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Structural changes of polystyrene particles in subcritical and supercritical water revealed by in situ small-angle neutron scattering

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:0 パーセンタイル:56.45(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 (D$$_{2}$$O) 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 D$$_{2}$$O 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 D$$_{2}$$O-rich regions.


Preparation, characterization, and dilute solution properties of four-branched cage-shaped poly(ethylene oxide)

野田 昂志*; 土肥 侑也*; 太田 豊*; 高田 慎一; 高野 敦志*; 松下 裕秀*

Journal of Polymer Science, 58(15), p.2098 - 2107, 2020/08

A four-branched cage-shaped poly(ethylene oxide) (4C-PEO) was prepared by a coupling reaction at very dilute condition between two kinds of end-functional four-armed star-shaped PEOs having amino and $$N$$-hydroxysuccinimide groups on their four ends, followed by purification using $$alpha$$-cyclodextrin ($$alpha$$-CD). The raw coupling reaction product shows multiple peaks including various high molecular weight multimeric products in size-exclusion chromatography measurements, while the product after $$alpha$$-CD purification shows a single peak eluted slightly earlier than the precursor star PEOs. These results suggest that the targeted 4C-PEO polymer was successfully isolated through the $$alpha$$-CD purification. Small-angle neutron scattering (SANS) measurements of the final product in dilute solution were conducted, and its chain conformation was evaluated from the scattering profile in comparison with linear and star polymers.


Chain dynamics in spin-coated films of poly(methyl methacrylate) in a solvent annealing process

青木 裕之

Polymer Journal, 51(6), p.611 - 616, 2019/06

 被引用回数:5 パーセンタイル:20.76(Polymer Science)

The dynamics of poly(methyl methacrylate) chains in spin-coating films during solvent annealing was studied. The neutron reflectometry (NR) measurement revealed that the absorbed solvent molecules homogeneously distributed in the spin-coated film and the solvent fraction increased to 0.35 in toluene vapor. From the real-time NR measurement for a stacked film of deuterated and hydrogenated PMMA in thermal annealing, the diffusion dynamics of the PMMA chain is strongly dependent on the distance from the surface: the polymer chain at the substrate is restricted. On the other hand, the depth dependence of the chain dynamics was weak in the spin-coated film in a solvent annealing process. Whereas the ratio of the diffusion constants of the PMMA chain at the surface and substrate was 50 in thermal annealing, that in toluene vapor was as small as 2. Therefore, the solvent annealing provide sufficient mobility to the polymer chain near the substrate. This result indicates that the solvent annealing method enables the equilibration of a spin-coated polymer film from the surface to the substrate interface.


Molecular dynamics simulation of telomeric single-stranded DNA and POT1

冠城 雅晃; 山田 寛尚*; 宮川 毅*; 森河 良太*; 高須 昌子*; 加藤 宝光*; 上坂 充*

Polymer Journal, 48(2), p.189 - 195, 2016/02


 被引用回数:5 パーセンタイル:19(Polymer Science)



Combining small-angle and intermediate-angle neutron scattering to study the hierarchical structure in microbial cellulose

Zhao, Y.; 小泉 智

European Polymer Journal, 66, p.437 - 443, 2015/05

 被引用回数:2 パーセンタイル:6.74(Polymer Science)

In this study, we employed intermediate angle neutron scattering (IANS) technique to correct the small angle neutron scattering (SANS) data of the water-swollen microbial cellulose (MC) sample, the system of which has a significant incoherent contribution from the water solvent, and we described the effects that the corrections have on the structural analysis. In order to elucidate the structure efficiently, the solvent was exchanged in situ between protonated water and deuterated water to give different scattering contrasts, and the water-exchange processes were followed by time-resolved SANS and IANS simultaneously. Our results showed that: (1) after incoherent correction, the microstructure of MC sample was proved to be invariant with solvents; (2) the scattering intensity depended only on the contrast factor, revealing a two-phase system composed of waterresistant crystalline cellulose phase and hydrated amorphous phase; (3) the cellulosecrystallites have a constant scattering length density of 2.0$$times$$10$$^{10}$$ cm$$^{-2}$$, determined by the matching point at which the scattering contrast between the two phases is minimum. This value was consistent with that of 1.9$$times$$10$$^{10}$$ cm$$^{-2}$$ estimated from its chemical structure.


