TWI827911B - 貴金屬濺鍍靶材 - Google Patents
貴金屬濺鍍靶材 Download PDFInfo
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- 238000005477 sputtering target Methods 0.000 title claims abstract description 65
- 239000010970 precious metal Substances 0.000 title claims description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 31
- 239000001257 hydrogen Substances 0.000 claims abstract description 31
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000005266 casting Methods 0.000 claims abstract description 15
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 9
- 239000013077 target material Substances 0.000 claims abstract description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 21
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 21
- 229910052698 phosphorus Inorganic materials 0.000 claims description 21
- 239000011574 phosphorus Substances 0.000 claims description 21
- 229910052717 sulfur Inorganic materials 0.000 claims description 21
- 239000011593 sulfur Substances 0.000 claims description 21
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 11
- 239000010931 gold Substances 0.000 claims description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 238000012545 processing Methods 0.000 abstract description 21
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000005096 rolling process Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 5
- 238000005242 forging Methods 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 5
- 239000000155 melt Substances 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 238000004544 sputter deposition Methods 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000003746 surface roughness Effects 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 238000007664 blowing Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000005058 metal casting Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000717 platinum sputter deposition Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009291 secondary effect Effects 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/02—Alloys based on gold
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/04—Alloys based on a platinum group metal
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
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Abstract
