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田村 由起子*; 荒川 勝利*; 竹中 幹人*; 中西 洋平*; 藤波 想*; 柴田 基樹*; 山本 勝宏*; 宮田 登*; 山田 雅子*; 瀬戸 秀紀*; et al.
Polymer, 333, p.128662_1 - 128662_8, 2025/08
被引用回数：0To investigate the relationship between the mechanical properties of silica-filled styrene-butadiene rubber (SBR) and the amount of bound rubber at the filler/rubber interface, the polymer matrix was extracted from silica-filled SBR using toluene at room temperature. In this study, this extraction process was reproduced by leaching a thermally annealed SBR layer deposited on a Si substrate in toluene at room temperature, where the adsorption layer of the SBR was grown at the interface with the substrate by thermal annealing. The SBR adsorption layer on the Si substrate has two-layer structures consisting of an inner and outer adsorption layers, which correspond to the tightly and loosely bound rubbers on the filler surface of the silica-filled SBR, respectively. For the sample annealed for less than 6 h, the outer adsorption layer, loosely bound to the substrate, was easily leached in toluene for 5 min, leaving only the inner adsorption layer on the substrate. For the samples annealed for more than 24 h, a large portion of the outer adsorption layer remained on top of the inner adsorption layer as a terrace structure. However, even for the sample annealed for 24 h, treating with toluene for 24 h completely leached the outer adsorption layer from the inner adsorption layer, although the inner adsorption layer remained on the substrate. It was found that the loosely bound rubber in the silica-filled SBR could be easily extracted from the filler surface, along with the free polymer chains in the polymer matrix during extraction with toluene at room temperature. In contrast, the tightly bound rubber was not leached by toluene at room temperature. This may be because the interfacial polymer chains within approximately 1 nm of the substrate surface were strongly constrained to the substrate, and even toluene molecules were excluded.
田口 美岐*; 宮田 登*; 宮崎 司*; 青木 裕之; Ozawa, Satoru*; 長谷川 龍一 *; 盛満 裕真*; 川口 大輔*; 山本 悟*; 田中 敬二*
Polymer Journal, 7 Pages, 2025/03
被引用回数：0 パーセンタイル：0.00(Polymer Science)Polyrotaxane (PR) exhibits unique mechanical properties due to the ability of its cyclic molecules to move or slide along the axial chain. Thus, to design advanced polymer-based composite materials and organic devices, it is crucial to better understand the aggregation states at the surface and substrate interface in polymer films containing PR. Here, we report the depth profile of PR along the direction normal to the interface when it is mixed with polystyrene (PS). Neutron reflectivity and X-ray photoelectron spectroscopy revealed that PS and PR segregated at the surface and substrate interface, respectively, and that the extent of segregation depended on the length of PS. The surface enrichment of PS is driven by both energy and entropy, whereas the enrichment of PR at the substrate interface is energy driven.
Liu, Y.*; 宮田 登*; 宮崎 司*; 春藤 淳臣*; 川口 大輔*; 田中 敬二*; 青木 裕之
ACS Applied Materials & Interfaces, 8 Pages, 2025/00
The performance of structural adhesives is strongly influenced by the interfacial structure between the adhesive and adherend. In this study, we developed a nanometric stable interfacial layer derived from an epoxy resin system containing excess hardener. This layer, formed on solid substrates, exhibited excellent structural stability, even after extensive solvent washing. Neutron reflectometry (NR) was employed to investigate its structure under both dry and humid conditions, revealing a robust and well-defined interface that suppressed moisture accumulation at the adherend interface. FT-IR spectroscopy confirmed an excess of unreacted amino groups in the adsorbed layer, enabling further curing reactions with freshly applied epoxy resin. Re-coating experiments demonstrated that the adsorbed layer remained intact after thermal curing, suggesting strong interfacial compatibility. Notably, the presence of the adsorbed layer led to a significant enhancement in adhesive performance. Lap shear tests showed that the adhesion strength of the epoxy resin nearly doubled when the adsorbed layer was introduced at the interface. This approach does not rely on external coupling agents or primers, but instead utilizes a homologous material system to tailor interfacial properties through molecular-level design. The strategy presented here offers a practical and scalable method for improving adhesion in epoxy systems. By directly engineering the adhesive interface using components intrinsic to the epoxy formulation, this method enables reliable and enhanced bonding performance without altering the bulk material.
