CN109134546B - 钨前驱体及使用其形成含钨层的方法 - Google Patents
钨前驱体及使用其形成含钨层的方法 Download PDFInfo
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- CN109134546B CN109134546B CN201810556182.9A CN201810556182A CN109134546B CN 109134546 B CN109134546 B CN 109134546B CN 201810556182 A CN201810556182 A CN 201810556182A CN 109134546 B CN109134546 B CN 109134546B
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- tungsten
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- tungsten precursor
- vapor deposition
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 150
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 150
- 239000010937 tungsten Substances 0.000 title claims abstract description 149
- 239000002243 precursor Substances 0.000 title claims abstract description 122
- 238000000034 method Methods 0.000 title claims abstract description 37
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 22
- 238000005229 chemical vapour deposition Methods 0.000 claims description 46
- -1 tert-amyl Chemical group 0.000 claims description 31
- 238000000231 atomic layer deposition Methods 0.000 claims description 18
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 14
- 239000000758 substrate Substances 0.000 claims description 13
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 12
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 10
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 9
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 6
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 claims description 4
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 claims description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 4
- 125000001973 tert-pentyl group Chemical group [H]C([H])([H])C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 4
- 238000002230 thermal chemical vapour deposition Methods 0.000 claims description 4
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 4
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- 230000008021 deposition Effects 0.000 abstract description 25
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- 239000000463 material Substances 0.000 description 38
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- 238000002474 experimental method Methods 0.000 description 3
- YDGSUPBDGKOGQT-UHFFFAOYSA-N lithium;dimethylazanide Chemical compound [Li+].C[N-]C YDGSUPBDGKOGQT-UHFFFAOYSA-N 0.000 description 3
