JP2017008351A - 有機イリジウム化合物からなる化学蒸着用原料及び化学蒸着法、並びに、電気化学用触媒の製造方法 - Google Patents
有機イリジウム化合物からなる化学蒸着用原料及び化学蒸着法、並びに、電気化学用触媒の製造方法 Download PDFInfo
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- 239000002994 raw material Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 31
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- 229910000457 iridium oxide Inorganic materials 0.000 claims abstract description 49
- 229910052741 iridium Inorganic materials 0.000 claims abstract description 40
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- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 14
- 239000010703 silicon Substances 0.000 claims abstract description 14
- 125000004665 trialkylsilyl group Chemical group 0.000 claims abstract description 10
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- 125000001424 substituent group Chemical group 0.000 claims description 16
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- 125000000217 alkyl group Chemical group 0.000 claims description 13
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- 125000004432 carbon atom Chemical group C* 0.000 claims description 9
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 5
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- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- 229910001882 dioxygen Inorganic materials 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 28
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- 229910021607 Silver chloride Inorganic materials 0.000 description 6
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
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- ZKPHEWYDICTCGD-UHFFFAOYSA-N CC1=C(C(=C(C1(C)[IrH2]([Si](CC)(CC)CC)[Si](CC)(CC)CC)C)C)C Chemical compound CC1=C(C(=C(C1(C)[IrH2]([Si](CC)(CC)CC)[Si](CC)(CC)CC)C)C)C ZKPHEWYDICTCGD-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 239000010931 gold Substances 0.000 description 1
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- 239000011261 inert gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002503 iridium Chemical class 0.000 description 1
- MMAGMBCAIFVRGJ-UHFFFAOYSA-J iridium(3+);1,2,3,4,5-pentamethylcyclopenta-1,3-diene;tetrachloride Chemical compound Cl[Ir+]Cl.Cl[Ir+]Cl.CC=1C(C)=C(C)[C-](C)C=1C.CC=1C(C)=C(C)[C-](C)C=1C MMAGMBCAIFVRGJ-UHFFFAOYSA-J 0.000 description 1
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- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
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Abstract
【解決手段】有機イリジウム化合物からなり、化学蒸着法によりイリジウム及びケイ素を含む薄膜を製造するための化学蒸着用原料であって、前記有機イリジウム化合物は、イリジウムに、シクロペンタジエン又はその誘導体及びトリアルキルシリル基が配位した次式で示される有機イリジウム化合物である化学蒸着用原料。
(R1〜R5は各々独立にH又はC1〜3のアルキル;R6〜R11は各々独立にC1〜6のアルキル)
【選択図】図1
Description
