http://support.spring8.or.jp/Report_JSR/PDF_IAe_ALL/IAe_10B1815.pdf 2010B1815 BL46XU 㧗࢚ࢿࣝࢠ࣮ග㟁Ꮚศගἲࡼࡿ Gd ῧຍ AlN ⷧ⭷ࡢ῝ࡉ᪉ྥࡢゎᯒ Depth Analysis of the Gd Addition AlN Thin Film by Hard X-ray Photoelectron Spectroscopy ᑠᯘ ᖿᘯ a, ▼ཎ Ⴙ⏕ b, Ἠ ᏹ b, すᮏ ဴᮁ a, ⏣୰ ᐶஅ a, ᒣ ┿ஓ c, ႐ከ 㝯 c Mikihiro Kobayashia, Tsuguo Ishiharab, Hirokazu Izumib, Tetsurou Nishimotoa, Hiroyuki Tanakaa, Shinya Kitayamac, Takashi Kitac a a 㻔ᰴ㻕࣓ࣘࢵࢡࢫ, b රᗜ┴❧ᕤᴗᢏ⾡ࢭࣥࢱ࣮, c ⚄ᡞᏛ YUMEX Inc., bHyogo Prefectural Institute of Technology, cKobe University ᡃࠎࡀ῝⣸እග※⏝⺯ගయࡋ࡚㛤Ⓨࡋ࡚࠸ࡿ Gd ῧຍ AlN ⷧ⭷ࡣࠊ࢝ࢯ࣮ࢻ࣑ࣝࢿࢵࢭࣥࢫ ᐃࢆࡍࡿࡓࡵ㟁ὶࢆ༳ຍࡍࡿⓎගᙉᗘࡀᛴ⃭ῶ⾶ࡍࡿ⌧㇟ࡀ⏕ࡌ࡚࠸ࡿࠋࡑࡢཎᅉ ࡋ࡚ࠊ㟁Ꮚࣅ࣮࣒ࡼࡾ Gd ῧຍ AlN ⷧ⭷ࡀࢲ࣓࣮ࢪࢆཷࡅࡓࡇࡀ⪃࠼ࡽࢀࡿࠋᮏሗ࿌࡛ࡣ Gd ῧຍ AlN ⷧ⭷ࡢ⾲㠃῝ᒙ㒊ࡢᵓᡂඖ⣲ࡘ࠸࡚Ꮫ⤖ྜ≧ែࡢኚࢆ᫂ࡽࡍࡿࡓࡵࠊ BL46XU ࡚◳ X ⥺ග㟁Ꮚศග ᐃࡋࡓ⤖ᯝࢆ㏙ࡿࠋ ࣮࣮࢟࣡ࢻ㸸 Gd ῧຍ AlNࠊ῝⣸እග※ࠊXAFS ⫼ᬒ◊✲┠ⓗ㸸 ᡃࠎࡣỈ㖟ࣛࣥࣉࡢ௦᭰⏝ࢆ┠ⓗࠊ❅࣑ࣝࢽ࣒࢘㻔AlN㻕ࢆẕయࡋ࡚ᕼᅵ㢮ඖ⣲࢞ࢻࣜ ࢽ࣒࢘㻔Gd㻕ࢆῧຍࡋࠊGd ࡢ f-f 㟁Ꮚ㑄⛣ࢆ⏝ࡋࡓỈ㖟ࣇ࣮ࣜ῝⣸እග※ࡋ࡚᭷ᮃ࡞ Gd ῧຍ AlN ⷧ⭷ࡢ㛤Ⓨࢆ⾜ࡗ࡚ࡁࡓ[1][2][3]ࠋࡋࡋࠊGd