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論文

Ion beam induced luminescence of complexes formed in adsorbent for MA recovery process

渡部 創; 片井 雄也*; 松浦 治明*; 加田 渉*; 江夏 昌志*; 佐藤 隆博*; 新井 剛*

Nuclear Instruments and Methods in Physics Research B, 450, p.61 - 65, 2019/07

Ion-beam induced luminescence (IBIL) analysis on MA recovery adsorbent was performed to give chemical states of complexes formed in the adsorbent as fundamental information for process design, and EXAFS analysis was also carried out to support discussions. The IBIL spectra of the binary extractants system seemed to be superposition of individual ones, however it has also original peaks. As intensities of those peaks rapidly decreased with iteration time of measurements and the original peaks were not observed for the adsorbent without charging Eu(III), they were attributed to complexes of Eu(III) with organic compounds. Contributions of CMPO and HDEHP extractants for Eu(III) extraction must be not only individual ones but also cooperative.

論文

Module design of silica membrane reactor for hydrogen production via thermochemical IS process

Odtsetseg, M.; 田中 伸幸; 野村 幹弘*; 久保 真治

International Journal of Hydrogen Energy, 44(21), p.10207 - 10217, 2019/04

The potential of the silica membrane reactors for use in the decomposition of hydrogen iodide (HI) was investigated by simulation with the aim of producing CO$$_{2}$$-free hydrogen via the thermochemical water-splitting iodine-sulfur process. Simulation model validation was done using the data derived from an experimental membrane reactor. The simulated results showed good agreement with the experimental findings. The important process parameters determining the performance of the membrane reactor used for HI decomposition, namely, reaction temperature, total pressures on both the feed side and the permeate side, and HI feed flow rate were investigated theoretically by means of a simulation. It was found that the conversion of HI decomposition can be improved by up to four times (80%) or greater than the equilibrium conversion (20%) at 400$$^{circ}$$C by employing a membrane reactor equipped with a tubular silica membrane. The features to design the membrane reactor module for HI decomposition of thermochemical iodine-sulfur process were discussed under a wide range of operation conditions by evaluating the relationship between HI conversion and number of membrane tubes.

論文

Influences of pore and particle sizes of CMPO/SiO$$_{2}$$-P adsorbent on extraction chromatography process

渡部 創; 佐野 雄一; 三田 修平*; 桜井 翔太*; 新井 剛*

日本イオン交換学会誌, 30(1), p.8 - 16, 2019/01

In order to optimize operability of the adsorbents in the extraction chromatography system and to enhance the performance of the adsorbent, CMPO/SiO$$_{2}$$-P adsorbents with various pore and particle sizes were prepared, and characteristics of the adsorbents were evaluated through distribution coefficient, adsorption isotherm, adsorption rate, and breakthrough/elution behavior. Adsorption capacity was dominated not by the structure of the adsorbent but by amount of the extractant impregnated. The adsorbent with the largest pore size were revealed to show quick elution with short tail. Enlargement in the pore size must be one of the most effective improvements of the adsorbents to enhance the adsorption/elution performance. Adsorbent with particle size of more than 200 $$mu$$m formed channeling or voids inside the bed. They are suspected to lead slow adsorption/elution behavior, and smaller adsorbents must be desirable in the respect of performance of the column.

論文

Hydrogen production tests by hydrogen iodide decomposition membrane reactor equipped with silica-based ceramics membrane

Odtsetseg, M.; 田中 伸幸; 野村 幹弘*; 久保 真治

International Journal of Hydrogen Energy, 42(49), p.29091 - 29100, 2017/12

 被引用回数:2 パーセンタイル:76.91(Chemistry, Physical)

熱化学水素製造法ISプロセスにおいて水素生成する反応であるHI分解反応の分解率を向上させるため、水素分離膜を用いた膜反応器の適用を検討している。本研究では、高性能な水素分離膜を開発するため、HTMOSをシリカ源に用い$$alpha$$-アルミナ基材上に対向拡散CVD法を用いて製膜したシリカ膜の性能を調べた。$$alpha$$-アルミナに直接製膜した膜よりも$$gamma$$-アルミナをコーティングした$$alpha$$-アルミナ基材上に製膜した膜の方が、高い水素透過性を示すこと、および、450$$^{circ}$$Cの製膜条件で高い水素選択性ならびに水素透過性が得られることを見い出した。さらに、製膜した膜を適用した膜反応器において、HI分解反応を行い、平衡分解率(20%)を超える0.48の水素転化率を得ることができた。

