TWI429771B - 氧化鋅蒸鍍材料及由其所形成之氧化鋅膜 - Google Patents
氧化鋅蒸鍍材料及由其所形成之氧化鋅膜 Download PDFInfo
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- TWI429771B TWI429771B TW096114298A TW96114298A TWI429771B TW I429771 B TWI429771 B TW I429771B TW 096114298 A TW096114298 A TW 096114298A TW 96114298 A TW96114298 A TW 96114298A TW I429771 B TWI429771 B TW I429771B
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- Prior art keywords
- zinc oxide
- film
- pellets
- osmium
- mass
- Prior art date
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- 239000000463 material Substances 0.000 title claims description 60
- 238000007740 vapor deposition Methods 0.000 title claims description 20
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 275
- 239000011787 zinc oxide Substances 0.000 claims description 131
- 239000008188 pellet Substances 0.000 claims description 34
- 238000001704 evaporation Methods 0.000 claims description 27
- 230000008020 evaporation Effects 0.000 claims description 27
- 229910052746 lanthanum Inorganic materials 0.000 claims description 21
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 21
- 229910052762 osmium Inorganic materials 0.000 claims description 21
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 claims description 21
- 229910052684 Cerium Inorganic materials 0.000 claims description 18
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 18
- 229910052741 iridium Inorganic materials 0.000 claims description 15
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 13
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 12
- 229910052707 ruthenium Inorganic materials 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 239000002002 slurry Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 6
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 239000000853 adhesive Substances 0.000 claims description 5
- 230000001070 adhesive effect Effects 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 5