ῧຍ AlN ⷧ⭷ࡣࠊ㟁ὶࢆ༳ຍࡍࡿ࢝ࢯ࣮ ࢻ࣑ࣝࢿࢵࢭࣥࢫᙉᗘࡀᛴ⃭ῶ⾶ࡍࡿ⌧㇟ࡀ⏕ࡌ࡚࠾ࡾࠊࡑࡢཎᅉࡋ࡚ࡣࠊ㟁Ꮚࣅ࣮࣒ࡼ ࡿ⭷ࡢᦆയࢆ⪃࠼࡚࠸ࡿࠋࡑࡇ࡛ᡃࠎࡣᐇ㦂ᐊ࡛ࣞ࣋ࣝࡢ X ⥺ග㟁Ꮚศග ᐃἲࡼࡾࠊⷧ⭷ᵓ ᡂඖ⣲ࡢᏛ⤖ྜ≧ែࢆ᫂ࡽࡋࠊⓎගᙉᗘࡢ㛗㛫Ᏻᐃ⧅ࡀࡿᅉᏊࡢゎ᫂ࢆヨࡳ࡚ࡁࡓࠋ ࡑࡢ⤖ᯝࠊ㟁Ꮚࣅ࣮࣒↷ᑕᚋࡢⷧ⭷࡛ࡣࠊ㟁Ꮚࣅ࣮࣒↷ᑕࡼࡾ୍㒊ཎᏊࡀࡣࡌࡁ㣕ࡤࡉࢀࡓࡓ ࡵࠊAl2pࠊGd3d5/2ࠊN1s ࣆ࣮ࢡࡢᙉᗘࡀᑠࡉࡃ࡞ࡾࠊࡲࡓఱࢀࡶ㧗࢚ࢿࣝࢠ࣮ഃࢩࣇࢺࡋ࡚࠾ ࡾࠊࡑࢀࡒࢀᏛ⤖ྜ≧ែࡀኚࡋ࡚࠸ࡿࡇࢆぢฟࡋࡓࠋࡋࡋ࡞ࡀࡽࠊࡇࢀࡲ࡛⏝ࡋ࡚ࡁ ࡓᐇ㦂ᐊ⣔ࡢ XPS ࡛ࡣග㟁Ꮚࡢ⬺ฟ῝ࡉࡀᩘ nm ␃ࡲࡿࡓࡵࠊᴟ⾲㠃ࡢᏛ⤖ྜ≧ែࡢኚࡋ ☜ㄆ࡛ࡁ࡚࠸࡞࠸ࠋ ࡑࡇ࡛ᮏᐇ㦂࡛ࡣࠊࡼࡾ῝ᒙ㒊ࡢሗࢆ㠀◚ቯ࡛ホ౯࡛ࡁࡿᨺᑕගࢆ⏝ࡋࡓ◳ X ⥺ග㟁Ꮚศ ගἲ㻔HAXPES㻕ࢆ⏝࠸⭷ෆ㒊ࡢᏛ⤖ྜ≧ែࢆゎᯒࡍࡿࡇ࡛ࠊ࢝ࢯ࣮ࢻ࣑ࣝࢿࢵࢭࣥࢫᙉᗘࡢ ᖜ࡞ῶ⾶ᶵᵓࢆ᫂ࡽࡋࠊ㧗㍤ᗘⓎගᮦᩱࡢ㛤Ⓨᣦ㔪ࢆᚓࡿࡇࢆ┠ⓗࡋࡓࠋ͒ ᐇ㦂㸸 ᐃヨᩱ࡛࠶ࡿ Gd ῧຍ AlN ⷧ⭷ࡣࠊᛂᛶ㧗࿘Ἴ࣐ࢢࢿࢺࣟࣥࢫࣃࢵࢱࣜࣥࢢἲࡼࡾస〇 ࡋࡓࠋ4N 㔠ᒓ Al ࢱ࣮ࢤࢵࢺୖ 3N 㔠ᒓ Gd ࢳࢵࣉࢆ㓄⨨ࡋࡓྠࢫࣃࢵࢱࣜࣥࢢ࡛ࠊࣝࢦࣥ ❅⣲ΰྜ࢞ࢫ୰ࠊ200Υࡢ ᗘ᮲௳࡛▼ⱥ࢞ࣛࢫᇶᯈୖ⭷ཌ 540 nm ⛬ᗘࡢᡂ⭷ࢆ⾜ࡗࡓࠋ㟁Ꮚ ࣅ࣮࣒↷ᑕᚋࡢⷧ⭷ࡣࠊຍ㏿㟁ᅽ 5 kVࠊຍ㏿㟁ὶ 200 μA ࡢ᮲௳࡛㟁Ꮚࣅ࣮࣒ࢆ↷ᑕࡋࠊ࢝ࢯ࣮ࢻ ࣑ࣝࢿࢵࢭࣥࢫᙉᗘࡀ 1/2ࠊཬࡧ 1/4 ῶ⾶ࡋࡓヨᩱࢆ‽ഛࡋࡓࠋ 㧗㍤ᗘ㹖⥺↷ᑕࡼࡿࢳ࣮ࣕࢪࢵࣉࢆ㜵Ṇࡍࡿࡓࡵ㟁Ꮚࣅ࣮࣒↷ᑕ๓ᚋࡢヨᩱ⾲㠃ࠊཌ ࡉ⣙ 4 nm ࡢ㔠ⷧ⭷ࢆ╔ࡋ࡚ࠊCu 〇ࡢࢧࣥࣉࣝ࣍ࣝࢲ࣮ᑟ㟁ᛶ࣮࢝࣎ࣥࢸ࣮ࣉ࡛ᅛᐃࡋࡓࡶ ࡢࢆ ᐃ౪ࡋࡓࠋ ᐃࡣ BL46XU ࠾࠸࡚༙⌫ᆺࢼࣛࢨ࣮㻔VG-SCIENTA 〇 R-4000㻕ࢆഛ࠼ࡓ HAXPES