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 3
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- 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
- 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
- C23C16/22—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 deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F11/00—Compounds containing elements of Groups 6 or 16 of the Periodic Table
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F11/00—Compounds containing elements of Groups 6 or 16 of the Periodic Table
- C07F11/005—Compounds containing elements of Groups 6 or 16 of the Periodic Table compounds without a metal-carbon linkage
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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Abstract
本发明公开一种钨前驱体及一种形成含钨层的方法。所述钨前驱体具有由以下式1表示的结构。
在式1中，R1、R2及R3独立地包括包含经取代或未经取代的C1到C5的直链或分支的烷基；R4及R5独立地包括包含C1到C5的直链或分支的烷基、卤素元素、具有C2到C10的二烷基氨基或者包含C3到C12的三烷基硅烷基；n为1或2，且m为0或1。此外，n+m＝2(例如，当n为1时，m为1)。当n为2时，m为0且R1及R2各有两个。两个R1彼此独立，且两个R2彼此独立。本公开的钨前驱体适用于沉积且限制及/或防止半导体器件的劣化。
Description
[相关申请的交叉参考]
本申请主张在2017年6月15日提出申请的韩国专利申请第10-2017-0076029号的优先权，所述韩国专利申请的全部内容并入本申请供参考。
技术领域
本发明概念涉及一种钨前驱体及一种使用其形成含钨层的方法。
背景技术
半导体器件由于其尺寸小、多功能及/或制作成本低而被视为电子行业中的重要因素。半导体器件可随着电子行业的发展而高度集成。半导体器件的图案线宽因其高集成度(integration)而正在不断减小。因此，电线(electric line)的电阻正在不断增加。使用具有低电阻的钨作为电线材料来减小电线的电阻。还使用钨来形成栅极电极、掩模等。
发明内容
本发明概念的一些示例性实施例提供一种适用于沉积且限制及/或防止半导体器件劣化的钨前驱体。
本发明概念的一些示例性实施例提供一种形成会限制及/或防止半导体器件劣化的含钨层的方法。
根据本发明概念的一些示例性实施例，钨前驱体可由以下式1来表达。
[式1]
在式1中，R1、R2及R3可独立地包括包含经取代或未经取代的C1到C5的直链或分支的烷基，R4及R5可独立地为包含C1到C5的直链或分支的烷基、卤素元素、包含C2到C10的二烷基氨基或者包含C3到C12的三烷基硅烷基，n可为1或2，且m可为0或1。此外，n+m可满足关系：n+m＝2。当n为2时，m可为0且R1及R2中的每一者可提供有两个。两个R1可彼此独立。两个R2可彼此独立。
根据本发明概念的一些示例性实施例，一种形成含钨层的方法可包括在衬底上提供钨前驱体，且所述钨前驱体可由以上式1来表达。
附图说明
图1示出根据本发明概念一些示例性实施例的由式(1-3)表达的钨前驱体的质子核磁共振(1H-NMR)分析数据。
图2示出根据本发明概念一些示例性实施例的由式(1-3)表达的钨前驱体的大气压力热重量及示差热分析(thermogravimetry and differential thermal analysis，TG-DTA)特性的曲线图。
图3示出根据本发明概念一些示例性实施例的由式(1-3)表达的钨前驱体的减压热重量及示差热分析(TG-DTA)特性的曲线图。
图4示出根据本发明概念一些示例性实施例的由式(1-38)表达的钨前驱体的质子核磁共振(1H-NMR)分析数据。
图5示出根据本发明概念一些示例性实施例的由式(1-64)表达的钨前驱体的质子核磁共振(1H-NMR)分析数据。
具体实施方式
以下，将结合附图详细阐述本发明概念的一些示例性实施例以有助于清晰地理解本发明概念。在本说明书中，附加到符号C的后缀数(suffix number)可表示碳原子的数目。举例来说，符号C1可意指一个碳原子，且符号C12可意指十二个碳原子。当在具有后缀的两个C之间放置连字符时，则此种表达可提供范围。举例来说，表达C1到C5可标示以下基团中的一者：甲基、乙基、丙基(及/或异丙基)、丁基(例如，正丁基、异丁基)或戊基(例如，正戊基、异戊基等)。在本说明通篇中，叔戊基(tertiary amyl group)也可被称为叔戊基(tertiary pentyl group)。
根据本发明概念的一些示例性实施例，一种钨前驱体可由以下式1来表达。
[式1]
