TWI396675B - 氧化鋅系靶材 - Google Patents
氧化鋅系靶材 Download PDFInfo
- Publication number
- TWI396675B TWI396675B TW098131168A TW98131168A TWI396675B TW I396675 B TWI396675 B TW I396675B TW 098131168 A TW098131168 A TW 098131168A TW 98131168 A TW98131168 A TW 98131168A TW I396675 B TWI396675 B TW I396675B
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- Prior art keywords
- zinc oxide
- gallium
- range
- titanium
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- Prior art date
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- 235000014692 zinc oxide Nutrition 0.000 title 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 title 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 73
- 239000010936 titanium Substances 0.000 claims description 50
- 229910052719 titanium Inorganic materials 0.000 claims description 38
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 36
- 239000011787 zinc oxide Substances 0.000 claims description 36
- 229910052733 gallium Inorganic materials 0.000 claims description 32
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 30
- 230000007613 environmental effect Effects 0.000 description 22
- 238000012360 testing method Methods 0.000 description 21
- 238000000034 method Methods 0.000 description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 229910052760 oxygen Inorganic materials 0.000 description 13
- 239000001301 oxygen Substances 0.000 description 13
- 238000000465 moulding Methods 0.000 description 12
- 239000000843 powder Substances 0.000 description 8
- 238000005477 sputtering target Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 238000004544 sputter deposition Methods 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000007733 ion plating Methods 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000003566 sealing material Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 229910001195 gallium oxide Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C04B35/632—Organic additives