- 238000005566 electron beam evaporation Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000013077 target material Substances 0.000 claims description 3
- 244000166124 Eucalyptus globulus Species 0.000 claims 1
- 239000010408 film Substances 0.000 description 78
- 230000015572 biosynthetic process Effects 0.000 description 16
- 238000002156 mixing Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- 229910003437 indium oxide Inorganic materials 0.000 description 6
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 6
- DLINORNFHVEIFE-UHFFFAOYSA-N hydrogen peroxide;zinc Chemical compound [Zn].OO DLINORNFHVEIFE-UHFFFAOYSA-N 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 229910000420 cerium oxide Inorganic materials 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 3
- 238000005477 sputtering target Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000009694 cold isostatic pressing Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003826 uniaxial pressing Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 1
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229910000929 Ru alloy Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001785 cerium compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- 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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- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- Non-Insulated Conductors (AREA)
Description
本發明係關於為將如：太陽電池等所用之透明導電膜、或液晶顯示裝置、電致發光顯示裝置、觸控面板裝置之透明壓電感測器的透明電極，或構成顯示裝置之主動矩陣驅動裝置、防靜電導電膜塗敷、氣感測器、電磁遮蔽面板、壓電設備、光電變換裝置、發光裝置，薄膜型蓄電池等所用之膜成膜所用之氧化鋅蒸鍍材料及由其所形成之氧化鋅膜。
本發明係根據2006年4月26日於日本所申請之特願2006-121403號，2006年9月8日於日本所申請之特願2006-244144號及2007年3月9日於日本所申請之特願2007-060081號主張優先權，並援用該內容。
近年，製造太陽電池等之光電變換裝置等時，須使用透明導電膜。習知以往將氧化銦膜(摻雜錫之銦氧化物膜)作為透明導電膜。氧化銦膜具有透明性優異、低電阻之優點。
另一方面，太陽電池或液晶顯示裝置等，要求其低成本化。但因銦昂貴，若將氧化銦膜作為透明導電膜之用時，結果必使該太陽電池亦為昂貴物之缺點。又，製造太陽電池等時，須於透明導電膜上藉電漿化學相氣積層(CVD)法使非晶質矽成膜，此時，透明導電膜若為氧化銦膜時
