Nanoscale polymer discs, toroids and platelets: a survey of their syntheses and potential applications

Emma R. L. Brisson ^a, Max J. H. Worthington ^a, Simran Kerai ^a and Markus Müllner *^ab
aKey Centre for Polymers and Colloids, School of Chemistry, The University of Sydney, Sydney 2006 NSW, Australia. E-mail: markus.muellner@sydney.edu.au
^bThe University of Sydney Nano Institute (Sydney Nano), The University of Sydney, Sydney 2006 NSW, Australia

First published on 4th January 2024

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Emma R. L. Brisson

Emma R. L. Brisson completed her PhD in 2018 at the University of Melbourne with Dr Luke Connal and Professor George V. Franks, where she investigated the synthesis of dynamic, amino acid functional materials and their self-assembly. After a year as a Research Chemist in the Polymer Team at DuluxGroup, Emma became a Postdoctoral Researcher at the University of Sydney in the Polymer Nanostructures Group, using molecular polymer bottlebrushes as templates for the self-assembly of block copolymers into discs. Emma translated her skills to the world of lipid-based drug delivery for one year in the Self-Assembled Systems Group at the University of Newcastle. Emma is now a Senior Materials Chemist at MicroTau in Sydney, Australia, where she develops high-performance, microstructured coatings for the aviation and marine industries, mimicking shark skin to reduce skin friction and improve fuel efficiency.

Max J. H. Worthington

Max J. H. Worthington completed his PhD at Flinders University in 2020 under the supervision of Prof. Justin Chalker where he investigated renewable polymers for applications in environmental remediation, biochemistry, and agriculture. After an additional year of postdoctoral study working with industry partners translating lab processes for commercialisation, he expanded his synthetic experience with a postdoctoral research position in the Polymer Nanostructures Group at The University of Sydney, where he studied the synthesis and self-assembly of polymeric 2D materials for nanomedicine. Max has a keen interest in green and renewable chemistries, and the development of new tools to benefit the environment and human health.

Simran Kerai

Simran Kerai completed her B. Pharmaceutical Science Advanced (Hons) at Monash University under the supervision of Dr Kristian Kempe focusing on novel functionalised poly(2-oxazoline) based nanoparticles for drug delivery. She then joined the Polymer Nanostructures Group at The University of Sydney in 2022. Her PhD investigates the self-assembly of polymeric discoid nanoparticles for biomedical applications under the supervision of A/Prof Markus Müllner.

Markus Müllner

Markus Müllner heads the Polymer Nanostructures Group in the Key Centre for Polymers and Colloids at The University of Sydney, Australia. His research group has extensive expertise in the synthesis and application of molecular polymer bottlebrushes. Markus and his team are interested in a variety of polymer-related topics, from the synthesis of polymer architectures and their use in self-assembly or nanomedicine applications, and polymer-templated nanomaterials. Markus is currently an Associate Professor and Australian Research Council Future Fellow in the School of Chemistry. He studied polymer and colloid chemistry at the University of Bayreuth, Germany, where he also received his doctorate in polymer chemistry under the supervision of Prof. Axel H. E. Müller. Before starting at The University of Sydney, Markus was a McKenzie Fellow working with Prof. Frank Caruso at the University of Melbourne from 2013–2015.

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1. Introduction

Nanomaterials are critical to our future.^1–4 The ability to manipulate materials at the nanoscale has been revolutionary,^5–9 where the ability to control their composition and morphology has enabled new possibilities. The precision by which functional inorganic matter can be synthesised is extraordinary, with numerous, reliable procedures guaranteeing control over (nano)material characteristics in three dimensions.^10–12 Turning to soft matter, immense progress has been made in developing approaches to achieve polymer nanomaterials. Polymers are soft, and their chemistry and other properties are easily tuned to the desired application by synthetic procedures, making them outstanding building blocks for nanomaterials synthesis.^13,14 Bottom-up approaches based on self-assembly are state-of-the-art when it comes to polymer nanomaterials fabrication. Amphiphilic block copolymers can self-assemble into aggregates of controlled size and shape. The volume fractions of the amphiphile (as with lipids and surfactants) and their interaction with their surroundings largely dictate this process. Most block copolymer self-assembly is driven by thermodynamics and the minimisation of surface energies, causing the prevalence of spheres, cylinders, and vesicles. The ability to make more complex shapes and morphologies is limited, as other interactions must be strong enough to pay the energy cost to flatten a curved surface, as an example. The synthesis of more complex and 2D structures is becoming increasingly vital as their anisotropic properties make them highly valuable to fundamental and applied research.^15–17 Recent progress in polymer self-assembly, for example via polymerisation-induced self-assembly (PISA) or microfluidic processes, grant access to a plethora of structures.^18,19 In addition, top-down methods, such as ‘particle replication in nonwetting templates’ (PRINT), 3D printing and lithography,^20–22 provide access to polymer (nano)particles that do not require amphiphilicity or specific supramolecular interaction.