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- 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
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Description
本發明係有關一種以氧化鋅做為主成分之氧化鋅系靶材。
透明導電膜用於紅外線遮蔽板或靜電遮蔽板的用途、面發熱體或觸控開關(touch switch)等之導電膜、顯示裝置等之透明電極的需要性正在升高。以此種透明導電膜而言，以往一般係利用摻雜有錫之氧化銦膜(ITO)，但由於ITO之價格高，故期望有價廉的透明導電膜出現。
於是，屬於較ITO更價廉之膜的氧化鋅系透明導電膜正受到注目，市售品中，有在氧化鋅中添加氧化鋁而成之AZO、和添加有氧化鎵而成之GZO等。
然而，此等氧化鋅系透明導電膜與ITO相比，係為導電性和耐久性較差者，因此為尋求高導電性和安定化而添加各種元素之製品(參照專利文獻1至4等)正在研究中。此外，特別是，添加有做為添加元素之Ga者(參照專利文獻5至7等)正在研究中。
然而，此種氧化鋅系透明導電膜在實際使用時，有蝕刻速率過快而難以圖案化之問題，且有耐環境性差之問題。
〔專利文獻1〕日本特開昭62-154411號公報(申請專利範圍)
〔專利文獻2〕日本特開平9-45140號公報(申請專利範圍)
〔專利文獻3〕日本特開2002-75061號公報(申請專利範圍)
〔專利文獻4〕日本特開2002-75062號公報(申請專利範圍)
〔專利文獻5〕日本特開平10-306367號公報(申請專利範圍)
〔專利文獻6〕日本特開平11-256320號公報(申請專利範圍)
〔專利文獻7〕日本特開平11-322332號公報(申請專利範圍)
本發明係有鑑於上述情形而研創者，其目的(課題)在提供一種耐環境性優良之氧化鋅系靶材。
為解決前述課題，本發明第1態樣為一種氧化鋅系靶材，其具備氧化物燒結體，該氧化物燒結體係以氧化鋅做為主成分，並且含有鈦(Ti)及鎵(Ga)兩元素，且在鈦1.1at%以上或鎵4.5at%以上之範圍含有該兩元素。
在該第1態樣中，藉在預定範圍含有鈦(Ti)及鎵(Ga)兩元素，而製得可形成耐環境性優良之膜的氧化鋅系靶材。
本發明之第2態樣係在第1態樣之氧化鋅系靶材中，鎵含量y(at%)係在鈦含量x(at%)所示之值(-2x+10.4)以下之範圍且在鈦含量x(at%)所示之值(-0.5x
+1.1)以上之範圍。
在該第2態樣中，藉由將鈦及鎵設在所需範圍，而製得可形成膜之電阻率更小且導電性更良好之氧化鋅系透明導電膜的氧化鋅系靶材。
本發明之第3態樣係在第1或第2態樣之氧化鋅系靶材中，鎵含量y(at%)係在鈦含量x(at%)所示之值(-x+3.4)以下、(x-0.9)以下或(-2.3x+10.1)以上之範圍。
在該第3態樣中，藉由將鈦及鎵設在所需範圍，所製得的氧化鋅系靶材可形成載體密度特別小且相當於近紅外光區域之長波長的光之穿透性更為提高，特別是適於太陽電池用途的膜。
本發明之氧化鋅系靶材藉由在預定範圍含有鈦(Ti)及鎵(Ga)兩元素，而可發揮可形成耐環境性優良之膜的效果。
本發明之氧化鋅系靶材係依據下述發現所完成者：若製作成以氧化鋅做為主成分並且同時添加鎵與鈦而成之燒結體，則可形成耐環境性顯著提高之氧化鋅系透明導電膜。
本發明之氧化鋅系靶材係具備含有鈦(Ti)及鎵(Ga)兩元素做為添加元素之氧化物燒結體者，且為在鈦1.1at%以上或鎵4.5at%以上之範圍(亦即，在鈦未達1.1at%且鎵未達4.5at%之範圍以外的範圍)含有兩元素者。其原
因為，若在此等範圍含有兩元素，則可形成耐環境性提高之膜，若在範圍外，則無法得到顯著的可形成耐環境性提高之膜的效果。
在此，所謂氧化鋅系靶材，係指具備氧化鋅系燒結體之靶，且除了藉由濺鍍進行透明導電膜之成膜時所使用之濺鍍靶以外，還包含藉由離子鍍覆進行透明導電膜之成膜時所使用之離子鍍覆用靶(也稱為顆粒)者。
換言之，本發明之範圍係如後述，經進行耐環境測試結果，可製得電阻率之變化減小至7%以下且具有可耐實用之耐環境性之膜的靶。
再者，在本申請案中，各金屬元素之含量(at%)係以Ti及Ga的莫耳數相對於全金屬元素的莫耳數之比例(Ti/(Zn+Ti+Ga)、Ga/(Zn+Ti+Ga))表示。
在此，耐環境測試係測定在放置於60℃、相對濕度90%之環境下250小時後之前後電阻率之變化者。只要電阻率之變化(增加)在7%以內，則在裝置設計上不會產生大的問題，而可判斷為可耐實用。
在此，電阻率之變化率(%)係如下述式所示。再者，當電阻率減少時，由於在裝置設計上不會成為大的問題，故認為是滿足變化為7%以下之條件者。