山本 勝宏*; 今井 達也*; 河合 純希*; 伊藤 恵利*; 宮崎 司*; 宮田 登*; 山田 悟史*; 瀬戸 秀紀*; 青木 裕之
ACS Applied Materials & Interfaces, 16(48), p.66782 - 66791, 2024/11
被引用回数：0 パーセンタイル：0.00(Nanoscience & Nanotechnology)In this study, a silicon-based copolymer, poly(tris(trimethylsiloxy)-3-methacryloxypropylsilane)-co-poly(N,N-dimethyl acrylamide), thin film was subjected to plasma surface treatment to make its surface hydrophilic (biocompatible). Neutron reflectivity (NR) measurement of the plasma-treated thin film showed a decrease in the film thickness (etching width: similar to 20 nm) and an increase in the scattering length density (SLD) near the surface (similar to 15 nm). The region with a considerably high SLD adsorbed water (D
O) from its saturated vapor, indicating its superior surface hydrophilicity. Nevertheless of the hydrophilicity, the swelling of the thin film was suppressed. Hard X-ray photoelectron spectroscopy (HAXPES) performed at various takeoff angles revealed that the thin-film surface (similar to 20 nm depth) underwent extensive oxidation. NR and HAXPES analysis quantitatively yielded the depth profiling of elemental compositions in a few tens of nm scale. Si oxidation and hydrogen elimination (probably CH
groups) in the vicinity of the surface region increased the SLD and decreased the hydrophobicity. A combination of Soft X-ray photoelectron spectroscopy and NR measurements revealed the surface chemical composition and mass density. It was considered that the surface near the film was chemically composed close to SiO, forming a gel-like (three-dimensional network) structure that is hydrophilic and suppresses swelling due to moisture, indicating it can be expected to maintain stable hydrophilicity on the film surface.
宮崎 司*; 宮田 登*; 有馬 寛*; 下北 啓輔*; 山本 勝宏*; 竹中 幹人*; 中西 洋平*; 柴田 基樹*; 青木 裕之; 山田 悟史*; et al.
Colloids and Surfaces A; Physicochemical and Engineering Aspects, 701, p.134928_1 - 134928_8, 2024/11
被引用回数：0 パーセンタイル：0.00(Chemistry, Physical)Isotactic polypropylene (PP) thin films deposited on Si substrates were subjected to neutron reflectivity (NR) measurements under various humidity conditions to evaluate the isothermal adsorption of water accumulated between the PP layer and Si substrate, with focus on the temperature-dependence of the adsorption isotherm. The adsorption of accumulated water followed a single type II isotherm according to the Brunauer-Emmett-Teller (BET) classification, regardless of temperature. This can be attributed to the weak interactions between the PP layer and Si substrate, and between the PP layer and water molecules. Hydrophobic PP does not significantly interact with water molecules and the hydrophilic Si surface. Therefore, the interfacial water molecules are simply adsorbed on the native oxide layer on Si via simple interaction between the water molecules and the silicon oxide surface without being affected by the PP layer. Consequently, the adsorption isotherm of the accumulated water follows the single type II adsorption isotherm regardless of temperature, similar to the adsorption isotherm of water simply adsorbed on exposed silica surfaces. These weak interactions of the PP layer with the Si surface and water molecules also lead to fast diffusion kinetics for the accumulated water along the interface.