論文

Microanalysis of silica-based adsorbent for effective recovery of radioactive elements

佐野 雄一; 渡部 創; 松浦 治明*; 名越 航平*; 新井 剛*

Journal of Nuclear Science and Technology, 54(10), p.1058 - 1064, 2017/10

 パーセンタイル:100(Nuclear Science & Technology)

ポリマー架橋度が吸着材の吸着・溶離性能に与える影響についてポリマー架橋度をパラメータとした吸着材を用いた試験により評価するとともに、その要因をSTXM分析及びEXAFS分析により考察した。吸着材中に形成された金属錯体構造については、ポリマー架橋度により大きな違いは生じないことを確認した。一方、ポリマー架橋度の増加に伴いポリマーは細孔中に均一に広がる様子が認められるとともに、架橋度が高い条件では細孔が狭小化し、水分子が捕捉されやすくなるため、溶離率が低下するものと考えられた。

論文

Local structure and distribution of remaining elements inside extraction chromatography adsorbents

渡部 創; 佐野 雄一; 塩飽 秀啓; 矢板 毅; 大野 真平*; 新井 剛*; 松浦 治明*; 江夏 昌志*; 佐藤 隆博*

Nuclear Instruments and Methods in Physics Research B, 404, p.202 - 206, 2017/08

 パーセンタイル:100(Instruments & Instrumentation)

Extraction chromatography is one of the most promising technology for minor actinide (MA(III): Am and Cm) recovery from high level liquid waste generated in the reprocessing. A brand-new adsorbent proposed by our group are expected to achieve more efficient MA(III) recovery than usual procedure. Fundamental MA(III) adsorption/elution performances of the adsorbents have been demonstrated. An appropriate washing process of lanthanides (Ln(III)) is necessary to be established to design a process flow. In this study, chemical state and distribution of Eu inside the adsorbent before and after contacting with candidate eluents for MA(III) or Ln(III) were evaluated by EXAFS measurements and micro-PIXE analysis, respectively. Two-dimensional PIXE images showed that adsorbed Eu and residual Eu after contacting with the eluents for MA(III) were uniformly distributed on the particle. However, EXAFS oscillation revealed that local structure around Eu drastically changes by the contact. Those results suggest that the Eu remained inside the particle without distinct shift and that they form various complexes with extractants in the particle.

論文

Microscopic analyses of complexes formed in adsorbent for Mo and Zr separation chromatography

安倍 諒治*; 名越 航平*; 新井 剛*; 渡部 創; 佐野 雄一; 松浦 治明*; 高木 秀彰*; 清水 伸隆*; 江夏 昌志*; 佐藤 隆博*

Nuclear Instruments and Methods in Physics Research B, 404, p.173 - 178, 2017/08

 パーセンタイル:100(Instruments & Instrumentation)

Molybdenum and zirconium obstruct the efficient recovery of minor actinides (MA(III): Am(III) and Cm(III)) by extraction chromatography; hence, the removal of these elements prior to MA(III) recovery is desirable. The use of an adsorbent impregnated with bis(2-ethylhexyl) hydrogen phosphate (HDEHP) for Mo and Zr decontamination was evaluated in this report. The adsorption/elution and column separation experiments showed that Mo and Zr in the simulated HLLW were selectively adsorbed on the particles, and that Mo was eluted by H$$_{2}$$O$$_{2}$$. EXAFS analysis and SAXS patterns of the adsorbent containing Zr revealed that the Zr-HDEHP complex had a crystal-like periodic structure similar to the structure of the precipitate produced in the solvent extraction system. Micro-PIXE analysis revealed that distribution of the residual Zr on the adsorbent was uniform.

