JP2020076084A - 蛍光ダイヤモンドおよびその製造方法 - Google Patents
蛍光ダイヤモンドおよびその製造方法 Download PDFInfo
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 139
- 239000010432 diamond Substances 0.000 title claims abstract description 139
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 claims abstract description 66
- 239000002184 metal Substances 0.000 claims abstract description 66
- 229910052752 metalloid Inorganic materials 0.000 claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 37
- 150000002738 metalloids Chemical class 0.000 claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 claims description 32
- 238000000137 annealing Methods 0.000 claims description 15
- 229910052759 nickel Inorganic materials 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 238000010884 ion-beam technique Methods 0.000 claims description 13
- 238000010894 electron beam technology Methods 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 230000001678 irradiating effect Effects 0.000 claims description 6
- 229910052732 germanium Inorganic materials 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 238000005474 detonation Methods 0.000 claims description 3
- 238000001308 synthesis method Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 description 28
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 25
- 239000000523 sample Substances 0.000 description 24
- 238000005259 measurement Methods 0.000 description 23
- 238000001069 Raman spectroscopy Methods 0.000 description 12
- 239000002994 raw material Substances 0.000 description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 11
- 150000002500 ions Chemical class 0.000 description 11
- 239000010703 silicon Substances 0.000 description 10
- 230000005284 excitation Effects 0.000 description 8
- 238000004050 hot filament vapor deposition Methods 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 238000005468 ion implantation Methods 0.000 description 7
- 125000004429 atom Chemical group 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000000879 optical micrograph Methods 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 239000002113 nanodiamond Substances 0.000 description 5
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 5
- 238000000295 emission spectrum Methods 0.000 description 4
- 238000004020 luminiscence type Methods 0.000 description 4
- 238000000387 optically detected magnetic resonance Methods 0.000 description 4