箕輪 一希*; 渡部 創; 中瀬 正彦*; 高畠 容子; 宮崎 康典; 伴 康俊; 松浦 治明*
Nuclear Instruments and Methods in Physics Research B, 556, p.165496_1 - 165496_6, 2024/11
被引用回数：0 パーセンタイル：0.00(Instruments & Instrumentation)X線吸収端構造(XANES)分析とカラム試験により希土類のアルキルジアミドアミン(ADAAM)含浸吸着材への選択性を考察した。さらに高レベル放射性廃液に含まれるマイナーアクチノイド(MA)の模擬物質として希土類を実験に利用する蓋然性の高さを、ADAAMの窒素原子と希土類イオンの相互作用により証明した。LaとCeはADAAM中のアミンの窒素原子と相互に作用することを証明し、N-K端におけるXANESスペクトルにて検討に供した希土類においてピークシフトが観察されたことから、ソフトな相互作用が希土類の選択性に関与することを明らかにした。また、ADAAM含浸吸着材において希土類の選択性に関する要因はMAのそれと同じであることから、希土類がMAの模擬物質として適していることを示した。
下北 啓輔*; 山本 勝宏*; 宮田 登*; 柴田 基樹*; 中西 洋平*; 荒川 勝利*; 竹中 幹人*; 木田 拓充*; 徳満 勝久*; 田中 亮*; et al.
Langmuir, 40(30), p.15758 - 15766, 2024/07
被引用回数：1 パーセンタイル：0.00(Chemistry, Multidisciplinary)To investigate the structure of the interface between polyethylene films and substrates, the neutron reflectivity (NR) of deuterated polyethylene (dPE) thin films deposited on Si substrates was measured, demonstrating water accumulation at the interface, even under ambient conditions. After leaching the thermally annealed dPE films in hot p-xylene, NR measurements were conducted on the layers remaining on the substrate, clearly revealing that the adsorption layer of dPE grew during annealing and consisted of two layers, an inner adsorption layer and an outer adsorption layer, as previously proposed for amorphous polymers. The inner adsorption layer was approximately 3.7 nm thick with a density comparable to that of the bulk. The outer adsorption layer was several nanometers thick and appeared to grow insufficiently on top of the inner adsorption layer under the annealing conditions examined in this study. This study clarifying the growth of the adsorption layer of polyethylene at the interface with an inorganic substrate is useful for improving the performance of polymer/inorganic filler nanocomposites due to the wide utility of crystalline polyolefins as polymer matrix materials in nanocomposites.
Kawano, Masayuki*; 盛満 裕真*; Liu, Y.*; 宮田 登*; 宮崎 司*; 青木 裕之; 川口 大輔*; 山本 悟*; 田中 敬二*
Macromolecules, 57(14), p.6625 - 6633, 2024/07
被引用回数：0 パーセンタイル：0.00(Polymer Science)A better understanding of the dynamic behavior of polymer chains on solid surfaces is indispensable for the design and construction of high-performance polymer composites. We herein visualized the in-plane movement of isolated poly(methyl methacrylate) (PMMA) and poly(tert-butyl methacrylate) (PtBMA) single chains on hydrophilic silicon wafers under ambient conditions by atomic force microscopy. Isolated PMMA chains adsorbed to the substrate, whereas PtBMA chains diffused, the degree of which was dependent on the humidity. Neutron reflectivity revealed the formation of a layer of condensed water on the substrate. All-atomistic molecular dynamics simulations implied that the diffusivity difference of the two polymers was based on the submerged depth in which a part of a chain existed. That is, the interaction of a polymer with the surface of the hydrophilic substrate primarily governs its lateral movement, or adsorption behavior, facilitated by the presence of water.
岡藤 孝史*; 三浦 一浩*; 佐郷 ひろみ*; 村上 久友*; 渡壁 智祥; 安藤 勝訓; 宮崎 真之
Proceedings of ASME 2024 Pressure Vessels & Piping Conference (PVP 2024) (Internet), 8 Pages, 2024/07
免震システムが適用された高速炉の容器に適用可能な座屈強度評価式の開発を行っている。既往報告において、一定の水平荷重を受けつつ、周期的な軸方向圧縮荷重が作用する条件下での一連の座屈試験と解析を行い、座屈評価式の適用性を確認している。本報告では、大きな初期不整がある場合に座屈強度が低下する効果を取入れるための補正係数を提案した。様々な寸法、初期不整形状、垂直/水平荷重比を有する改良9Cr-1Mo鋼(Grade91)及びオーステナイト系ステンレス鋼の容器に対して、大変形大ひずみ理論による一連の弾塑性座屈解析を実施した。その結果、補正係数は全体的に初期不整の程度に対応して座屈強度が減少する傾向にあり、補正係数を考慮した座屈評価式は肉厚の半分を超える大きな初期不整がある場合でも高速炉の容器に適用できることを示した。
渡壁 智祥; 山本 智彦; 岡村 茂樹; 宮崎 真之; 宮川 高行; 内田 昌人*; 平山 智之*; 杣木 孝裕*; 湯川 正貴*; 深沢 剛司*; et al.