Spherical nanomaterials, such as micelles, dominate literature; however, cylindrical micelles and nanoparticles are now readily accessible by self-assembly and have been thoroughly studied in recent years.^23,24 Unlike most spherical nanomaterials, cylinders or rods are anisotropic and thus present new opportunities to tune nanomaterials properties. The ability to control the aspect ratio or stiffness of these nanoparticles has been demonstrated to be especially advantageous in the areas of nanomedicine.^25–27 Further advances in this area are anticipated from 2D nanoparticles, as their increased surface area and altered movement in flow grant them valuable attributes for targeted drug delivery.²⁸ As powerful as the self-assembly of polymers has become, access to assemblies or nanomaterials beyond the traditional phase diagrams are rare. Two dimensional, or planar, particles are difficult to synthesize. The self-assembly of polymers into flattened structures often requires design and engineering beyond solvent–polymer interactions and block segment ratios. To overcome the energetically favoured surface curvature, polymer phase separation, strong chain–chain interactions, and/or polymer crystallisation are required.

The exploration of non-spherical particle syntheses from polymeric materials has been occurring since the 1990s.^29,30 The reporting of the synthesis and characterization of these materials is prevalent in the literature; however, reports of their applications remain limited. We would like to take the opportunity and highlight recent progress in this area. The focus of this review lays primarily on self-assembly strategies and the various polymer building blocks that have been used to produce polymeric nanomaterials in the shapes of discs, toroids, and platelets. By focussing on these three particle types, we seek to highlight the interconnectedness of these structures, in terms of their assembly methods as well as their areas of application. We will therefore also highlight anticipated and emerging applications of these nanomaterials.

2. Polymer nanoscale discs

In this section we focus on wholly synthetic polymer-based (with exception for minor small-molecule components) nanoscale assemblies with disc or disc-like geometry. Readers are directed to other recent reviews where nanodiscs from polymer–lipid or polymer–protein hybrids have been summarised.^31,32 A select few studies fit the criterion of polymer-only nanodiscs, and by omitting studies on lipid and biomolecule assembly, we achieve a strict focus on objects synthesised via contemporary controlled polymerisation techniques, combined with conventional and emerging polymer self-assembly processes. Each of the methods present in the literature can be divided in to two general categories: the direct(ed) self-assembly in solution and the disassembly of a superstructure to form polymer nanodiscs (Scheme 1). Self-assembly in solution can be further grouped into two broader concepts with some overlap. In the first and simplest concept, it is useful to think of disc synthesis in terms of overcoming the energy penalty to compress or bend molecular assemblies into a planar shape; this could encompass compressing or stretching a sphere into a flat disc or rounding-off the edges of a planar structure. In this direct self-assembly approach, the polymer is built including chemical moieties with predominant interactions such that some component preferentially packs into a flat surface. Examples mainly include multiblock polymers with a crystallisable or rod-like segment, where the rigid component directs planar packing. However, there are some instances where this is achieved via accessing the superstrong segregation regime (SSSR), when the interfacial tension dictates the morphology, rather than a balance between interfacial tension and chain crowding, or non-crystalline packing methods (i.e., via π–π stacking or rod-like polymers). Related to this direct self-assembly, is the second concept that we term directed self-assembly. This assembly approach is predominately governed by extrinsic factors, where careful control of extraneous conditions is utilised to overcome bending energies and to complete disc formation. The energy required to overcome bending penalties is imposed by extraneous forces, such as templates, solvent mixtures or small-molecule chaperones that guide formation. Contrasting to the direct(ed) solution self-assembly of polymers, is the hierarchical multistep assembly approach, where larger assemblies are first formed, and then deconstructed to yield individual discs. Here we focus on those processes that clearly lead to a characterizable intermediate that is then processed further into the final nano-object. Table 1 provides an overview of the various copolymers and self-assembly strategies used to yield polymer nanodiscs.