在式1中，R1、R2及R3可独立地包括具有经取代或未经取代的C1到C5的直链(例如，线状)或分支的烷基；R4及R5可独立地包括具有经取代或未经取代的C1到C5的直链或分支的烷基、卤素元素、具有C2到C10的二烷基氨基(dialkylamino group)或者具有C3到C12的三烷基硅烷基(trialkylsilyl group)；n为1或2；且m为0或1。当n为1时，m可为1。当n为2时，m可为0且R1及R2中的每一者可提供有两个。两个R1可彼此独立，且两个R2可彼此独立。当n为2时，两个R1可设置在钨原子的左侧及右侧，且同样地，两个R2也可设置在钨原子的左侧及右侧。当n为2时，式1可对应于以下具体式(1-70)到具体式(1-75)中的一者。
具有C1到C5的直链或分支的烷基可包含氢原子，所述氢原子中的至少一者可被具有C3到C12的三烷基硅烷基取代。具有C1到C5的直链或分支的烷基可包括选自由甲基、乙基、丙基、异丙基、丁基、异丁基、仲丁基、叔丁基、戊基及异戊基组成的群组的一者。卤素元素可包括氟、氯、溴及碘中的一者。具有C2到C10的二烷基氨基可包括选自由以下组成的群组的一者：二甲基氨基(dimethylamino group)、乙基甲基氨基(ethylmethylaminogroup)、甲基丙基氨基(methylpropylamino group)、甲基异丙基氨基(methylisopropylamino group)、二乙基氨基(diethylamino group)、乙基丙基氨基(ethylpropylamino group)、乙基异丙基氨基(ethylisopropylamino group)、二异丙基氨基(diisopropylamino group)、二仲丁基氨基(disecondarybutylamino group)及二叔丁基氨基(ditertiarybutylamino group)。具有C3到C12的三烷基硅烷基可包括三甲基硅烷基(trimethylsilyl group)或三乙基硅烷基(triethylsilyl group)。
当n为1时，R1、R2及R3中的每一者可独立地包括具有C3到C5的直链或分支的烷基，且R4及R5可独立地包括具有C1到C5的直链烷基。当n为1时，R1及R2中的每一者可独立地包括异丙基、叔戊基、叔丁基或叔戊基；R3可包括异丙基、正丙基、叔丁基或叔戊基；且R4及R5可独立地包括卤素、甲基或乙基。当n为1时，R3可包括异丙基，且R4及R5可包括甲基。
当n为2时，R1、R2及R3中的每个可独立地包括具有C3到C5的直链或分支的烷基。作为另外一种选择，当n为2时，R1、R2及R3中的每个可独立地包括具有C3到C4的支链烷基。不同地，当n为2时，R1、R2及R3中的每个可独立地包括异丙基、仲丁基或叔丁基，且在这种情况下，钨前驱体可具有低的熔点(melting point)。
举例来说，钨前驱体可具有由以下具体式(1-1)到具体式(1-75)表达的化学结构中的一者：
在以上具体式(1-1)到具体式(1-75)中，Me可表示甲基，Et可表示乙基，nPr可表示正丙基(n-丙基)，iPr可表示异丙基，nBu可表示正丁基(n-丁基)，sBu可表示仲丁基，tBu可表示叔丁基，tAm可表示叔戊基，TMS可表示三甲基硅烷基，且TES可表示三乙基硅烷基。
可利用以下反应1来形成(或合成)钨前驱体且无任何特别限制。
[反应1]
以下是关于根据本发明概念一些示例性实施例的具体化合物的形成例的说明。
<由式(1-3)表达的钨前驱体的形成例>
在形成由式(1-3)表达的钨前驱体的以上反应序列中，TMS可表示三甲基硅烷基，Et可表示乙基，iPr可表示异丙基，且DAD可表示二氮杂二烯(diazadiene)。Me可表示甲基，且THF可表示四氢呋喃。
由六氯化钨(WCl6)合成了氧基四氯化钨(WOCl4)。基于在《有机金属(Organometallics)》(1991年，第10卷，第1546页)中出版的让皮埃尔勒尼(Jean Pierre LeNy)所报道的次序来执行由WOCl4合成W(NiPr)Cl4(OEt2)及对W(NiPr)Cl4(OEt2)的分析。举例来说，在氩气气氛下，向1升的四颈烧瓶中添加了WOCl4(40.0g，117mol)及氧杂环丁烷(oxetane)(570ml)以生成溶液1。在室温下滴加了50ml的溶液1之后，另外滴加了异氰酸异丙酯(15.9g，0.187mol)并接着在回流的同时加热了约16小时。然后，在略微减低的压力下移除了溶剂以获得微红棕色固体物质。添加了二乙醚(400ml)并在室温下搅拌了一小时。又在略微减低的压力下移除了溶剂以获得33.5g(产率为63％)橘色固体物质或四氯(二乙醚)(异丙基酰亚胺)钨[W(NiPr)Cl4(OEt2)]。
接着，在氩气气氛下，向100ml的两颈烧瓶中添加了叔戊基二氮杂二烯(4.52g，0.023mol)及四氢呋喃(约50ml)，且另外添加了锂(0.30g，0.0438mol)，并且接着在室温下将其混合物搅拌了一夜，以合成二氮杂二烯络合物(diazadiene complex)。然后，向200ml的四颈烧瓶中添加了所合成的四氯(二乙醚)(异丙基酰亚胺)钨[W(NiPr)Cl4(OEt2)](10.0g，0.0219mol)及二乙醚(约80ml)，且接着将其混合物冷却到-55℃。向此混合物中滴加了二氮杂二烯络合物，且然后将此混合物加热到室温并在室温下搅拌了一夜。然后，在略微减低的压力下对溶剂进行了蒸馏以获得黑色固体物质。将黑色固体物质在减压(15Pa)下加热到170℃的浴温度(bath temperature)，以合成(叔戊基二氮杂二烯)(二氯)(异丙基酰亚胺)钨(以下被称为中间物A)。在氩气气氛下，向200ml的四颈烧瓶中添加了中间物A(20.21g，0.0398mol)及四氢呋喃(tetrahydrofuran，THF)(约90ml)并接着冷却到-55℃。