本發明係一種貴金屬濺鍍靶材,其係由鑄造錠構成之濺鍍靶材,其特徵在於氫含量未達5wtppm。本發明係以提供一種於濺鍍靶製造時加工特性被改善之貴金屬濺鍍靶材作為課題。濺鍍靶材意指藉由鑄造或壓延等之塑性加工形成濺鍍靶形狀前之鑄造錠的狀態。
Description
本發明係關於一種最適於半導體領域中之薄膜之形成的貴金屬濺鍍靶材。
濺鍍被使用於形成半導體領域中之細微配線、MEMS、光裝置、LED、有機EL、高頻裝置、水晶等中之薄膜。濺鍍係指如下技術:在真空中導入非活性氣體(主要為氬氣),向靶(板狀之成膜材料)施加負的電壓使其發生輝光放電,將非活性氣體原子離子化,使氣體離子以高速衝撞靶表面進行激烈地打擊而使構成靶之成膜材料之粒子(原子、分子)激烈地彈出,強力地附著、堆積於基材或基板之表面而形成薄膜。
濺鍍具有如下特長:即便是高熔點金屬或合金等難以真空蒸鍍之材料亦可成膜,可對應廣大範圍之成膜材料。一般來說,濺鍍靶係以如下方法製作:使用熔解鑄造法形成鑄錠後,藉由鍛造、壓延加工為濺鍍靶形狀,其後,進行熱處理,進而切削表面。
貴金屬濺鍍靶亦同樣地係對鑄造錠進行鍛造、壓延等而被製造,然而,對鑄造錠進行鍛造或壓延時,存在發生微細之龜裂(micro crack,微裂)之問題。由於微裂成為濺鍍時異常放電之原因,故被要求極力降低上述之情形。再者,下述文獻作為貴金屬濺鍍靶之相關先前技術為人所知。
先前技術文獻
專利文獻
專利文獻1:國際公開第2017/209281號
[發明所欲解決之課題]
本發明係以提供一種於濺鍍靶製造時加工特性被改善之貴金屬濺鍍靶材作為課題。於本案說明書中,濺鍍靶材意指藉由鑄造、壓延等塑性加工形成濺鍍靶形狀前之鑄造錠的狀態。
[解決課題之技術手段]
可解決上述課題之本發明之一種態樣為一種貴金屬濺鍍靶材,其特徵在於氫含量為5wtppm以下。
[發明之效果]
根據本發明,具有可改善濺鍍靶製造時之加工特性之優異效果。
本發明之實施型態為一種由貴金屬鑄造錠構成之濺鍍靶材,其特徵在於氫含量為5wtppm以下。氫雜質使貴金屬之硬度增加,而使加工特性惡化。藉由將氫含量設為5wtppm以下,則可提升加工特性,防止於濺鍍靶之製造時微裂之發生。較佳為設為1wtppm以下。又,藉由減少濺鍍靶材之氫含量,可獲得如下次要效果:抑制濺鍍時真空度之降低,進而可減少濺鍍膜中之氫雜質。
本實施型態之由貴金屬鑄造錠構成之濺鍍靶材較佳為根據貴金屬之種類設定以下之維氏硬度之範圍。
金靶材:維氏硬度25Hv以上45Hv以下
白金靶材:維氏硬度37Hv以上55Hv以下
鈀靶材:維氏硬度45Hv以上140Hv以下
銀靶材:維氏硬度25Hv以上55Hv以下
若維氏硬度較低,則貴金屬過軟,無法保持加工時之水平性,加工特性惡化。另一方面,若維氏硬度較高,則貴金屬濺鍍靶中會發生裂痕(crack)或自連接(bonding)面之剝落。貴金屬濺鍍靶材之硬度亦根據濺鍍靶材中之氫、磷、硫等雜質含量而變化。
於本案說明書中,貴金屬濺鍍靶材意指由金、白金、鈀、銀之任一單一金屬構成之濺鍍靶材,並非意指銀合金等於部分含有貴金屬這般的合金濺鍍靶材。由單一金屬構成之情形時,濺鍍靶之材質與合金之情形不同,最適於加工特性之硬度會變化,故難以直接應用最適於合金之情形之表面狀態。再者,於本案說明書中,單一之金屬並非意指連微量含有作為雜質之其他之金屬成分者都要排除,具體而言,亦可含有金屬雜質合計1000wtppm以下。金屬雜質可使用輝光放電質量分析(GD-MS)進行分析。又,各金屬雜質之含量未達分析下限值之情形時,將分析下限值作為其含量而算出。
進而,本發明之實施型態之貴金屬濺鍍靶材較佳為磷含量為1wtppm以下,硫含量為1wtppm以下。此等雜質會析出至晶界,有加工硬化,加工特性惡化之情形。藉由將磷、硫之任一者之含量設為1wtppm以下,會阻礙此種析出,可使加工特性提升。
以下,使用下述方法進行了本案說明書所記載之貴金屬濺鍍靶材之各物性評價。供測定之試樣為自濺鍍靶材之2處所切割取出之端材。對於切割取出之試樣僅進行丙酮洗淨後,使其乾燥。洗淨後,對2個試樣進行測定,並求其平均值。再者,避免自濺鍍靶材之極端之處(例如:外周端等)之端材的切割取出。
(維氏硬度之測定)
測定維氏硬度所使用之裝置如下所示:
測定裝置:微小硬度試驗機(Mitutoyo Corporation)
型號:HM-221
推壓荷重:200kgf
(氫含量之測定)
測定裝置:堀場製作所製造之氫分析裝置(非分散紅外線吸收法)
(磷含量之測定、硫含量之測定)
測定裝置:輝光放電質量分析(GD-MS)。
其次,對本發明之實施例等進行說明。再者,以下實施例僅作為代表之例示,本發明不必受此等實施例之限制,而應根據申請專利範圍所記載之技術思想之範圍進行解釋。
(Au濺鍍靶)
將純度4N之Au原料以高純度碳坩鍋進行大氣熔解後,將Au之熔液注入鑄模,其後,於水中進行急速冷卻而製作Au鑄造錠(濺鍍靶材)。於進行大氣熔解時,藉由將微量水蒸氣或氫氣吹入適量之熔液中,調整鑄錠中之氫含量。又,關於硫、磷,亦藉由於熔液中微量添加來調整硫含量、磷含量。如此獲得之濺鍍靶材之雜質(氫、磷、硫)含量及維氏硬度如表1所示。
其次,對Au鑄造錠(濺鍍靶材)實施熱鍛後,藉由車床加工(切削),將表面粗度Ra調整成平均0.4~1.6 μm。藉由光學顯微鏡觀察由此獲得之濺鍍靶材之表面,調查有無微裂(尺寸:以圓等效直徑(equivalent circle diameter)計為10 µm以上)。結果,確認氫含量為5wtppm以上之濺鍍靶材發生微裂。
[表1]
