TWI512134B - 使用氣體混合物之自由基的原子層沈積 - Google Patents

使用氣體混合物之自由基的原子層沈積 Download PDF

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TWI512134B
TWI512134B TW101105141A TW101105141A TWI512134B TW I512134 B TWI512134 B TW I512134B TW 101105141 A TW101105141 A TW 101105141A TW 101105141 A TW101105141 A TW 101105141A TW I512134 B TWI512134 B TW I512134B
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Sang In Lee
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    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
    • C23C16/45536—Use of plasma, radiation or electromagnetic fields
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
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    • C23C16/45548—Atomic layer deposition [ALD] characterized by the apparatus having arrangements for gas injection at different locations of the reactor for each ALD half-reaction
    • C23C16/45551—Atomic layer deposition [ALD] characterized by the apparatus having arrangements for gas injection at different locations of the reactor for each ALD half-reaction for relative movement of the substrate and the gas injectors or half-reaction reactor compartments

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Description

使用氣體混合物之自由基的原子層沈積
本發明係關於使用原子層沈積(atomic layer deposition，ALD)在基板上沈積一或多個材料層。
本申請案根據35 U.S.C.§ 119(e)主張2011年2月16日申請的同在申請中之美國臨時專利申請案第61/443,556號之優先權，其係以全文引用的方式併入本文中。
原子層沈積(ALD)為用於在基板上沈積一或多個材料層之薄膜沈積技術。ALD使用兩種類型之化學品，一種為源前驅體，另一種為反應物前驅體。一般而言，ALD包括四個階段：(i)注入源前驅體，(ii)移除源前驅體之物理吸附層，(iii)注入反應物前驅體，及(iv)移除反應物前驅體之物理吸附層。ALD可為緩慢製程，其在可獲得所需厚度之層之前可能花費大量時間或重複許多次。因此，為加快製程，可使用如美國專利申請公開案第2009/0165715號中所描述之具有單元模組(所謂的線性注入器)之氣相沈積反應器或其他類似裝置以加快ALD製程。單元模組包括用於源材料之注入單元及排放單元(源模組)，及用於反應物之注入單元及排放單元(反應物模組)。
