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論文

Bithiophene with winding vine-shaped molecular asymmetry; Preparation, structural characterization, and enantioselective synthesis

豊森 佑夏*; 辻 悟*; 光田 紫乃布*; 岡山 陽一*; 芦田 汐未*; 森 敦紀*; 小林 徹; 宮崎 有史; 矢板 毅; 荒江 祥永*; et al.

Bulletin of the Chemical Society of Japan, 89(12), p.1480 - 1486, 2016/09

 被引用回数:3 パーセンタイル:71.91(Chemistry, Multidisciplinary)

Preparation of 2,2'-bithiophene derivatives bearing $$omega$$-alkenyl groups at the 3,3'-positions and ring-closing metathesis reactions of the obtained compound were performed. The reaction of bithiophene bearing 3-butenyl substituents with 5mol% Grubbs 1st generation catalyst underwent ring-closing metathesis (RCM) to afford the cyclized product 7 showing winding vine-shaped molecular asymmetry in up to 88% yield. Enantioselective RCM was also achieved by the use of chiral Schrock Hoveyda molybdenum-alkylidene catalyst in up to 87% ee.

論文

Effects of growth temperature and growth rate on polytypes in gold-catalyzed GaAs nanowires studied by in situ X-ray diffraction

高橋 正光; 神津 美和*; 佐々木 拓生

Japanese Journal of Applied Physics, 55(4S), p.04EJ04_1 - 04EJ04_4, 2016/04

 被引用回数:4 パーセンタイル:66.57(Physics, Applied)

The polytypism of GaAs nanowires was investigated by in situ X-ray diffraction using a molecular-beam eppitaxy chamber combined with an X-ray diffractometer. The growth of nanowries was found to start with the formation of zincblende structure, followed by the growth of the wurtzite structure. The wurtzite structure tended to form at a low growth temperature and a high growth rate.

論文

Real-time observation of rotational twin formation during molecular-beam epitaxial growth of GaAs on Si (111) by X-ray diffraction

鈴木 秀俊*; 仲田 侑加*; 高橋 正光; 池田 和磨*; 大下 祥雄*; 諸原 理*; 外賀 寛崇*; 森安 嘉貴*

AIP Advances (Internet), 6(3), p.035303_1 - 035303_6, 2016/03

 被引用回数:3 パーセンタイル:66.57(Nanoscience & Nanotechnology)

The formation and evolution of rotational twin (TW) domains introduced by a stacking fault during molecular-beam epitaxial growth of GaAs on Si (111) substrates were studied by in situ X-ray diffraction. To modify the volume ratio of TW to total GaAs domains, GaAs was deposited under high and low group V/group III (V/III) flux ratios. For low V/III, there was less nucleation of TW than normal growth (NG) domains, although the NG and TW growth rates were similar. For high V/III, the NG and TW growth rates varied until a few GaAs monolayers were deposited; the mean TW domain size was smaller for all film thicknesses.

論文

Anomalous lattice deformation in GaN/SiC(0001) measured by high-speed ${{it in situ}}$ synchrotron X-ray diffraction

佐々木 拓生; 石川 史太朗*; 高橋 正光

Applied Physics Letters, 108(1), p.012102_1 - 012102_5, 2016/01

AA2015-0769.pdf:2.43MB

 被引用回数:1 パーセンタイル:88.37(Physics, Applied)

We report an anomalous lattice deformation of GaN layers grown on SiC(0001) by molecular beam epitaxy. The evolution of the lattice parameters during the growth of the GaN layers was measured by in situ synchrotron X-ray diffraction. The lattice parameters in the directions parallel and normal to the surface showed significant deviation from the elastic strains expected for lattice-mismatched films on substrates up to a thickness of 10 nm. The observed lattice deformation was well explained by the incorporation of hydrostatic strains due to point defects. The results indicate that the control of point defects in the initial stage of growth is important for fabricating GaN-based optoelectronic devices.

論文

Direct observation of strain in InAs quantum dots and cap layer during molecular beam epitaxial growth using ${{it in situ}}$ X-ray diffraction

下村 憲一*; 鈴木 秀俊*; 佐々木 拓生; 高橋 正光; 大下 祥雄*; 神谷 格*

Journal of Applied Physics, 118(18), p.185303_1 - 185303_7, 2015/11

 被引用回数:4 パーセンタイル:67.17(Physics, Applied)

Direct measurements on the growth of InAs quantum dots (QDs) and various cap layers during molecular beam epitaxy are performed by ${{it in situ}}$ X-ray diffraction (XRD). The evolution of strain induced both in the QDs and cap layers during capping is discussed based on the XRD intensity transients obtained at various lattice constants. Transients with different features are observed from those obtained during InGaAs and GaAs capping, attributed to In-Ga intermixing between the QDs and the cap layer. Photoluminescence wavelength can be tuned by controlling the intermixing and the cap layer thickness. It is demonstrated that such information about strain is useful for designing and preparing novel device structures.