氫含量 | 磷含量 | 硫含量 | 維氏硬度 | 加工特性 | |
wtppm | wtppm | wtppm | Hv | ||
Au靶材 (鑄造錠) | 未達1 | 未達1 | 未達1 | 25 | 無微裂 |
2 | 未達1 | 未達1 | 32 | 無微裂 | |
4 | 未達1 | 未達1 | 41 | 無微裂 | |
4 | 1 | 1 | 45 | 無微裂 | |
5 | 3 | 3 | 62 | 發生微裂 | |
15 | 5 | 8 | 75 | 發生微裂 |
(白金濺鍍靶材)
將純度3N5之Pt原料使用高純度氧化鋯坩鍋進行大氣熔解後,將Pt熔液注入鑄模,其後,於水中進行急速冷卻而製作Pt鑄造錠(濺鍍靶材)。於進行大氣熔解時,藉由將微量水蒸氣或氫氣吹入適量之熔液中,調整鑄錠中之氫含量。又,關於硫、磷,亦藉由於熔液中微量添加來調整硫含量、磷含量。如此獲得之濺鍍靶材之雜質(氫、磷、硫)含量及維氏硬度如表2所示。
其次,對Pt鑄造錠(濺鍍靶材)實施熱鍛後,藉由車床加工(切削),將表面粗度Ra調整成平均0.4~1.6 μm。藉由光學顯微鏡觀察由此獲得之濺鍍靶材之表面,調查有無微裂(尺寸:數μm)。結果,確認氫含量為5wtppm以上之濺鍍靶材發生微裂。
[表2]
氫含量 | 磷含量 | 硫含量 | 維氏硬度 | 加工特性 | |
wtppm | wtppm | wtppm | Hv | ||
Pt靶材 (鑄造錠) | 未達1 | 未達1 | 未達1 | 37 | 無微裂 |
未達1 | 未達1 | 未達1 | 40 | 無微裂 | |
1 | 未達1 | 未達1 | 43 | 無微裂 | |
4 | 1 | 1 | 53 | 無微裂 | |
4 | 1 | 1 | 55 | 無微裂 | |
5 | 3 | 3 | 60 | 發生微裂 | |
12 | 5 | 8 | 70 | 發生微裂 |
(鈀濺鍍靶材)
將純度3N5之Pd原料使用高純度氧化鋯坩鍋進行真空熔解後,將Pd熔液注入鑄模,其後,於水中進行急速冷卻而製作Pd鑄造錠(濺鍍靶材)。於進行真空熔解時,藉由使微量水蒸氣或氫氣混入,調整鑄錠中之氫含量。又,關於硫、磷,亦藉由於熔液中微量添加來調整硫含量、磷含量。如此獲得之濺鍍靶材之雜質(氫、磷、硫)含量及維氏硬度如表3所示。
其次,對Pd鑄造錠(濺鍍靶材)實施熱鍛後,藉由車床加工(切削),將表面粗度Ra調整成平均0.4~1.6 μm。藉由光學顯微鏡觀察由此獲得之濺鍍靶材之表面,調查有無微裂(尺寸:數μm)。結果,確認氫含量為5wtppm以上之濺鍍靶材發生微裂。
[表3]
氫含量 | 磷含量 | 硫含量 | 維氏硬度 | 加工特性 | |
wtppm | wtppm | wtppm | Hv | ||
Pd靶材 (鑄造錠) | 未達1 | 未達1 | 未達1 | 45 | 無微裂 |
1 | 未達1 | 未達1 | 50 | 無微裂 | |
4 | 未達1 | 未達1 | 105 | 無微裂 | |
4 | 1 | 1 | 140 | 無微裂 | |
6 | 1 | 1 | 200 | 發生微裂 | |
20 | 5 | 8 | 410 | 發生多量微裂 |
(銀濺鍍靶材)
將純度4N5之Ag原料使用高純度氧化鋯坩鍋進行大氣熔解後,將Ag熔液注入鑄模,其後,於水中進行急速冷卻而製作Ag鑄造錠(濺鍍靶材)。於進行大氣熔解時,藉由將微量水蒸氣或氫氣吹入適量之熔液中,調整鑄錠中之氫含量。又,關於硫、磷,亦藉由於熔液中微量添加來調整硫含量、磷含量。如此獲得之濺鍍靶材之雜質(氫、磷、硫)含量及維氏硬度如表4所示。
其次,對Ag鑄造錠(濺鍍靶材)實施熱鍛後,藉由車床加工(切削),將表面粗度Ra調整成平均0.4~1.6 μm。藉由光學顯微鏡觀察由此獲得之濺鍍靶材之表面,調查有無微裂(尺寸:數μm)。結果,確認氫含量為5wtppm以上之濺鍍靶材發生微裂。
[表4]
[產業上之可利用性]
氫含量 | 磷含量 | 硫含量 | 維氏硬度 | 加工特性 | |
wtppm | wtppm | wtppm | Hv | ||
Ag靶材 (鑄造錠) | 未達1 | 未達1 | 未達1 | 25 | 無微裂 |
2 | 未達1 | 未達1 | 33 | 無微裂 | |
4 | 1 | 1 | 51 | 無微裂 | |
4 | 1 | 1 | 55 | 無微裂 | |
10 | 3 | 3 | 60 | 發生微裂 | |
13 | 5 | 8 | 65 | 發生微裂 |
藉由本發明,具有可改善濺鍍靶製造時之加工特性之優異效果。本發明之實施型態之貴金屬濺鍍靶材可應用於形成高頻裝置、水晶、MEMS、光裝置、LED、有機EL等中之薄膜。
無。
無。
無。
Claims (6)
- 一種貴金屬濺鍍靶材,其為由鑄造錠構成之濺鍍靶材,且氫含量未達5wtppm,磷含量為1wtppm以下,硫含量為1wtppm以下。
- 如請求項1之貴金屬濺鍍靶材,其由金之鑄造錠構成,且維氏硬度為25~45Hv。
- 如請求項1之貴金屬濺鍍靶材,其由白金之鑄造錠構成,且維氏硬度為37~55Hv。
- 如請求項1之貴金屬濺鍍靶材,其由鈀之鑄造錠構成,且維氏硬度為45~140Hv。
- 如請求項1之貴金屬濺鍍靶材,其由銀之鑄造錠構成,且維氏硬度為25~55Hv。
- 如請求項1至5中任一項之貴金屬濺鍍靶材,其氫含量為1wtppm以下。
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