ᐇ㦂 ⨨ࢆ⏝࠸ᐊ ࡚⾜ࡗࡓࠋධᑕ X ⥺࢚ࢿࣝࢠ࣮ࡣ 8 keVࠊࢼࣛࢨ࣮ධᑕࢫࣜࢵࢺࡣ curved 0.5 mmࠊࣃࢫ࢚ࢿࣝࢠ࣮ࡣ 200 eV ࡑࢀࡒࢀタᐃࡋࡓࠋ ࡲࡓᚓࡽࢀࡓࢫ࣌ࢡࢺࣝࡢ࢚ࢿࣝࢠ࣮⿵ṇࡣࠊྠ ᐃࡋࡓ Au4f7/2 ࣆ࣮ࢡࢆ⏝࠸࡚⾜ࡗࡓࠋ Intensity (arb.units) Intensity (arb.units) ⤖ᯝ࠾ࡼࡧ⪃ᐹ㸸 ᅗ 1 㟁Ꮚࣅ࣮࣒↷ᑕ๓ᚋ࠾ࡅࡿ Gd ῧຍ AlN ⷧ⭷ࡢ N1s ࢫ࣌ࢡࢺࣝࢆ♧ࡍࠋᅗ୰ࡢ after 㻔1㻕 ࡣࠊ㟁Ꮚࣅ࣮࣒↷ᑕࡼࡾ᭱ึࡢⓎගᙉᗘࡽ 1/2 ࡲ࡛ᙉᗘࡀῶ⾶ࡋࡓヨᩱ࡛ࠊafter 㻔2㻕 ࡣࠊ1/4 ࡲ࡛ᙉᗘࡀῶ⾶ࡋࡓヨᩱ࡛࠶ࡿࠋ㟁Ꮚࣅ࣮࣒↷ᑕᚋࡢⷧ⭷࡛ࡣࠊ㟁Ꮚࣅ࣮࣒↷ᑕࡼࡾ N ཎᏊࡀ ᢤࡅࡓࡓࡵࠊࣆ࣮ࢡᙉᗘࡀᑠࡉࡃ࡞ࡗ࡚࠸ࡿ⪃࠼ࡽࢀࡿࠋࡲࡓࣆ࣮ࢡ⨨ࡣప࢚ࢿࣝࢠ࣮ഃ ࢩࣇࢺࡋ࡚࠾ࡾࠊࣆ࣮ࢡ⨨ࡀ㧗࢚ࢿࣝࢠ࣮ഃࢩࣇࢺࡋ࡚࠸ࡓᐇ㦂ᐊ⣔ XPS ᐃࡢ⤖ᯝࡣ ㏫᪉ྥࣆ࣮ࢡࡀࢩࣇࢺࡋ࡚࠸ࡿࠋ N1s 䠉before 䠉after (1) 䠉after (2) 405 400 395 390 Binding Energy (eV) ᅗ 1㸬㟁Ꮚ⥺↷ᑕ๓ᚋ࠾ࡅࡿ Gd ῧຍ AlN ⷧ⭷ࡢ N1s ࢫ࣌ࢡࢺࣝ ᅗ 2 ♧ࡋࡓ Al2sࠊཬࡧᅗ 3 ♧ࡋࡓ Gd3d ࢫ࣌ࢡࢺࣝࡶྠᵝࠊ㟁Ꮚࣅ࣮࣒↷ᑕᚋࡢࣆ࣮ࢡ ᙉᗘࡣᑠࡉࡃ࡞ࡗ࡚࠾ࡾࠊࣆ࣮ࢡ⨨ࡣᐇ㦂ᐊ⣔ XPS ᐃ࡛ࡣ㧗࢚ࢿࣝࢠ࣮ഃࢩࣇࢺࡋ࡚࠸ࡓ ࡢᑐࡋ࡚ࠊHAXPES ᐃ࡛ࡣప࢚ࢿࣝࢠ࣮ഃࢩࣇࢺࡋ࡚࠸ࡓࠋࡇࢀࡽࡢኚࡀࠊ㟁Ꮚࣅ࣮࣒ ບ㉳ࡢ㝿 Gd ῧຍ AlN ⷧ⭷ࡽⓎ⏕ࡍࡿ࢝ࢯ࣮ࢻ࣑ࣝࢿࢵࢭࣥࢫᙉᗘࡀపୗࡍࡿཎᅉ㛵ಀࡀ ࠶ࡿ⪃࠼ࡽࢀࡿࠋ Al 2s 䠉before 䠉after (1) 䠉after (2) 124 122 120 118 116 Binding Energy (eV) ᅗ 2㸬㟁Ꮚ⥺↷ᑕ๓ᚋ࠾ࡅࡿ Gd ῧຍ AlN ⷧ⭷ࡢ Al2s