論文

Mechanisms determining the structure of gold-catalyzed GaAs nanowires studied by in situ X-ray diffraction

高橋 正光; 神津 美和*; 佐々木 拓生; Hu, W.*

Crystal Growth & Design, 15(10), p.4979 - 4985, 2015/10

 被引用回数:9 パーセンタイル:27.34(Chemistry, Multidisciplinary)

The evolution of polytypism during GaAs nanowire growth was investigated by in situ X-ray diffraction. The growth of nanowires was found to start with the formation of zincblende structure, followed by the growth of wurtzite structure. The growth process was well reproduced by a simulation based on a layer-by-layer nucleation mode. The good agreement between the measured and simulated results confirms that nucleation costs higher energy for the stackings changing the crystal structure than for those conserving the preceding structure. The transition in prevalent structure can be accounted for by the change of local growth conditions related to the shape of triple phase line rather than by the change in supersaturation level, which quickly reaches equilibrium after starting growth.

論文

その場放射光X線回折によるIII-Vエピ成長のひずみ解析

佐々木 拓生; 高橋 正光

日本結晶成長学会誌, 42(3), p.210 - 217, 2015/10

AA2015-0738.pdf:2.23MB

Dislocation-mediated strain relaxation during lattice-mismatched InGaAs/GaAs(001) heteroepitaxy was studied through in situ X-ray reciprocal space mapping (${{it in situ}}$ RSM). At the synchrotron facility SPring-8, a hybrid system of molecular beam epitaxy and X-ray diffractometry with a two-dimensional detector enabled us to perform ${{it in situ}}$ RSM at high-speed and high-resolution. Using this experimental setup, the strain relaxation processes were classified into four thickness ranges with different dislocation behavior. In order to discuss this observation quantitatively, a strain relaxation model was proposed based on the Dodson-Tsao's kinetic model, and its validity was demonstrated by good agreement with the experimental residual strain. In addition to the single InGaAs layer, strain relaxation processes in multi-layer structures are discussed.

論文

放射光その場X線回折による半導体成長機構の解明

高橋 正光

日本結晶成長学会誌, 42(3), p.201 - 209, 2015/10

AA2015-0739.pdf:0.82MB

An experimental approach to crystal growth dynamics using synchrotron X-ray diffraction is discussed. In the study of crystal growth, analysis of imperfect crystals lacking three-dimensional periodicity is inevitably required. Though diffuse scattering generated by such imperfect crystals is much weaker than the bulk Bragg diffraction, recent development of the synchrotron light source has enabled the in situ measurement of it during crystal growth. In this article, studies on surface structures, evolution of defects in growing films and the growth of nanostructures under molecular-beam epitaxy conditions are presented as well as a brief overview of the instrumentation.

論文

${it In situ}$ three-dimensional X-ray reciprocal-space mapping of InGaAs multilayer structures grown on GaAs(001) by MBE

佐々木 拓生; 高橋 正光; 鈴木 秀俊*; 大下 祥雄*; 山口 真史*

Journal of Crystal Growth, 425, p.13 - 15, 2015/09

 パーセンタイル:100(Crystallography)

${it In situ}$ three-dimensional X-ray reciprocal space mapping (${it in situ}$ 3D-RSM) was employed for studying molecular beam epitaxial (MBE) growth of InGaAs multilayer structures on GaAs(001). Measuring the symmetric 004 diffraction allowed us to separately obtain film properties of individual layers and to track the real-time evolution of both residual strain and lattice tilting. In two- layer growth of InGaAs, significant plastic relaxation was observed during the upper layer growth, and its critical thickness was experimentally determined. At the same thickness, it was found that the direction of lattice tilting drastically changed. We discuss these features based on the Dunstan model and confirm that strain relaxation in the multilayer structure is induced by two kinds of dislocation motion (dislocation multiplication and the generation of dislocation half-loops).