論文

抽出クロマトグラフィーに用いる含浸吸着材への表面処理が吸着・溶離挙動に及ぼす影響

名越 航平*; 新井 剛*; 渡部 創; 佐野 雄一; 竹内 正行; 佐藤 睦*; 及川 博史*

日本イオン交換学会誌, 28(1), p.11 - 18, 2017/01

抽出クロマトグラフィーによる高レベル放射性廃液からのマイナーアクチノイド分離回収プロセスへの適用が期待される含浸吸着材の改良を目的として、含浸吸着材の基体として用いる多孔質シリカ粒子に種々の表面処理を施すことで表面極性を変化させたTODGA含浸吸着材を作製し、硝酸水溶液中におけるNdの吸着溶離挙動を評価した。多孔質シリカ粒子の表面極性を変化させることで吸着分配係数、吸着速度、溶離性能のいずれも顕著に変化することを確認した。

論文

Electroplating of Ni microstructures on the cross section of Cu wire using PMMA mother fabricated by proton beam writing

田邊 祐介*; 岩本 隆志*; 高橋 潤一*; 西川 宏之*; 佐藤 隆博; 石井 保行; 神谷 富裕

JAEA-Review 2012-046, JAEA Takasaki Annual Report 2011, P. 129, 2013/01

In this study, the Ni microstructures were attempted to be fabricated on a distal surface of Cu wires with a diameter of 1.0 mm aiming at the use for imprint lithography. Firstly a PMMA master block was fabricated on the distal surface by exposing PB with beam size of 1.1 $$mu$$m at 3.0 MeV and developing it by IPA-water for electroplating. The master block was composed of the 4-$$mu$$m wide lines with pitches of 25 $$mu$$m and depths of 20 $$mu$$m. Secondly the electroplating was performed on the PMMA master block using a nickel sulfamate bath. Thirdly the electroplated Ni surface was mechanically polished easily to remove PMMA by smoothing its surface. Finally, the Ni microstructures with 20.5 $$mu$$m were fabricated by removing the PMMA after polishing. We additionally performed UV imprint lithography of the photosensitive polymer using the Ni microstructures as a mold. The observation result of SEM images of Ni microstructures and UV imprinted grooves showed that their imprinted grooves were successfully transferred by way of the Ni microstructures from the PMMA master block using the combination of the electroplating and imprinting.

論文

Visualization of focused proton beam dose distribution by atomic force microscopy using blended polymer films based on polyacrylic acid

大道 正明*; 高野 勝昌*; 佐藤 隆博; 神谷 富裕; 石井 保行; 大久保 猛; 江夏 昌志; 加田 渉; 杉本 雅樹; 西川 宏之*; et al.

Journal of Nanoscience and Nanotechnology, 12, p.7401 - 7404, 2012/09

 被引用回数:2 パーセンタイル:84.67(Chemistry, Multidisciplinary)

A new visualization method for dose distribution of a focused proton beam in sub-micrometer scale was developed using a formation of a bulky cross-linked structure of polyacrylic acid -$$N$$, $$N$$'-methylence bisacrylamide, blend film. The areas irradiated by the focused proton beam were swelled on the film. The height of the swelling was significantly increased according to the beam fluence and the increase of containing ratio of the methylence bisacrylamide. The height was saturated at the fluence of 5$$times$$10$$^5$$ ions/$$mu$$m$$^{2}$$. The proton beam-sensitive polymer film was used for the analysis of dose distribution on its surface. The irradiated surface was observed by employing an atomic force microscope. This observation result showed that the method could be used to confirm the writing patterns and the beam-spot shape. Nanostructures with a crescent shape are visualized clearly at a misaligned beam-spot shape in the set up of the beam-optics.