，因電漿化學相氣積層時之氫電漿，亦產生氧化銦膜劣化的問題點。
為解決此問題點，建議使用可進一步廉價製作的鋁、硼、矽等之導電活性元素摻雜氧化鋅系膜作為太陽電池等之透明導電膜，建議藉濺鍍用以形成此氧化鋅系膜之氧化鋅系濺鍍用靶(例如參照專利文獻1)。若藉此氧化鋅系濺鍍用靶，使該導電活性元素含有預定量的鋅，可得極低電阻的氧化鋅燒結體，此燒結體其原料粉末微細且具高分散性可提高燒結密度並提高導電性。
〔專利文獻1〕特開平6-2130號公報(申請專利範圍第2項、第3項及第4項)
但使用該以往的氧化鋅系濺鍍用靶為高速成膜須開動高電壓同時進行濺鍍，易產生異常放電，因放電狀態不穩定靶不均勻消耗，所得之膜產生組成偏差產生很難得到低電阻之膜之不適情況。反之，若減少投入電力以降低電壓，使成膜速度變慢，產生大幅降低氧化鋅系膜之成膜效率之不適情況。
本發明之目的，係提供得高速成膜較低電阻之膜之氧化鋅蒸鍍材料及使用此之氧化鋅膜。
本發明的第1型態，係為使透明導電膜成膜所用之氧化鋅蒸鍍材料。
該有特徵的構成，為由氧化鋅純度為98%以上之由氧化鋅粉末所製成的氧化鋅粒料所成，粒料含1種或2種以上選自由釔、鑭、鈧、鈰、鐠、釹、鉅及釤所成群之元素。
此時之氧化鋅蒸鍍材料，係使用由氧化鋅粒料所含之1種或2種以上選自由釔、鑭、鈧、鈰、鐠、釹、鉅及釤所成群之元素的濃度於該範圍內之氧化鋅蒸鍍材料形成氧化鋅膜時，該氧化鋅膜可得涉及溫度範圍廣之優良的導電性。
本發明之另一型態，其特徵為氧化鋅粒料為多晶體或單晶體。
此氧化鋅蒸鍍材料，其中氧化鋅粒料為多晶體或單晶體的組織並無差異，因依組成的差異其效果有明顯地變化，氧化鋅粒料可為多結晶，亦可為單結晶具有申請專利範圍第1項所載之範圍內的組成，使用該氧化鋅蒸鍍材料形成氧化鋅膜時，該氧化鋅膜可得涉及溫度範圍廣的優良的導電性。
本發明的其他型態，係將氧化鋅蒸鍍材料作為靶材料藉真空成膜法所形成之氧化鋅膜。
此真空成膜法係以電子束蒸鍍法、離子披覆法或濺鍍法為宜。
如上所述，根據本發明，由氧化鋅純度為98%以上之由氧化鋅粉末所製成的氧化鋅粒料所成，此粒料因含預定量之1種或2種以上選自由釔、鑭、鈧、鈰、鐠、釹、鉅及釤所成群之元素，若使用此氧化鋅蒸鍍材料膜形成氧化鋅膜時，該氧化鋅膜可得優良的導電性。
又，氧化鋅粒料可為多晶亦可為單晶，使用具有該範圍內組成之氧化鋅蒸鍍材料形成氧化鋅膜時，該氧化鋅膜可得優良的導電性。
其次說明用以實施本發明之最佳形態。
本發明者們針對氧化鋅蒸鍍材料及使用此蒸鍍材料經成膜之氧化鋅膜中之雜質種及該含量中導電性的影響詳細調查的結果，確認深受氧化鋅粒料所含之1種或2種以上選自由釔、鑭、鈧、鈰、鐠、釹、鉅及釤所成群之元素的濃度之影響。氧化鋅粒料中之1種或2種以上選自由釔、鑭、鈧、鈰、鐠、釹、鉅及釤所成群之元素的濃度愈增加，大體上氧化鋅膜之導電性則變得良好，但若再增加反而劣化，考量若要適用於製品，得知最適當為存於1種或2種以上選自由釔、鑭、鈧、鈰、鐠、釹、鉅及釤所成群之元素的濃度範圍。又，該1種或2種以上選自由釔、鑭、鈧、鈰、鐠、釹、鉅及釤所成群之元素，含以鑭、鈰、釹為主要成分為混合物之鈰合金料(以Mm示之)。
調整本發明之1種或2種以上選自由釔、鑭、鈧、鈰、鐠、釹、鉅及釤所成群之元素的濃度之氧化鋅蒸鍍材料，係為將透明導電膜成膜所用之氧化鋅蒸鍍材料。此粒料的直徑為5~50mm，厚度為2~30mm為宜。將此粒料的直徑設為5~50mm，係為實施穩定且高速的成膜，該直徑若低於5mm會產生濺油等不適情況，若超過50mm因對爐(儲存蒸鍍材料)的填充率降低，造成蒸鍍中之膜的不均勻及成膜速度降低的不適情況。又該厚度設為2~30mm係為實施穩定且高速的成膜。該厚度若低於2mm會產生濺油等不適情況，若超過30mm因對爐(儲存蒸鍍材料)的填充率降低，造成蒸鍍中之膜的不均勻及成膜速度降低的不適情況。
又，此氧化鋅蒸鍍材料，係由氧化鋅純度為98%以上，以98.4%以上之由氧化鋅粉末所製成的多晶氧化鋅粒料所成為宜。在此，氧化鋅粉末中之氧化鋅純度限定為98%以上，係因若低於98%因雜質的影響造成氧化鋅膜的導電性降低。又，此氧化鋅蒸鍍材料係相對密度為90%以上，以95%以上的多晶氧化鋅粒料為宜。相對密度設為90%以上，係因若低於90%成膜時的濺油増加。又，此實施形態的氧化鋅粒料組織為多晶，亦可為單晶。
氧化鋅蒸鍍材料中之該釔、鑭、鈧等元素為2~20質量%，以3~6質量%為宜。該釔、鑭、鈧等元素設為2~20質量%係為提高氧化鋅膜的導電性。該元素若低於2質量%並無助於提高導電性，若超過20質量%產生氧化鋅膜
