TW202208664A - 導電氮化物膜的成核方法 - Google Patents
導電氮化物膜的成核方法 Download PDFInfo
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- TW202208664A TW202208664A TW110122054A TW110122054A TW202208664A TW 202208664 A TW202208664 A TW 202208664A TW 110122054 A TW110122054 A TW 110122054A TW 110122054 A TW110122054 A TW 110122054A TW 202208664 A TW202208664 A TW 202208664A
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- reaction zone
- metal
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- nitride
- pulse sequence
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- 238000000034 method Methods 0.000 title claims abstract description 60
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- 238000010899 nucleation Methods 0.000 title claims abstract description 29
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011800 void material Substances 0.000 claims abstract description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 12
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- 238000006243 chemical reaction Methods 0.000 claims description 50
- 238000001208 nuclear magnetic resonance pulse sequence Methods 0.000 claims description 46
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- LXEXBJXDGVGRAR-UHFFFAOYSA-N trichloro(trichlorosilyl)silane Chemical group Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl LXEXBJXDGVGRAR-UHFFFAOYSA-N 0.000 claims description 19
- 229910003074 TiCl4 Inorganic materials 0.000 claims description 18
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 9
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- H01L21/02186—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal the material containing titanium, e.g. TiO2
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- H01L21/0228—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition deposition by cyclic CVD, e.g. ALD, ALE, pulsed CVD
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Abstract
提供利用某些含矽鹵化物、含矽醯胺及某些金屬前體連同含氮還原氣體用於某些金屬氮化物基板表面之成核的經改良方法。在利用預處理步驟的同時,該方法顯示極大經改良成核,其中微電子裝置基板具有沉積於其上之具有約10 Å至約15 Å之厚度及小於約1%之空隙面積的這種金屬氮化物膜。一旦達成該成核,便可快速實施傳統的層疊沉積。
Description
本發明概言之係關於在微電子裝置上形成某些薄膜之方法。具體而言,本發明係關於金屬氮化物膜在微電子裝置之表面上的成核方法。
在積體電路之製造中,氮化鈦因其相對較低電阻率及與CMOS (互補金屬氧化物半導體)製程之相容性而備受關注。因此,氮化鈦通常用作襯墊障壁且可沉積於矽基板上。該等氮化鈦層可用作障壁層以抑制金屬擴散至障壁層下面之區域中。導電金屬層(例如,含銅層或含鎢層)通常沉積於氮化鈦層上。鈦層可藉由化學氣相沉積(CVD)製程、原子層沉積(ALD)製程及/或物理氣相沉積(PVD)製程形成。舉例而言,氮化鈦層可藉由在CVD製程期間四氯化鈦與還原劑(例如氨)反應形成且氮化鈦層可藉由在CVD製程中使四氯化鈦與氨反應形成。此後,可將導電材料沉積於微電子裝置基板上。參見例如美國專利第7,838,441號。然而,諸如氮化鈦及氮化矽鈦之材料的沉積為在微電子裝置基板上起始沉積之困難所困擾,且在所謂的初始非線性生長區域中,膜厚度基於沉積序列數量之構建相對較差。參見例如「Growth Mechanism and Continuity of Atomic Layer Deposited TiN films on Thermal SiO2
」, A. Satta等人,Journal of Applied Physics
, 第92卷, 第12期, 第7641-7646頁(2002)。
因此,業內需要用於在微電子裝置基板上沉積含鈦膜之經改良方法,特定地在基板表面利用該等含鈦材料之起始形成或成核期間。
概言之,本發明提供利用某些含矽鹵化物、含矽醯胺及某些金屬前體連同含氮還原氣體用於某些金屬氮化物基板表面之成核的經改良方法。在利用預處理步驟的同時,該方法顯示極大經改良成核,其中微電子裝置基板具有沉積於其上之具有約10 Å至約15 Å之厚度及小於約1%之空隙面積的這種金屬氮化物膜。一旦達成該成核,便可快速實施傳統的層疊沉積。
相關申請案之交叉參考
本申請案係於2020年6月17日提交並以引用的方式併入本文之美國序列號16/904,179之部分延續申請案,並根據35 USC § 120主張其優先權。
除非上下文另外明確指示,否則如本說明書及隨附申請專利範圍中所用,單數形式「一(a, an)」及「該」包括複數個指示物。除非上下文另外明確指示,否則如本說明書及隨附申請專利範圍中所用,術語「或」通常以其含義使用,包括「及/或」。
術語「約」通常係指認為與所述值等效(例如,具有相同功能或結果)之數值範圍。在許多情況中,術語「約」可包括四捨五入至最接近的有效數字之數值。
使用端點所表達之數值範圍包括屬該範圍內之所有數值(例如,1至5包括1、1.5、2、2.75、3、3.80、4及5)。
在第一態樣中,本發明提供用於金屬氮化物在反應區中在微電子裝置基板之表面上成核之預處理方法,其包含:
I. 在脈衝氣相沉積條件下將選自A、B及C之化合物引入至反應區中,其中該等脈衝氣相沉積條件包含複數個脈衝序列,其中將化合物A、B及C中之至少兩者依序且以任何順序引入至該反應區中,其中之一者為A,每一者視情況隨後係利用惰性氣體之吹掃步驟,以界定脈衝序列之第一循環,其中該複數個包含至少三個循環,其中A、B及C定義為:
A. 選自含矽鹵化物及含矽醯胺之前體;
B. 金屬前體,其中該金屬選自鈦、鉭、鉬、鎢及鈮;及
C. 含氮還原氣體,其中該含氮還原氣體在每一脈衝序列之每循環引入至該反應區中一次或兩次。
在一個實施例中,脈衝序列之循環在此預處理步驟中重複約3至約15次。在另一實施例中,A係雙-第三戊基伸乙基矽烯且B係TiCl4
。在另一實施例中,脈衝序列之第一循環係六氯二矽烷;NH3
;TiCl4
;及NH3
。在另一實施例中,脈衝序列之第一循環係(i)六氯二矽烷及NH3
;(ii) 六氯二矽烷及N2
H4
;(iii) 六氯二矽烷及1,1-二甲基肼;或(iv) 六氯二矽烷及1,2-二甲基肼。
在第二態樣中,本發明提供用於金屬氮化物在反應區中在微電子裝置基板之表面上成核之方法,其包含:
I. 在脈衝氣相沉積條件下將選自A、B及C之化合物引入至反應區中,其中該等脈衝氣相沉積條件包含複數個脈衝序列,其中將化合物A、B及C中之至少兩者依序且以任何順序引入至該反應區中,其中之一者為A,每一者視情況隨後係利用惰性氣體之吹掃步驟,以界定脈衝序列之第一循環,其中該複數個包含至少三個循環,其中A、B及C定義為:
A. 選自含矽鹵化物及含矽醯胺之前體;
B. 金屬前體,其中該金屬選自鈦、鉭、鉬、鎢及鈮;及
C. 含氮還原氣體,其中該含氮還原氣體在每一脈衝序列之每循環引入至該反應區中一次或兩次;隨後
II. 將脈衝序列之第二循環引入至該反應區中,脈衝序列之該第二循環包含將化合物D及E以任一順序引入至該反應區中,每一者視情況隨後利用惰性氣體吹掃:
D. 金屬前體,其中該金屬選自鈦、鉭、鉬、鎢及鈮;及
E. 含氮還原氣體;及
將脈衝序列之該第二循環重複足夠反覆次數以在基板上建立金屬氮化物成核,以提供代表在具有約10 Å至約15 Å之厚度之膜中小於約1%空隙面積之覆蓋區。
在一個實施例中,基板表面包含二氧化矽。在另一實施例中,基板表面選自氧化鋁、氧化鋯、二氧化鉿及其混合物。
如本文所用,術語「金屬氮化物」包括具有不同比例之選自鈦、鉭、鉬、鎢及鈮之金屬與氮之膜。在該等膜中,膜中金屬之原子百分比可端視金屬及沉積方法而變。另外,含有金屬氮化物之膜可進一步包含約2%至約20%原子百分比之矽。該等金屬氮化物膜可使用其已知金屬前體製備,例如TiCl4
;TiI4
;四(二甲基醯胺基)鈦(TDMAT);Ti(NCH2
CH3
)x
Cly
;TaCl5
;TaF5
;MoCl5
;WCl5
;WF6
;NbCl5
;及諸如此類。本文所闡述之前體可單獨使用,或與不同前體組合或依次使用。舉例而言,在一個實施例中,可利用鈦前體四(二甲基醯胺基)鈦直至達成約1個單層之膜,且之後可利用氯化前體(例如TiCl4
)以進一步構建膜。對於實例性金屬氮化物前體,參見例如Journal of Applied Physics
113, 021301 (2013) 「Crystallinity of inorganic films grown by atomic layer deposition: overview and general trends」表IV (第48-50頁)。實例包括(但不限於) TiCl4
、TiI4
、Ti(N(CH3
)2
)4
、Ti(N(CH3
CH2
)(CH3
))4
、TaCl5
、TaClS(CH3
CH2
)2
、TaBr5
、Ta(N(CH3
)2
)5
、Ta(N(CH3
CH2
)CH3
)5
、Ta(異丙基-N)(N(CH3
CH2
)CH3
)3
、Ta(第三丁基N)(N(CH3
CH2
)2
)3
、Ta(第三戊基-N)(N(CH3
)2
)3
、NbCl5
、WF6
、W(tBu-N)2
(N(CH3
)2
)2
、W2
(N(CH3
)2
)6
及諸如此類。
在一個實施例中,金屬前體選自TiCl4
、TiI4
、Ti(NCH2
CH3
)x
Cly
(其中x + y =4)、式Ti(NR2
