スライド 1
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- かずき むこやま
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1 第 京大原子炉実験所, SANS SAXS によるソフトマター研究 ー高分子ミセルのナノ構造解析を中心としてー 京都大学 工学研究科 高分子化学専攻 松岡秀樹
2 Research Interests Non-Surface Activity Surface tension (mn/m) UV absorbance Ionic Amphiphlic Block Copolymers C (wt%) Living Anionic Polymerization,Living Radical Anomalous behavior by polymerity Polymerization (DEPN, RAFT) Polymer conc. No Salt Salt F Si COOH SO 3 - XR,NR Polymer monolayer, polyelectrolyte brush on water surface Structural Transition Critical Brush Density DP of PSS chain n Salt Conc 塩効果 Micellization イオン性コロナブラシ ミセルコア イオン濃度 Analytical: 1~M Effective: 0.1~0.M 小イオン SANS, SAXS Chain length, ratio Stability against salt, Sphere / rod transition
3 X 線小角散乱装置 (SAXS) Upgrade!! 超小角 X 線散乱装置 (USAXS)
4 ポリスチレンスルホン酸ナトリウム
5 Colloidal Crystal of polyelectrolyte grafted latex particles S S Colloidal Crystal of polyelectrolyte grafted latex particles S G 5
6 コロイド結晶の解析例
7 コロイド結晶の三次元パラクリスタル理論による解析
8
9 Polymer Micelle diffusion Breathing?
10 These Polymers are Non-Surface Active! Non-surface active but form micelles in solution n m m C O O n n m SO 3 - Na+ CH CH CH O S O ONa SO 3 - Na + CH 3 Amphiphilic Ionic Di(Tri)block Copolymers Et Si Et H Et Si Et H Ph Ph Ph Me COOCH CH CH SO 3- Na + Ph Ph Ph Me COOH - Na + These polymers become Non-Surface Active under suitable conditions of m:n and ionic strength 11
11 Micelle Formation but No-Adsorption Surface tension does not decrease, but cmc is detected by dye solubilization : surface tension of aqueous solution : UV absorbance of aqueous solution Surface tension (mn/m) Surface Tension Dye Solubilization C (wt%) Surface tension of (Ip-h) 6 -b-(ssna) 50 aqueous solutions and hydrophobic dye adsorption (495 nm) as a function of polymer concentration. Surface tension does not reduce. Very low foam formation activity. (no salt) However, there are micelles in solution UV absorbance n m SO 3 - Na+ N N HO Oil Orange SS (Hydrophobic dye) UV absorbance 1
12 Foam Formation and Salt Effect Good foam formation by salt addition, which is quite different from normal surfactant Low-molecular weight ionic surfactant Ionic amphiphilic diblock copolymer H m n SO 3 Na SO - H + NaCl NaCl 13
13 14
14 Image Charge at the Interface The Origin of Non-Surface Activity The image charges repulsion prevents polymer adsorption at water surface
15 高分子と低分子における鏡像電荷効果 高分子 低分子 C10 C0 電荷数 1 個 電荷数が多く, 疎水吸着に勝る場合がある. 鏡像電荷効果はあるが, 疎水吸着が勝る
16 Structure Analysis of Polymer Micelle by SANS d(q)/dω (cm -1 ) Core-Shell Model R C = 3 Å R S = 69 Å raw data core-shell model fit q ( A -1 ) d(q)/dω (cm -1 ) Pedersen Model R C = 31 Å S = 38 Å R g = 14 Å raw data Pedersen model fit q ( A -1 ) R S n m S R g R C SO 3 - Na+ R C (5:40) 17
17 Core-Corona Model and Effect of Polydispersity SAXS Ref: M.Nakano et al., Macromolecules 1999, 3,
18 Structure Analysis of Polymer Micelle by SANS Core-Shell Model Pedersen Model R S S R g R C R C 19
19 Cryo-TEM Image of Polyelectrolyte Grafted Latex Particles J. Am. Chem. Soc., 17, 9688 (005)
20 SANS Profiles for PIph -b-pssna Micelles Sphere to rod transition by longer hydrophobic chain and by salt addition n m SO 3 - Na+ Longer hydrophobic chains High salt concentration 10 B (5:40) 10 C (38:50) 10 D (6:40) 10 F (131:54) d Σ(q)/dΩ (cm- 1 ) d Σ(q)/dΩ (cm- 1 ) d Σ(q)/dΩ (cm- 1 ) d Σ(q)/dΩ (cm- 1 ) q q ( Å -1 ) q ( Å -1 ) q ( Å -1 ) q ( Å -1 ) 10-4 SANS profiles for PIph-b-PSSNa DO solutions (1 wt %) without salt (filled circle) and with1 M NaCl aq (open circle). Solid lines are fitting curves by a simple core-shell model.