習知ALD氣相沈積室具有用於在基板上沈積ALD層之一或多組反應器。當基板在反應器下方穿過時，基板暴露於源前驅體、沖洗氣體及反應物前驅體。沈積於基板上之源前驅體分子與反應物前驅體分子反應或源前驅體分子由反 應物前驅體分子置換，以在基板上沈積材料層。在基板暴露於源前驅體或反應物前驅體之後，可使基板暴露於沖洗氣體以自基板移除過量之源前驅體分子或反應物前驅體分子。
為減少沈積所需厚度之材料所需之重複次數，宜增加每一ALD循環之沈積速率。
實施例係關於在基板上沈積材料層，其藉由產生含有第一氣體及第二氣體之氣體混合物之自由基且接著將該等自由基注入基板上來執行。第一氣體包括氮化合物。基板事先已注有源前驅體。自由基充當反應物前驅體，與基板上之源前驅體分子反應或置換源前驅體分子，且在基板上沈積材料層。
在一個實施例中，第二氣體包括另一氮化合物。第一氣體可包括NH3 且第二氣體可包括N2 O。
在一個實施例中，所沈積材料包含氮氧化鋁(aluminum oxynitride，AlON)。
在一個實施例中，N2 O與NH3 之比率為70：30至90：10。更佳地，N2 O與NH3 之比率為80：20。
在一個實施例中，將氣體混合物注入自由基反應器內之電漿室中。在電漿室中之第一電極與電漿室周圍之第二電極之間施加電壓，以在電漿室中產生電漿。電漿產生氣體混合物之自由基。
在一個實施例中，自電漿室至基板之距離為小於80 mm。
在一個實施例中，源前驅體係選自由四乙基甲胺基鋯(Tetraethylmethylaminozirconium，TEMAZr)、三甲基矽烷(Trimethylsilane，TMS)、三(二甲胺)聚矽氧(Tridimethylaminesilicone，3DMAS)及四乙基甲基鋁鈦(Tetraethylmethylaluminumtitanium，TEMATi)組成之群。
在一個實施例中，第一氣體包含NH3 且第二氣體包含CH4 。
實施例亦係關於自由基反應器，其包含主體及電極，用以在原子層沈積(ALD)製程中產生充當反應物前驅體之自由基。主體經形成具有用於供應氣體之通道、連接至通道以接收所供應氣體且產生所供應氣體之自由基的電漿室、連接至電漿室以接收所產生自由基且位於基板上方以使基板暴露於自由基的反應室、及排出過量氣體及/或自由基之一或多個排放部分。電極在主體內延伸。在電極與主體兩端施加電壓以在電漿室內產生電漿。
在此參看隨附圖式描述實施例。然而，在此揭示之原理可以許多不同形式予以體現，且不應被解釋為限於在此闡述之實施例。在描述中，可省略熟知特徵及技術之細節，以避免不必要地使實施例之特徵不明確。
在圖式中，圖式中之類似參考數字表示類似元件。為了清晰起見，可誇示圖式之形狀、大小及區域，及其類似者。
實施例係關於使用氣體混合物產生充當反應物前驅體以在基板上沈積材料層之自由基來執行原子層沈積(ALD)。氣體混合物包括含氮化合物，諸如NH3 或N2 O。基板事先已注有源前驅體材料。因此，當基板注有反應物前驅體時，在基板上沈積材料層。藉由使用氣體混合物代替單一氣體產生自由基，可增加材料之沈積速率。
圖1為根據一個實施例之線性沈積裝置100之截面圖。圖2為根據一個實施例之線性沈積裝置100之透視圖(不含室壁以有助於說明)。線性沈積裝置100可尤其包括支撐柱118、處理室110及一或多個反應器136。反應器136可包括一或多個注入器及自由基反應器。各注入器將源前驅體、反應物前驅體、沖洗氣體或此等材料之組合注入基板120上。如下文參考圖5詳細描述，源前驅體及/或反應物前驅體可為氣體混合物之自由基。
由壁封閉之處理室可維持在真空狀態下，以防止污染物影響沈積製程。處理室110含有容納基板120之基座128。基座128置放於用以滑動移動之支撐板124上。支撐板124可包括溫度控制器(例如加熱器或冷卻器)以控制基板120之溫度。線性沈積裝置100亦可包括起模頂桿(lift pin)(未圖示)，其幫助將基板120裝載至基座128上或將基板120自基座128上卸除。
