Watching RAFT PISA grow spheres, worms, vesicles
In situ SAXS shows PGMA45-PHPMA200 aqueous RAFT PISA nucleating in 9–10 min and finishing as ~227 nm vesicles.
Source
<i>In situ</i> SAXS studies of a prototypical RAFT aqueous dispersion polymerization formulation: monitoring the evolution in copolymer morphology during polymerization-induced self-assembly
Study at a glance
- Design
- Other — In situ SAXS of aqueous RAFT HPMA polymerization from a PGMA45 macro-CTA
- N
- ~2 mL SAXS cell polymerization tracking — no sample N
- Population
- Aqueous RAFT polymerization forming micelles, worms, and vesicles
- Outcome
- Time-resolved nucleation and morphological transitions during polymerization
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Inspect source passages
Watching RAFT PISA grow spheres, worms, vesicles
These passages occur verbatim in the stored paper text. They support the points listed below; they do not verify every statement in the explanation.
Micellar nucleation occurs within 9–10 min.
In situ SAXS studies indicate that micellar nucleation occurs within 9–10 min.
First short worms form at a PHPMA DP of around 134.
The first short worms are formed at a PHPMA DP of around 134.
What they did
Authors polymerized HPMA from a PGMA45 macro-CTA at 70 °C in a ~2 mL SAXS cell and tracked scattering while checking conversion, GPC, DLS, and TEM after the run.
What they found
Micelles nucleate at 9–10 min; worms appear near PHPMA DP 134 after 28–29 min; vesicles reach Dv = 227 ± 16 nm. HPMA conversion exceeds 99% within 80 min; GPC Mn is 51 200 g mol−1 with Đ = 1.25.
The limits
What it doesn't show
The SAXS nucleation clock is faster than the lab 1H NMR rate jump; other PISA monomers and concentrations are not mapped at the same time resolution.
Key terms
- PISA
- Polymerization-induced self-assembly: a growing insoluble block triggers in situ nanoparticle formation.
- RAFT
- Reversible addition–fragmentation chain-transfer living radical polymerization.
- PGMA-PHPMA
- Glycerol monomethacrylate stabilizer with a 2-hydroxypropyl methacrylate core-forming block.
- SAXS
- Small-angle X-ray scattering used here in situ to assign spheres, worms, and vesicles.
- Jellyfish intermediate
- Transient branched-worm structure en route from worms to vesicles.
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SAXS nucleation of micelles occurs at:
Common questions
When do micelles nucleate?
Within 9–10 minutes by SAXS intensity upturn.
When do worms start?
Near PHPMA DP 134, around 28–29 min.
Final vesicle size?
227 ± 16 nm by SAXS.
How complete is HPMA conversion?
More than 99% within 80 min at 70 °C.
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