的導電性降低及穿透率惡化等不適情況。反之，該等元素若為微量時，非以粒狀的析出物存於氧化鋅矩陣的粒界或粒內，而是均勻分散於氧化鋅蒸鍍材料中。又該元素係以氧化物存於氧化鋅蒸鍍材料中。認為如釔係以Y2O3的形態存在，鑭以La2O3的形態存在。又，鈧以Sc2O3的形態存在，鈰以CeO2或Ce2O3的形態存在。認為鐠以Pr6O12的形態存在，釹以Nd2O3的形態存在。再之鉅以Pm2O3的形態存在，釤以Sm2O3的形態存在。
如此所構成的本發明之氧化鋅蒸鍍材料，因添加3價或4價以上的烯土類元素，使對為2價的鋅產生剩餘的載體電子。又於氧化鋅蒸鍍材料添加稀土類時，係為易引起蒸鍍時組成偏差的材料，得維持膜所期的組成比例。又，除強制投入載體電子以外亦有藉缺氧作為導電的機構。一般蒸鍍法係導入氧氣，但通常膜組成時呈現氧不足的狀態。透明導電膜形成時雖採用使產生缺氧以降低電阻的手法，但添加稀土類元素時，因蒸發性能優易具有易於控制的特徵。本發明係利用此特徵使用鋁或鎵以外的添加元素，可得齊於氧化銦的導電性。
其次，以添加元素為鈰，藉結燒法製作時為代表，說明本發明的氧化鋅蒸鍍材料的製造方法。
首先將純度為98%以上的高純度氧化鋅粉末，和鈰的濃度為2~20質量%之範圍所成之量的高純度之氧化鈰粉末，和黏著劑，和有機溶媒加以混合，調製成濃度為30~75質量%的淤漿。以調製40~65質量%的淤漿為宜。
將淤漿的濃度限定為30~75質量%，係因若超過75質量%因該淤漿為非水系，有很難穩定混合造粒的問題點，若低於30質量%無法得到具有均勻性組織的緊密的氧化鋅燒結體。氧化鋅粉末的平均粒徑以在0.1~5.0μm的範圍內為宜。將氧化鋅粉末的平均粒徑限於於該範圍內，係因若低於下限值粉末太細而凝結，粉末的控制不佳，有很難調製成高濃度淤漿的問題點，若超過上限值，因很難控制微細結構，有無法得到緊密的粒料的問題點。
氧化鈰粉末若考量防止鈰存在量的不均和與氧化鋅矩陣的反應性及鈰化合物的純度時，以添加1次粒徑為奈米尺度的氧化鈰粒子為宜。
使用聚乙二醇或聚乙烯醇縮丁醛等作為黏著劑，有機溶媒係使用乙醇或丙醇等為宜。黏著劑以添加0.2~5.0質量%為宜。
又，高純度粉末和黏著劑和有機溶媒的濕式混合，尤以高純度粉末和為分散媒的有機溶媒的濕式混合，係藉濕式球磨機或攪拌混合機進行。
濕式球磨機，若使用二氧化鋅製之球時，使用直徑5~10mm的複數二氧化鋅製之球經8~24小時，以20~24小時濕式混合為宜。將二氧化鋅製之球的直徑限定為5~10mm，係因若低於5mm呈現混合不足，但若超過10mm時有雜質增加之不適情況。又，混合時間若長於最長24小時，因即使長時間連續混合很少產生雜質。
攪拌混合機，係使用直徑1~3mm的二氧化鋅製之球
經濕式混合0.5~1小時。將二氧化鋅製之球的直徑限定為1~3mm，係因若低於1mm呈現混合不足，但若超過3mm有雜質增加的不適情況。又混合時間最長為1小時以內，若超過1小時不僅是原料的混合，因球本身磨損，成為產生雜質的原因，又因1小時間即可充分混合。
其次將該淤漿噴霧乾燥，得到平均粒徑為50~250μm，以50~200μm的混合造粒粉末為宜。將此造粒粉末放入預定的模型以預定的壓力成形。該噴霧乾燥以使用噴霧乾燥機進行為宜，預定的模型使用單軸加壓裝置或冷等靜壓成形裝置(CIP(Cold Isostatic Press)成形裝置)。
單軸加壓裝置，係將造粒粉末以750~2000kg/cm2(73.55~196.1MPa)，以1000~1500kg/cm2(98.1~147.1MPa)的壓力單軸加壓成形為宜。
冷等靜壓成形裝置，係將造粒粉末以1000~3000kg/cm2(98.1~294.2MPa)，以1500~2000kg/cm2(147.1~196.1MPa)的壓力冷等靜壓成形為宜。
將壓力限定於該範圍，係為提高成形體的密度並防止燒結後變形，省略後加工。
再之以預定溫度燒結成形體。燒結係於大氣、惰性氣體、真空或還原氣體大氣中以1000℃以上、以1200~1400℃的溫度為宜，進行1~10小時，以2~5小時為宜。藉此得到相對密度90%以上的粒料。該燒結係於大氣壓下進行，以熱壓(HP)燒結或熱等均壓機(HIP,Hot
Isostatic Press)燒結之類的進行加壓燒結時，於惰性氣體、真空或還原氣體大氣中以1000℃以上的溫度進行1~5小時為宜。將如此所得之粒料的多晶氧化鋅蒸鍍材料作為靶材料，藉真空成膜法於基板表面形成氧化鋅膜。