論文

Spontaneous formation of suboxidic coordination around Co in ferromagnetic rutile Ti$$_{0.95}$$Co$$_{0.05}$$O$$_2$$ film

Hu, W.*; 林 好一*; 福村 知昭*; 赤木 和人*; 塚田 捷*; 八方 直久*; 細川 伸也*; 大和田 謙二; 高橋 正光; 鈴木 基寛*; et al.

Applied Physics Letters, 106(22), p.222403_1 - 222403_5, 2015/06

 被引用回数:21 パーセンタイル:16.17(Physics, Applied)

The local atomic structures around Co in high temperature diluted ferromagnetic semiconductor Co-doped TiO$$_2$$ has been investigated using X-ray fluorescence holography and X-ray absorption fine structure experiments. While the Co atoms in the Ti$$_{0.99}$$Co$$_{0.01}$$O$$_2$$ simply substituted for Ti sites in the rutile structure, a suboxidic arrangement of CoO$$_2$$Ti$$_4$$ was found to form around Co in the Ti$$_{0.95}$$Co$$_{0.05}$$O$$_2$$ films. First-principles calculations supported the stability of the aggregated suboxidic clusters in the rutile TiO$$_2$$. The suboxidic coordination may be the source of strong exchange interaction, resulting in the high Curie temperature in Co-dopedTiO$$_2$$.

論文

Role of liquid indium in the structural purity of wurtzite InAs nanowires that grow on Si(111)

Biermanns, A.*; Dimakis, E.*; Davydok, A.*; 佐々木 拓生; Geelhaar, L.*; 高橋 正光; Pietsch, U.*

Nano Letters, 14(12), p.6878 - 6883, 2014/12

 被引用回数:17 パーセンタイル:26.37(Chemistry, Multidisciplinary)

The dynamic relation between the growth conditions and the structural composition of the catalyst-free InAs nanowires was investigated using time-resolved X-ray scattering and diffraction measurements during the growth by molecular beam epitaxy. A spontaneous build-up of liquid indium is directly observed in the beginning of the growth process and associated with the simultaneous nucleation of InAs nanowires predominantly in the wurtzite phase. After their nucleation, the nanowires grow in the absence of liquid indium, and with a highly defective wurtzite structure. A pathway to pure wurtzite nanowires is presented through this work.

論文

Present state of TEM-SXES analysis and its application to SEM aiming chemical analysis of bulk materials

寺内 正己*; 高橋 秀之*; 飯田 信雄*; 村野 孝訓*; 小池 雅人; 今園 孝志; 小枝 勝*; 長野 哲也*; 笹井 浩行*; 大上 裕紀*; et al.

Microscopy and Microanalysis, 20(Suppl.3), p.682 - 683, 2014/08

電子顕微鏡(TEM及びEPMA)に取り付け可能な軟X線発光分光器(SXES)を開発した。これは4枚の不等間隔溝回折格子を備え、50$$sim$$4000eVのエネルギー範囲を測定できる。これとTEMを組み合わせたTEM-SXES装置は、電子エネルギー損失分光器やエネルギー分散型分光器では計測困難な局所領域の価電子帯に関する情報を取得できる。SXES装置を材料開発・評価の現場へ広く普及させる観点から、試料の薄膜化を必要としないSEMにも搭載できるようにした。SEMはTEMに比して空間分解能で劣るもののプローブ電流量が大きい上、幅広い物質、特に、バルク物質を扱えるため汎用性が高い。本研究では、Al金属間化合物(Al$$_2$$Au, Al$$_2$$Co)のバルク試料からのAl-L発光測定において結晶構造の違いAl(FCC), Al$$_2$$Au(CaF$$_2$$), Al$$_2$$Co(CsCl)に起因するバンド構造の差異が反映されたスペクトルを得ることができた。このように、SEMによるSXES測定は、バルク試料に対して状態密度の顕微マッピング分析が可能な技術として有用であると考えられる。

論文

Exciting possibilities of soft X-ray emission spectroscopy as chemical state analysis in EPMA and FESEM

高橋 秀之*; 飯田 信雄*; 村野 孝訓*; 寺内 正己*; 小池 雅人; 河内 哲哉; 今園 孝志; 長谷川 登; 小枝 勝*; 長野 哲也*; et al.