)4
之化合物(其中R2
係C1
-C4
烷基)(例如四(二甲基醯胺基)鈦)、第三戊基醯亞胺基-參(二甲基醯胺基)鈦、TaCl5
、MoCl5
、WCl5
及NbCl5
。在一個實施例中,鈦前體選自TiCl4
、TiI4
、Ti(NCH2
CH3
)x
Cly
(其中x + y = 4)、式Ti(NR2
)4
之化合物(其中R2
係C1
-C4
烷基)(例如四(二甲基醯胺基)鈦)、第三戊基醯亞胺基-參(二甲基醯胺基)鈦。<0}{0>在另一實施例中,鈦前體係TiCl4
。
在一個實施例中,金屬氮化物選自氮化鈦、氮化鉭、氮化鎢及氮化鈮。
在一個實施例中,前體化合物A係六氯二矽烷。
在一個實施例中,脈衝序列之循環重複約3至約15次。
在第三態樣中,本發明提供用於氮化鈦在反應區中在微電子裝置基板之表面上成核之方法,其包含:
I. 在脈衝氣相沉積條件下將選自A、B及C之化合物引入至反應區中,其中該等脈衝氣相沉積條件包含複數個脈衝序列,其中將化合物A、B及C中之至少兩者依序且以任何順序引入至該反應區中,其中之一者為A,每一者視情況隨後係利用惰性氣體之吹掃步驟,以界定脈衝序列之第一循環,其中該複數個包含至少三個循環,其中A、B及C定義為:
A. 下式之化合物,
B. TiCl4
,及
C. 氨;隨後
II. 將脈衝序列之第二循環引入至該反應區中,脈衝序列之該第二循環包含將化合物D及E以任一順序引入至該反應區中:
D. 鈦前體;及
E. 含氮還原氣體;及
將脈衝序列之該第二循環重複足夠反覆次數以在基板上建立氮化鈦成核,以提供代表在具有約10 Å至約15 Å之厚度之膜中小於約1%空隙面積之覆蓋區。
在第四態樣中,本發明提供用於氮化鈦在反應區中在微電子裝置基板之表面上成核之方法,其包含:
I. 在脈衝氣相沉積條件下將六氯二矽烷、氨、TiCl4
及氨依序引入至反應區中以界定第一脈衝序列之一個循環,其中該等脈衝氣相沉積條件包含該等循環中之至少三者,每一者視情況隨後係利用惰性氣體之吹掃步驟;隨後
II. 將第二脈衝序列之循環引入至該反應區,第二脈衝序列之該循環包含將化合物D及E以任一順序引入至該反應區中,每一者視情況隨後係利用惰性氣體之吹掃步驟:
D. 鈦前體;及
E. 含氮還原氣體;及
將該第二脈衝序列循環重複足夠反覆次數以在基板上建立氮化鈦成核,以提供代表在具有約10 Å至約15 Å之厚度之膜中小於約1%空隙面積之覆蓋區。
在第五態樣中,本發明提供用於金屬氮化物在反應區中在微電子裝置基板之表面上成核之方法,其包含:
I. 在脈衝氣相沉積條件下將六氯二矽烷及還原氣體依序引入至反應區中,其中該等脈衝氣相沉積條件包含複數個脈衝序列,每一者視情況隨後係利用惰性氣體之吹掃步驟,以界定脈衝序列之第一循環,其中該複數個包含至少三個循環,
II. 將脈衝序列之第二循環引入至該反應區中,脈衝序列之該第二循環包含將化合物A及B以任一順序引入至該反應區中:
A. 金屬前體,其中該金屬選自鈦、鉭、鉬、鎢及鈮;及
B. 含氮還原氣體;及
將該第二脈衝序列循環重複足夠反覆次數以在基板上建立金屬氮化物成核,以提供具有約10 Å至約15 Å之厚度的膜。
在另一實施例中,所得膜將展現較未利用步驟I所形成之相應膜小至少約25%之AFM粗糙度。
在第六態樣中,本發明提供用於氮化鈦在反應區中在微電子裝置基板之表面上成核之方法,其包含:
I. 在脈衝氣相沉積條件下將六氯二矽烷及含氮還原氣體依序引入至反應區中以界定第一脈衝序列之第一循環,其中該等脈衝氣相沉積條件包含該等循環中之至少三者,每一者視情況隨後係利用惰性氣體之吹掃步驟;隨後
II. 將脈衝序列之第二循環引入至該反應區中,脈衝序列之該第二循環包含將化合物D及E以任一順序引入至該反應區中,每一者視情況隨後係利用惰性氣體之吹掃步驟:
D. 鈦前體;及
E. 含氮還原氣體;及
將脈衝序列之該第二循環重複足夠反覆次數以建立氮化鈦成核,以提供具有約10 Å至約15 Å之厚度的膜。
在另一實施例中,所得膜展現較未利用步驟I所形成之相應膜小至少約25%之AFM粗糙度。