又，雖以Ce作為代表已進行了說明，使用鑭、鈧、鐠、釹、鉅及釤作為添加元素時，使用釔、鑭、鈧、鐠、釹、鉅及釤以取代該鈰，以同於該方法製造氧化鋅蒸鍍材料。
另一方面，用以形成該氧化鋅膜的真空成膜法，例舉如電子束蒸鍍法或離子披覆法或濺鍍法等。
其次，詳細說明本發明之實施例與比較例。
作為氧化鋅蒸鍍材料，其相對密度為95%，此氧化鋅蒸鍍材料中所含鈰的濃度為5質量%之多晶氧化鋅粒料。此氧化鋅蒸鍍材料的直徑及厚度分別為5mm及1.6mm。另外，氧化鋅粉末的氧化鋅純度為99%。
接著，於玻璃基板上，藉電子束蒸鍍法使該氧化鋅蒸鍍材料，形成膜厚為200nm的氧化鋅膜。成膜條件係到達真空度為1.0×10-4Pa，氧氣分壓為1.0×10-2Pa，基板溫度為200℃，成膜速度為0.5nm/秒。
係藉除使用藉燒結法製作之氧化鋅多晶粒料(縱、橫及厚度分別為5mm、5mm及2mm程度的板狀粒料)所含之鈧的濃度為3~6質量%的氧化鋅蒸鍍材料之外，其餘同於實施例1的方法形成氧化鋅膜。
係藉除使用藉燒結法製作之氧化鋅多晶粒料(縱、橫及厚度分別為5mm、5mm及2mm程度的板狀粒料)所含之釔的濃度為3~6質量%的氧化鋅蒸鍍材料以外，其餘同於實施例1的方法形成氧化鋅膜。
係藉除使用藉燒結法製作之氧化鋅多晶粒料(縱、橫及厚度分別為5mm、5mm及2mm程度的板狀粒料)所含之鑭的濃度為3~6質量%的氧化鋅蒸鍍材料以外，其餘同於實施例1的方法形成氧化鋅膜。
係藉除使用藉燒結法製作之氧化鋅多晶粒料(縱、橫及厚度分別為5mm、5mm及2mm程度的板狀粒料)所含之鐠的濃度為3~6質量%的氧化鋅蒸鍍材料以外，其餘同於實施例1的方法形成氧化鋅膜。
係藉除使用藉燒結法製作之氧化鋅多晶粒料(縱、橫及厚度分別為5mm、5mm及2mm程度的板狀粒料)所含之釹的濃度為3~6質量%的氧化鋅蒸鍍材料以外，其餘同於實施例1的方法形成氧化鋅膜。
係藉除使用藉燒結法製作之氧化鋅多晶粒料(縱、橫及厚度分別為5mm、5mm及2mm程度的板狀粒料)所含之鉅的濃度為3~6質量%的氧化鋅蒸鍍材料以外，其餘同於實施例1的方法形成氧化鋅膜。
係藉除使用藉燒結法製作之氧化鋅多晶粒料(縱、橫及厚度分別為5mm、5mm及2mm程度的板狀粒料)所含之釤的濃度為3~6質量%的氧化鋅蒸鍍材料以外，其餘同於實施例1的方法形成氧化鋅膜。
作為氧化鋅蒸鍍材料，相對密度為95%之結晶氧化鋅粒料。即準備氧化鋅中不含釔、鑭、鈧、鈰、鐠、釹、鉅及釤其中任1種的氧化鋅粒料。此氧化鋅蒸鍍材料的直徑及厚度分別為5mm及1.6m。藉除使用此氧化鋅蒸鍍材料
之外，其餘同於實施例1的方法形成氧化鋅膜。另外，氧化鋅粉末之氧化鋅純度為99%。
測定於實施例1~8及比較例1所得之氧化鋅膜的電阻率和穿透率。電阻率係使用三菱化學股份有限公司製商品名為Loresta(HP型、MCP-T410、探針為串列1.5mm間距)作為測定器，於大氣為25℃的一般常溫藉施加定電流的4端子4探針法測定。穿透率係使用日立製作所股份有限公司製分光光度計U-4000作為測定器測定，對於可見光波長區域(380~780mm)，垂直地設置成膜後之基板以測定測定光。此等之測定結果示於表1。
由表1清楚表示，若較之比較例1的93%，實施例1~8中之穿透率雖低，最低值為實施例2的87%，得知因
實施例1~8中之氧化鋅膜得以充分實際使用的透過率。反之，自表1清楚得知，實施例1~8中之電阻率明顯低於比較例1之值。因此，得知本發明之氧化鋅蒸鍍材料可高速成膜比較性低電阻的膜。
如上所述，根據本發明，係由氧化鋅純度為98%以上的氧化鋅粒料所成，此粒料因含預定量1種或2種以上選自由釔、鑭、鈧、鈰、鐠、釹、鉅及釤所成群之元素，若使用此氧化鋅蒸鍍材料形成氧化鋅膜，此氧化鋅膜可得優良的導電性。
又，氧化鋅粒料為多晶，亦可為單結，若使用具有該範圍內組成的氧化鋅蒸鍍材料形成氧化鋅膜，該氧化鋅膜可得優良的導電性。因此，本發明極有助於產業上。
Claims (6)
- 一種氧化鋅(ZnO)蒸鍍材料，其係為將透明導電膜成膜所用之氧化鋅蒸鍍材料，其特徵為由氧化鋅純度為98%以上之由氧化鋅粉末所製成的氧化鋅粒料所構成，該粒料包含1種或2種以上選自由鑭、鈰、鐠、釹、鉅及釤所成群之稀土類元素2~20質量%。
- 如申請專利範圍第1項之氧化鋅蒸鍍材料，其中氧化鋅粒料為多晶體或單晶體。
- 一種氧化鋅膜，其特徵為將申請專利範圍第1或2項之氧化鋅蒸鍍材料作為靶材料藉由電子束蒸鍍法所形成。
- 如申請專利範圍第1項之氧化鋅蒸鍍材料，其中該稀土類元素係為存在於氧化鋅蒸鍍材料中之氧化物。
- 如申請專利範圍第1項之氧化鋅蒸鍍材料，其中該氧化鋅粒料之直徑為5~50mm。