使用滴液漏斗滴加了金属锂100ml(1.17M，68ml，0.0796mol)，且然后将其混合物加热到室温并在室温下搅拌了一夜。在略微减低的压力下对溶剂进行了蒸馏，以获得微黑棕色固体物质。利用己烷对微黑棕色固体物质进行了萃取及过滤，并接着又在略微减低的压力下进行了蒸馏从而获得微红棕色固体物质。在略微减低的压力(15Pa)下在150℃的浴温度下对微红棕色固体物质进行了蒸馏，以获得15.84g(产率为85％)的微红色固体物质或由式(1-3)表达的钨前驱体。图1示出根据本发明概念一些示例性实施例的由式(1-3)表达的钨前驱体的质子核磁共振(1H-NMR)分析数据。图2示出根据本发明概念一些示例性实施例的由式(1-3)表达的钨前驱体的大气压力热重量及示差热分析(TG-DTA)特性的曲线图。图3示出根据本发明概念一些示例性实施例的由式(1-3)表达的钨前驱体的减压热重量及示差热分析(TG-DTA)特性的曲线图。物理性质分析的结果如下。
(1)1H-NMR(苯-d6)(化学位移(chemical shift)：多重性：H的数目)
(0.67:t:6)(0.78:s:6)(1.25:d:6)(1.26:s:6)(1.40:s:6)(1.55-1.58:m:4)(4.11:sep:1)(6.11:s:2)
(2)元素分析(金属分析：电感耦合等离子体原子发射光谱法(InductivelyCoupled Plasma-Atomic Emission Spectrometry，ICP-AES))
W：39.2重量％、C：43.7重量％、H：8.1重量％、N：9.0重量％
(理论值；W：39.34重量％、C：43.69重量％、H：7.98重量％、N：8.99重量％)
(3)大气压力热重量及示差热分析
质量减小50％的温度：231℃(Ar流速：100ml/min，温度上升速率：10℃/min)
(4)减压热重量及示差热分析
质量减小50％的温度：142℃(10托，Ar流速：50ml/min，温度上升速率：10℃/min)
<由式(1-38)表达的钨前驱体的形成例>
在氩气气氛下，向200ml的四颈烧瓶中添加了叔丁基二氮杂二烯(7.75g，0.0461mol)及四氢呋喃(约80ml)，且另外添加了锂(0.61g，0.0876mol)，并接着在室温下搅拌了一夜，从而合成二氮杂二烯络合物。接着，向300ml的四颈烧瓶中添加了二乙醚(约130ml)及如在由式(1-3)表达的钨前驱体的形成例中所论述而合成的四氯(二乙醚)(异丙基酰亚胺)钨(20.01g，0.0438mol)，并接着将其混合物冷却到-55℃。向此混合物中滴加了二氮杂二烯络合物，且将此混合物加热到室温并在室温下搅拌了一夜。然后，在略微减低的压力下对溶剂进行了蒸馏，以获得棕色固体物质。将棕色固体物质在减压(20Pa)下加热到浴温度190℃，以合成中间物B。在氩气气氛下，向200ml的四颈烧瓶中添加了中间物B(6.00g，0.0125mol)及四氢呋喃(约40ml)并接着冷却到-55℃。使用滴液漏斗滴加了(三甲基硅烷基)甲基锂100ml(1.0M，25ml，0.0250mol)，且将其混合物加热到室温并在室温下搅拌了一夜。在略微减低的压力下，对溶剂进行了蒸馏以获得微黑棕色固体物质。利用己烷对微黑棕色固体物质进行了萃取及过滤，并接着又在略微减低的压力下进行了蒸馏从而获得微红棕色固体物质。在略微减低的压力(20Pa)下在140℃的浴温度下对微红棕色固体物质进行了蒸馏，以获得3.45g(产率为47％)的微红色固体物质或由式(1-38)表达的钨前驱体。图4示出根据本发明概念一些示例性实施例的由化学式(1-38)表达的钨前驱体的质子核磁共振分析数据。物理性质分析的结果如下。
(1)1H NMR(苯-d6)(化学位移：多重性：H的数目)
(0.33：s：18)(0.51-0.54：m：4)(1.20：d：6)(1.26：s：18)(4.32:sep:1)(6.22：s：2)
(2)元素分析(金属分析：电感耦合等离子体原子发射光谱法)
W：31.6重量％、C：43.1重量％、H：8.3重量％、N：7.3重量％、Si：9.7重量％
(理论值；W：31.5重量％、C：43.22重量％、H：8.46重量％、N：7.20重量％、Si：9.62重量％)
(3)大气压力热重量及示差热分析
质量减小50％的温度：251℃(Ar流速：100ml/min，温度上升速率：10℃/min)
(4)减压热重量及示差热分析
质量减小50％的温度：168℃(10托，Ar流速：50ml/min，温度上升速率：10℃/min)
<由式(1-64)表达的钨前驱体的形成例>
在氩气气氛下，向200ml的四颈烧瓶中添加了二乙醚(约70ml)并冷却到-30℃，且接着将二甲胺气体(约5g，约0.11mol)引入到烧瓶中。在使用滴液漏斗滴加正丁基锂100ml(1.63M，18ml，0.0292mol)之后，将其混合物加热到室温并在室温下搅拌了三小时，从而生成二甲基氨锂(lithium dimethylamide)溶液。接着，向300ml的四颈烧瓶中添加了四氢呋喃(约50ml)及如在由式(1-38)表达的钨前驱体的形成例中所论述而合成的中间物B(7.03g，0.0146mol)并接着冷却到-55℃。使用滴管滴加了二甲基氨锂溶液并接着加热到室温。将混合物在室温下搅拌了一夜，以在略微减低的压力下对溶剂进行蒸馏，从而获得微黑棕色固体物质。利用己烷对微黑棕色固体物质进行了萃取及过滤，并接着又在略微减低的压力下进行了蒸馏，以获得粘性微红棕色固体物质。在减压(40Pa)下在140℃的浴温度下对微红棕色固体物质进行了蒸馏，以获得2.47g(产率为34％)的粘性微红色液体物质或由式(1-64)表达的钨前驱体。图5示出根据本发明概念一些示例性实施例的由化学式(1-64)表达的钨前驱体的质子核磁共振分析数据。物理性质分析的结果如下。