- 238000004435 EPR spectroscopy Methods 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000000799 fluorescence microscopy Methods 0.000 description 3
- 238000002513 implantation Methods 0.000 description 3
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000002096 quantum dot Substances 0.000 description 3
- 238000006862 quantum yield reaction Methods 0.000 description 3
- 229910052718 tin Inorganic materials 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000005283 ground state Effects 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052768 actinide Inorganic materials 0.000 description 1
- 150000001255 actinides Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 230000004397 blinking Effects 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910021480 group 4 element Inorganic materials 0.000 description 1
- 229910021478 group 5 element Inorganic materials 0.000 description 1
- 229910021474 group 7 element Inorganic materials 0.000 description 1
- 229910021472 group 8 element Inorganic materials 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
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Abstract
Description
MVセンター:Metal-Vacancy Center
NVセンター:Nitrogen-Vacancy Center
SiVセンター:Silicon-Vacancy Center
〔1〕MVセンター(Mは金属又は半金属であり、Vは空孔を示す)を1×1014/cm3以上の濃度で含む、蛍光ダイヤモンド。
〔2〕下記(i)〜(iii)の少なくとも1つを満たす、〔1〕に記載の蛍光ダイヤモンド。:
(i) 導入する空孔数と金属又は半金属の原子数の比(V数/M数)が0.1〜10000である、
(ii) 金属又は半金属(M)が0.0001〜1原子%含まれる、
(iii) NVセンターの濃度が1×1017/cm3以下である
〔3〕金属または半金属元素がSi、Ge又はSnである、〔1〕又は〔2〕に記載の蛍光ダイヤモンド。
〔4〕半金属元素がSiである、〔1〕又は〔2〕に記載の蛍光ダイヤモンド。
〔5〕MVセンターを構成する金属または半金属元素以外の金属または半金属元素を含む、〔1〕〜〔4〕の何れか1項に記載の蛍光ダイヤモンド。
〔6〕上記MVセンターを構成する金属または半金属元素以外の金属または半金属元素が、Fe, CoまたはNiである、〔5〕記載の蛍光ダイヤモンド。
〔7〕下記の第1段階及び第2段階
第1段階:ダイヤモンドの合成過程で適当な濃度の金属又は半金属(M)を導入して金属又は半金属(M)を含むダイヤモンドを提供すること、
第2段階:金属又は半金属(M)を含むダイヤモンドに高エネルギー線を照射して空孔を形成し、次いでアニールして蛍光を発するMVセンターを形成すること
を含む、〔1〕〜〔6〕に記載の蛍光ダイヤモンドの製造方法。
〔8〕上記の高エネルギー線がHeもしくはHのイオンビーム又は電子線である、〔7〕に記載の蛍光ダイヤモンドの製造方法。
〔9〕上記の第1段階において、MVセンターを構成する金属または半金属元素以外の金属または半金属を存在させる、〔7〕に記載の蛍光ダイヤモンドの製造方法。
〔10〕上記MVセンターを構成する金属または半金属元素以外の金属または半金属が、Fe, CoまたはNiである〔9〕に記載の蛍光ダイヤモンドの製造方法。
〔11〕第1段階のダイヤモンド合成の方法が化学気相合成法(CVD法)である、〔7〕〜〔10〕の何れか1項に記載の蛍光ダイヤモンドの製造方法。
〔12〕第1段階のダイヤモンド合成の方法が爆轟法である、〔7〕〜〔10〕の何れか1項に記載の蛍光ダイヤモンドの製造方法。
〔13〕第1段階のダイヤモンド合成の方法が爆縮法である、〔7〕〜〔10〕の何れか1項に記載の蛍光ダイヤモンドの製造方法。
蛍光ダイヤモンドは、MVセンター(Mは金属または半金属)、M原子及び空孔(V)を含む。
蛍光ダイヤモンドは、金属又は半金属(M)を含むダイヤモンドを原料として用い、このダイヤモンド原料に高エネルギー線を照射して空孔を形成する工程、空孔を形成したダイヤモンドをアニールしてMVセンターを形成する工程を含む方法により製造することができる。