21 Micelle Structure: Sphere to Rod Transition by Salt Addition SANS raw data Pedersen model fit. Core-shell model fit. n m SO 3 - Na+ d(q)/d Ω (cm -1 ) sphere 100% d(q)/d Ω (cm -1 ) d(q)/d Ω (cm -1 ) salt-free 0.01M NaCl 0.1M NaCl q ( A -1 ) q ( A -1 ) q ( A -1 ) 10 sphere 94% 10 sphere 80% 10 sphere 75% sphere + rod 10-1 sphere only M NaCl d(q)/d Ω (cm -1 ) M NaCl d(q)/d Ω (cm -1 ) q ( A -1 ) d(q)/d Ω (cm -1 ) q ( A -1 ) M NaCl 1M NaCl q ( A -1 ) 3
22 Sphere/Rod Transition and Micelle Structure Parameters SANS Analysis 4.5 Critical salt concentration shell thickness (nm) (65:40) (Ip-h ) 65 -b-(ssna) C (%) S Salt concentration[mol/l] %Sphere d(q)/d Ω (cm -1 ) (65:40) q ( A -1 ) 0 M 1 M NaCl Very Stable against Salt P.Kaewsaiha, K.Matsumoto, H.Matsuoka, Langmuir, 3(18), (007). n m SO 3 - Na+ 4
23 Mechanism of High Stability against Salt Addition of Polyelectrolyte Grafted Particles Polyelectrolyte brush (corona) イオン性コロナブラシ micelle ミセルコアcore small ions イオン濃度 ion concentration Analytical: 1~M Effective: 0.1~0.M 小イオン Matsuoka Laboratory, Department of Polymer of Polymer Chemistry, Kyoto Kyoto University 5
24 Ionic Amphiphilic Diblock Copolymers Synthesis of block copolymers by living polymerization Water soluble Insoluble Molecular properties such as surface activity Non-Surface Activity Monolayer on the water surface Nanostructure and Transition SAXS SANS Micelle Formation Nanostructure Transition Polyelectrolyte Brush at the Air/Water Interface 6 6 XR NR
25 Air-Water Interface X-ray Reflectometer (XR) RINT TTR-MA in our laboratory Air-Water Interface Neutron Reflectometer (NR) ARISA-II at J-Parc, Japan (formerly at KEK) Ge(111) XG Incident x-ray Monochrometer Ge(111) Slit θ s Reflected x-ray LB trough cover Kapton window Pressure sensor Wilhelmy plate θ d Slit Attenuator Scintillation counter Monitor LB trough Barrier Sample stage XR Electron Density NR Scattering Length Density 7 7 7
26 Salt Concentration Dependence --- NR Profiles hydrophobic Et Si hydrophilic H Reflectivity [-] No Fit XR can be fitted Et SB+MAA Et SB layer 35mN/m Q [Å ] b/v (x10-6 ) [Å - ] without salt 0.01M 0.1 1M fit. fit. fit. 35mN/m Et SB Increase of Roughness MAA+D O + without salt 0.01M 0.1M Z [Å ] Ph poly ( Et SB -b -MAA) D O m Ph C n Me COOH Fig. NR profiles and scattering density profiles for poly(et SB-d 10 ) 3 -bpoly(maa) 49 monolayer monolayer on subphase with different NaCl concentrations at 35mN/m. 8 8
27 Reflectivity [-] hydrophobic Ph Et Si Contrast-Variation by NR --- Small Ion distribution 1M NaCl (D O) 1M NaBr (D O) 1M Na Cl (D O:H O=8: ) fit. fit. hydrophilic H m Ph C n MeCOOH poly (Et SB-b-MAA) Nb(Cl - )=Nb(D O/H O) The same monolayer structure was evaluated from 1M NaBr system and 1M NaCl(D O/H O) system(no contribution from Cl- ions) ---> No contribution from Br- ions in NaBr system. Nb [10-6 Å - ] NaBr (H O) NaCl (D O/H O) NaBr (H O) NaCl (D O/H O) z [Å ] q [Å -1 ] Fig. NR profiles and scattering density profiles for poly(et SB-d 10 ) 3 -b-poly(maa) 49 monolayer monolayer at 35mN/m on various subphase. No good agreement for 1M NaCl system --> Contribution from Cl- ion distribution? f [-] 9 9