Microscopy and Microanalysis, 20(Suppl.3), p.684 - 685, 2014/08

電子プローブアナライザ(EMPA)としてX線エネルギー範囲が公称50$$sim$$210eVの新しい波長分散型軟X線発光分光計(SXES)を開発した。このEPMA-SXESは2枚の不等間隔溝回折格子を用いた平面結像型分光器で、従来の波長分散型分光器では困難であったパラレル計測が可能であり、そのエネルギー分解はAl-L端で約0.2eVと、光電子分光器や電子エネルギー損失分光器と比して同程度である。これらの特長から様々なバルク試料の化学結合状態について有意義な情報を得ることができる。本研究では、このEPMA-SXESを用いた実試料の測定を行い、リチウムイオン電池の負極及び金属リチウムからのLi-K発光スペクトルの比較、$$sigma$$結合と$$pi$$結合に起因するキッシュ黒鉛からのC-K発光スペクトルの結晶方位依存性、3種類の希土類フッ化物(LaF$$_3$$, CeF$$_3$$, NdF$$_3$$)からのLa, Ce, NdのN発光スペクトルの比較について報告する。

論文

Application of capillary electrophoresis with laser-induced fluorescence detection for the determination of trace neodymium in spent nuclear fuel using complexation with an emissive macrocyclic polyaminocarboxylate probe

原賀 智子; 齋藤 伸吾*; 佐藤 義行; 浅井 志保; 半澤 有希子; 星野 仁*; 渋川 雅美*; 石森 健一郎; 高橋 邦明

Analytical Sciences, 30(7), p.773 - 776, 2014/07

 被引用回数:4 パーセンタイル:75.67(Chemistry, Analytical)

高レベル放射性廃棄物の発生源である使用済燃料について、燃焼率の指標の一つであるネオジムイオンを簡易・迅速に分析するため、蛍光性環状型6座ポリアミノカルボン酸配位子を用いたキャピラリー電気泳動-レーザー励起蛍光検出法の適用性を検討した。本検討では、ウラニルイオンやランタノイドイオン群など、様々な金属イオンが共存する使用済燃料溶解液において、微量のネオジムイオンを定量することに成功し、その際、ランタノイドイオン間の分離には分離用泳動液に含まれる水酸化物イオンが重要な役割を担っていることを明らかした。従来の陰イオン交換による分離法では、ネオジムの単離に約2週間を要するが、本法では数十分で分離検出が可能であり、分析に要する時間を大幅に短縮することができ、作業者の被ばくの低減が期待できる。

論文

Chemical state information of bulk specimens obtained by SEM-based soft-X-ray emission spectrometry

寺内 正己*; 越谷 翔悟*; 佐藤 二美*; 高橋 秀之*; 飯田 信雄*; 村野 孝訓*; 小池 雅人; 今園 孝志; 小枝 勝*; 長野 哲也*; et al.

Microscopy and Microanalysis, 20(3), p.692 - 697, 2014/06

 被引用回数:11 パーセンタイル:21.61(Materials Science, Multidisciplinary)

電子ビーム励起軟X線発光分光法(SXES)によりバルク材料の化学結合状態を評価するために回折格子分光器を走査型電子顕微鏡(SEM)に導入した。この分光器は、平面結像型不等間隔溝回折格子と、マルチチャンネルプレートに電荷結合素子カメラを組み合わせた検出器を搭載した斜入射平面結像光学系として設計した。マグネシウムL発光(50eV)において最高のエネルギー分解は0.13eVであることを確認した。これは、最近の専用の電子エネルギー損失分光装置に匹敵する。このSXES-SEM装置は、バルクMgおよびLiの純粋金属の状態密度を評価できる。SiウェハのSi-L発光、GaPウェハのP-L発光、及び金属間化合物AlCo, AlPd, Al$$_2$$Pt及びAl$$_2$$AuのAl-L発光において明確なバンド構造効果を観察した。

論文

Anomalous temperature dependence of current-induced torques in CoFeB/MgO heterostructures with Ta-based underlayers

Kim, J.*; Sinha, J.*; 三谷 誠司*; 林 将光*; 高橋 三郎*; 前川 禎通; 山ノ内 路彦*; 大野 英男*

Physical Review B, 89(17), p.174424_1 - 174424_8, 2014/05

 被引用回数:55 パーセンタイル:4.96(Materials Science, Multidisciplinary)

磁気トンネル接合素子に用いられるCoFeB/Mgoヘテロ構造膜の下地に用いられるTa膜の影響を調べた。Ta下地膜は電流による磁化反転に大きな効果を持っていることがわかった。この結果はスピン拡散モデルで解析された。

論文

Acute and obtuse rhombohedrons in the local structures of relaxor ferroelectric Pb(Mg$$_{1/3}$$Nb$$_{2/3}$$)O$$_3$$