(I) 導入したい金属又は半金属元素(M)を含む基板をダイヤモンド合成に用いる、
(II) 導入したい金属又は半金属元素(M)を含む基板上に他の金属等を全面あるいは部分的に蒸着し、ダイヤモンド合成に用いる、
(III) 導入したい金属又は半金属元素(M)を含む気体を原料気体に添加する、
(IV) 導入したい金属又は半金属元素(M)の蒸発源、スパッタ源を基板の近傍に配置し、ダイヤモンド成膜中に導入したい元素をダイヤモンド膜に供給する。
市販品のシリコン基板を約2cm角に劈開(cleavage)した試料を基板として用いる。市販品のナノダイヤモンド分散液(たとえばMicrodiamant製MSY0-0.5GAF)をシリコン基板上にスポイドで1、2滴を滴下し綿棒により基板表面に擦り付ける。これはシリコン基板表面に微小な傷を生じさせてのちに成長するダイヤモンド膜の付着の起点とすると同時に、基板上に残留するナノダイヤモンドをダイヤモンド成長の核とすることを意図したものである。このようにして前処理を行ったシリコン基板を熱フィラメントCVD装置に導入した。
シリコン基板片の前処理はシリコン基板上に粉体状の市販ナノダイヤモンド(たとえばMicrodiamont製MSY0-0.5)を少量乗せ、綿棒を用いてシリコン基板表面に擦り付けた。このようにして前処理を行った基板をマグネトロンスパッタ装置を用いて試料表面のおよそ半分の面積部分に膜厚約50nmのニッケルを蒸着した。この基板を用いて実施例1と同様に図2に示す熱フィラメントCVD装置を用いてダイヤモンドの成膜を行った。
実施例2と同様にシリコン基板に市販のナノダイヤモンドを用いて前処理をおこなったのちに、マグネトロンスパッタ装置を用いて試料表面の約半分の面積にコバルトの成膜を行った。コバルトの膜厚は約50nmであった。この基板を用いて実施例1、2と同様に図2に示す熱フィラメントCVD装置を用いてダイヤモンドの成膜を行った。成膜条件は実施例1、2とほぼ同様で、フィラメントを基板より約7mmの位置に固定し、真空系により1×10-3Pa以下を基準に真空引きをし、高真空ポンプを停止したのち原料ガスをCH4が3sccm、H2が200sccmで流し、真空チェンバー内圧力が約10kPaで安定したのち、フィラメントに電力を投入した。成膜はフィラメント電力250Wで2時間行った。その結果、基板全体にダイヤモンド膜は成長し、実施例1、2とほぼ同様な粒子径、膜厚の分布が得られた。このうち、コバルト蒸着領域における試料表面の光学顕微鏡写真を図11に、周辺領域で測定したラマン散乱スペクトルを図12に、またPL測定結果を図13に示す。それらの結果は実施例1、2と同様にラマン散乱測定において明瞭な1332/cmのダイヤモンドピークが見えており、質の良いダイヤモンドが形成されていることを示している。PL測定の結果は実施例1の3倍程度、実施例2の約0.6倍程度であり、金属スパッタリングなしの場合とニッケル膜が存在する場合の間に位置する濃度(同様な濃度評価法によれば1.8×1013/cm3)のSiVセンターが成膜直後に形成されていることを示している。
Claims (13)
- MVセンター(Mは金属又は半金属であり、Vは空孔を示す)を1×1014/cm3以上の濃度で含む、蛍光ダイヤモンド。
- 下記(i)〜(iii)の少なくとも1つを満たす、請求項1に記載の蛍光ダイヤモンド:
(i) 導入する空孔数と金属又は半金属の原子数の比(V数/M数)が0.1〜10000である、
(ii) 金属又は半金属(M)が0.0001〜1原子%含まれる、
(iii) NVセンターの濃度が1×1017/cm3以下である。 - 金属または半金属元素がSi、Ge又はSnである、請求項1又は2に記載の蛍光ダイヤモンド。
- 半金属元素がSiである、請求項1又は2に記載の蛍光ダイヤモンド。
- MVセンターを構成する金属または半金属元素以外の金属または半金属元素を含む、請求項1〜4の何れか1項に記載の蛍光ダイヤモンド。
- 上記MVセンターを構成する金属または半金属元素以外の金属または半金属元素が、Fe, CoまたはNiである、請求項5記載の蛍光ダイヤモンド。
- 下記の第1段階及び第2段階
第1段階:ダイヤモンドの合成過程で適当な濃度の金属又は半金属(M)を導入して金属又は半金属(M)を含むダイヤモンドを提供すること、
第2段階:金属又は半金属(M)を含むダイヤモンドに高エネルギー線を照射して空孔を形成し、次いでアニールして蛍光を発するMVセンターを形成すること
を含む、請求項1〜6のいずれか1項に記載の蛍光ダイヤモンドの製造方法。 - 上記の高エネルギー線がHeもしくはHのイオンビーム又は電子線である、請求項7に記載の蛍光ダイヤモンドの製造方法。
- 上記の第1段階において、MVセンターを構成する金属または半金属元素以外の金属または半金属を存在させる、請求項7に記載の蛍光ダイヤモンドの製造方法。
- 上記MVセンターを構成する金属または半金属元素以外の金属または半金属が、Fe, CoまたはNiである請求項9に記載の蛍光ダイヤモンドの製造方法。
- 第1段階のダイヤモンド合成の方法が化学気相合成法(CVD法)である、請求項7〜10の何れか1項に記載の蛍光ダイヤモンドの製造方法。
- 第1段階のダイヤモンド合成の方法が爆轟法である、請求項7〜10の何れか1項に記載の蛍光ダイヤモンドの製造方法。
- 第1段階のダイヤモンド合成の方法が爆縮法である、請求項7〜10の何れか1項に記載の蛍光ダイヤモンドの製造方法。
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