在一個實施例中，基座128緊固於托架210上，托架210在整個延伸桿138上移動，其中延伸桿138上形成有螺旋。托架210在其容納延伸桿138之孔中形成有相應螺旋。延伸 桿138緊固於馬達114之軸上，且因此當馬達114之軸旋轉時，延伸桿138跟著旋轉。延伸桿138之旋轉引起托架210(且因此基座128)在支撐板124上線性移動。藉由控制馬達114之速度及旋轉方向，可控制基座128線性移動之速度及方向。使用馬達114及延伸桿138僅為用於移動基座128之機構的一個實例。亦可使用多種其他移動基座128之方式(例如，在基座128之底部、頂部或側面使用齒輪及小齒輪)。此外，代替移動基座128，可使基座128保持靜止且可使反應器136移動。
圖3為根據一個實施例之旋轉沈積裝置300之透視圖。代替使用圖1之線性沈積裝置100，根據另一個實施例，可使用旋轉沈積裝置300來執行沈積製程。旋轉沈積裝置300可尤其包括反應器320A、320B、334A、334B、364A、364B、368A、368B，基座318及封閉此等組件之容器324。如上文參考圖1所描述，旋轉沈積裝置300之一組反應器(例如，320A及320B)對應於線性沈積裝置100之反應器136。基座318將基板314緊固於適當位置。反應器320A、320B、334A、334B、364A、364B、368A、368B係置放於基板314及基座318上方。基座318或反應器320、334、364、368旋轉以使基板314經受不同製程。
一或多個反應器320A、320B、334A、334B、364A、364B、368A、368B連接至氣管(未圖示)以提供源前驅體、反應器前驅體、沖洗氣體及/或其他材料。氣管提供之材料可(i)藉由反應器320A、320B、334A、334B、364A、 364B、368A、368B直接注入基板314上，(ii)在於反應器320A、320B、334A、334B、364A、364B、368A、368B內之腔室中混合之後注入基板314上，或(iii)在藉由於反應器320A、320B、334A、334B、364A、364B、368A、368B內產生之電漿轉化為自由基之後注入基板314上。在材料注入基板314上之後，多餘材料可經由出口330、338排放。旋轉沈積裝置300之內部亦可維持在真空狀態下。
儘管以下實例實施例主要參考線性沈積裝置100中之反應器136描述，但相同原理及操作可應用於旋轉沈積裝置300或其他類型之沈積裝置。
圖4為根據一個實施例之圖1之沈積裝置100中之反應器136A、136B(統稱為「反應器136」)的透視圖。在圖4中，反應器136A及136B彼此鄰接串聯置放。在其他實施例中，反應器136A、136B可彼此相隔一定距離置放。當基板120自左向右移動(如箭頭450所示)時，基板120依序藉由反應器136A及136B注入材料以在基板120上形成沈積層410。代替移動基板120，可在注入源前驅體材料或反應物前驅體材料時自右向左移動反應器136A、136B。
在一或多個實施例中，反應器136A為氣體注入器，其將源前驅體材料注入基板120上。反應器136A連接至管(未圖示)以接收來自源(例如罐)之源前驅體。源前驅體注入基板120上，在基板120上形成一或多個源前驅體分子層。過量源前驅體分子經由排放管422A、422B排放。
反應器136B可為產生自一或多個源(例如罐)接收之氣體 或氣體混合物之自由基的自由基反應器。氣體或氣體混合物之自由基可充當反應物前驅體，其結合源前驅體在基板120上形成材料之原子層。氣體或氣體混合物經由管(未圖示)注入反應器136B中，且藉由在電極兩端施加電壓在反應器136B內轉化為自由基。自由基注入基板120上，且恢復至非活性狀態之餘留自由基及/或氣體自反應器136B經由排放管438A、438B排出。
圖5A為根據一個實施例之說明沿圖4之線A-B截取之反應器136A、136B的截面圖。注入器136A包括主體500，其經形成具有氣體通道516、穿孔(狹縫或孔)520、反應室514、收縮區518A、518B及排放部分510A、510B。源前驅體經由氣體通道516及穿孔520注入反應室514中。反應室514下方之基板120之區域與源前驅體接觸，且在其表面吸收源前驅體分子。過量源前驅體(亦即，在源前驅體沈積於基板120上之後餘留之源前驅體)穿過收縮區518A、518B，且經由排放部分510A、510B排出。排放部分510A、510B連接至排放管422A、422B。