28 Possible Cl - ion Distribution 1M NaCl (DO) profile was well fitted with taking the Cl- ion distribution into account with the same monolayer structure determined by contrast matching method M NaCl (D O) Concentrated Cl- ion layer just beneath the carpet layer fit. with small ion distribution Reflectivity [-] box model fit. Nb [10-6 Å - ] Cl - ion Profile for monolayer only 35mN/m 1M NaBr (D O) 1M NaCl (D O) q [Å -1 ] H. Matsuoka, E. Mouri, P. Kaewsaiha, Y. Furuya, Y. Suetomi, K. Matsumoto, N. Torikai, Trans. MRS-J, 3(1), (007). Fig. NR profiles with fitting curve in which Cl - ion distribution is considered. (left) Scattering length density obtained by the fitting. (right) z [Å ] bc(cl)=9.6, (Br)=6.8)
29 Counterion and Salt Ion Distribution in the Polyelectrolyte Brush is unknown. Polyelectrolyte brush (corona) イオン性コロナブラシ micelle ミセルコアcore small ions イオン濃度 ion concentration Analytical: 1~M Effective: 0.1~0.M 小イオン Matsuoka Laboratory, Department of of Polymer Chemistry, Kyoto Kyoto University 31
30 Visual Observation of Phase Transition PNIPAm PNIPAm PNIPAM 3-34 o C Diblock Diblock 38-4 o C PNIPAM-b-PMAPTAC Conc n 1 mg/ml 3
31 温度による界面不活性 / 界面活性転移の制御 RT PNIPAM( 非イオン性水溶性 ) 界面活性 界面活性! PMAPTAC ( カチオン性 ) やや界面活性? LCST 3 C 45 C PNIPAM( 疎水性 ) 界面活性 PMAPTAC ( カチオン性 ) やや界面活性? 界面不活性! 分子が 疎水性 になると, 界面 不 活性になる!? 33
32 界面不活性性の発現機構 1) ) 三成分が平衡にある. 鏡像電荷のため, 水面での居心地が悪い 界面不活性 + ミセル形成疎水性増加 水面での居心地よりミセルでの居心地がより良くなる? 34
33 水 / 有機溶媒混合系での界面不活性性とミセル形成挙動 鏡像電荷による静電反発 水 / 有機溶媒混合系を用いる事により誘電率を変化させて界面不活性性およびミセル形成挙動に与える影響の調査 二つのモデル (Core-Shell model) 1 コア中に溶媒は存在しない コアに有機溶媒だけ取り込まれている Organic solvent?
34 第 63 回コロイドおよび界面化学討論会 主催 : 日本化学会コロイドおよび界面化学部会 会期 :011 年 9 月 7 日 ( 水 ) 9 日 ( 金 ) 会場 : 京都大学吉田キャンパス百周年時計台記念館 共催 : 京都大学大学院工学研究科 協賛 : 京都大学 物質 細胞統合システム拠点 工学部 工業化学科講義室 後援 : 日本化学会コロイドおよび界面化学部会関西支部 高分子学会, 応用物理学会, 日本中性子科学会など, 約 30 の学協会に申請手続中 URL: (011 年 4 月 1 日開設予定 )
35 一般セッション シンポジウム 分子集合体の科学と技術 組織化膜の科学と技術 微粒子分散系の科学と技術 固体表面 界面の科学と技術 応用 開発セッション -(1): 界面活性剤 ( 界面活性剤単独系 混合系 エマルションを含む ) -(): 界面活性剤と他物質の相互作用 -(3): 超分子 高次分子集合体 -(4): ゲル -(5): 高分子溶液 -(6): その他 3-(1): 単分子膜 LB 膜 3-(): 自己組織化膜 3-(3): 二分子膜 ( ベシクル リポソームなど ) 3-(4): 界面物性 ( 気 - 液 液 - 液 ) 3-(5): その他 4-(1): サスペンション 4-(): 微粒子 ナノ粒子 4-(3): 高分子コロイド 4-(4): 界面電気現象 4-(5): レオロジー 4-(6): その他 5-(1): 固体表面構造と物性 機能 5-(): 吸着と触媒 5-(3): 表面力 トライボロジー 走査プローブ顕微鏡 5-(4): 散乱 回折 分光法 5-(5): ミクロファブリケーション 5-(6): その他 6-(1): 企業開発研究 ( 製品配布可 ) 6-(): アカデミアにおける応用研究 S-1: 界面 分散系の新デザイン : サーファクタントフリー分散系と界面吸着粒子の科学と工学 S-: 細胞と粒子の相互作用は, コロイド 界面科学でどこまで理解できるのか? S-3: 液体のクラスター化にともなう新現象 S-4: ソフト界面分子膜科学の新展開 S-5: ナノ細孔物質の新現象 新機能 S-6: 界面動電現象の科学と技術 - 計測とサイエンス イノベーション S-7: 蛋白質 / 水界面の熱力学と ATP エネルギー バイオ関連セッション追加の方針
コスメトロジー研究報告 Vol.24, 2016 図 3 界面不活性性 発現機構の模式図 図 5 界面不活性高分子水溶液に対する添加塩の効果 の模式図 図 4 界面不活性高分子の cmc の添加塩濃度依存性 低分子イオン性界面活性剤と真逆に 上昇傾向を示す 図 6 本研究で用いた ３種のイオン性両親
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