在一個實施例中,在該等第五及第六態樣中,含氮還原氣體係氨。在另一實施例中,含氮還原氣體選自肼;1,1-二甲基肼;及1,2-二甲基肼。
因此,在本發明之第二、第三、第四、第五及第六態樣中,提供基板表面(例如微電子裝置基板)利用金屬氮化物之經改良成核方法。因此,在第七態樣中,本發明提供其上沉積有金屬氮化物膜之微電子裝置基板,該金屬氮化物膜具有約10 Å至約15 Å之厚度及小於約1%空隙面積。在一個實施例中,金屬氮化物包含氮化鈦。
一旦達成成核,即具有約10-15 Å之厚度以及小於約1%空隙面積之膜,即可以逐層模式進行金屬氮化物物種之進一步沉積。
因此,在第八態樣中,本發明提供在基板表面上沉積金屬氮化物之方法,其包含以上態樣中任一者之方法,其進一步包含將(i) 至少一種金屬前體及(ii) 至少一種含氮還原氣體以任一順序引入至反應區中,每一者隨後係利用惰性氣體之可選吹掃步驟,以界定脈衝序列之第三循環,並重複脈衝序列之該第三循環,直至獲得期望厚度之金屬氮化物膜為止。
在某些實施例中,上文所描述化合物A、B或C之脈衝時間(即,前體暴露於基板之持續時間)在約1與60秒之間之範圍內。當利用吹掃步驟時,該吹掃步驟之持續時間係約1至60秒、1至4秒或1至2秒,此取決於所利用之工具且取決於化合物A、B及C之身份以及在其上發生沉積之基板。在其他實施例中,每一化合物之脈衝時間在0.1至60秒或20至40秒之範圍內,再次所利用之工具。在其他實施例中,每一化合物之脈衝時間在約5至約10秒之範圍內。
在一個實施例中,氣相沉積條件包含約250℃至約750℃之溫度及約0.5至約1000托(Torr)或1至30托之壓力。在另一實施例中,氣相沉積條件包含約350℃至約450℃之溫度,此取決於所利用之工具且取決於化合物A、B及C之身份以及在其上發生沉積之基板。
可用於形成高純度薄金屬(例如含鈦膜)之製程包括任何適宜氣相沉積技術(例如,數位或脈衝CVD、ALD及脈衝電漿製程)。可利用該等氣相沉積製程以在微電子裝置之至少一個基板表面上形成含鈦膜,以形成具有約20埃至約2000埃之厚度的膜。
在本發明之方法中,以上化合物可依任何脈衝機制(例如在單晶圓CVD、ALD及/或PECVD或PEALD室中或在含有多個晶圓之爐中)與期望微電子裝置基板反應。
另一選擇,本發明方法可作為ALD或類似ALD製程實施。如本文所用,術語「ALD或類似ALD」係指諸如以下之製程:(i) 將每一反應物A、B及C依序引入至反應器,例如單晶圓ALD反應器、半間歇式ALD反應器或間歇式爐ALD反應器,或(ii) 藉由移動或旋轉基板至反應器之不同區段將每一反應物暴露於基板或微電子裝置表面且每一區段由惰性氣體簾隔開,即空間ALD反應器或卷對卷ALD反應器。
如本文所用,術語「含氮還原氣體」包括選自肼(N2
H4
)、甲基肼、第三丁基肼、1,1-二甲基肼、1,2-二甲基肼及NH3
之氣體。
本文所揭示之沉積方法可涉及一或多種吹掃氣體。用於吹掃掉未消耗反應物及/或反應副產物之吹掃氣體係不與前體反應之惰性氣體。實例性吹掃氣體包括(但不限於)氬、氮、氦、氖及其混合物。在某些實施例中,將吹掃氣體(例如Ar)以約10至約2000 sccm範圍內之流速供應至反應器達約0.1至1000秒,由此吹掃可留在反應器中之未反應材料及任何副產物。類似地,該等惰性氣體可用作上文各種前體A、B及C之載體氣體。濃度及流速可端視所利用之特定工具而變。
將能量施加至前體化合物及還原氣體或其組合以誘導反應並在微電子裝置基板上形成含金屬氮化物之膜。該能量可由(但不限於)熱、脈衝熱、電漿、脈衝電漿、螺旋波電漿、高密度電漿、感應耦合電漿、光子、遠端電漿方法及其組合提供;在電漿能量之情況下,該等機制可用於如上所述的前體C。在某些實施例中,可使用二次RF頻率源以改質基板表面處之電漿特徵。在其中沉積涉及電漿之實施例中,電漿生成製程可包含直接電漿生成製程,其中電漿直接在反應器中生成;或另一選擇遠端電漿生成製程,其中電漿係在反應區及基板之「遠端」生成,被供應至反應器中。氣相沉積方法之其他實例闡述於美國專利第10,526,701號,其以引用的方式併入本文中。