當源前驅體分子穿過收縮區518A、518B時，歸因於源前驅體分子之較高流動速率，物理吸附之源前驅體分子至少部分自此等區域518A、518B下方之基板120之區域移除。
在一或多個實施例中，注入器136A亦可將沖洗氣體注入基板120上以自基板120移除物理吸附之源前驅體分子，在基板120上僅留下化學吸附之源前驅體分子。以此方式， 可獲得產生高品質原子層之ALD製程。
自由基反應器136B與注入器136A具有類似結構，除了自由基反應器進一步包括電漿產生器。電漿產生器包括內部電極576及電漿室578周圍之外部電極572(外部電極572可為金屬主體550之一部分)。主體550尤其經形成具有氣體通道564、穿孔(狹縫或孔)568、電漿室578、注入器狹縫580、反應室562及排放部分560A、560B。氣體或氣體混合物經由通道564及穿孔568注入電漿室578中。藉由在內部電極576與外部電極572之間施加電壓差，在電漿室578內產生電漿。電漿之結果是，在電漿室578內產生氣體或氣體混合物之自由基。產生之自由基經由注入器狹縫580注入反應室562中。反應室562下方之基板120之區域與自由基接觸，在基板120上形成沈積層410。
電漿室578與基板120之間的距離H經組態以使足量自由基以活性狀態到達基板120。自由基具有預定壽命。因此，當自由基經由注入器狹縫580及反應室562行進至基板120時，一些自由基恢復回至非活性氣體狀態。隨著行進距離增大，恢復至非活性氣體狀態之自由基的量增加。因此，宜設置距離H為小於某一長度。舉例而言，距離H設置為10 mm至100 mm。
當使用含氮氣體混合物(例如N2 O與NH3 混合物)之自由基時，自由基之壽命相對較短，且若距離H為80 mm或大於80 mm，則大部分自由基恢復回至非活性狀態。因此，當使用含氮氣體混合物之自由基時，距離H設置為小於80 mm。
圖5B為說明沈積層中之氮濃度與基板120離電漿室578之距離H之間的關係的圖。在圖5B之實驗中，基板120注有三甲基鋁(Trimethylaluminium，TMA)，且接著注有包括50% N2 O及50% NH3 的氣體混合物之自由基，由此在基板120上沈積原子層AlON。因更多氮自由基(N＊ )保持活性，故更多氮原子併入沈積之AlON層中。因此，沈積層中之氮含量隨以活性狀態到達基板120表面之活性自由基之量而變化。隨著距離H增大，沈積層中之氮含量減少。氮含量減少指示氮自由基N＊ 未能有效到達基板120。參考圖5B，若距離H增加至80 mm或大於80 mm，則沈積層中之氮含量明顯下降。因此，當使用氮自由基N＊ 作為反應物前驅體時，宜維持距離H小於80 mm。
出於圖5B中說明之實驗之目的，基板120之溫度維持在80℃且TMA氣罐之溫度維持在5℃。藉由施加200瓦特下120 kHz之DC脈衝在電漿室578中產生電漿。所得AlON膜之沈積速率為1.70埃/循環。
圖6為根據另一個實施例之說明自由基反應器600之截面圖。自由基反應器600包括主體610及在整個自由基反應器600內延伸之內部電極614。內部電極具有半圓形截面，其中平面表面面向基板120且圓形表面背向基板120。
氣體或氣體混合物經由自由基反應器之主體610內形成之通道618及穿孔622注入自由基反應器600中。主體610之部分624充當外部電極。藉由在內部電極614與外部電極 624之間施加電壓，可在電漿區域628中產生自由基。自由基經由收縮區642A、642B流入排放部分626A、626B中。在自由基反應器600中沈積原子層之原理及操作與自由基反應器136B實質上相同，為簡潔起見在此略去。亦可使用多種其他組態之自由基反應器。
當產生氮自由基時，宜使用氣體混合物代替使用單一氣體。舉例而言，基於實驗，與使用僅N2 O氣體或NH3 氣體相比，自N2 O氣體與NH3 氣體之混合物產生之自由基產生較高沈積速率。然而，在氣體之某一混合比率下，形成粒子。因此，如下文參考表1詳細描述，執行實驗以確認產生較高沈積速率同時避免在自由基反應器136B中形成粒子之混合比率之範圍。