- 一種氧化鋅(ZnO)蒸鍍材料之製造方法，其係如申請專利範圍第1項之氧化鋅蒸鍍材料之製造方法，其特徵為將1種或2種以上選自由鑭、鈰、鐠、釹、鉅及釤所成群之稀土類元素作為添加元素，混合平均粒徑在0.1~5.0μm之範圍內之純度98%以上之氧化鋅粉末、該添加元素之濃度為2~20質量%之範圍之量之1次粒徑為奈米尺度之氧化物粉末、黏著劑、及有機溶媒而調製成濃度為30~75質量%之淤漿，噴霧乾燥該淤漿而調製成平均粒徑50~250μm之混合 造粒粉末，將該造粒粉末放入預定之模型且以73.55~196.1MPa之壓力使其成形，使該成形體在大氣、惰性氣體、真空或還原氣體之環境下以1200~1400℃溫度燒結1~10小時而得到粒料。
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| JP5129772B2 (ja) * | 2008-03-28 | 2013-01-30 | タテホ化学工業株式会社 | Ｓｒ−Ｃａ−Ｏ焼結体 |
| JP5402520B2 (ja) * | 2008-10-27 | 2014-01-29 | 三菱マテリアル株式会社 | ＺｎＯ蒸着材の製造方法 |
| CN101748405B (zh) * | 2008-11-28 | 2014-02-12 | 北京北方微电子基地设备工艺研究中心有限责任公司 | 透明导电膜及其制造方法、太阳能电池及平板显示装置 |
| JP5381724B2 (ja) * | 2009-01-13 | 2014-01-08 | 三菱マテリアル株式会社 | ＺｎＯ蒸着材の製造方法 |
| JP5428870B2 (ja) * | 2009-01-13 | 2014-02-26 | 三菱マテリアル株式会社 | ＺｎＯ蒸着材の製造方法 |
| JP5428871B2 (ja) * | 2009-01-13 | 2014-02-26 | 三菱マテリアル株式会社 | ＺｎＯ蒸着材の製造方法 |
| JP5428872B2 (ja) * | 2009-01-13 | 2014-02-26 | 三菱マテリアル株式会社 | ＺｎＯ蒸着材の製造方法 |
| JP5428873B2 (ja) * | 2009-01-13 | 2014-02-26 | 三菱マテリアル株式会社 | ＺｎＯ蒸着材の製造方法 |
| JP5381725B2 (ja) * | 2009-01-13 | 2014-01-08 | 三菱マテリアル株式会社 | ＺｎＯ蒸着材の製造方法 |
| JP5519959B2 (ja) * | 2009-06-10 | 2014-06-11 | 三菱マテリアル株式会社 | 積層シート |
| TWI531276B (zh) * | 2010-10-21 | 2016-04-21 | 行政院原子能委員會核能研究所 | 有機電激發光元件之封裝方法及其結構 |
| CN102723376A (zh) * | 2012-06-29 | 2012-10-10 | 苏州嘉言能源设备有限公司 | 太阳能电池光吸收透明薄膜 |
| JP2015113512A (ja) * | 2013-12-13 | 2015-06-22 | 三菱マテリアル株式会社 | 酸化物スパッタリングターゲット |
| CN105713596B (zh) * | 2014-12-05 | 2018-10-19 | 有研稀土新材料股份有限公司 | 混合ref3变色镀膜材料及其制备方法和用途 |
| CN107001145B (zh) * | 2014-12-15 | 2020-05-19 | 日本特殊陶业株式会社 | 导电性氧化物烧结体、导电用构件、气体传感器、压电元件以及压电元件的制造方法 |
| JP6817020B2 (ja) * | 2016-02-22 | 2021-01-20 | 株式会社タムロン | 赤外線透過膜、光学膜、反射防止膜、光学部品、光学系及び撮像装置 |
| CN108183173A (zh) * | 2017-12-14 | 2018-06-19 | 中国科学院广州能源研究所 | 一种基于掺钇氧化锌电子传输层的量子点发光二极管及其制备方法 |
| KR102255537B1 (ko) * | 2018-01-12 | 2021-05-25 | 주식회사 엘지에너지솔루션 | 파우치 필름 및 그의 제조 방법 |
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