Proceedings of ASME 2024 Pressure Vessels & Piping Conference (PVP 2024) (Internet), 10 Pages, 2024/07
ナトリウム冷却高速炉では、薄肉の機械部品や配管の耐震安全性を厳しい設計地震レベルで確保するため、3次元免震装置を開発している。開発成果の進捗をシリーズ(Part7
Part9)発表する。Part7では、研究開発の全体概要、各要素を組み立てた状態での3次元免震装置の試験計画、および構成要素の性能について紹介する。Part8では、各要素を組み立てた状態での3次元免震装置の性能を負荷試験を通じて調査した。Part9では、試験結果で得た知見に基づき検証した解析モデルによる3次元免震装置の効果を報告する。
中西 洋平*; 柴田 基樹*; 澤田 諭*; 近藤 寛朗*; 元川 竜平; 熊田 高之; 山本 勝宏*; 三田 一樹*; 宮崎 司*; 竹中 幹人*
Polymer, 306, p.127209_1 - 127209_7, 2024/06
被引用回数：2 パーセンタイル：50.19(Polymer Science)Adding silane coupling agents to rubber/silica particles systems improves their mechanical properties and the dispersion of the particles. The improvement is believed to be attributed to the enhanced adsorption of rubber molecules on the surface of silica particles by the silane coupling agent. However, the enhancement of the adsorption by silane coupling agent has not been clarified quantitatively yet. In this study, we have investigated the difference in (i) the adsorption of rubber on silica surfaces and (ii) the aggregation of silica particles in rubber/silica particle systems with and without silane coupling agents by using contrast variation neutron scattering (CV-SANS). The CVSANS results quantitatively clarified the adsorption layer's thickness and the degree of aggregation for both systems. In the case of the system without silane coupling agents, the adsorption layers do not exist around the particles, and the particles tend to aggregate. On the other hand, the adsorption layers of about 5.3 nm are formed on the surface of the particles in the system with silane coupling agents, and the addition of silane coupling agents suppressed the aggregation.
宮崎 加奈子*; 武原 政人*; 蓑毛 健太*; 堀江 憲路*; 竹原 真美*; 山崎 信哉*; 斉藤 拓巳*; 大貫 敏彦*; 高野 公秀; 塩津 弘之; et al.
Journal of Hazardous Materials, 470(15), p.134104_1 - 134104_11, 2024/05
被引用回数：1 パーセンタイル：31.14(Engineering, Environmental)Radioactive Cs contamination has been one of the central issues in Fukushima and other legacy sites; however, atomic-scale characterization of radioactive Cs has never been successful. Here we report, for the first time, the direct imaging of radioactive Cs atoms using high-resolution high-angle annular dark-field scanning transmission electron microscopy. As inclusions in Cs-rich microparticles, 27-36 wt.% of Cs (as CsO) occurs in a type of zeolite called pollucite. The normalized formula for pollucite are expressed as (Cs,K,Ba)
(Fe
,Zn,X
)Si
O
, (Cs,K,Ba)
(Fe
Zn
X
)
Si
O, and (Cs,K,Ba)
(Fe
ZnX
)
Si
O after normalization with 12 oxygen atoms (X includes other trace cations; Ti, Mn, Rb, Zr, Mo, and Sn). Atomic-resolution image of radioactive Cs atoms are obtained when viewing along the [111] zone axis, a view supported by image simulations using the multi-slice method. The occurrence of pollucite indicates that locally enriched Cs reacted with siliceous substances during meltdowns, presumably through hydrothermal reactions. In case of predominant occurrence of pollucite in debris, incorporation in pollucite structure retards leaching of radioactive Cs. Still, the atomic-resolution imaging of radioactive Cs is an important advance for better understanding the fate of radioactive Cs inside and outside of damaged reactors during severe accidents like Fukushima Daiichi.