如本文所用,術語「微電子裝置」對應於經製造用於微電子、積體電路或電腦晶片應用之半導體基板(包括3D NAND結構)、平板顯示器及微機電系統(MEMS)。應理解,術語「微電子裝置」並不意欲以任何方式進行限制且包括任何基板,該基板包括負通道金屬氧化物半導體(nMOS)及/或正通道金屬氧化物半導體(pMOS)電晶體並最終將成為微電子裝置或微電子總成。該等微電子裝置含有至少一個基板,其可選自例如矽、SiO2
、Si3
N4
、氧化鋁、氧化鋯、二氧化鉿、OSG、FSG、碳化矽、氫化碳化矽、氮化矽、氫化氮化矽、碳氮化矽、氫化碳氮化矽、氮化硼、抗反射塗層、光阻劑、鍺、含鍺、含硼、Ga/As、撓性基板、多孔無機材料、金屬(例如銅及鋁)及擴散障壁層(例如但不限於TiN、Ti(C)N、TaN、Ta(C)N、Ta、W或WN)。該等膜與各種後續處理步驟(例如化學機械平坦化(CMP)及各向異性蝕刻製程)相容。實例
在此實例中,將TiN沉積於未經處理及經預處理熱SiO2
表面上。
TiN膜係藉由ALD製程使用四氯化鈦(TiCl4
)作為第一前體及氨(NH3
)作為第二前體沉積。每一沉積循環係在350℃之溫度及3托之反應室壓力利用基板實施。每一沉積循環包括0.2秒之TiCl4
蒸氣抽取、20秒之惰性氬吹掃、0.5秒之NH3
脈衝及20秒之惰性氬吹掃。
第一預處理層係藉由ALD製程使用TAS作為第一前體及TiCl4
作為第二前體沉積。每一沉積循環係在350℃之溫度及3托之反應室壓力利用基板實施。每一沉積循環包括1.0秒之TAS蒸氣脈衝、20秒之惰性氬吹掃、0.2秒之TiCl4
蒸氣抽取及20秒之惰性氬吹掃。實施總共10個循環,且隨後係TiN製程。
第二預處理層係藉由ALD製程使用TAS作為第一前體、TiCl4
作為第二前體且NH3
作為第三前體沉積。每一沉積循環係在350℃之溫度及3托之反應室壓力利用基板實施。每一沉積循環包括1.0秒之TAS蒸氣脈衝、20秒之惰性氬吹掃、0.2秒之TiCl4
蒸氣抽取、20秒之惰性氬吹掃、0.5秒之NH3
脈衝及20秒之惰性氬吹掃。實施總共10個循環,且隨後係TiN製程。
第三預處理層係藉由ALD製程使用HCDS作為第一前體、TiCl4
作為第二前體且NH3
作為第三前體沉積。每一沉積循環係在350℃之溫度及3托之反應室壓力利用基板實施。每一沉積循環包括1.0秒之HCDS脈衝、20秒之惰性氬吹掃、0.5秒之NH3脈衝、及20秒之惰性氬吹掃、0.2秒之TiCl4
蒸氣抽取、20秒之惰性氬吹掃、0.5秒之NH3脈衝及20秒之惰性氬吹掃。實施總共10個循環,且隨後係TiN製程。
說明:所有沉積及預處理均在熱SiO2
基板上進行。每一沉積循環係在350℃之溫度及3托之反應室壓力利用基板實施。當TiN膜直接沉積於熱SiO2
上時,10個循環僅給出2.2 Ti原子/nm2
,相比之下,TAS-TiCl4
-NH3
及HCDS-NH3
-TiCl4
-NH3
預處理方法可增加相同循環次數所沉積Ti之量,此證實在TiN ALD之前實施預處理之正面效應。
序列 | 目的 | 循環數 | 所量測Ti密度(原子/nm2 ) |
TiCl4 -NH3 | 沉積 | 10 | 2.2 |
TAS-TiCl4 | 預處理 | 10 | 1.3 |
TAS-TiCl4 -NH3 | 預處理 | 10 | 4.4 |
HCDS-NH3 -TiCl4 -NH3 | 預處理 | 10 | 3.1 |
在此實例中,將TiN沉積於未經處理及經預處理熱SiO2
表面上。
此預處理層係藉由ALD製程使用HCDS作為第一前體及NH3
作為第二前體沉積。每一沉積循環係在350℃之溫度及3托之反應室壓力利用基板實施。每一沉積循環包括30秒之HCDS脈衝、20秒之惰性氬吹掃、2秒之NH3
脈衝及20秒之惰性氬吹掃。實施總共10個循環,且隨後係TiN製程。
試驗 | 預處理 | TiN循環 | XRF 厚度(Å) | 電阻率(µΩ-cm) | 粗糙度(Å) |