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2.1 Direct(ed) self-assembly in solution

In principle, the construction of open lamellae nanostructures becomes more feasible by boosting nonspecific interactions within hydrophobic segments that increase membrane rigidity and the corresponding curvature energy penalty. Self-assembled polymer disc-like morphologies first started appearing in the literature in the mid-1990s as crystalline-core diblock copolymers began to be investigated. Richter et al. investigated polyethylene-block-poly(ethylenepropylene) (PE-b-PEP) diblock copolymers and their self-assembly in decane.³³ They found that at lower temperatures, lamellar sheets with 40–80 Å thicknesses were formed, while spheres were present at temperatures above the melting point of PE. The driving force for these self-assemblies was the crystallisation of the PE in the core, while PEP extended out from the surface like a brush. These sheets could easily assemble into hierarchical superstructures with needle-like shapes via van der Waals interactions of the PEP lamellar surfaces. The exploration of block copolymers with crystallisable domains became an early feature to generate disc-like polymer nano-objects. Section 4 will discuss the use of crystallisation-driven self-assembly (CDSA) as a tool for 2D nanoparticle formation. Here, we will provide an overview of examples that used block copolymers and polymer architectures to yield nanodiscs in solution. Starting off with formative studies, emphasis is placed on showcasing strategies beyond crystallisation to achieve planar polymer assemblies.

2.2 Template-assisted assembly

In addition to solvent choice, temperature, or monomer selection as modes to steer the formation of self-assembled aggregates, it is also possible to employ structure-guiding templates that facilitate the formation of a particular morphology. In one such example of structure-guiding templates in the self-assembly of triblock terpolymers, Yang and co-workers used PEO-block-poly(3-triethoxysilylpropyl methacrylate)-block-PS to form Janus nanodiscs at a paraffin-in-water emulsion interface.⁷⁴ In an emulsion, the amphiphilic triblock terpolymer acted as a surfactant and stabilised the water/paraffin interface (Fig. 4A). Lowering the pH initiated the polycondensation of the triethoxysilylpropyl middle block to form a silsesquioxane layer around the surface of the paraffin droplets. The incorporation of a non-gelable PEO-b-PS amphiphilic copolymer meant that the forming silsesquioxane layer became discontinuous around the droplets. Dissolving the paraffin droplet freed individual amphiphilic Janus discs that, depending on the solvent quality, aggregated to dimers, or were individually dispersed. The discs themselves could be used as surfactants to stabilise emulsions of water and cyclohexane for months. In follow-up work, the same group used a template system consisting of silica particles with distinct imidazole patches.⁷⁵ PAA-b-PS was amassed at the surface through a strong electrostatic interaction of carboxylic acid groups at the imidazole domains, and after crosslinking of PAA, discs were formed (Fig. 4B). Such discs were ∼20 nm in diameter with heights respective of the PAA chain length, for example, PAA₆₆-b-PS₄₈ resulted in 1.6 × 20 nm discs and PAA₁₃₂-b-PS₂₂ resulted in 3.3 × 20 nm discs. The system was also found to tolerate combinations of PAA-b-PS of different block lengths, for example, a 1:1 mixture of PAA₁₅-b-PS₁₁₅ and PAA₁₃₂-b-PS₂₂ resulted in 2.3 × 20 nm discs and the height could be tuned by altering the feed ratio.