ࢫ࣌ࢡࢺࣝ Intensity (arb.units) Gd 3d5/2 䠉before 䠉after (1) 䠉after (2) 1200 1190 1180 Binding Energy (eV) ᅗ 3㸬㟁Ꮚ⥺↷ᑕ๓ᚋ࠾ࡅࡿ Gd ῧຍ AlN ⷧ⭷ࡢ Gd3d ࢫ࣌ࢡࢺࣝ ᡃࠎࡣᐇ㦂⤖ᯝࡼࡾࠊ┿✵୰࡛㟁Ꮚࣅ࣮࣒↷ᑕࡼࡗ࡚ヨᩱ⾲㠃ࡣ㑏ඖࡉࢀࠊࡑࡢᚋࠊẼ୰ ྲྀࡾฟࡋࡓࠊヨᩱࡢᴟ⾲㠃ࡔࡅࡀ㓟ࡉࢀࡓ࠸࠺ᶵᵓࢆ⪃࠼࡚࠸ࡿࡀࠊࡑࡢࡶヨᩱ ⾲㠃ࡢᖏ㟁ࡼࡿᙳ㡪ࡸࡢᅉᏊࡶ⪃࠼ࡽࢀࠊヲ⣽ࡘ࠸࡚ࡣᚋࡉࡽㄪᰝࡀᚲせ࡛࠶ࡿࠋ ᅇ HAXPES ᐃࡼࡾࠊ㟁Ꮚࣅ࣮࣒↷ᑕࢆཷࡅࡓ Gd ῧຍ AlN ῝⣸እ⺯ගⷧ⭷ࡘ࠸࡚ࠊᐇ 㦂ᐊ⣔ XPS ᐃ࡛ࡣᚓࡽࢀ࡞ࡗࡓ▱ぢࢆᚓࡿࡇࡀ࡛ࡁࡓࠋ ᚋࡢㄢ㢟㸸 ᚋࠊ㟁Ꮚࣅ࣮࣒↷ᑕࡼࡾヨᩱࡢ XPS ࢫ࣌ࢡࢺࣝࡀࡢࡼ࠺ኚࡍࡿࢆヲ⣽ㄪࠊヨ ᩱຎࡢཎᅉ㧗㍤ᗘࡢせᅉࢆࡉࡽㄪᰝࡍࡿᚲせࡀ࠶ࡿࠋᮏᐇ㦂ࡢ⤖ᯝࡽࠊ㟁Ꮚࣅ࣮࣒↷ ᑕࡼࡗ࡚ⷧ⭷ࡣ㑏ඖࡉࢀࠊࡑࡢᚋࠊᴟ⾲㠃ࡢࡳࡀ㓟ࡉࢀࡓ࠸࠺ᶵᵓࢆ⪃ᐹࡋ࡚࠸ࡿࡀࠊ ᅇࡢ ᐃ࡛ࡣᖏ㟁㜵Ṇ⏝╔ࡋࡓ㔠ⷧ⭷ࡀཌࡗࡓࡓࡵࠊฟᑕゅ౫Ꮡᛶࡢ ᐃࡀ࡛ࡁ࡞ࡗࡓࠋ ḟᅇࡣ㔠ⷧ⭷ࡢཌࡉࢆ 1㹼4 nm ࡢ⠊ᅖෆ࡛ኚ࠼ࡓヨᩱࢆ‽ഛࡋࠊග㟁Ꮚࡢฟᑕゅᗘ౫Ꮡᛶࡢ ᐃ ࡼࡾ⭷ཌ᪉ྥ࡛ࡢྛᵓᡂඖ⣲ࡢᏛ≧ែศᯒࢆ⾜࠸ࠊຎᶵᵓࡢጇᙜᛶࢆ᳨ウࡋࡓ࠸ࠋ ཧ⪃ᩥ⊩㸸 [1] T. Kita et al., Appl. Phys. Lett., 93, 21190,㻌㻔2008㻕. [2] S.Kitayama et al., IOP Conf. Series: Materials Science and Engineering, 1, 012001, 㻔2009㻕. [3]ᑠᯘᖿᘯ, ᖹᡂ 22 ᖺᗘ SPring-8 㔜Ⅼ⏘ᴗ⏝ㄢ㢟ᡂᯝሗ࿌᭩, 㻔2010A1711㻕.
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