Pulse radiolysis study on a highly sensitive chlorinated resist ZEP520A

保坂 勇志*; 大山 智子; 大島 明博*; 榎本 智至*; 鷲尾 方一*; 田川 精一*

Journal of Photopolymer Science and Technology, 26(6), p.745 - 750, 2013/12

 被引用回数:11 パーセンタイル:35.17(Polymer Science)



Nanoscale structures of radiation-grafted polymer electrolyte membranes investigated via a small-angle neutron scattering technique

澤田 真一; 山口 大輔; Putra, A.; 小泉 智*; 前川 康成

Polymer Journal, 45(8), p.797 - 801, 2013/08

 被引用回数:9 パーセンタイル:32.31(Polymer Science)



Effects of crosslinker density on the polymer network structure in poly-$$N$$,$$N$$-dimethylacrylamide hydrogels

深澤 倫子*; 池田 尚弘*; 田畑 麻友*; 服部 正孝*; 相澤 守*; 柚木 俊二*; 関根 由莉奈

Journal of Polymer Science, Part B; Polymer Physics, 51(13), p.1017 - 1027, 2013/07

 被引用回数:32 パーセンタイル:74.42(Polymer Science)

To investigate the effects of crosslinker density on the properties of hydrogels, compression tests, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and Raman measurements were performed on poly-$$N$$,$$N$$-dimethylacrylamide hydrogels. The results of the compression tests showed that the Young's modulus increases as the crosslinker density increases. In addition, the results suggest that the bound water plays an important role in strengthening the hydrogel. The water structure may be one of the dominant factors governing the chemical and physical properties of hydrogels.


Effect of partial delignification of kenaf bast fibers for radiation graft copolymerization

Mohamed, N. H.*; 玉田 正男; 植木 悠二; 瀬古 典明

Journal of Applied Polymer Science, 127(4), p.2891 - 2895, 2013/02

 被引用回数:12 パーセンタイル:38.01(Polymer Science)



$$gamma$$-ray irradiated organic thin film transistors based on perfluoropentacene with polyimide gate insulator

高柳 佑太郎*; 大内 啓邦*; Duan, Z.*; 奥川 孝紀*; 柳 雄一郎*; 吉田 哲*; 田口 光正; 平尾 敏雄; 西岡 泰城*

Journal of Photopolymer Science and Technology, 25(4), p.493 - 496, 2012/08

 被引用回数:0 パーセンタイル:0.01(Polymer Science)



Microprocessing of arched bridge structures with epoxy resin by proton beam writing

高野 勝昌*; 麻野 敦資*; 前吉 雄太*; 丸井 裕美*; 大道 正明*; 佐伯 昭紀*; 関 修平*; 佐藤 隆博; 石井 保行; 神谷 富裕; et al.

Journal of Photopolymer Science and Technology, 25(1), p.43 - 46, 2012/07

 被引用回数:2 パーセンタイル:6.61(Polymer Science)

The proton beam writing (PBW) with energy of several MeV ranges is a unique tool of three-dimensional microprocessing for a polymer material. Three-dimensional structures like a bridge structure can be fabricated by the double exposures of PBW with two deferent energies followed by the one-time development using etching solution. In this study, the fabrication of an arched bridge was attempted by means of the supercritical drying with liquid carbon dioxide to a SU-8 photoresist film, as the polymer material, coated on a substrate of epoxy sheet, after the PBW process. In the exposures, two patterns of bridge girders and piers were written with 0.5 and 3 MeV proton beams to the SU-8 photoresist films, respectively. After these writings, the photoresist films were developed with the solution of diacetone alcohol and rinsed with the solution of isopropyl alcohol. Then the supercritical drying with liquid carbon dioxide was used at 12 MPa, 40$$^{circ}$$C. As the results, the bridge structures with curved girders to the vertical direction were formed due to the swelling effect of the photoresist film on the drying. In the conference, the microprocessing method of the bridge structure and the swelling effect of the photoresist film will be represented in detail.


Surface modification of vulcanized rubber by radiation grafting, 2; Improvement in performance of wiper rubber

溝手 範人*; 片貝 秋雄; 玉田 正男

Journal of Applied Polymer Science, 123(4), p.2172 - 2176, 2012/02

 被引用回数:4 パーセンタイル:13.49(Polymer Science)



Structure and dynamics of poly(vinyl alcohol) gels in mixtures of dimethyl sulfoxide and water

金谷 利治*; 高橋 伸明; 竹下 宏樹*; 大倉 正敏*; 西田 幸次*; 梶 慶輔*

Polymer Journal, 44(1), p.83 - 94, 2012/01

 被引用回数:25 パーセンタイル:67.11(Polymer Science)

We review our structure studies on poly(vinyl alcohol) (PVA) gels formed in mixtures of dimethyl sulfoxide (DMSO) and water using various scattering methods including wide-, small- and ultra small-angle neutron scattering and light scattering. These studies revealed the hierarchic structure of PVA gels formed in DMSO/water (60/40 v/v) in a very wide spatial scale from 1 ${AA}$ to several micron: the crosslinking points are crystallites with radius of $$sim$$70 ${AA}$, the distance between the neighboring crystallites is 180-200 ${AA}$, and the bicontinuous structure due to liquid-liquid phase separation is in mm scale. We also review our dynamic studies on three kinds of PVA gels in nm scale using neutron spin echo technique to separate the concentration fluctuations observed by small-angle neutron scattering into the static and dynamics contributions.