These illustrative examples still employ polymers in solution and aim at directing them to form a disc at an interface. Liu and co-workers demonstrated an innovative method of disc formation with tuneable curvature by forming spheres and flattening them within decane droplets.⁷⁶ A dispersion polymerisation process (in decane:methanol) was followed to encapsulate spheres of PS in a shell of poly(2-ethylhexyl methacrylate) (PEHMA). Due to the swelling of the PS component, phase separation moulded the spheres into discs. With removal of decane and the PEHMA shell individual discs were achieved. In addition to PS, spheres of PS copolymerised with sodium styrene sulfonate (NaSS), acrylic acid (AA), or (2(methacryloyloxy)ethyl)trimethylammonium chloride (METAC) were also demonstrated. The process was general and did not show specific differences between monomers. To form the initial sphere two approaches were followed: either the direct addition of the second monomer or the synthesis of a ∼100 nm copolymer shell onto a micron-sized PS sphere. The latter method was found preferable as it allowed for finer control over the synthesis of the core PS spheres. Cavity depth was tuneable as curvature was correlated with hydrophilic monomer content; at low or no hydrophilic content the discs were convex, with increasing content (from 0.035% NaSS) they became concave. Optical microscopy was used to investigate the contact angle between the PS particles and adsorbed decane to understand how curvature is imparted. In addition, packing behaviours of disc populations were demonstrated by LCSM with fish-scale-like and crosshatch patterns formed with monoform concave or convex discs, and long chains of stacked, alternating concave and convex discs formed in a mixed sample. At >1 μm these discs decidedly exceed the nanoscale, but the authors demonstrated the process on various spheres with 1.23, 1.42 and 1.71 μm diameters with similar results. Larger microspheres formed larger discs and smaller spheres formed smaller discs, consequently it was suggested that the method would not be size-dependent and could theoretically translate to nanodiscs. While this method is not solution phase self-assembly based, it highlights the power of shaping a preformed polymer particle to a disc-like shape.

2.3 Disassembly of superstructures

In contrast to the bottom-up approaches to form polymer nanodiscs summarized in Sections 2.1 and 2.2, approaches that utilised a pre-formed superstructure broken into nanodiscs will be the next focus. In this approach, a polymer bulk or microparticle is first produced before it is broken down or disassembled into individual polymer discs. In this context, the self-assembly of copolymers in bulk (e.g., via solvent evaporation) or within a drying solvent droplet (e.g. confinement self-assembly) offer avenues in fabricating micro-phase separated polymer thin films and microparticles, where especially lamellar domains lend themselves to produce 2D nanomaterials, such as discs. Phase-separating copolymers will assemble into well-known bulk microdomains (dictated by the χ parameter and block ratios) once the solvent has been removed. This bulk self-assembly strategy has been used extensively to work nanostructured films, membranes, or templates for inorganic nanostructures.^24,77–80 The same self-assembly principles dictate microdomain structure formation in a drying emulsion droplet, allowing the generation of polymer particles with controllable internal morphology. However due to a water-oil interphase, surfactants amongst other parameters can largely affect the orientation of the internal domains. A recent review by Yan et al. comprehensively summarised the progress and potential of confinement self-assembly.⁸¹

3. Polymer nanoscale toroids

Micelles resembling closed-looped rings were first reported in 1999 by In et al. from the assembly of a cationic tetramer surfactant in water.⁹⁶ Closed loop micelles were mixed among worm-like micelles and it was found that the rigidity of micelles affected the size of the closed loops by limiting their bending into smaller loops. The concept of manipulating the flexibility of cylindrical assemblies and bending them into closed loops or micelles is also translatable in polymer self-assembly. In general, polymeric toroids can be yielded via several approaches: (i) the direct assembly of a toroid-forming (co)polymer, (ii) the aforementioned transformation of a pre-assembled morphology (e.g. a cylinder) into a toroid, or (iii) through the disassembly of a hierarchical superstructure (similar to the formation of polymer discs via microparticles discussed in Section 2.3) (Scheme 2). As the formation pathway for toroids is difficult to observe in situ and the success of formation is typically proven by microscopy, it is likely that approaches (i) and (ii) may therefore co-exist or remain difficult to distinguish. Therefore, the following section broadly groups the fabrication of toroids into two categories: direct self-assembly and disassembly of pre-formed superstructures. Individually, each section will be subdivided by the type of building blocks. Table 2 provides an overview of the various copolymers and self-assembly strategies used to yield polymer toroids. For a recent review on toroidal self-assemblies, including computational modelling on their formation, we suggest Xu et al.⁹⁷