電阻率之變化率(%)={(耐環境測試後之電阻率/耐環境測試前之電阻率)-1}×100
此外，特別是，氧化鋅系靶材以製成鎵含量y(at%)在鈦含量x(at%)所示之值(-2x+10.4)以下範圍且在
鈦含量x(at%)所示之值(-0.5x+1.1)以上範圍為佳。
此外，特別是，鎵含量y(at%)在鈦含量x(at%)所示之值(-2.5x+9.8)以下且(-0.5x+1.1)以上之範圍時，電阻率成為1.5×10-3
Ω cm以下，而製得可形成更良好之膜的靶。
其原因為，藉由在如此之範圍含有鎵及鈦，特別是電阻率減小為2.5×10-3
Ω cm以下或1.5×10-3
Ω cm以下且而製得可形成導電性更優良之膜的靶。
電阻率以2.5×10-3
Ω cm以下或1.5×10-3
Ω cm以下為佳之原因為，以例如在液晶顯示器之陣列側電極而言，由於電阻率為1×10-3
Ω cm左右即可使用，故在實用上為佳。
並且，特別是，以製成特徵在於鎵含量y(at%)在鈦含量x(at%)所示之值(-x+3.4)以下、(x-0.9)以下或(-2.3x+10.1)以上之範圍的氧化鋅系靶材為佳。
藉由在如此之範圍含有鎵及鈦，可製得可形成載體密度更小且容易使相當於近紅外光區域之長波長的光穿透的膜，因而可形成適於例如太陽電池用途的透明導電膜。
若設在上述之適當的範圍，則載體密度成為4.0×1020
cm-3
以下，而成為適於太陽電池用途之製品。
在此，相當於近紅外光區域之長波長側之穿透率，造成光之吸收/反射之自由電子之電漿振盪(plasma oscillation)係在長波長側者較高。造成電漿振盪之電漿波長係以下述式所示，載體密度越少，則電漿波長越偏向長波長側。
在此，c：光速3.0×1010
〔cm/s〕，e：電子電荷4.8×10-10
esu，ne
：載體密度〔cm-3
〕，ε0
=π/4，ε：介電常數(=折射率之平方，n2
=2.02
=4.0)，m*
：氧化鋅之電子之有效質量(0.28×9.1×10-28
〔g〕)，μ：移動度〔cm2
/V．s〕。
當載體密度為4×1020
cm-3
時，電漿波長為1650nm左右，長波長的光也會充分穿透。
茲說明做為本發明對象之氧化鋅系靶材之製造方法，但以下說明僅為例示性，製造方法並無特別限定。
首先，構成本發明之靶的起始原料一般為氧化鋅(ZnO)、氧化鎵(Ga2
O3
)、氧化鈦(TiO2
)之粉末，亦可以此等單體、化合物、複合氧化物等做為原料。當使用單體、化合物時，係經過預先製作成氧化物之步驟。
將此等原料粉末以所需之調配率混合並進行成形之方法無特別限定，可使用至今習知之各種濕式法或乾式法。
以乾式法而言，可舉例如冷壓(Cold Press)法或熱壓(Hot Press)法等。冷壓法係將混合粉末填充於成形模具中製作成形體後進行煅燒。熱壓法係在成形模具內將混合粉煅燒、燒結。
以濕式法而言，以使用例如過濾式成形法(參照日本特開平11-286002號公報)為佳。此過濾式成形法係使用過濾式成形模具，並調製由混合粉末、離子交換水及有機添加劑組成之漿液後，將此漿液注入該過濾式成形模具中，僅從過濾器面側將漿液中之水分減壓排出而製作成形體，並將所得之陶瓷成形體乾燥脫脂後進行煅燒。前述過濾式成形模具係由用以從陶瓷原料漿液中將水分減壓排出而得到成形體之非水溶性材料所構成者，其中，該模具係由具有1個以上之排水孔之成形用下模、載置於此成形用下模上且具有通水性之過濾器、及隔著密封用之密封材從上面側挾持過濾器之成形用模框所構成，將前述成形用下模、成形用模框、密封材及過濾器以可各自分解之方式組裝，並僅從該過濾器面側將漿液中之水分減壓排出。
以冷壓法或濕式法所成形者之煅燒溫度以1000至1500℃為佳、以1000至1300℃更佳，其氛圍環境為大氣環境、氧氣環境、非氧化性環境、和真空環境等。另一方面，當為熱壓法時，以在900至1300℃燒結為佳，其環境為非氧化性環境或真空環境等。再者，在各方法中進行煅燒後，進行用以成形/加工為預定尺寸之機械加工而製作成靶。
以下，依據以濺鍍靶為例子之實施例說明本發明，但並不限定於此。
以Ti及Ga的莫耳數相對於全金屬元素的莫耳數之比例(Ti/(Zn+Ti+Ga)、Ga/(Zn+Ti+Ga))相當於在下述表1及表2中表示為樣品A1至A50之莫耳比之比例，準備全量為約1.0kg之BET=3.59m2
/g之ZnO粉、BET=7.10m2
/g之TiO2
粉、及BET=13.45m2
/g之Ga2
O3
粉，並使用球磨機將此等粉料混合。之後，相對於混合粉末添加6.6wt%的4wt%聚乙烯醇水溶液做為黏合劑並混合後，進行冷壓而得到成形體。