在以下實驗中，首先在基板上注入TMA且接著注入氣體之自由基以形成AlN、Al2 O3 或AlON膜。基板之溫度維持在80℃且TMA之溫度維持在5℃。為產生用作反應物前驅體之自由基，使用NH3 、N2 O或其混合物。為產生電漿，在內部電極576與外部電極572之間施加200瓦特下120 kHz之電壓信號。基板與電漿室之間的距離H(參見圖5)為17 mm。自由基反應器之長度為260 mm。固持基板之基座之直徑為80 cm且基座旋轉速度為5 rpm。
所量測AlN、Al2 O3 或AlON層之沈積速率及此等層之特徵列於表1中。當將比率為x(NH3 氣體，其中x取0與1之間的值)比(1-x)(N2 O氣體)之NH3 及N2 O注入自由基反應器時，所得層為Al2 O3 (當x=1時)、AlN(當x=0時)或 (x)Al2 O3 +(1-x)AlN。
由表1可知，當N2 O氣體與NH3 氣體之間的比率為80：20時，沈積速率最大(1.96埃/循環)。在此比率下，自由基反應器中無粒子產生。當NH3 增多或減少超出此比率時，沈積速率減小。此外，當NH3 之比率增至40%時，自由基反應器中形成粒子。具體而言，當N2 O與NH3 之比率在40：60至60：40範圍內時，自由基反應器中偵測到粒子。當NH3 之比率增至70%及大於70%時，未偵測到粒子。表1顯示宜使用含氮氣體混合物之自由基代替使用僅N2 O或NH3 ，以提高沈積速率。
在另一個實施例中，可使用四乙基甲胺基鋯(TEMAZr)作為源前驅體，且可使用(1-x)N2 O與(x)NH3 (其中x為大於0且小於0.5之值)之類似混合物來產生自由基作為反應物前驅體，以在基板上產生ZrO(1-x) Nx 層。
在另一個實施例中，可使用三甲基矽烷(TMS，(CH3 )3 SiH)或三(二甲胺)聚矽氧(3DMAS)作為源前驅體，且可使用(1-x)NH3 與(x)N2 O(其中x為大於0且小於0.5)之氣體來產生自由基充當反應物前驅體，以獲得SiOx N(1-x) 層。
用於產生自由基之氣體混合物不限於含氮氣體。舉例而言，可使NH3 與CH4 混合以產生N＊ 及C＊ 自由基。在一個實施例中，使用四乙基甲基鋁鈦(TEMATi)作為源前驅體且使用自(1-x)NH3 及(x)CH4 (其中x大於0且小於0.5)產生之自由基作為反應物前驅體，以在基板上形成TiC(1-x) Nx 層。
在另一個實施例中，使用TiCl4 作為源前驅體且使用自N2 或NH3 氣體產生之自由基作為反應物前驅體，以在基板上產生TiN膜之原子層。
在以上實施例中，自基板至電漿室之距離H可設置為小於80 mm，以使大部分自由基可在未恢復回至非活性狀態的情況下到達基板。
圖7為根據一個實施例之說明使用含氮氣體混合物之自由基執行原子層沈積之製程的流程圖。首先，藉由注入器136A將源前驅體注入基板之區域上(710)。接著，使基板120與注入器總成136之間相對移動(720)，以使基板120之區域置放於自由基反應器136B下方。
自由基反應器136B經注有氣體混合物。氣體混合物可包括第一氣體及第二氣體。第一氣體可為NH3 且第二氣體可為N2 O。藉由使用兩種不同氣體之混合物，可增加ALD製程之沈積速率。在此實例中，沈積層為AlON。
儘管上文已就若干實施例描述本發明，但可在本發明之範疇內進行各種修改。因此，本發明之揭示內容意欲為說明性的而不限制本發明之範疇，本發明之範疇在以下申請專利範圍中闡述。
100‧‧‧線性沈積裝置
110‧‧‧處理室
114‧‧‧馬達
118‧‧‧支撐柱
120‧‧‧基板
124‧‧‧支撐板
128‧‧‧基座
136‧‧‧反應器/注入器總成
136A‧‧‧反應器/氣體注入器
136B‧‧‧反應器/自由基反應器
138‧‧‧延伸桿
210‧‧‧托架
300‧‧‧旋轉沈積裝置
314‧‧‧基板
318‧‧‧基座
320A‧‧‧反應器
320B‧‧‧反應器
324‧‧‧容器
330‧‧‧出口
334A‧‧‧反應器
334B‧‧‧反應器
338‧‧‧出口
364A‧‧‧反應器
364B‧‧‧反應器
368A‧‧‧反應器
368B‧‧‧反應器
410‧‧‧沈積層
422A‧‧‧排放管
422B‧‧‧排放管
438A‧‧‧排放管
438B‧‧‧排放管
450‧‧‧箭頭
500‧‧‧主體
510A‧‧‧排放部分
510B‧‧‧排放部分
514‧‧‧反應室