(1)1H NMR(苯-d6)(化学位移：多重性：H的数目)
(1.29：d：6)(1.33：s：18)(3.33：s：12)(4.84：sep：1)(6.73:s：2)
(2)元素分析(金属分析：电感耦合等离子体原子发射光谱法)
W：37.1重量％、C：40.8重量％、H：7.8重量％、N：14.3重量％
(理论值；W：36.96重量％、C：41.05重量％、H：7.90重量％、N：14.08重量％)
(3)大气压力热重量及示差热分析
质量减小50％的温度：219℃(Ar流速：100ml/min，温度上升速率：10℃/min)
(4)减压热重量及示差热分析
质量减小50％的温度：144℃(10托，Ar流速：50ml/min，温度上升速率：10℃/min)
<由式(1-72)表达的钨前驱体的形成例>
在氩气气氛下，向100ml的两颈烧瓶中添加了异丙基二氮杂二烯(1.53g，0.0109mol)及四氢呋喃(约30ml)，且另外添加了锂(0.14g，0.0208mol)，并接着在室温下搅拌了一夜，从而合成二氮杂二烯络合物。接着，在氩气气氛下，向200ml的四颈烧瓶中添加了四氢呋喃(约30ml)及如在由式(1-38)表达的钨前驱体的形成例中所论述而合成的中间物B(5.03g，0.0105mol)并接着冷却到-55℃。向此混合物中滴加了二氮杂二烯络合物，且将此混合物加热到室温并在室温下搅拌了一夜。在略微减低的压力下，对溶剂进行了蒸馏，以获得墨绿色(blackish green)固体物质。利用己烷对墨绿色固体物质进行了萃取及过滤，并接着又在略微减低的压力下进行了蒸馏从而获得墨绿色固体物质。在略微减低的压力(15Pa)下在150℃的浴温度下对墨绿色固体物质进行了蒸馏，以获得墨绿色固体物质或由式(1-72)表达的钨前驱体。由化学式(1-72)表达的钨前驱体的物理性质分析结果如下。
(1)1H NMR(苯-d6)(化学位移：多重性：H的数目)
(1.27：d：12)(1.29：s：18)(1.33：br s：6)(4.59：sep：1)(4.65:sep:1)(4.65：sep：2)(6.51：s：2)(6.58：s：2)
(2)元素分析(金属分析：电感耦合等离子体原子发射光谱法)
W：33.7重量％、C：46.3重量％、H：7.6重量％、N：12.4重量％
(理论值；W：33.46重量％、C：45.91重量％、H：7.89重量％、N：12.75重量％)
(3)大气压力热重量及示差热分析
质量减小50％的温度：242℃(Ar流速：100ml/min，温度上升速率：10℃/min)
(4)减压热重量及示差热分析
质量减小50％的温度：158℃(10托，Ar流速：50ml/min，温度上升速率：10℃/min)
<钨前驱体的评价实验1：熔点>
进行测量以确定如上所述形成的具有由式(1-3)、式(1-38)及式(1-64)表示的化学结构的钨前驱体以及对照钨前驱体或六氯化钨(WCl6)的熔点。此实验是在30℃下在大气压力下进行，且下表1显示出在30℃下维持固态的钨前驱体的测量结果或熔点。
<表1>
根据表1中的结果，具有由式(1-3)、式(1-38)及式(1-64)表达的化学结构的钨前驱体可在30℃下在大气压力下为液态，或者当略微加热例如到71℃时可进入液态，且可能被认为具有相比于对照钨前驱体即六氯化钨(WCl6)的熔点低得多的熔点。高熔点化合物可能需要高的供给能量来进行例如化学气相沉积(chemical vapor depositon，CVD)或原子层沉积(atomic layer deposition，ALD)等沉积工艺，因而不适用于沉积工艺。当输送槽在室温及大气压力下递送固体化合物时，固体化合物可能会与输送槽的壁碰撞，且因此可能使其表面受损从而使得当使固体化合物蒸发时引起蒸气压力差异。这种趋势可能导致难以维持稳定的工艺条件。本发明概念的钨前驱体可具有相对低的熔点从而在沉积工艺中需要低的能量，且在其液态下可进行安全地递送以维持稳定的工艺条件。如上所述，本发明概念的钨前驱体可适用于例如化学气相沉积或原子层沉积等沉积工艺。
<钨前驱体的评价实验2：蒸发率>
使用热重量及示差热分析测量设备在压力为760托、介于室温到600℃范围内的温度、氩气流速为100ml/min且温度上升速率为10℃/min的条件下对具有由式(1-2)、式(1-3)、式(1-17)及式(1-72)表达的化学结构的钨前驱体进行加热。下表2显示出通过对所得残余物的数量进行测量而计算的蒸发率。
<表2>
根据表2的结果，具有由式(1-2)、式(1-3)、式(1-17)及式(1-72)表达的化学结构的钨前驱体可具有大于97.5％的高蒸发率。根据本发明概念的一些示例性实施例，认为钨前驱体可非常好地蒸发，且所生成的残余物可非常少。当蒸发率减小时，在加热时生成的残余物可能非常多。
以下将阐述一种根据本发明概念一些示例性实施例的使用钨前驱体形成含钨层的方法。
在例如热化学气相沉积、等离子体增强型(Plasma Enhanced，PE)化学气相沉积、光化学气相沉积、光等离子体化学气相沉积、原子层沉积或等离子体增强型原子层沉积等沉积工艺中，可供应由式1表达的钨前驱体来形成含钨层。在热化学气相沉积中，利用热量来使化学气相沉积材料反应并将化学气相沉积材料沉积在衬底上。在等离子体增强型化学气相沉积中，可使用热量及等离子体来使化学气相沉积材料反应。在光化学气相沉积中，可使用热量及光来使化学气相沉积材料反应。在光等离子体化学气相沉积中，可使用热量、光及等离子体来使化学气相沉积材料反应。
