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Exploring the Upper Size Limit for Sterically Stabilized Diblock Copolymer Nanoparticles Prepared by Polymerization-Induced Self-Assembly in Non-Polar Media.
Langmuir ( IF 3.7 ) Pub Date : 2020-04-02 , DOI: 10.1021/acs.langmuir.0c00211
Bryony R Parker 1 , Matthew J Derry 1 , Yin Ning 1 , Steven P Armes 1
Affiliation  

Reversible addition-fragmentation chain transfer (RAFT) dispersion polymerization of benzyl methacrylate is used to prepare a series of well-defined poly(stearyl methacrylate)-poly(benzyl methacrylate) (PSMA-PBzMA) diblock copolymer nanoparticles in mineral oil at 90 °C. A relatively long PSMA54 precursor acts as a steric stabilizer block and also ensures that only kinetically trapped spheres are obtained, regardless of the target degree of polymerization (DP) for the core-forming PBzMA block. This polymerization-induced self-assembly (PISA) formulation provides good control over the particle size distribution over a wide size range (24-459 nm diameter). 1H NMR spectroscopy studies confirm that high monomer conversions (≥96%) are obtained for all PISA syntheses while transmission electron microscopy and dynamic light scattering analyses show well-defined spheres with a power-law relationship between the target PBzMA DP and the mean particle diameter. Gel permeation chromatography studies indicate a gradual loss of control over the molecular weight distribution as higher DPs are targeted, but well-defined morphologies and narrow particle size distributions can be obtained for PBzMA DPs up to 3500, which corresponds to an upper particle size limit of 459 nm. Thus, these are among the largest well-defined spheres with reasonably narrow size distributions (standard deviation ≤20%) produced by any PISA formulation. Such large spheres serve as model sterically stabilized particles for analytical centrifugation studies.

中文翻译:


探索非极性介质中聚合诱导自组装制备的空间稳定二嵌段共聚物纳米颗粒的尺寸上限。



采用甲基丙烯酸苄酯的可逆加成-断裂链转移(RAFT)分散聚合在90℃矿物油中制备一系列结构明确的聚(甲基丙烯酸硬脂酯)-聚(甲基丙烯酸苄酯)(PSMA-PBzMA)二嵌段共聚物纳米粒子。相对较长的 PSMA54 前体充当空间稳定剂嵌段,并且还确保仅获得动力学捕获的球体,无论形成核的 PBzMA 嵌段的目标聚合度 (DP) 是多少。这种聚合诱导的自组装 (PISA) 配方可在较宽的尺寸范围(直径 24-459 nm)内很好地控制粒径分布。 1H NMR 光谱研究证实,所有 PISA 合成都获得了高单体转化率 (≥96%),而透射电子显微镜和动态光散射分析显示出明确的球体,目标 PBzMA DP 与平均粒径之间存在幂律关系。凝胶渗透色谱研究表明,随着更高 DP 的目标,分子量分布逐渐失去控制,但 PBzMA DP 高达 3500 时可以获得明确的形态和窄粒度分布,这对应于粒度上限459 纳米。因此,这些是由任何 PISA 配方生产的最大的明确球体之一,具有相当窄的尺寸分布(标准偏差≤20%)。这种大球体可作为分析离心研究的空间稳定颗粒模型。
更新日期:2020-04-03
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