將此成形體在大氣中以60℃/h之升溫速度升溫後，在600℃進行脫脂10小時。接著，在大氣中以100℃/h從室溫升溫至1300℃後，在1300℃煅燒8小時，之後以100℃/h冷卻至室溫，而得到燒結體。對所得之燒結體實施平面研磨，而得到φ 100mm×6mmt之靶。
再者，以ICP分析所得之燒結體後，確認其與原料調配組成幾乎相同。
以Al的莫耳數相對於全金屬元素的莫耳數之比例(Al/(Zn+Al))相當於2.4at%之比例，準備全量為約1.0kg之BET=3.59m2
/g之ZnO粉、BET=3.89m2
/g之Al2
O3
粉，並使用球磨機將此等粉料混合。之後，對於混合粉末添加6.6wt%的4wt%聚乙烯醇水溶液做為黏合劑並混合後，進行冷壓而得到成形體。
將此成形體在大氣中以60℃/h升溫後，在600℃進行脫脂10小時。接著，在大氣中以100℃/h從室溫升溫
至1300℃後，在1300℃煅燒8小時，之後以100℃/h冷卻至室溫，而得到燒結體。對所得之燒結體實施平面研磨，而得到φ 100mm×6mmt之靶。
在4英吋陰極之DC磁控濺鍍裝置中分別安裝各製造例之濺鍍靶及AZO濺鍍靶，在基板溫度250℃，一面使氧氣分壓每隔0.5sccm在0至2.0sccm變化(相當於0至6.6×10-3
Pa)，而得到透明導電膜。
如此進行而得之透明導電膜係為其組成與經濺鍍之透明導電膜用濺鍍靶之組成相同之氧化鋅系透明導電膜。如此之氧化鋅系透明導電膜之組成分析，可將單膜全部溶解後以ICP分析。此外，當膜本身呈元件構成等情形中，也可依需要利用FIB等將相當部分之剖面進行切取後，使用附屬於SEM或TEM等之元素分析裝置(EDS或WDS，歐傑(Auger)分析等)鑑定。
濺鍍條件係設定如下述，而得到厚度為1200 Å之膜。
靶尺寸：φ=100mm，t=6mm
濺鍍方式：DC磁控濺鍍
排氣裝置：旋轉泵+低溫泵(cryopump)
到達真空度：3×10-5
Pa以下
Ar壓力：4.0×10-1
Pa
氧氣壓力：0至6.6×10-3
Pa
基板溫度：250℃
濺鍍功率：130W(功率密度1.6W/cm2
)
使用基板：Corning#1737(液晶顯示器用玻璃)50mm×50mm×0.8mmt
將使氧氣分壓變化而成膜之透明導電膜分別切取10mm×10mm之大小後，分別藉由Van der Pauw法(Toyo Corporation製，霍耳(Hall)係數測定裝置ResiTest8300)測定電阻率。
第1圖(b)中顯示作為比較例之摻雜有鋁(Al)2.4at%之ZnO(AZO)膜之電阻率之氧氣分壓相關性。如此，當氧氣分壓為0時，電阻率最低。此外，摻雜有2at%之Ti及1at%之Ga之ZnO膜(樣品A24)之電阻率之氧氣分壓相關性係如第1圖(a)所示。樣品A24之氧氣分壓相關性係顯示與AZO膜相同的特性。此其他樣品組成中之TiGa系ZnO膜也皆顯示相同的特性。因此，表1及表2所示之特性值皆為氧氣分壓為0時之數據資料。
將在氧氣分壓為0時成膜之各透明導電膜分別切取10mm×10mm之大小後，首先藉由Van der Pauw法(Toyo Corporation製，霍耳係數測定裝置ResiTest8300)測定電阻率，之後封入恆溫恆濕器內(ESPEC製PR-2KP)，並放置於60℃ 90%RH環境中250小時後，再次測定電阻率，並算出放置前後之電阻率變化。再者，使恆溫恆濕器內升溫降溫時，係藉由控制溫度與濕度而使樣品不會結露水。
結果如表1及表2所示。
結果，鈦未達1.1at%且鎵未達4.5at%之範圍之樣品
A1至A10以及鎵為0%之樣品A16、A22，電阻率之變化率超過7%，除此之外之範圍之樣品，電阻率之變化率為7%以下。換言之，從表1之資料得知，鈦為1.2at%以上時，電阻率之變化率會成為7%以下，但由表1、2所示以外之資料之傾向可清楚得知，電阻率之變化率成為7%以下者係鈦為1.1at%以上、鎵為4.5at%以上。
在第2圖之耐環境性測試結果中，電阻率之變化率在7%以內之樣品以○表示，超過7%之樣品以●表示。
將在氧氣分壓為0時成膜之各透明導電膜分別切取10mm×10mm之大小後，藉由Van der Pauw法(Toyo Corporation製，霍耳係數測定裝置ResiTest8300)測定電阻率。
結果如表1及表2所示。
由結果可得知，鎵含量y(at%)在鈦含量x(at%)所示之值(-2x+10.4)以下之範圍且在鈦含量x(at%)所示之值(-0.5x+1.1)以上之範圍之透明導電膜，其電阻率為2.5×10-3
Ω cm以下。另一方面，得知超出此範圍之樣品之電阻率會大於2.5×10-3
Ω cm。再者，連同表1、2所示範圍以外之資料一起綜合判斷結果可清楚得知，電阻率成為2.5×10-3