举例来说，当利用化学气相沉积来形成含钨层时，可通过包括气体输送方法及液体输送方法的以下方法来供应化学气相沉积材料。在气体输送方法中，可通过对用于存储化学气相沉积材料的容器进行加热或减压来使化学气相沉积材料蒸发，且可将蒸发的化学气相沉积材料引入到化学气相沉积腔室中。当蒸发的化学气相沉积材料可与载气(例如氮气及/或氦气)一起引入时。在液体输送方法中，可将处于液态或溶液状态的化学气相沉积材料输送到蒸发腔室，以在蒸发腔室中将所输送的化学气相沉积材料加热并减压到蒸发状态，且接着化学气相沉积腔室可将蒸发的化学气相沉积材料接纳在其中。可利用气体输送方法及液体输送方法来供应由式1表达的钨前驱体本身。当利用液体输送方法时，可将钨前驱体溶解在溶剂中(或与溶剂混合)以生成溶液，且接着可供应钨前驱体溶液。化学气相沉积材料还可包括其他前驱体或亲核试剂(nucleophile)。
当含钨层仅包含金属原子中的钨时，可仅使用钨前驱体作为根据本发明概念一些示例性实施例的化学气相沉积材料。当含钨层还包含氮、氧、硅及/或其他金属时，根据本发明概念一些示例性实施例的化学气相沉积材料还可包含适合于所述化学气相沉积材料的反应性化合物、其他前驱体及有助于前驱体稳定性的亲核试剂中的一者或多者。在上述多组分化学气相沉积工艺中，可通过以下方法来供应化学气相沉积材料：使化学气相沉积材料的每一组分独立地蒸发的单一来源方法(single-source method)以及以所期望的组成将化学气相沉积材料预先混合并接着进行蒸发的混合来源方法(cocktail-sourcemethod)。即使利用混合来源方法，仍可将化学气相沉积材料溶解在有机溶剂中以生成溶液，且可供应化学气相沉积材料溶液。
有机溶剂并非仅限于任何特定物质，而是可包括例如以下中的一者或多者：乙酸酯，例如乙酸乙酯、乙酸丁酯及乙酸乙氧基乙酯；醚，例如四氢呋喃、四氢吡喃、乙二醇二甲醚、二乙二醇二甲醚、三乙二醇二甲醚、二丁醚及二噁烷；酮，例如甲基丁基酮、甲基异丁基酮、乙基丁基酮、二丙基酮、二异丁基酮、甲基戊基酮、环己酮及甲基环己酮；烃，例如己烷、环己烷、甲基环己烷、二甲基环己烷、乙基环己烷、庚烷、辛烷、甲苯及二甲苯；含氰基的烃，例如1-氰基丙烷、1-氰基丁烷、1-氰基己烷、氰基环己烷、氰基苯、1,3-二氰基丙烷、1,4-二氰基丁烷、1,6-二氰基己烷、1,4-二氰基环己烷及1,4-二氰基苯；吡啶；以及二甲基吡啶。在包含化学气相沉积材料及有机溶剂的溶液中，化学气相沉积材料的量可介于0.01mol/l到2.0mol/l或0.05mol/l到1.0mol/l的范围内。当化学气相沉积材料仅包含本发明概念的钨前驱体时，量的范围可指仅钨前驱体的量。当化学气相沉积材料包含其他前驱体以及本发明概念的钨前驱体时，量的范围可对应于其他前驱体以及本发明概念的钨前驱体的总计量。
其他前驱体可包括硅化合物及/或金属化合物，所述硅化合物及/或金属化合物分别具有包括以下中的一者或多者的配体：水合物、氢氧化物、卤化物、叠氮化物、烷基、烯基、环烷基、芳基、炔基、氨基、二烷基氨基烷基、单(烷基)氨基、二烷基氨基、二胺、二(硅烷基烷基)氨基、二(烷基硅烷基)氨基、二硅烷基氨基、烷氧基、烷氧基烷基、酰肼、磷化物、腈、二烷基氨基烷氧基、烷氧基烷基二烷基氨基、硅氧基(siloxy)、二酮酸根(diketonate)、环戊二烯基、硅烷基、吡唑根(pyrazolate)、胍根(guanidinate)、膦胍根(phosphorguanidinate)、脒根(amidinate)、酮亚胺根(ketoiminate)、二酮亚胺根(diketiminate)、羰基及膦脒根(phosphoramidinate)。金属可包括以下中的一者：镁、钙、锶、钡、镭、钪、钇、钛、锆、铪、铌、钽、铬、钼、钨、锰、铁、锇、钴、铑、铱、镍、钯、铂、铜、银、金、锌、镉、铝、镓、铟、锗、锡、铅、锑、铋、镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥及镱。
其他前驱体并非仅限于任何特定制造方法。举例来说，当使用醇化合物作为有机配体时，可通过使醇化合物的碱金属醇盐与金属的无机酸或金属的水合物之间发生反应来生成前驱体。在这种情况下，金属的无机酸或金属的水合物可包括金属的卤化物或硝酸盐，且碱金属醇盐可包括钠醇盐、锂醇盐及钾醇盐中的一者或多者。
当利用单一来源方法来供应本发明概念的化学气相沉积材料时，可能适宜的是，其他前驱体包括特性与本发明概念的钨前驱体的热特性或氧化/分解特性相似的化合物。当利用混合来源方法来供应本发明概念的化学气相沉积材料时，可能适宜的是，其他前驱体包括在混合时不会因化学反应而改变以及特性与本发明概念的钨前驱体的热特性或氧化/分解特性相似的化合物。
可添加亲核试剂来对本发明概念的钨前驱体或其他前驱体赋予稳定性。亲核试剂可包括选自由以下组成的群组的至少一者：乙二醇醚，例如甘醇二甲醚、二甘醇二甲醚、三甘醇二甲醚及四甘醇二甲醚；冠醚，例如18-冠-6、二环己基-18-冠-6、24-冠-8、二环己基-24-冠-8及二苯并-24-冠-8；多胺，例如乙二胺、N,N'-四甲基乙二胺、二亚乙基三胺、三亚乙基四胺、四亚乙基五胺、五亚乙基六胺、1,1,4,7,7-五甲基二亚乙基三胺、1,1,4,17,10,10-六甲基三亚乙基四胺及三乙氧基三乙胺；环状多胺，例如环拉胺(cyclam)及大环多胺(cyclen)；杂环化合物，例如吡啶、吡咯烷、哌啶、吗啉、N-甲基吡咯烷、N-甲基哌啶、N-甲基吗啉、四氢呋喃、四氢吡喃、1,4-二噁烷、噁唑、噻唑及噁噻戊环(oxathiolane)；β-酮酯，例如乙酰乙酸甲酯、乙酰乙酸乙酯及乙酰乙酸-2-甲氧基乙基；β-二酮，例如乙酰丙酮、2,4-己二酮、2,4-庚二酮、3,5-庚二酮及二叔戊酰甲烷(dipivaloylmethane)。当前驱体的总量为1mol时，所使用的亲核试剂的量可介于0.1mol到10mol或1mol到4mol的范围内。