Thermoresponsive extraction of cadmium(II) ions by poly(TPEN-NIPA) gels; Effect of chain length and branched spacer structure on gel formation and extraction behavior

稲葉 優介*; 津曲 貴幸*; 喜田 達也*; 渡部 渉*; 中島 靖隆*; 福岡 佐千緒*; 森 敦紀*; 松村 達郎; 中野 義夫*; 竹下 健二*

Polymer Journal, 43(7), p.630 - 634, 2011/07

 被引用回数:11 パーセンタイル:35.66(Polymer Science)

重合可能な二重結合を持つ官能基をピリジン環に結合させた${it N,N,N',N'}$-(tetrakis-2-pyridylmethyl)ethylenediamine (TPEN)の誘導体を合成し、重合開始剤としてazobisisobutyronitrile (AIBN)を使用して${it N}$-isopropylacrylamide (NIPA)との共重合を試みた。得られたTPEN-NIPA重合ゲルは、膨潤/収縮挙動に温度応答性が認められ、さらに抽出剤であるTPENの性能が発揮され水溶液中のカドミウム(II)イオンを抽出可能であった。重合ゲルは、側鎖にpropyl基, butyl基, decyl基及びisopropyl基を持つTPEN誘導体を用意して重合した。これらについて、カドミウムイオン抽出の温度依存性を比較した。これらのゲルによる水溶液中のカドミウム(II)イオン抽出は、膨潤状態である5$$^{circ}$$Cにおいて効率が高く、収縮状態である45$$^{circ}$$Cでは、ほとんど抽出されなかった。また、側鎖にisopropyl基を持つTPEN誘導体による重合ゲルが、抽出性能の高い温度応答性を有することを見いだした。


The Static structure of polyrotaxane in solution investigated by contrast variation small-angle neutron scattering

遠藤 仁; 眞弓 皓一*; 大坂 昇*; 伊藤 耕三*; 柴山 充弘*

Polymer Journal, 43(2), p.155 - 163, 2011/02

 被引用回数:7 パーセンタイル:27(Polymer Science)



Preirradiation graft polymerization of styrene in a poly(tetrafluoroethylene) film investigated by time-resolved small-angle neutron scattering

岩瀬 裕希*; 澤田 真一; 八巻 徹也; 前川 康成; 小泉 智

International Journal of Polymer Science, 2011(2011), p.301807_1 - 301807_7, 2011/00

 被引用回数:11 パーセンタイル:38.33(Polymer Science)



Micro-fabrication of biodegradable polymers using focused ion beam

大久保 聡*; 高橋 朋宏*; 高澤 侑也*; 五輪 智子*; 佐々木 隆*; 長澤 尚胤; 玉田 正男; 大島 明博*; 田川 精一*; 鷲尾 方一*

Journal of Photopolymer Science and Technology, 23(3), p.393 - 397, 2010/11

 被引用回数:4 パーセンタイル:13.86(Polymer Science)



High-rate crystallization of polycarbonate in spincast thin film

阿多 誠介*; 岡 壽崇; He, C.-Q.*; 大平 俊行*; 鈴木 良一*; 伊藤 賢志*; 小林 慶規*; 扇澤 敏明*

Journal of Polymer Science, Part B; Polymer Physics, 48(20), p.2148 - 2153, 2010/10

 被引用回数:4 パーセンタイル:20.32(Polymer Science)



Surface modification of vulcanized rubber by radiation grafting, 1; Improvement in friction behavior

溝手 範人*; 片貝 秋雄; 玉田 正男; 松岡 広成*

Journal of Applied Polymer Science, 117(5), p.2825 - 2830, 2010/09



Ion beam irradiation effects on resist materials

五輪 智子*; 高橋 朋宏*; 岡 壽崇; 村上 健*; 大島 明博*; 田川 精一*; 鷲尾 方一*

Journal of Photopolymer Science and Technology, 23(3), p.399 - 404, 2010/08

6 MeV/u ion beams (Si$$^{14+}$$, Ar$$^{18+}$$, etc.) and 30 kV Ga$$^{+}$$ focused ion beam (FIB) were irradiated to a chemical amplified deep-UV resist and electron beam resist. The resist sensitivities were correlated with the energy deposition of ion beams, we obtained clear patterns of the resists. In contrast, crosslinking reaction of resist polymer was induced by the FIB irradiation, positive-negative inversion took place.

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