TW563203B - Precursors for zirconium and hafnium oxide thin film deposition - Google Patents

Precursors for zirconium and hafnium oxide thin film deposition Download PDF

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TW563203B
TW563203B TW091122207A TW91122207A TW563203B TW 563203 B TW563203 B TW 563203B TW 091122207 A TW091122207 A TW 091122207A TW 91122207 A TW91122207 A TW 91122207A TW 563203 B TW563203 B TW 563203B
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tmhd
zirconium
precursor
vapor deposition
chemical vapor
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Wei-Wei Zhuang
David Russell Evans
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Sharp Kk
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    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
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    • H01L21/314—Inorganic layers
    • H01L21/3141—Deposition using atomic layer deposition techniques [ALD]

Description

563203 A7 ____B7_ 五、發明説明{) 發明領域 (請先閱讀背面之注意事項再填寫本頁) 本發明係有關給氯化物烷氧化物的合成，其可用於經 由化學蒸氣澱積法（CVD)或原子層化學蒸氣澱積法（ALCVD) 而用於鈴金屬氧化物薄膜澱積。 發明背景 現時，用於CVD或ALCVD的給和鍩先質爲HfCh， Hf(〇R)4,此處 R =院基，例如 CH(CH3)2，Hf(tmhd)4,此處 tmhd = 2 ，2,6,6-四甲基-3,5-庚二酮基，則的&(：)4，此處1£3(：二三氟乙醯 丙酮基，及Hf(NCh)4，及含锆成分的類似先質，對於金屬閘 氧化物應用而言，HfCh業經報導爲純Hf〇2薄膜澱積所用的 潛在來源。Ryan C.Smith et al.,Chemical Vapor Deposition of the Oxides of Titanium,Zirconium and Hafnium for Use as High-k Materials in Microelectronic Devices. A Carbon-free Precursor for the Synthesis of Hafnium Dioxide, Advanced Materials for Optics and Electronics 1 0,1 05-1 14,1 1 1- 1 1 3(2000)° 經濟部智慧財產局員工消費合作社印製 至於其他的先質，Hf(OR)4極具空氣和濕氣敏感性且難 以掌握；Hf(tmhd)4具穩定性，但會誘來難以移除的碳污染； Hf(tfac)4爲揮發性先質，但其使用會包括氟污染之危險。 尙未有Hf(N03)4在ALCVD中的應用之報導。 因爲給和鍩具有幾乎相同的電子組態，所以彼等具有 幾乎相同的化學性質。因此，如諳於此技者所熟知者，彼 等實際上可在化學化合物中互換，且在用於半導體器件中 本紙張尺度適用中國國家標準（CNS ) A4規格（210X：297公釐） -4 - 563203 A7 B7 經濟部智慧財產局員工消費合作社印製 五、發明説明4 ) 時展現出類似的特性。 發明槪述 一種製造以化學蒸氣澱積法形成的薄膜所用先質之方 法，其包括將ZC14與H(tmhd)3溶劑和烴溶劑例如苯混合形 成溶液，此處Z爲選自給和錆之中的元素；將該溶液於氬 氣圍中回流1 2小時；真空移除溶劑，由是製得一固體化合 物；及將該化合物在2 00°C和0.1 mmHg近真空下昇華。 一種用於化學蒸氣Μ積法的Z〇x先質，其包括選自zci(t mhd)3和ZCh((tmhd)2之中的含Z化合物。 本發明的目的爲提出鉛先質，其可用於透過CVD或AL CVD程序進行的給金屬氧化物薄膜澱積。 本發明的另一目的爲減低氯污染同時仍提供足夠揮發 性的先質。 本發明的一目的爲使用烷氧化物配位基來部份取代氯， 產生給二氯化物二烷氧化物或給氯化物三烷氧化物。 本發明此槪述和諸目的係提出以對本發明本質獲得快 速的理解。對本發明更徹底的了解可經由參照下面本發明 較佳具體實例配合所附圖式的詳細說明而得到。 圖式之簡略說明 第1圖繪示出HfCl(tmhd)3的EDS光譜。 第2圖繪示出HfCh(tmhd)2的EDS光譜。 第3圖繪示出HfCl(tmhd)3的TGA光譜。 (請先閱讀背面之注意事項再填寫本頁) 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -5- 563203 A7 B7 五、發明説明< ) 第4圖繪示出HfCl2(tmhd)2的TGA光譜。 (請先閲讀背面之注意事項再填寫本頁) 籃佳具體實例之詳細說明 如諳於此技者所熟知者，給和鉻具有很相似的化學性 質，且用於半導體器件中時有實際上相同的行爲表現。本文 中的實例係使用給，不過對於含鉻化合物和先質也都正確 可通用。 因爲HfCl4含有非常高濃度的氯，所以新的給先質應該 含有較少的氯且具有較高的揮發性。爲完成此項，乃使用 烷氧化物配位基部份地取代氯，導致給二氯化物二烷氧化 物或給氯化物三烷氧化物。化合物，HCl(tmhd)3和 HfCl2(tmhd)2，可產生合意的結果；氯是爲了在原子層化學 蒸氣澱積法（AL(VD)中的吸收要求而包含進去的，且在先質 中含有較少的氯，如此可減低氯污染且提供比HfCl4更高的 揮發性。 本發明給先質爲HfCl(tmhd)3和HfCl2(tmhd)2，其中含 經濟部智慧財產局員工消費合作社印製 有氯以在ALCVD應用中幫助分子吸收到晶圓表面上且其也 含有比HfCl2較少的氯以減低在給金屬氧化物薄膜中的氯污 染。 合成所用原料爲HfCl4，H(tmhd)和烴溶劑例如苯溶劑。 得自 Aldrich Chemical的HfCU係經由昇華予以純化。得 自 Strem Chemicals的H(tmhd)在使用之前予以分飽過。 苯係經由在二苯甲酮和金屬鈉上回流而純化。 要製造HfCl(tmhd)3時，係將HfCl4(50克，0.156莫耳） 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -6 - 563203 A7 B7 五、發明説明4 ) 與H(tmhd)3(86克，0.468莫耳）在1000毫升圓底兩頸燒瓶內 所裝的6 〇 〇毫升苯中混合。於混合後強烈攪拌該溶液。 (請先閲讀背面之注意事項再填寫本頁)
HfCl4逐漸地溶解且溶液顏色逐漸改變成稀黃色。將溶液在 氬氣圍中回流1 2小時。然後真空移除掉溶劑，得到白色固 體化合物。將該化合物在200°C，O.lmmHg近真空下昇華， 產生 76.3 克純 HfCl(tmhd)3,產率 64%。對 HfClC33H5706 的 計算組成爲：1^:23.37%;(：:5 1.90%;(：1:4.64%;11:7.52%;和〇: I2.57%。實際的分析結果指出下面的百分比：Hf:24.42%;C: 5 1.89%;C1:4.7 10/〇;Η:7.62%;和 Ο: 1 1.36% 〇 同樣地於HfCl2(tmhd)2的合成中，將HfCl4(50克， 經濟部智慧財產局員工消費合作社印製 0.156莫耳）與H(tmhd)3(58克，0.312莫耳）在1 000毫升圓底 雙頸燒瓶所裝的600毫升苯中混合。於混合後強烈攪拌該 溶液。HfCl4逐漸溶解，且溶液顏色逐漸變成稀黃色。於氬 氣圍下將溶液回流1 2小時。然後真空移除掉溶劑而得白色 固體化合物。之後在210°C，〇. ImmHg近真空下將化合物昇 華，產生53克純化的HfCl2(tmhd)2,產率爲55%。HfCl2C22H3 8〇4 的計算組成物：Hf:28.98%;C:42.90%;Cl: 1 1.5 1%;H:6.22%; 和0:10.39%。實際分析結果指示下列百分比：Hf:30.24%;C:4 3.13%;C1:11.67%;H:6.24%;和 0:8.72%。 於兩先質中的氯存在進一步用EDS予以確定，如第1和 2圖中所示者。兩化合物的揮發性都透過熱重力分析法（TG A)予以評估，如第3和4圖中所示者。結果指出兩種新的給 先質都具揮發性且可用爲ALCVD應用的來源。 該等先質可用來在半導體器件上形成HfCK薄膜。製備 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） 563203 A7 B7 五、發明説明4 ) 如適當的基板，其可包括在其上形成半導體結構。該半導 體結構可經遮蔽以阻止在不需要薄膜之處澱積Hf〇x薄膜。 該Hf〇x薄膜可用CVD或ALCVD澱積成，其後，將罩移除掉 。之後完成該半導體器件。 因爲給和鉻具有近乎相同的電子組態，所以彼等具有 近乎相同的化學性質。因此，如諳於此技者所熟知者，彼等 實際上可在化學化合物中互換，且於用於半導體器件中時 展現出相似的特性。該等元素可在化學式中以、、Z 〃表之， 此處Z爲選自給和鍩之中的元素。 如此，已揭示出用於給和鉻氧化物薄膜澱積中的先質 之製法。要了解者，在後附申請專利範圍所界定的本發明範 圍內對其可作出進一步的變異和修改。 (請先閲讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -8 -