A | 無 | 52 | 9.1 | n/a | 3.8 |
B | 10x HCDS-NH3 | 36 | 9.6 | 1.34 × 106 | 2.7 |
本發明之其他態樣:
在另一態樣(I)中,本發明提供用於金屬氮化物在反應區中在微電子裝置基板之表面上成核之方法,其包含以下步驟:
I. 在脈衝氣相沉積條件下將六氯二矽烷及還原氣體依序引入至反應區中,其中該等脈衝氣相沉積條件包含複數個脈衝序列,每一者視情況隨後係利用惰性氣體之吹掃步驟,以界定脈衝序列之第一循環,其中該複數個包含至少三個循環,及
II. 將脈衝序列之第二循環引入至該反應區中,脈衝序列之該第二循環包含將化合物A及B以任一順序引入至該反應區中:
A. 金屬前體,其中該金屬選自鈦、鉭、鉬、鎢及鈮;及
B. 含氮還原氣體;及
將該第二脈衝序列循環重複足夠反覆次數以在基板上建立金屬氮化物成核,以提供具有約10 Å至約15 Å之厚度的膜。
在另一態樣(II)中,本發明提供態樣(I)之方法,其中該含氮還原氣體係N2
H4
。
在另一態樣(III)中,本發明提供用於氮化鈦在反應區中在微電子裝置基板之表面上成核之方法,其包含:
I. 在脈衝氣相沉積條件下將六氯二矽烷及含氮還原氣體依序引入至反應區中以界定第一脈衝序列之第一循環,其中該等脈衝氣相沉積條件包含該等循環中之至少三者,每一者視情況隨後係利用惰性氣體之吹掃步驟;隨後
II. 將脈衝序列之第二循環引入至該反應區中,脈衝序列之該第二循環包含將化合物D及E以任一順序引入至該反應區中,每一者視情況隨後係利用惰性氣體之吹掃步驟:
D. 鈦前體;及
E. 含氮還原氣體;及
將脈衝序列之該第二循環重複足夠反覆次數以建立氮化鈦成核,以提供具有約10 Å至約15 Å之厚度的膜。
在另一態樣(IV)中,本發明提供在基板之表面上沉積金屬氮化物之方法,其包含下文技術方案6之方法,其進一步包含將(i) 至少一種金屬前體及(ii) 至少一種含氮還原氣體以任一順序引入至反應區中,每一者隨後係利用惰性氣體之可選吹掃步驟,以界定脈衝序列之第三循環,並重複脈衝序列之該第三循環,直至獲得期望厚度之金屬氮化物膜為止。
已經因此闡述本揭示內容之幾個說明性實施例,熟習此項技術者將易於理解,在隨附申請專利範圍之範圍內亦可做出及使用其他實施例。本文件所涵蓋之本揭示內容之若干優點已經在前面描述中闡釋。然而,應瞭解,本揭示內容在許多方面中僅係說明性的。當然,本揭示內容之範圍係在表達隨附申請專利範圍之語言中定義。
結合附圖考慮各種說明性實施例之以下描述,可更完全地理解本揭示內容。
圖1係在原子層沉積中厚度對氮化鈦循環次數之圖表。此數據顯示利用TAS/TiCl4
、TAS/TiCl4
/NH3
及HCDS/NH3
/TiCl4
/NH3
之微電子裝置基板的早期成核效應。對於TAS/TiCl4
/NH3
及HCDS/NH3
/TiCl4
/NH3
預處理,TiN (氮化鈦) ALD循環之次數包括預處理中之10個TiN循環;舉例而言,若次數=100,則其意味著10個HCDS/NH3
/TiCl4
/NH3
循環及90個使用例如TiCl4
/NH3
之氮化鈦沉積循環。「TAS」(雙-第三戊基伸乙基矽烯)係自Entegris, Inc., Billerica, MA市售購得之有機矽烯產品。
圖2係電阻率(以µΩ-cm表示)對氮化鈦厚度(以埃表示)之圖表。TiN電阻率繪示為未經處理及經預處理熱SiO2
基板上藉由XRF量測之TiN膜厚度的函數。
圖3係在無預處理之情形中在利用100個TiCl4
/NH3
循環之ALD後熱SiO2
基板表面之掃描電子顯微照片(SEM)。
圖4係經受10個TAS/TiCl4
循環、隨後50個TiCl4
/NH3
循環之ALD之熱SiO2
基板表面的SEM。與無預處理之類似實驗(但兩倍循環)相比,此SEM顯示展現相當少之空隙空間且因此更好成核之極大經改良表面。將圖4之空隙空間與圖3進行比較,圖4中之空隙空間為0.8%,相比之下圖3之空隙空間為2.7%。(使用自國立衛生研究院(National Institutes of Health)獲得之ImageJ軟體計算。)
