和72秒時間。在熱退火之前 35 1222961 和之後（4個小時，425°C，空氣氣氛）的〇FSG和〇s 的 IR光譜值列於表9中。 表9 退火前
0FSG
0SG 270 800
28. 3 1. 432 26. 7 沈積速率（nm/min 厚度（nm — 折射率（nm 電容（：pF) 介電常數 退火後 厚度（nm ) 厚度變化（％ ) 折射率 電容（pF) 介電常數 • 92 • 91 915
1. 393 1. 392 28. 1 28. 4 2. 88 2. 98 魯 如表9中資料表明，〇fsG膜在熱退火後電容和介電常 數均降低。相反，0SG膜在熱退火後電容和介電常數部增 加。 對本發明已經作了詳盡的闡述，並且給出了一些具體 實施例，所屬技術領域的技術人員非常清楚：可對本發明 進行各種變化和修改而不會脫離其本質和範圍。 36

Claims (1)

1222961 拾、申請專身
(2004年5月修正) Fz來表不的膜’其中，v+w + 35原子％，w從1〇到65原子 1 · 一種用公式 Siv〇wCxHyF x+ y + z= 100%，v 從 到 3 % ’ y從10到50原子％，χ從2到3〇原子％，z從〇·工 到15原子％，而且其中〇·5原子％或更少的氟鍵結於碳。 2如申明專利範圍第丨項所述的膜，其中大部分的氫 和破鍵結。 3 ·如申請專利範圍第i項所述的膜，其具有低於3. 5 的介電常數。 響 4 ·如申請專利範圍第1項所述的膜，其具有低於3. 0 的介電常數。 5 ·如申請專利範圍第1項所述的膜，其具有低於 2· Og/cm3的體積密度。 6 ·如申請專利範圍第【項所述的膜，其具有低於 1· 5g/cm3的體積密度。 7 ·如申請專利範圍第1項所述的膜，其具有低於5nm φ 當量球徑的孔尺度，該尺度用小角度中子散射儀或者正電 子毁滅壽命光譜儀測定。 8·如申請專利範圍第1項所述的膜，其具有低於2. 5nm 當量球徑的孔尺度，該尺度用小角度中子散射儀或者正電 子毁滅壽命光譜儀測定。 9 ·如申請專利範圍第1項所述的膜，其係藉由化學氣 相沈積而沈積在一半導體基板上。 10 ·如申請專利範圍第1項所述的膜，其是積體電路 38 1222961 (2004年5月修正) 中由以下層所組成之群中的至少一種··該群由絕緣層、層 間；丨電層孟屬層間介電層、覆蓋層、化學—機械平坦層 或者蝕刻終止層、阻絕層或者粘合層組成。 n ·如申請專利範圍第1項所述的膜，其在N2中425 °C 等溫條件下，平均質量損失低於1.0wt%/hr。 12 ·如申請專利範圍第1項所述的膜，其在空氣中 425°C等溫條件下，平均質量損失低於。 13·如申請專利範圍帛i項所述的膜，其具有低於 的體積密度；具有低於25_當量球徑的孔尺度， 名尺度用：角度中子散射儀或者正電子毁滅壽命光譜儀測 疋在帛導體基板上沈積析出；該膜是在積體電路中由 以下層所組成之群中的5小_ # ^ , 的至V 種’該群由絕緣層、層間介 電層，金屬層間介電屉、笋笨 9覆π層、化學〜機械平坦層或者 蚀刻終止層、阻絕層或者枯合層組成。 14 ·如申請專利筋圖 圍苐1項所述的膜，其中X/z>〇. 25。 15· —種用公式si〇CH X 表不的膜，其中，v+w + + y+z=10〇%，¥從 原子％，w從1〇到65原子 %，y攸10到5 0原子〇/ 〇，X從1到3 〇原子％，從 到15原子％，其限制 ^0*1 Η条件爲χ/ζ>〇·25，而且盆 子％或更少的氟鍵結於碳。 ，、中0.5原 16.如中請專利範圍第15項所述的膜，1 1.5g/cm3的體積密度；具有 .....有低於 · ; 2· 5nm當量跋和的$ p洚 該尺度用小角度中子散 里工的孔尺度， 丁政射儀或者正電子妒 ， 定。而且，該膜中大邱八^ 1又滅奇π光譜儀測 |八4分氣和碳鐽人· + t ^ 人埏α，在一半導體基板上 39 1222961 (2004年5月修正） 沈積析出，該膜是在積體電路中由以下層所組成之群中的· · 至少一種：該群由絕緣層、層間介電層、金屬層間介電層、 覆蓋層、化學一機械平坦層或者蝕刻終止層、阻絕層或者 粘合層所組成。 17 · 一種用公式Siv〇wCxHyFz表示的膜，其中，v+w+x + y+Z=l〇〇%，v從到35原子％，w從10到65原子 %，y從10到50原子％，χ從i到3〇原子％，z從〇 1 到15原子％，其中〇·5原子％或者更少的氟鍵結於碳，其 適合防止膜性能隨環境條件的變化而變化。 18 ·如申請專利範圍第17項所述的膜，其環境條件是 微電子處理過程。 19·如申請專利範圍第18項所述的膜，其微電子處理 過程是化學氧化或者熱氧化過程。 20·如申請專利範圍第17項所述的膜，其一個膜性能 爲介電常數，環境條件至少爲由以下步驟所紐成群中的一 個微電子處理步驟：該群由加溫退火、電介質蝕刻和後蝕 刻灰化過程所組成。 21.如申請專利範圍第20項所述的膜’其環境條件可 使介電常數增加10%或更少。 22·如申請專利範圍第2〇項所述的膜’其環境條件可 使介電常數增加〇 · 1 %或更少。 、，23.如申請專利範圍第20項所述的膜’其由環境條件 增加的介電常數值小於參考0SG膜由環境條件增加的參 介電常數值。 " 40 (_4年5月修E) 24 ·如申請專利範圍第23項所述的膜，其由環境條件 增加的介電常數值爲參考OSG膜由環境條件所增加的參 介電常數值的50%或者更小。 25 ·如申請專利範圍第24項所述的膜，其由環境條件 增加的介電常數值爲參考〇SG膜由環境條件所增加的參 介電常數值的20%或者更小。 ^ 26·如申請專利範圍第17項所述的膜，其一個膜性能 爲整個膜内氟分佈。 ％
27 ·如申請專利範圍第 爲膜内碳濃度。 17項所述的膜，其一個膜性 28·如申請專利範圍第27項所述的膜，其由環境條件 降低的碳濃度值爲參考0SG膜由環境條件所降低的表考炉 濃度值的5 0 %或者更小。 29 ·如申請專利範圍第28項所述的膜，其由環境條件 降低的碳濃度值爲參考OSG膜由環境條件所降低的參考碳 濃度值的20%或者更小。 30 · —種用公式Siv0wCxHyFz表示的膜，盆φ 八τ v十w + χ + y+ 100%，v從10到35原子％，w從1〇到65原子 %，y從10到50原子％，X從1到30原子％，z從〇工 到15原子％，其限制條件爲χ/ζ>〇· 25，1中0 ς7 八τ u· b原子％ 或者更少的氟鍵結於$反’該膜適合防止膜性能隨微電子户 理過程而變化。
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