嵌段共聚物自组装纳米薄膜
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吴立敏，王晓艳. 纳米、亚微米颗粒粒度的测量——光子相关光谱法,《上海计量测 试》， 2003年 30卷 3期
2.Experimental Part
Sythesis of the Triblock Copolymer
a. Esterification
PEO+Acryloyol Chloride（丙烯酰氯）
P(St317-co-AN262)-b-PEO795-b-P(St-co-AN)
Preparation of Polymer Films
a. Dissolving the Triblock Copolymer in a DMF/toluene mixture
b. Spin-coating the homogeneous solution onto a Si wafer
✓ No micelle could be detected in the solution by PCCS, even after increasing the concentration up to 200 mg/mL, which seems to indicate a high CMC in this solvent system. Beyond this concentration, the polymer solution was too viscous to be analyzed.
a dense insoluble core内核
micelles
a diffuse corona核冠
Self-Assembly Nanomaterials
✓ In this work，the preparation of stable nanostructure assemblies in one step from homogeneous solutions of ABA triblock copolymers.
✓ The success of this strategy is essentially due to the design of very stable micelles prepared and selfassembled in situ in few seconds by solvent evaporation
✓ BCs in selective solvent lຫໍສະໝຸດ Baiduad to the preparation of core-shell micelles with a dense insoluble core and a diffuse shell partially swollen by the solvent
PEO-acrylate(I)
b. Intermolecular Radical Addition
I+MAMA-SGI alkoxyamine
macroalkoxyamine-based PEO(II)
c. Preparation of Triblock Copolymer
II+Styrene+Arylonitrile
Main Reference
Outline
Introduction Experimental Part Results and Discussion Conclusions Innovations and Problems References
1. Introduction
✓ Amphiphilic block copolymers (BCs) could control material interfaces . The 3D construction is directed by the assembly of BCs micelles prepared in situ during the spin-coating of the block copolymer solution.
evaporate solvent
Synthetic Producure
3.Results and Discussion
Sythesis of the Triblock Copolymer Precursor Preparation of Particle Nanomaterial Preparation of “Spider Web” Nanomterial
looped
bridged
Photon Cross Correlation Spectroscopy
Photon Cross Correlation Spectroscopy（PCCS），光子交叉相 关光谱法 PCCS已用于纳米颗粒粒径测量,其技术日益成熟并成为纳米 颗粒粒径测量的有效方法。其测量原理是建立在颗粒的布朗 运动之上。随着颗粒的布朗运动,散射光强围绕某一平均值 不断起伏涨落。 PCCS可以直接测试高浓度试样而不需要稀释。测量结果完全 真实的反映了被测试样品的实际粒度及分布状态 PCCS测定的参数为：平均粒径和多分散指数
3.1 Preparation of Particle Nanomaterial
✓ The preparation of superstructure homogeneous solution : PSAN-b-PEO-b-PSAN selective solution： DMF/toluene (50/50 v/v) , 100 mg/mL spin-coated on Si wafer
✓ The glassy PSAN blocks will enable the formation of compact aggregates constraining the micelles to be kinetically frozen at room temperature
✓ whereas the flexible PEO block will enable the dynamic transitions between looped and bridged chain conformations.
2.Experimental Part
Sythesis of the Triblock Copolymer
a. Esterification
PEO+Acryloyol Chloride（丙烯酰氯）
P(St317-co-AN262)-b-PEO795-b-P(St-co-AN)
Preparation of Polymer Films
a. Dissolving the Triblock Copolymer in a DMF/toluene mixture
b. Spin-coating the homogeneous solution onto a Si wafer
✓ No micelle could be detected in the solution by PCCS, even after increasing the concentration up to 200 mg/mL, which seems to indicate a high CMC in this solvent system. Beyond this concentration, the polymer solution was too viscous to be analyzed.
a dense insoluble core内核
micelles
a diffuse corona核冠
Self-Assembly Nanomaterials
✓ In this work，the preparation of stable nanostructure assemblies in one step from homogeneous solutions of ABA triblock copolymers.
✓ The success of this strategy is essentially due to the design of very stable micelles prepared and selfassembled in situ in few seconds by solvent evaporation
✓ BCs in selective solvent lຫໍສະໝຸດ Baiduad to the preparation of core-shell micelles with a dense insoluble core and a diffuse shell partially swollen by the solvent
PEO-acrylate(I)
b. Intermolecular Radical Addition
I+MAMA-SGI alkoxyamine
macroalkoxyamine-based PEO(II)
c. Preparation of Triblock Copolymer
II+Styrene+Arylonitrile
Main Reference
Outline
Introduction Experimental Part Results and Discussion Conclusions Innovations and Problems References
1. Introduction
✓ Amphiphilic block copolymers (BCs) could control material interfaces . The 3D construction is directed by the assembly of BCs micelles prepared in situ during the spin-coating of the block copolymer solution.
evaporate solvent
Synthetic Producure
3.Results and Discussion
Sythesis of the Triblock Copolymer Precursor Preparation of Particle Nanomaterial Preparation of “Spider Web” Nanomterial
looped
bridged
Photon Cross Correlation Spectroscopy
Photon Cross Correlation Spectroscopy（PCCS），光子交叉相 关光谱法 PCCS已用于纳米颗粒粒径测量,其技术日益成熟并成为纳米 颗粒粒径测量的有效方法。其测量原理是建立在颗粒的布朗 运动之上。随着颗粒的布朗运动,散射光强围绕某一平均值 不断起伏涨落。 PCCS可以直接测试高浓度试样而不需要稀释。测量结果完全 真实的反映了被测试样品的实际粒度及分布状态 PCCS测定的参数为：平均粒径和多分散指数
3.1 Preparation of Particle Nanomaterial
✓ The preparation of superstructure homogeneous solution : PSAN-b-PEO-b-PSAN selective solution： DMF/toluene (50/50 v/v) , 100 mg/mL spin-coated on Si wafer
✓ The glassy PSAN blocks will enable the formation of compact aggregates constraining the micelles to be kinetically frozen at room temperature
✓ whereas the flexible PEO block will enable the dynamic transitions between looped and bridged chain conformations.