眞田 幸尚; 阿部 智久; 佐々木 美雪; 菅野 麻里奈*; 山田 勉*; 中曽根 孝政*; 宮崎 信之*; 押切 圭介*; 渡部 浩司*
Journal of Nuclear Science and Technology, 61(5), p.693 - 702, 2024/05
被引用回数：7 パーセンタイル：84.29(Nuclear Science & Technology)主な放射性物質を除去した「処理水」にはトリチウムが含まれており、日本のステークホルダーからはどのように処理するかが議論されている。施設内の処理水の量は限界に達しており、日本政府は、2023年度(年度:年度)までに海に放流することを決定した。本研究では、福島第一原子力発電所(FDNPS)のトリチウム水放出用のシンプルで実用的なトリチウムモニターを開発した。シンプルで実用的なトリチウムモニターは、薄いプラスチックシンチレーターシートに基づくFDNPSトリチウム水放出用に開発された。開発されたデバイスは、標準的なトリチウム溶液と最小検出可能活性を計算する方法を使用して較正された。厚さ0.25mmのシンチレータ15個を0.26Lのフローセルに配置して、サンプル水を供給し、3,200mm
の有効表面積を得ることができる。完全な水でのトリチウム水の効率は0.000035cpsBq
である。単純なシールド条件下で検出可能な最小活性は7,800BqLであった(測定時間は3,600秒であった)。
渡部 創; 高畠 容子; 長谷川 健太; 後藤 一郎*; 宮崎 康典; 渡部 雅之; 佐野 雄一; 竹内 正行
Mechanical Engineering Journal (Internet), 11(2), p.23-00461_1 - 23-00461_10, 2024/04
Japan Atomic Energy Agency is developing extraction chromatography technology to recover MA(III) from spent nuclear fuel. Developments in the extraction chromatography system especially focusing on safety and stable operation are required for practical application of the technology. This paper discusses the main tasks that have to be challenged preferentially based on achievements obtained by previous studies and potential MA(III) recovery process flow.
山本 智彦; 渡壁 智祥; 宮崎 真之; 岡村 茂樹; 宮川 高行; 横井 忍*; 深沢 剛司*; 藤田 聡*
Mechanical Engineering Journal (Internet), 11(2), p.23-00393_1 - 23-00393_21, 2024/04
A sodium-cooled fast reactor (SFR) considers adopting 3-dimensional seismic isolation devices for withstanding seismic loads not only horizontal but also vertical direction. A seismic isolation device consists of a laminated rubber bearing and horizontal oil dampers for horizontal direction, coned disc springs and vertical oil dampers for vertical direction, respectively. In order to investigate the performance of each component and the feasibility of integrated system for SFR, the experiments such as load-displacement tests, vibrating tests, etc., to each component of seismic isolation devices and seismic response analysis are carried out. As those experimental results, the mechanical characteristics of each component and the devices are grasped, then it is demonstrated that components and devices have expected performances to reduce the seismic loading within the design range. As the analytical results of seismic response, it is indicated that this 3-dimesional seismic isolation device and system can reduce the seismic response on horizontal and vertical simultaneously. Based on the analytical studies and experimental results, the feasibility of newly developed 3-dimensional seismic isolation system is obtained and the prospect of practical application of 3D seismic isolation system for fast reactor is implied in this paper.
長谷川 健太; 後藤 一郎*; 宮崎 康典; 安倍 弘; 渡部 創; 渡部 雅之; 佐野 雄一; 竹内 正行
Mechanical Engineering Journal (Internet), 11(2), p.23-00407_1 - 23-00407_8, 2024/04
JAEA has been working on development of extraction chromatography technology for recovery of trivalent minor actinides (MA(III)) from high-level radioactive waste generated in reprocessing of spent fuel. The technology utilizes porous silica particles with about 50 micrometre diameter for support of adsorbents. Pressure drop of the packed column depends on characteristics of the particle. Large pressure drop of the column is not favorable for safety assessment of the technology although a certain level of the pressure drop is indispensable for excellent separation performance. In this study, we applied a granulation technique using a spray dryer that is widely used in industry, and conducted experiments to find the optimal specifications for silica support particles and conditions for the granulation operation. A basic characterization of the adsorbent prepared from the produced particles was carried out by an adsorption test of simulated high level liquid waste.