可能期望本发明概念的沉积材料不包含例如金属残余物、卤素残余物及有机残余物等残余物。否则，可能期望含有相对于前驱体而言介于优选地少于100ppb以及更优选地少于10ppb范围内的金属残余物。可能期望含有相对于沉积材料的总量而言介于优选地少于1ppm以及更优选地为100ppb的范围内的金属残余物。当特别地使用本发明概念的含钨层作为栅极介电层、层间介电层、栅极层及/或势垒层时，可能需要使沉积材料不含对半导体器件的电特性产生影响的碱金属及碱土金属或者否则含有极少量的碱金属及碱土金属。可能期望含有介于优选地少于100ppm、更优选地少于10ppm以及甚至更优选地少于1ppm的范围内的卤素残余物。可能期望含有相对于沉积材料的总量而言介于少于500ppm以及优选地少于50ppm的范围内的有机残余物。还可建议沉积材料不包含水分。水分可在执行化学气相沉积工艺时的时间期间导致出现颗粒。为了避免上述问题，可从每一前驱体、有机溶剂及亲核试剂中预先移除水分。如果含有水分，则可能期望前驱体、有机溶剂及亲核试剂中的每一者含有介于优选地少于10ppm以及更优选地少于1ppm的范围内的水分。
可能要求本发明概念的沉积材料不含有颗粒。否则，当使用光散射自动颗粒计数器(light-scattering automatic particle counter)来检测处于液相的沉积材料中所含有的颗粒时，可能优选的是，大于0.3μm的颗粒的数目为每1ml液相少于100，且大于0.2μm的颗粒的数目为每1ml液相少于1,000。可能更优选的是，大于0.2μm的颗粒的数目为每1ml液相少于100。
在使用钨前驱体的沉积工艺中，可引入反应气体与钨前驱体反应。反应气体可包括氧化气体，例如氧气、臭氧、二氧化氮、一氧化氮、水蒸气、过氧化氢、乙酸及乙酸酐。反应气体可包括具有还原能力的氢气。另外或作为另外一种选择，反应气体可包括氮化气体(nitriding gas)，例如单(烷基)胺、二烷基胺、三烷基胺、亚烷基二胺、有机胺化合物、肼及氨气。
含钨层可沉积在包含以下的衬底上：玻璃、金属(例如钌)、硅及/或陶瓷(例如氮化硅、氮化钛、氮化钽、氧化钛、氧化钽、氧化钌、氧化锆、氧化铪及氧化镧)。衬底可具有板形状、球形状、纤维形状及/或鳞形状。衬底可具有平的表面或可在衬底上具有三维结构(例如沟槽)。
用于形成含钨层的沉积工艺可具有例如反应温度(或衬底温度)、反应压力、沉积速率等基本工艺参数。反应温度可落在足以使钨前驱体反应的高于100℃或从150℃到500℃的范围内。本发明概念的钨前驱体可在高于300℃的温度下具有热稳定性。因此，可适当地选择从250℃到450℃的温度范围作为反应温度。在热化学气相沉积或光化学气相沉积的情况下，反应压力可落在10Pa到大气压力的范围内。在等离子体化学气相沉积的情况下，反应压力可落在10Pa到2,000Pa的范围内。可基于材料供应条件(例如，蒸发温度、蒸发压力)、反应温度及反应压力来控制沉积速率。高的沉积速率可能使含钨层的膜品质劣化，而低的沉积速率可能会降低生产率。沉积速率可被控制在0.01nm/min到100nm/min或1nm/min到50nm/min的范围内。
用于形成含钨层的沉积工艺可另外具有例如沉积材料的蒸发温度及/或蒸发压力等工艺参数。在使用本发明概念的钨前驱体的沉积工艺中，可给出从0℃到150℃的温度范围作为沉积材料的蒸发温度。蒸发压力可落在从1Pa到10,000Pa的范围内。
当利用原子层沉积来形成本发明概念的含钨层时，原子层沉积可包括：对沉积腔室提供钨前驱体的蒸气以使晶片能够将钨前驱体吸附在晶片上，且接着对未吸附的钨前驱体的蒸气进行吹扫。当含钨层还包含除钨以外的元素时，含钨层的原子层沉积工艺还可包括：供应含有此元素的其他前驱体的蒸气或含有此元素的反应气体，以使吸附在晶片上的钨前驱体能够与所供应的蒸气或反应气体发生反应，且对其他前驱体的未反应的蒸气或未反应的反应气体进行吹扫。上述工艺可使钨前驱体分解以将经分解的钨与此元素结合，从而在晶片上形成单原子层式含钨层。在原子层沉积工艺中，可通过控制分别包括上述步骤的循环的次数来确定含钨层的厚度。
举例来说，当含钨层是通过原子层沉积而形成的氧化钨层时，可使本发明概念的钨前驱体蒸发且可制备氧化气体。蒸发温度或蒸发压力可与上述相同。晶片(衬底)的温度可落在室温到500℃、更窄地150℃到500℃以及甚至更窄地150℃到350℃的范围内。执行原子层沉积工艺的沉积腔室可具有介于1Pa到10,000Pa且更窄地介于10Pa到1,000Pa的范围内的内部压力。
当执行吹扫步骤时，吹扫步骤可使用惰性气体(例如氮气、氦气及氩气)，及/或可对沉积腔室进行减压。沉积腔室可减压到0.01Pa到300Pa以及更窄地0.01Pa到100Pa的范围。
本发明概念的钨前驱体可与氧化气体、氮化气体、还原气体、硅前驱体或其他金属前驱体具有良好的反应性。
在原子层沉积工艺中，可施加源自等离子体、光及/或电压的能量，且可视需要使用催化剂。举例来说，可在以下步骤处施加能量：在供应本发明概念的钨前驱体的步骤处；在沉积工艺中升高温度、进行吹扫及供应氧化气体的步骤处；或者上述步骤之间。
在利用化学气相沉积或原子层沉积形成本发明概念的含钨层之后，可对含钨层进一步执行退火工艺以增强半导体器件的电特性。退火工艺可在惰性气体、氧化气体或还原气体气氛下执行。可对含钨层进一步执行回焊工艺，使得可利用含钨层来填充阶梯式区(stepwise region)。在这种情况下，工艺温度可落在200℃到1,000℃以及更窄地250℃到500℃的范围内。