Ω cm以下之鈦含量x(at%)所示之值(-2x+10.4)以下範圍之邊界，係鎵含量y(at%)在鈦含量x(at%)所示之值(-0.5x+1.1)以上之範圍。
在第3圖中，耐環境性測試結果在7%以內者，電阻
率為2.5×10-3
Ω cm以下之樣品以□表示、電阻率超過2.5×10-3
Ω cm之樣品以■表示，耐環境性測試結果超過7%之樣品以●表示。
此外，亦可得知特別是鎵含量y(at%)在鈦含量x(at%)所示之值(-2.5x+9.8)以下且(-0.5x+1.1)以上之範圍之樣品，其電阻率係為1.5×10-3
Ω cm以下。再者，連同表1、2所示以外範圍之資料一起綜合判斷結果可清楚得知，電阻率成為1.5×10-3
Ω cm以下之鈦含量x(at%)所示之值(-2x+10.4)以下範圍之邊界，係鎵含量y(at%)在鈦含量x(at%)所示之值(-2.5x+9.8)以下且(-0.5x+1.1)以上之範圍。
在第4圖中，第3圖中電阻率成為1.5×10-3
Ω cm以下之樣品係以◇表示。
將在氧氣分壓為0時成膜之各透明導電膜切取後，從藉由Van der Pauw法之霍耳係數測定(Toyo Corporation製，霍耳係數測定裝置ResiTest8300)，分別測定各膜之載體密度及載體移動度。
結果如表1及表2所示。
由其結果得知，鎵含量y(at%)在鈦含量x(at%)所示之值(-x+3.4)以下、(x-0.9)以下或(-2.3x+10.1)以上範圍之樣品，其載體密度為4.0×1020
cm-3
以下。另一方面，亦得知除此以外之範圍之樣品之載體密度會大於4.0×1020
cm-3
。再者，連同表1、2所示以外資料一起綜
合判斷結果得知，載體密度成為4.0×1020
cm-3
以下之範圍，係鎵含量y(at%)在鈦含量x(at%)所示之值(-x+3.4)以下、(x-0.9)以下或(-2.3x+10.1)以上之範圍。
在第5圖中，耐環境性測試結果在7%以內之樣品中，載體密度為4.0×1020
cm-3
以下之樣品以△表示、載體密度超過4.0×1020
cm-3
之樣品以▲表示，耐環境性測試結果超過7%之樣品以●表示。
第1圖(a)及(b)係表示實施例及比較例中所製成之膜之電阻率之氧氣分壓相關性之曲線圖。
第2圖係表示耐環境性測試之測定結果之曲線圖。
第3圖係表示耐環境性測試及電阻率之測定結果之曲線圖。
第4圖係表示耐環境性測試及電阻率之測定結果之曲線圖。
第5圖係表示耐環境性測試及載體密度之測定結果之
曲線圖。
由於本案的圖為實驗結果數據，並非本案的代表圖。故本案無指定代表圖。
Claims (2)
- 一種氧化鋅系靶材，係具備氧化物燒結體，該氧化物燒結體係以氧化鋅做為主成分，並且含有鈦(Ti)及鎵(Ga)兩元素，且在鈦1.1at%以上或鎵4.5at%以上之範圍含有該兩元素，而且鎵含量y(at%)係在鈦含量x(at%)所示之值(-2.5x+9.8)以下之範圍，且在鈦含量x(at%)所示之值(-0.5x+1.1)以上之範圍。
- 如申請專利範圍第1項之氧化鋅系靶材，其中，鎵含量y(at%)係在鈦含量x(at%)所示之值(-x+3.4)以下、或(x-0.9)以下之範圍。
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| JP5003600B2 (ja) * | 2008-06-13 | 2012-08-15 | 住友金属鉱山株式会社 | 酸化物焼結体、ターゲット、およびそれを用いて得られる透明導電膜、導電性積層体 |
| JP5585046B2 (ja) * | 2009-10-27 | 2014-09-10 | 東ソー株式会社 | 複合酸化物焼結体、ターゲット及び酸化物透明導電膜 |
| WO2011102425A1 (ja) * | 2010-02-18 | 2011-08-25 | 住友化学株式会社 | 酸化物焼結体、酸化物混合体、それらの製造方法およびそれらを用いたターゲット |
| JP2011222687A (ja) * | 2010-04-08 | 2011-11-04 | Tosoh Corp | 太陽電池 |
| US9111663B2 (en) * | 2010-09-29 | 2015-08-18 | Tosoh Corporation | Sintered composite oxide, manufacturing method therefor, sputtering target, transparent conductive oxide film, and manufacturing method therefor |