論文

3D micro-fabrication utilized superimposing technique with focused MeV ion beams

高野 勝昌*; 佐藤 隆博; 神谷 富裕; 石井 保行; 大久保 猛; 江夏 昌志; 加田 渉; 杉本 雅樹; 関 修平*; 西川 宏之*

JAEA-Review 2011-043, JAEA Takasaki Annual Report 2010, P. 162, 2012/01

A unique micro-processing technique for epoxy resin films has been developed at the TIARA, utilizing the ion beam writing with multiple energies of light and heavy ion beams. In this study, nano-wire structure fabrication was tried by a superimposing with the proton beams and 520 MeV $$^{40}$$Ar$$^{14+}$$. And in order to reduce the surface tension in developing and drying processes, after a baking at 95 $$^{circ}$$C for 1 minute, developing and drying was performed with super-critical CO$$_{2}$$ at 12 MPa, 40 $$^{circ}$$C. As the result, the bridge structure which strung the wires fabricated by 520 MeV $$^{40}$$Ar$$^{14+}$$ hitting can be observed at the aimed points.

論文

Electroforming of Ni mold using high-aspect-ratio PMMA microstructures fabricated by proton beam writing

田邊 祐介*; 西川 宏之*; 佐藤 隆博; 石井 保行; 神谷 富裕

JAEA-Review 2011-043, JAEA Takasaki Annual Report 2010, P. 163, 2012/01

We report on Ni electroforming using high-aspect-ratio PMMA microstructures by Proton Beam Writing (PBW). There are several issues to be addressed in the fabrication process of Ni molds with a high-aspect-ratio using the PMMA microstructures. First, the residual PMMA was observed on the sidewall of PMMA master block by increasing the thickness of its master block. Second, the small voids were formed in the Ni molds when the high-aspect ratio PMMA master blocks were used. These problems ware resolved using the PMMA master blocks fabricated by PBW on the condition of the higher dose exposure than ordinal one and using a seed layer of a 600-$$mu$$m thick Cu substrate evaporated on the Si substrate before spin-coating the PMMA film. The 30-$$mu$$m PMMA master block with the aspect ratio of 30 was successfully fabricated using the above procedures. Using this PMMA master block, the Ni mold with 30-$$mu$$m thick on the Cu substrate was successfully electroformed without voids from the observation of the cross section revealed by a FIB. Furthermore, a Ni mold with grids and circle patterns was also successfully fabricated using a 15-$$mu$$m thick PMMA film spin-coated on a Cu substrate. The result of the thermal imprint using the Ni mold demonstrated that the high aspect structure was transferred on a PMMA film without damages of the Ni mold even after many trials.

論文

Optimizing composition of TODGA/SiO$$_{2}$$-P adsorbent for extraction chromatography process

渡部 創; 新井 剛*; 小川 剛*; 瀧澤 真*; 佐野 恭平*; 野村 和則; 駒 義和

Procedia Chemistry, 7, p.411 - 417, 2012/00

 被引用回数:5 パーセンタイル:7.57

As a part of developing extraction chromatography technology for minor actinides (MA(III); Am and Cm) recovery from spent fast reactor fuels, improvement on the TODGA/SiO$$_{2}$$-P adsorbent to enhance its desorption efficiency was carried out. Batchwise adsorption/elution experiments revealed that 20wt% of the adsorbent concentration impregnated and 10% of cross linkage of polymer gave better desorption ratio than the reference adsorbent. Inactive column separation experiments with the simulated high level liquid waste and the optimized adsorbent revealed that decontamination factors of fission products can also be improved as well as the recovery yields.

論文

Microbeam complex at TIARA; Technologies to meet a wide range of applications

神谷 富裕; 高野 勝昌; 佐藤 隆博; 石井 保行; 西川 宏之*; 関 修平*; 杉本 雅樹; 奥村 進; 福田 光宏*

Nuclear Instruments and Methods in Physics Research B, 269(20), p.2184 - 2188, 2011/10

 被引用回数:10 パーセンタイル:27.41(Instruments & Instrumentation)

In order to meet wide variety of ion beam applications, three different types of ion microbeam systems were developed. These systems have shown the spatial resolutions of less than 1 $$mu$$m and have made it possible to irradiate minute targets or areas with positioning accuracies of less than 1 $$mu$$m. For micro-analyses, an in-air micro-PIXE system was originally developed on the light ion microbeam system. For micro-fabrication, technique of mask-less ion beam lithography was developed on the light-ion microbeam and other systems. Single-ion-hit technique was also realized to study single-event phenomena in semiconductors or biological cells induced by high-energetic heavy particles. On the other hand, the qualities of the beam from accelerators were important, such as stability of the intensity and the energy of the beams. In this paper, the latest progress and a future prospect of them were discussed.