本发明概念的含钨层可在化学气相沉积及/或原子层沉积设施中形成。加热器可对存储有本发明概念的钨前驱体的存储容器进行加热，且因此可生成蒸气并将蒸气供应到沉积腔室中。作为另外一种选择，蒸发器可对存储在存储容器中的处于液相的钨前驱体进行蒸发，且因此可将经蒸发的钨前驱体供应到沉积腔室中。不同的是，在化学气相沉积及/或原子层沉积设施中可包括射频(radio frequency，RF)匹配系统及射频产生器，使得可对反应气体进行等离子体处理。本发明概念的含钨层可在单晶片型制造设施中形成，且也可在批次型制造设施(例如熔炉)中形成。举例来说，批次型制造设施可同时对多个晶片执行沉积工艺。
本发明概念的含钨层可包括钨层、氮化钨层、氧化钨层、钨硅层、碳化钨层等。本发明概念的含钨层可用作金属氧化物半导体场效应晶体管(metal-oxide-semiconductorfield effect transistor，MOSFET)的栅极电极、栅极介电层、掩模层、源极/漏极接触件及/或存储器器件的字线。
<实验例：制造原子层沉积氧化钨层>
在沉积设备中加载了形成有氮化钛层的衬底。将衬底控制到250℃的温度。在氮化钛层上提供作为本发明概念的含钨层的实例的氧化钨层。利用原子层沉积方法形成了氧化钨层。从本发明概念的钨前驱体中选择由式(1-3)表示的钨前驱体，且使用所选择的钨前驱体来形成氧化钨层。供应臭氧(O3)作为反应气体。在100℃的温度下对钨前驱体进行了蒸发。如下执行单一循环：(1)将通过使钨前驱体蒸发而生成的蒸气供应到沉积腔室中达10秒以在衬底上沉积钨前驱体的沉积步骤；(2)使用氩气气体达30秒以从沉积腔室吹除钨前驱体的未反应的蒸气的吹扫步骤；(3)供应臭氧达30秒以在133Pa的压力下与钨前驱体反应的反应步骤；(4)使用氩气气体达30秒以从沉积腔室吹扫未反应的臭氧的吹扫步骤。如此便形成了氧化钨(WO3)层。氧化钨层的厚度在每一个循环增加约0.03nm。将此循环重复约500次以形成总厚度为约15nm的氧化钨层。氧化钨层含有介于少于0.1重量％范围内的碳残余物。
根据本发明概念的一些示例性实施例，钨前驱体可表现出高蒸气压力，且可在室温下或当略微加热时变为液相。在使钨前驱体蒸发之后，可生成少量的副产物及/或残余物。本发明概念的钨前驱体可适用于沉积工艺(例如化学气相沉积或原子层沉积)，可易于输送，且其被供应到衬底中的量可容易受到控制。因此，可形成高品质的含钨层，且可提高生产率。此外，钨前驱体可包含数目相对少的卤素原子以限制及/或防止半导体器件因在所述工艺之后剩余的卤素原子而劣化。
Claims (10)
1.一种钨前驱体，其特征在于，具有由式1表示的结构，
[式1]
其中，在式1中，
R1、R2及R3独立地为未经取代的C1到C5的直链或分支的烷基，
R4及R5独立地为未经取代的直链或分支的C1到C5烷基、经三甲基硅烷基取代的C1到C5的直链或分支的烷基或二甲基氨基，
R4及R5相同，
n为1，且
m为1。
2.根据权利要求1所述的钨前驱体，其特征在于，
R1、R2及R3中的至少一者为甲基、乙基、丙基、丁基或戊基中的一者，且
R4及R5为甲基、乙基、丙基、丁基或戊基中的一者。
3.根据权利要求1所述的钨前驱体，其特征在于，R1、R2及R3独立地为异丙基、仲丁基或叔丁基。
4.根据权利要求1所述的钨前驱体，其特征在于，所述钨前驱体的结构是由以下式(1-1)到式(1-6)、式(1-16)到式(1-24)、式(1-34)到式(1-39)、式(1-43)到式(1-45)、式(1-61)、式(1-64)及式(1-67)中的一者表示：
其中，Me表示甲基，Et表示乙基，nPr表示正丙基，iPr表示异丙基，tBu表示叔丁基，且tAm表示叔戊基，且TMS表示三甲基硅烷基。
5.根据权利要求1所述的钨前驱体，其特征在于，
R1、R2及R3独立地为未经取代的C3到C5的直链或分支的烷基。
6.根据权利要求5所述的钨前驱体，其特征在于，
R1及R2独立地为叔丁基或叔戊基，且
R3为异丙基、叔丁基或叔戊基。
7.根据权利要求5所述的钨前驱体，其特征在于，R4及R5为甲基或乙基。
8.一种形成含钨层的方法，其特征在于，所述方法包括：
在衬底上提供钨前驱体，所述钨前驱体具有由以下式1表示的结构，
[式1]
其中，在式1中，
R1、R2及R3独立地为未经取代的C1到C5的直链或分支的烷基，
R4及R5独立地为未经取代的直链或分支的C1到C5烷基、经三甲基硅烷基取代的C1到C5的直链或分支的烷基或二甲基氨基，
R4及R5相同，
n为1，且
m为1。
9.根据权利要求8所述的方法，其特征在于，所述提供所述钨前驱体包括：利用热化学气相沉积、等离子体化学气相沉积、光化学气相沉积或原子层沉积来提供所述钨前驱体。
10.根据权利要求8所述的方法，其特征在于，
利用化学气相沉积工艺来提供所述钨前驱体，且
所述化学气相沉积工艺包括：将所述钨前驱体的蒸气跟随载气一起提供。
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| KR20180137064A (ko) | 2018-12-27 |
| US10900119B2 (en) | 2021-01-26 |
| JP2019004138A (ja) | 2019-01-10 |
| JP7064945B2 (ja) | 2022-05-11 |
| CN109134546A (zh) | 2019-01-04 |
| US20180363131A1 (en) | 2018-12-20 |
| KR102474876B1 (ko) | 2022-12-07 |
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