Hu, W.*; 林 好一*; 大和田 謙二; Chen, J.*; 八方 直久*; 細川 伸也*; 高橋 正光; Bokov, A.*; Ye, Z.-G*

Physical Review B, 89(14), p.140103_1 - 140103_5, 2014/04

 被引用回数:24 パーセンタイル:16.22(Materials Science, Multidisciplinary)

The local structures around Nb and Pb in the relaxor ferroelectric Pb(Mg$$_{1/3}$$Nb$$_{2/3}$$)O$$_3$$ were investigated by X-ray fluorescence holography. The Pb atomic images around Nb showed a rhombohedral distortion of the crystal unit cells. The Pb-Pb correlated images showed a local structure of body-center-like $$2a_0times 2a_0 times 2a_0$$ superlattice, proving a rigid three-dimensional network structural model combining the two kinds of rhombohedrons. This superstructure and the fluctuating Pb and Nb atoms play an important role in the relaxor behavior of this material.

論文

RI施設における排気中$$^{14}$$Cモニタリング; 捕集及び酸化方法の比較評価

上野 有美; 小嵐 淳; 岩井 保則; 佐藤 淳也; 高橋 照彦; 澤畠 勝紀; 関田 勉; 小林 誠; 角田 昌彦; 菊地 正光

保健物理, 49(1), p.39 - 44, 2014/03

原子力科学研究所第4研究棟(RI施設)では、排気中の$$^{14}$$Cを1か月間連続で捕集し、施設から大気中へ放出される$$^{14}$$Cのモニタリングを行っている。しかし、CuO触媒を600$$^{circ}$$C以上に加熱する必要があることやモノエタノールアミン(MEA)が毒劇物に指定されていることから、管理区域内でのモニタリング手法として改良の余地が残っている。本試験では、異なる捕集剤を用いた捕集法の比較、使用する捕集剤の量とCO$$_{2}$$捕集効率の関係についての検討、異なる酸化触媒の異なる温度条件下における酸化性能の比較を行った。CO$$_{2}$$捕集剤の検討では、MEAに加えて、Carbo-Sorb Eを評価の対象とした。酸化触媒の検討では、CuO触媒に加えて、Ptアルミナ触媒、Pd/ZrO$$_{2}$$触媒を評価の対象とした。試験の結果、Carbo-Sorb Eはガスの通気による気化量が大きく、1か月の連続捕集には適さず、MEAは1か月間を通して安定したCO$$_{2}$$捕集能力があることが確認できた。各触媒の酸化効率を比較した結果、Pd/ZrO$$_{2}$$触媒のCH$$_{4}$$に対する酸化性能が最も優れており、加熱炉の温度を200$$^{circ}$$C以上下げることができ、モニタリングの安全性を向上できる。

論文

Defect characterization in compositionally graded InGaAs layers on GaAs (001) grown by MBE

佐々木 拓生; Norman, A. G.*; Romero, M. J.*; Al-Jassim, M. M.*; 高橋 正光; 小島 信晃*; 大下 祥雄*; 山口 真史*

Physica Status Solidi (C), 10(11), p.1640 - 1643, 2013/11

 被引用回数:3 パーセンタイル:12.82

Defect characterization in compositionally step graded In$$_{x}$$Ga$$_{1-x}$$As layers with different thickness of the overshooting (OS) layer was performed using cathodoluminescence (CL) and transmission electron microscopy (TEM). We found that the type and in-plane distribution of defects generated in the top InGaAs layer grown on step graded layers strongly depend on the thickness of the OS layer. In the thin OS layer, a high density of threading dislocations aligned along [110] was observed. In the thick OS layer, significant line defects associating composition variation were dominantly present. These features on defect type and distribution would relate to strain and configuration of the OS layer.

論文

Real-time observation of crystallographic tilting InGaAs layers on GaAs offcut substrates

西 俊明*; 佐々木 拓生; 池田 和磨*; 鈴木 秀俊*; 高橋 正光; 下村 憲一*; 小島 信晃*; 大下 祥雄*; 山口 真史*

AIP Conference Proceedings 1556, p.14 - 17, 2013/09

 パーセンタイル:100

${it In situ}$ X-ray reciprocal space mapping during In$$_{x}$$Ga$$_{1-x}$$As/GaAs(001) MBE growth is performed to investigate effects of substrate misorientations on crystallographic tilting. It was found that evolution of the crystallographic tilt for the InGaAs films is strongly dependent on both layer structures and substrate misorientations. We discuss these observations in terms of an asymmetric distribution of dislocations.

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