宮川 晃尚*; 林 直輝*; 岩本 響*; 新井 剛*; 長友 重紀*; 宮崎 康典; 長谷川 健太; 佐野 雄一; 中谷 清治*
Analytical Sciences, 40(2), p.347 - 352, 2024/02
被引用回数：2 パーセンタイル：23.37(Chemistry, Analytical)複数のランタノイドイオンを含む錯体溶液中における単一抽出剤含浸高分子被覆シリカ粒子中のEu(III)分配機構を蛍光顕微分光法を用いて調べた。律速段階はEu(III)と2つの抽出剤分子との反応であった。得られた機構と速度定数は、Eu(III)溶液中でEu(III)が粒子に分配される単元素系の機構と一致した。
O/HO vapor generator for contrast-variation neutron scattering有馬 寛*; 高田 慎一; 笠井 聡*; 大内 啓一*; 森川 利明*; 宮田 登*; 宮崎 司*; 青木 裕之; 岩瀬 裕希*; 廣井 孝介; et al.
Journal of Applied Crystallography, 56(6), p.1802 - 1812, 2023/12
被引用回数：6 パーセンタイル：81.06(Chemistry, Multidisciplinary)The contrast-variation technique in neutron scattering experiments plays a pivotal role in distinguishing partial structures within multi-component complexes, facilitating the elucidation of distinct sample constituents. This differentiation is achieved using different isotopes, namely hydrogen and deuterium, which possess varying neutron scattering characteristics. This study presents a novel vapor generator designed for neutron scattering experiments, enabling continuous control of the DO/HO ratio of the vapor. This feature is especially useful for contrast-variation studies. The generator features two saturators and four mass flow controllers, allowing for the rapid and independent generation of DO/HO vapors. Additionally, the incorporation of the two-temperature method ensures accurate dew point control within a margin of 
0.2
Cdp. This setup proves useful for conducting time-resolved experiments and can accelerate research on functional polymers, such as polymer electrolyte membranes for fuel cells, where water potential assumes critical importance.
柴田 基樹*; 中西 洋平*; 阿部 淳*; 有馬 寛*; 岩瀬 裕希*; 柴山 充弘*; 元川 竜平; 熊田 高之; 高田 慎一; 山本 勝宏*; et al.
Polymer Journal, 55(11), p.1165 - 1170, 2023/11
被引用回数：2 パーセンタイル：17.57(Polymer Science)Marine ecosystem degradation due to micro plastics is a significant environmental problem, as acknowledged by Sustainable Development Goal 14. Decomposition of plastics using near critical or supercritical water is one of the promising methods to reduce micro plastics. To attain the optimization of the method for improving environmental friendliness, it is necessary to clarify the structural change of materials during the process. We, thus, investigated the decomposition processes of polystyrene particles dispersed in deuterated water (DO) during heating under near critical or supercritical conditions by using in situ small-angle neutron scattering. Under subcritical conditions, the PS particles were swollen by DO due to increased compatibility with temperature. Near the critical point in subcritical conditions, the cleavage of PS chains in the particles occurred, so that the swollen ratio was much enhanced though the PS particles kept their shapes. In a supercritical condition, the PS particles were degraded into oil including oligomers or monomers and the phase-separated structures with styrene-rich and DO-rich regions.
宮川 晃尚*; 林 直輝*; 岩本 響*; 新井 剛*; 長友 重紀*; 宮崎 康典; 長谷川 健太; 佐野 雄一; 中谷 清治*
Bulletin of the Chemical Society of Japan, 96(9), p.1019 - 1025, 2023/09
被引用回数：4 パーセンタイル：41.44(Chemistry, Multidisciplinary)本研究では、ニトリロトリアセトアミド(NTA)抽出液を含浸させたポリマーコートシリカ単粒子において、Eu(III)とSm(III)のこれらのイオンを含む溶液中での物質移動機構を明らかにした。質量移動の律速過程は、NO
イオンが関与しないイオンとNTA分子の反応過程であり、これは単一イオン分配系で得られたものと一致した。