| US9885108B2 (en) * | 2012-08-07 | 2018-02-06 | Semiconductor Energy Laboratory Co., Ltd. | Method for forming sputtering target |
| KR101526157B1 (ko) * | 2014-12-08 | 2015-06-04 | 주식회사3차버너 | 업소용 대형 국솥 |
| JP6776931B2 (ja) * | 2016-03-23 | 2020-10-28 | 三菱マテリアル株式会社 | 積層反射電極膜、積層反射電極パターン、積層反射電極パターンの製造方法 |
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| US5236632A (en) * | 1989-08-10 | 1993-08-17 | Tosoh Corporation | Zinc oxide sintered body, and preparation process and use thereof |
| JPH08264022A (ja) | 1995-03-27 | 1996-10-11 | Gunze Ltd | 透明導電膜 |
| JPH0945140A (ja) | 1995-07-28 | 1997-02-14 | Sumitomo Metal Mining Co Ltd | 酸化亜鉛系透明導電性膜 |
| JPH10306367A (ja) | 1997-05-06 | 1998-11-17 | Sumitomo Metal Mining Co Ltd | スパッタリングターゲット用ＺｎＯ−Ｇａ２Ｏ３系焼結体およびその製造方法 |
| JP3571540B2 (ja) | 1998-02-04 | 2004-09-29 | 三井金属鉱業株式会社 | 濾過式成形型およびその型を用いたセラミックス焼結体の製造方法 |
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| JPH11256320A (ja) | 1998-03-13 | 1999-09-21 | Sumitomo Metal Mining Co Ltd | ＺｎＯ系焼結体 |
| JPH11322332A (ja) * | 1998-05-21 | 1999-11-24 | Sumitomo Metal Mining Co Ltd | ＺｎＯ系焼結体およびその製造方法 |
| JP2002075061A (ja) | 2000-08-30 | 2002-03-15 | Uchitsugu Minami | 透明導電膜 |
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| KR101004981B1 (ko) * | 2005-06-28 | 2011-01-04 | 제이엑스 닛코 닛세키 킨조쿠 가부시키가이샤 | 산화갈륨-산화아연계 스퍼터링 타겟, 투명 도전막의 형성방법 및 투명 도전막 |
| JP4926977B2 (ja) * | 2005-12-08 | 2012-05-09 | Ｊｘ日鉱日石金属株式会社 | 酸化ガリウム−酸化亜鉛系焼結体スパッタリングターゲット |
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| JP2000195101A (ja) * | 1998-12-28 | 2000-07-14 | Japan Energy Corp | 光ディスク保護膜及び同保護膜形成用スパッタリングタ―ゲット |
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| TW201022178A (en) | 2010-06-16 |
| KR100958665B1 (ko) | 2010-05-20 |
| US20100065424A1 (en) | 2010-03-18 |
| JP2010070796A (ja) | 2010-04-02 |
| CN101914754A (zh) | 2010-12-15 |
| JP4295811B1 (ja) | 2009-07-15 |
| CN101914754B (zh) | 2012-10-31 |
| KR20100032335A (ko) | 2010-03-25 |
| US7790644B2 (en) | 2010-09-07 |
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