論文

Electroforming of Ni mold for imprint lithography using high-aspect-ratio PMMA microstructures fabricated by proton beam writing

田邊 祐介*; 西川 宏之*; 関 佳裕*; 佐藤 隆博; 石井 保行; 神谷 富裕; 渡辺 徹*; 関口 淳*

Microelectronic Engineering, 88(8), p.2145 - 2148, 2011/08

 被引用回数:6 パーセンタイル:54.54(Engineering, Electrical & Electronic)

Proton Beam Writing (PBW) is a direct-write technique using focused MeV proton beams. Electroforming Ni molds with high-aspect-ratio are developed for imprint lithography using master blocks of PMMA micro-structures fabricated by PBW. In this development, two problems happened as follows; the master blocks with unmelted PMMA remaining into the PMMA micro-structure in the etching process after PBW and the Ni molds with defectively transcriptional structures electroformed on the clear master blocks of its PMMA micro-structure. In this report, the two relations between the PMMA structures and the etching process and between their structures and the electroforming process were individually studied to solve the problems. In the conference, we will present the two problems, the several researches for their solutions and the trial production results of the electroforming Ni molds using the master blocks of the high-aspect-ratio PMMA micro-structures fabricated by PBW.

論文

Soft-lithographic methods for the fabrication of dielectrophoretic devices using molds by proton beam writing

椎根 康晴*; 西川 宏之*; 古田 祐介*; 金光 薫*; 佐藤 隆博; 石井 保行; 神谷 富裕; 中尾 亮太*; 内田 諭*

Microelectronic Engineering, 87(5-8), p.835 - 838, 2010/05

 被引用回数:4 パーセンタイル:63.67(Engineering, Electrical & Electronic)

Proton Beam Writing (PBW) is a direct writing process using a MeV focused proton beam. The previous performance examinations of the dielectrophoretic (DEP) devices, the high-aspect-ratio micro-structures with the pillar arrays and the fluidic channels fabricated by PBW, showed that spatially modulated electric fields were effective for trapping Escherichia coli. The reproduction of the DEP device using PBW only is, however, unsuitable because it takes a lot of time to fabricate complicated and large area structures. In this study, the fabrication technique of the micro fluidic channel, combining a soft lithography and PBW techniques, was introduced to improve the productivity of the DEP devices. The prototypes of DEP deceives including SU-8 high-aspect-ratio pillar arrays in the micro fluidic channel were developed using the fabrication technique. Especially the pillar arrays in these devices were produced by 1.0 or 1.7 MeV proton beams focused around 1 $$mu$$m in diameter. The observation of the DEP devices using an optical microscope image showed that the pillar arrays were successfully included in the micro fluidic channel. The prototyping capability of PBW combined with the soft lithography technique was highlighted by increasing the productivity of the DEP devices.

論文

Fabrication of nanowires by varying energy microbeam lithography using heavy ions at the TIARA

神谷 富裕; 高野 勝昌; 石井 保行; 佐藤 隆博; 及川 将一*; 大久保 猛; 芳賀 潤二*; 西川 宏之*; 古田 祐介*; 打矢 直之*; et al.

Nuclear Instruments and Methods in Physics Research B, 267(12-13), p.2317 - 2320, 2009/06

 被引用回数:5 パーセンタイル:56.05(Instruments & Instrumentation)

In TIARA facility of Japan Atomic Energy Agency (JAEA) Takasaki, three-dimensional micro/nano structures with high aspect ratio based on cross linking process in negative resist such as SU-8 have been produced by a technique of mask less ion beam lithography. By bombarding high-energy heavy ions such as 450 MeV Xe$$^{23+}$$ to SU-8, a nanowire could be produced just with a single ion hitting. Then we tried to produce nanowires, of which both ends were fixed in the three-dimensional structure. This paper shows a preliminary experiment using a combination of 15 MeV Ni$$^{4+}$$ ion microbeam patterning and the 450 MeV $$^{129}$$Xe$$^{23+}$$ hitting on SU-8.