516‧‧‧氣體通道
518A‧‧‧收縮區
518B‧‧‧收縮區
520‧‧‧穿孔/狹縫/孔
550‧‧‧主體
560A‧‧‧排放部分
560B‧‧‧排放部分
562‧‧‧反應室
564‧‧‧氣體通道
568‧‧‧穿孔/狹縫/孔
572‧‧‧外部電極
576‧‧‧內部電極
578‧‧‧電漿室
580‧‧‧注入器狹縫
600‧‧‧自由基反應器
610‧‧‧主體
614‧‧‧內部電極
618‧‧‧氣體通道
622‧‧‧穿孔
624‧‧‧外部電極
626A‧‧‧排放部分
626B‧‧‧排放部分
628‧‧‧電漿區域
642A‧‧‧收縮區
642B‧‧‧收縮區
H‧‧‧距離
圖1為根據一個實施例之線性沈積裝置之截面圖。
圖2為根據一個實施例之線性沈積裝置之透視圖。
圖3為根據一個實施例之旋轉沈積裝置之透視圖。
圖4為根據一個實施例之沈積裝置中之反應器的透視圖。
圖5A為根據一個實施例之說明沿圖4之線A-B截取之反應器的截面圖。
圖5B為說明沈積層中之氮濃度與基板離電漿室之距離之間的關係的圖。
圖6為根據另一個實施例之說明自由基反應器之截面圖。
圖7為根據一個實施例之說明使用含氮氣體混合物之自由基執行原子層沈積之製程的流程圖。
120‧‧‧基板
128‧‧‧基座
136A‧‧‧反應器/氣體注入器
136B‧‧‧反應器/自由基反應器
500‧‧‧主體
510A‧‧‧排放部分
510B‧‧‧排放部分
514‧‧‧反應室
516‧‧‧氣體通道
518A‧‧‧收縮區
518B‧‧‧收縮區
520‧‧‧穿孔/狹縫/孔
550‧‧‧主體
560A‧‧‧排放部分
560B‧‧‧排放部分
562‧‧‧反應室
564‧‧‧氣體通道
568‧‧‧穿孔/狹縫/孔
572‧‧‧外部電極
576‧‧‧內部電極
578‧‧‧電漿室
580‧‧‧注入器狹縫
H‧‧‧距離

Claims (10)

  1. 一種在基板上沈積材料層之方法，其包含：將源前驅體注入基板上；將NH3 氣體與N2 O氣體之混合物注入自由基反應器中，該混合物中N2 O與NH3 之比率為70：30至90：10；於該自由基反應器中產生該混合物之自由基；及將所產生之自由基注入該基板上，其中自該自由基反應器至該基板之距離為小於80mm，該等所產生之自由基與源前驅體分子反應或置換該等源前驅體分子，以在該基板上沈積材料層。
  2. 如請求項1之方法，其中該沈積材料包含氮氧化鋁(AlON)。
  3. 如請求項1之方法，其中該N2 O與NH3 之比率為80：20。
  4. 如請求項1之方法，其中產生該等自由基包含：將該混合物注入該自由基反應器內之電漿室中；及在該電漿室中之第一電極與該電漿室周圍之第二電極兩端施加電壓。
  5. 如請求項1之方法，其中該源前驅體係選自由四乙基甲胺基鋯(TEMAZr)、三甲基矽烷(TMS)、三(二甲胺)聚矽氧(3DMAS)及四乙基甲基鋁鈦(TEMATi)組成之群。
  6. 一種用於產生氣體自由基之自由基反應器，其包含：主體，其經形成有用於供應氣體之通道、連接至該通道以接收該所供應氣體且產生該所供應氣體之自由基的電漿室、連接至該電漿室以接受該等所產生之自由基且 位於基板上方以使該基板暴露於該等自由基的反應室、及排出過量氣體或自由基之一或多個排放部分，其中該所供應氣體包含NH3 與N2 O之混合物，該混合物中N2 O與NH3 之比率為70：30至90：10，其中自該電漿室至該基板之距離為小於80mm；及在該主體內延伸之電極，在該電極與該主體兩端施加電壓以在該電漿室內產生電漿。
  7. 如請求項6之自由基反應器，其中該基板暴露於該等自由基在該基板上沈積氮氧化鋁(AlON)。
  8. 如請求項6之自由基反應器，其中該主體進一步經形成有連接該電漿室與該反應室之穿孔。
  9. 如請求項6之自由基反應器，其中至少一部分該自由基反應器係置放於真空狀態下。
  10. 如請求項6之自由基反應器，其中該基板含有選自由四乙基甲胺基鋯(TEMAZr)、三甲基矽烷(TMS)、三(二甲胺)聚矽氧(3DMAS)及四乙基甲基鋁鈦(TEMATi)組成之群之材料層。
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