圖5係在原子層沉積中TiN厚度(藉由XRF量測)對TiN循環次數之圖表。此數據顯示利用10x HCDS/NH3
預處理之微電子裝置基板的早期成核之效應。
圖6係粗糙度(以埃表示)對藉由XRF量測之氮化鈦厚度(以埃表示)之圖表。粗糙度係藉由量測探針與樣品間之力之原子力顯微鏡(AFM)量測。空心菱形點代表未處理SiO2
上之TiN;實心正方形點代表在10x HCDS/NH3
預處理之SiO2
上之TiN。此數據顯示在10x HCDS/NH3
預處理之SiO2
上之TiN膜較未經處理者光滑至少25%,尤其對於厚度小於15 Å之氮化鈦而言。
圖7係在無預處理之情形中在利用70個TiCl4
/NH3
循環之ALD後熱SiO2
基板表面之SEM。
圖8係經受10個HCDS/NH3
循環、隨後50個TiCl4
/NH3
循環之ALD之熱SiO2
基板表面的SEM。與無預處理之類似實驗相比,此SEM顯示展現相當少之空隙空間且因此更好成核之極大經改良表面。將圖8之空隙空間與圖7進行比較,圖8中之空隙空間為0.2%,相比之下圖7之空隙空間為3.7%。(使用自國立衛生研究院獲得之ImageJ軟體計算。)
雖然本揭示內容可進行各種修改及替代形式,但其細節在圖式中藉由實例方式顯示並將詳細闡述。然而,應理解,其目的並非將本揭示內容之態樣限制為所闡述之特定說明性實施例。與此相反,目的係涵蓋屬本發明之精神及範圍內之所有修改、等效內容及替代。
Claims (10)
- 一種用於金屬氮化物在反應區中在微電子裝置基板之表面上成核之預處理方法,其包含: I. 在脈衝氣相沉積條件下將選自A、B及C之化合物引入至反應區中,其中該等脈衝氣相沉積條件包含複數個脈衝序列,其中將化合物A、B及C中之至少兩者依序且以任何順序引入至該反應區中,其中之一者為A,每一者視情況隨後係利用惰性氣體之吹掃步驟,以界定脈衝序列之循環,其中該複數個包含至少三個循環,其中A、B及C定義為: A. 選自含矽鹵化物及含矽醯胺之前體; B. 金屬前體,其中該金屬選自鈦、鉭、鉬、鎢及鈮;及 C. 含氮還原氣體,其中該含氮還原氣體在每一脈衝序列之每循環引入至該反應區中一次或兩次。
- 如請求項1之方法,其中A係雙-第三戊基伸乙基矽烯且B係TiCl4 。
- 如請求項1之方法,其中該脈衝序列係六氯二矽烷;NH3 ;TiCl4 ;及NH3 。
- 如請求項1之方法,其中脈衝序列之該第一循環選自(i) 六氯二矽烷及NH3 ;(ii) 六氯二矽烷及N2 H4 ;(iii) 六氯二矽烷及1,1-二甲基肼;或(iv) 六氯二矽烷及1,2-二甲基肼。
- 一種用於金屬氮化物在反應區中在微電子裝置基板之表面上成核之方法,該方法包含如請求項1之方法,其進一步包含: 將脈衝序列之第二循環引入至該反應區中,脈衝序列之該第二循環包含將化合物D及E以任一順序引入至該反應區中,每一者視情況隨後利用惰性氣體吹掃: D. 金屬前體,其中該金屬選自鈦、鉭、鉬、鎢及鈮;及 E. 含氮還原氣體;及 將脈衝序列之該第二循環重複足夠反覆次數以在基板上建立金屬氮化物成核,以提供代表在具有約10 Å至約15 Å之厚度之膜中小於約1%空隙面積之覆蓋區。
- 如請求項5之方法,其中該金屬前體選自TiCl4 ;TiI4 ;Ti(NCH2 CH3 )Cl;四(二甲基醯胺基)鈦;TaCl5 ;MoCl3 ;WCl5 ;及NbCl5 。
- 如請求項5之方法,其中該金屬氮化物選自氮化鈦、氮化鉭、氮化鉬、氮化鎢及氮化鈮。
- 如請求項5之方法,其中該含氮還原氣體選自氨、肼、甲基肼、第三丁基肼、1,1-二甲基肼及1,2-二甲基肼。
- 一種微電子裝置基板,其具有沉積於其上之金屬氮化物膜,該金屬氮化物膜具有約10Å至約15Å之厚度及小於約1%空隙面積。
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