第1実施形態:本実施形態では、化学蒸着の原料となる有機イリジウム化合物として、上記化4で示した有機イリジウム化合物である、ジヒドリド(ペンタメチルシクロペンタジエニル)ビス(トリエチルシリル)イリジウム([{(C5Me5)Ir(H)2(SiEt3)2}]):化1のR1、R2、R3、R4、R5が全てメチル基であり、R6、R7、R8、R9、R10、R11が全てエチル基である)を用意した。そして、この有機イリジウム化合物にて成膜を行い、得られた薄膜を酸化処理して複合材料からなる薄膜を製造した。
ペンタメチル−シクロペンタジエニルイリジウム(III)ジクロリド二量体([{(C5Me5)Ir}2Cl4])0.5g(0.62mmol)とトリエチルシラン(SiEt3)2cm3(12.6mmol)、更に、トリエチルアミン2cm3の混合溶液(溶媒:ベンゼン(10cm3))を15分間還流して反応させた。このとき溶液の色は緑色から黄色に変化した。反応後、トリエチルアンモニウムをフィルター除去すると共に、溶媒を減圧留去した。得られた油分について、有機シリコン組成物等の不純物を除去するため、メタノールで洗浄して白色の固形分採取した。この固形分をヘキサンとフロリジルを用いたクロマトグラフィーで分離精製して目的の有機イリジウム化合物結晶(無色)を得た。
上記で製造した有機イリジウム化合物について、TG−DTA分析により、熱分解特性と蒸気圧を評価した。TG−DTA分析は、窒素気流下(200cc(標準状態)/min)、試料を昇温速度2℃/minにて室温から450℃まで加熱した際の試料の重量変化を観察した。この測定結果を図1に示す。
本実施形態の有機イリジウム化合物を原料とし(反応ガス:酸素)、チューブ型化学気相蒸着(CVD)装置を用い、イリジウム薄膜を成膜した。この成膜試験に用いた基板は、FTO(フッ素ドープ酸化錫)がコートされたガラス基板である。このCVDによる成膜直後のイリジウム薄膜は、イリジウム中に酸化ケイ素がドープされた薄膜である。以下、この酸化ケイ素がドープされたイリジウム薄膜を「A1膜」と称して説明する。成膜条件は、次の通りである。
原料気化温度:95℃
基板加熱温度:400℃
反応ガス:酸素40sccm(キャリアガスを兼ねる)
反応器圧力:55−60Pa
成膜時間:5分
上記で成膜したA1膜を酸化処理してIrを酸化し、酸化イリジウムと酸化ケイ素とからなる薄膜を製造した。以下、A1膜の酸化処理により製造された複合材料膜について、「A2膜」と称する。
Claims (10)
- 有機イリジウム化合物からなり、化学蒸着法によりイリジウム及びケイ素を含む薄膜を製造するための化学蒸着用原料であって、
前記有機イリジウム化合物は、イリジウムに、シクロペンタジエン又はその誘導体及びトリアルキルシリル基が配位した次式で示される有機イリジウム化合物である化学蒸着用原料。
- R6、R7、R8、R9、R10、R11の全ての置換基がエチル基である請求項1記載の化学蒸着用原料。
- R1、R2、R3、R4、R5の全ての置換基が水素である請求項1又は請求項2記載の化学蒸着用原料。
- R1、R2、R3、R4、R5の少なくとも一つの置換基がメチル基であり、他の置換基が水素である請求項1又は請求項2記載の化学蒸着用原料。
- R1、R2、R3、R4、R5の少なくとも一つの置換基がエチル基であり、他の置換基が水素である請求項1又は請求項2記載の化学蒸着用原料。
- 有機イリジウム化合物からなる原料を気化して原料ガスとし、前記原料ガスを反応器に導入した後、前記有機イリジウム化合物を分解して、イリジウム及びケイ素を含む薄膜を製造する化学蒸着法において、
前記原料として請求項1〜請求項5のいずれかに記載の化学蒸着用原料を用いる化学蒸着法。 - 反応ガスとして酸素ガスを適用する請求項6記載の化学蒸着法。
- 更に、薄膜を酸化処理する工程を含む請求項6又は請求項7記載の化学蒸着法。
- 基材上に形成され、イリジウム酸化物及びケイ素酸化物を含む電気化学用触媒を製造するための方法であって、
請求項6〜請求項8のいずれかに記載の化学蒸着法により、基材上にイリジウム及びケイ素を含む薄膜を製造する工程を含む電気化学用触媒の製造方法。 - イリジウム及びケイ素を含む電気化学用触媒層を備える電解用電極であって、
前記電気化学用触媒層は請求項9記載の方法により製造される電気化学用触媒からなるものである電解用電極。
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Cited By (3)
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JP6321252B1 (ja) * | 2017-03-24 | 2018-05-09 | 田中貴金属工業株式会社 | イリジウム錯体からなる化学蒸着用原料及び該化学蒸着用原料を用いた化学蒸着法 |
JP2019167620A (ja) * | 2018-03-22 | 2019-10-03 | 株式会社東芝 | 触媒積層体、膜電極複合体、電気化学セル、スタック、水電解装置および水利用システム |
US11515552B2 (en) | 2018-03-22 | 2022-11-29 | Kabushiki Kaisha Toshiba | Catalyst laminate, membrane electrode assembly, electrochemical cell, stack, water electrolyzer, and hydrogen utilizing system |
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WO2018173724A1 (ja) * | 2017-03-24 | 2018-09-27 | 田中貴金属工業株式会社 | イリジウム錯体からなる化学蒸着用原料及び該化学蒸着用原料を用いた化学蒸着法 |
US11084837B2 (en) | 2017-03-24 | 2021-08-10 | Tanaka Kikinzoku Kogyo K.K. | Chemical deposition raw material including iridium complex and chemical deposition method using the chemical deposition raw material |
JP2019167620A (ja) * | 2018-03-22 | 2019-10-03 | 株式会社東芝 | 触媒積層体、膜電極複合体、電気化学セル、スタック、水電解装置および水利用システム |
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