論文

Development of micromachining technology in ion microbeam system at TIARA, JAEA

神谷 富裕; 西川 宏之*; 佐藤 隆博; 芳賀 潤二; 及川 将一*; 石井 保行; 大久保 猛; 打矢 直之; 古田 祐介*

Applied Radiation and Isotopes, 67(3), p.488 - 491, 2009/03

 被引用回数:4 パーセンタイル:62.73(Chemistry, Inorganic & Nuclear)

原子力機構高崎量子応用研究所のイオン加速器施設(TIARA)のマイクロビームにおいて、芝浦工業大学との共同研究で、マスクレスイオンビームリソグラフィ技術の開発が進められている。マイクロビームサイズ評価とレンズ系の最適化、又は空間分解能として最小100nmのレベルの高空間分解能の測定手段を確立するために、開発している加工技術自身と電鋳技術との組合せにより二次電子マッピングに使用する標準試料としてNiレリーフパターンを作成した。本発表ではこの標準試料を用いて、100nmレベルの最小のビームサイズを測定することができたことを述べるとともに、その試料中をイオンが透過する際の散乱効果が測定結果に与える影響をモンテカルロシミュレーションコードを使用して評価した結果について報告する。

口頭

集束イオンビーム描画によるレジスト材料のマイクロマシニング

打矢 直之*; 原田 卓弥*; 村井 将人*; 西川 宏之*; 芳賀 潤二; 佐藤 隆博; 及川 将一*; 酒井 卓郎; 石井 保行; 福田 光宏*; et al.

no journal, , 

レジスト材料の露光には一般にX線,EUV,電子線等の描画媒体が用いられているが、これらの描画媒体は物質中での原子及び電子との散乱のため、物質深部での加工性が極めて悪い。一方、MeV領域集束プロトンビームは、従来の媒体に比べて物質中での横方向への散乱が少なく、直進性が良いため、従来の媒体では製作が困難であった十$$mu$$を超える加工厚に適しており、高アスペクト比を有する3D構造体の形成が可能である。本研究ではポジ型レジスト(PMMA)及びネガ型レジスト(SU-8)へのMeV領域プロトンビーム照射により描画実験を行い、有機溶剤によるエッチング、すなわち現像を行うことで3D構造体を作製した。さらに、この構造の形状観察を走査型電子顕微鏡(SEM)を用いて行い、加工精度に関する評価を行った。この評価により高アスペクト比を有する3D構造体の製作に成功していることが確認できたので、結果をシンポジウムで報告する。

口頭

集束プロトンビーム描画による3次元構造体の作製

古田 祐介*; 打矢 直之*; 西川 宏之*; 芳賀 潤二; 及川 将一*; 佐藤 隆博; 石井 保行; 神谷 富裕

no journal, , 

有機物への自由度の高い微細加工を可能とするため、マイクロからサブマイクロメートル径の高エネルギー集束プロトンビームを用いた直接描画(PBW)技術の研究開発を進めている。この高エネルギー集束プロトンビームは従来技術の電子線に比べ横方向の散乱が少なく、物質中での飛程をビームエネルギーにより制御できるため、高アスペクト比の3D有機物構造体の製作に適している。この3次元有機物構造体製作における深さ制御技術の開発のため、ネガ型レジスト(SU-8)への高エネルギープロトンマイクロビーム照射を、レンジシフターによる飛程制御及びビームエネルギー可変による飛程制御を行った後、現像し、2種類の3次元有機物構造体を作製した。これらの構造体における深さの制御性は走査型電子顕微鏡(SEM)を用いた観察により行い、二つとも設計した3D図形をマイクロメートル級の精度で有機物に忠実に転写できることがわかった。今回の講演ではこれらの3次元有機物構造体の製作とSEM像観察に基づく深さ制御の評価について発表するとともに、今回使用した材料以外でのPBW技術使用による3次元構造体の製作の可能性についても言及する。

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