Claims (1)

  1. 六、申請專利範圍1 1. 一種製造以化學蒸氣澱積法形成的薄膜所用先質之方 法，其包括： (請先閲讀背面之注意事項再填寫本頁) 將ZCh與H(tmhd)3溶劑和烴溶劑混合形成溶液，此處Z 爲選自給和锆之中的元素； 將該溶液於氬氣圍中回流1 2小時； 真空移除溶劑，由是製得一固體化合物；及 將該化合物在200°C和O.lmmHg近真空下昇華。 2. 如申請專利範圍第1項之方法，其中該混合包括將 50克，0.156莫耳的HfCl4和86克，0.468莫耳的H(tmhd)3在 600毫升烴溶劑內混合以製造HfCl2(tmhd)3。 3 ·如申請專利範圍第1項之方法，其中該混合包括將 50克，0.156莫耳的HfCh和58克，0.312莫耳的H(tmhd)在 600毫升烴溶劑內混合以製造HfCl2(tmhd)2。 4·一種在半導體器件上形成Z〇x薄膜的方法，此處z爲 選自給和锆之中的元素；該方法包括： 經濟部智慧財產局員工消費合作社印製 製備一適當的基板，包括於其上構成^半導體結構體； 經由選自化學蒸氣澱積法和原子層化學蒸氣澱積法之 中的方法，使用選自ZCl(tmhd)3和ZCl2(tmhd)2所構成的ZCK 先質組合之中的Ζ〇χ先質在該半導體結構體上澱積一 20,層 ;及 完成該半導體器件。 5.—種用於化學蒸氣澱積法之Ζ〇χ先質，此處ζ爲選自 給和鍩之中的元素，該ζ〇χ先質包括： 選自ZCl(tmhd)3和ZCl2(tmhd)2所構成的化合物組合之 本紙張尺度適用中國國家梂準（CNS ) A4規格（210X297公釐） 563203 A8 B8 C8 D8 、申請專利乾圍 2中的含Ζ化合物。 (請先閲讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 本紙張尺度適用中國國家揉準（CNS ) Α4規格（210Χ297公釐） -10-
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