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3.1 Direct(ed) self-assembly

Whilst we note there are also examples of evaporation-induced formation of ring-shaped polymer objects on surfaces, such as block copolymers (on carbon-coated mica,⁹⁸ or nitrided silicon⁹⁹), dendrimers (on quartz¹⁰⁰), poly(n-hexyl isocyanate) and poly(9,9-di-n-decylfluorene) (on mica^101,102) as well as biomaterial-derived assemblies (e.g. from polysaccharides,^103,104 actin,¹⁰⁵ polypeptides^106,107 and DNA^108–112), we will focus on polymeric systems and systems assembled in solution. However, a noteworthy example of self-assembly on a substrate that illustrates well the morphological transition of a micelle towards a toroid was shown by Qiu and co-workers.¹¹³ They reported an elegant example of how solution-assembled micelles can be controllably altered in the local confinement of a surface using solvent vapours to transform micelles into complex morphologies, including toroids (Fig. 7). The primary principle at play in this example is the use of solvent vapour to cause coronal inversion of the blocks forming the assemblies.

3.2 Disassembly of hierarchical superstructures

Just as the use of confinement self-assembly was a rigorous approach to the formation of polymer nanodiscs, its application in the formation of toroids is just as powerful.^81,151 As the internal morphology can be adjusted by the selection of the block copolymer and their composition, it becomes feasible to produce structured microparticles that can be disassembled into toroidal polymer particles. Yang, Zhu and co-workers used a PS₁₉₂-b-P4VP₁₆₂ diblock copolymer in conjunction with a small-molecule hydrogen bond donor (pentadecylphenol, PDP) to control the morphology of the phase separation inside a drying emulsion droplet.¹⁵² Tuning the P4VP:PDP ratio altered the volume fraction of the P4VP domain and allowed for producing polymer particles with internal morphology including stacked lamellae or stacked toroids. Selectively dissolving the P4VP domain led to the disassembly of the superstructure to yield individual discs or toroids. Gröschel and co-workers used the concept of confinement assembly to generate polymer particles made of stacked polymer toroids (Fig. 11A).¹⁵³ A triblock terpolymer SBM was dissolved in chloroform and emulsified in an aqueous CTAB solution. The volume ratios of the blocks meant that the triblock phase separated into PB cylinders wrapping around the polymer particle like rings, while the PS and PMMA formed lamellar domains that sandwiched the PB cylinders. After a crosslinking step to stabilise the PB domain, the microparticles could be disassembled in solution to yield Janus nanorings with various diameters. Increasing the volume fraction of the PB middle block also meant that Janus nanodiscs could be generated via the same method.

A different approach was taken by Monteiro and co-workers who developed a temperature-directed morphology transformation (TDMT) method to synthesize a wide range of nanostructures, including toroids.^154,155 RAFT emulsion polymerisation was used to chain extend a PNIPAM macro-CTA with styrene yielding spherical seed particles at 70 °C (Fig. 11B). Upon cooling to 23 °C, the morphology of the particles altered and started to become kinetically trapped to produce hollow particles composed of stacked toroids. Addition of small amounts of toluene broke apart the superstructure to yield individual toroids in solution. Altering the end-group functionality of the macro-CTA allowed for introducing a variety of functional groups, which were later exclusively presented on the toroid surface which rendered them useful for protein binding or post-functionalisation reactions.

4. Polymeric nanoscale platelets

Disc-shaped cell fragments, for example, found in blood are commonly referred to as platelets. Polymer chemists borrowed this name to describe platelet-like objects, like self-assembled 2D materials. In this review, we have made the distinction between polymer discs and platelets: discs have smooth circular contours (see Section 2), while platelets feature a distinctly edged or facetted contour, stemming from their assembly method. The formation of 2D platelet-like nanoparticles and nanosheets has primarily been achieved through crystallisation-driven self-assembly (CDSA) and has come a long way from the early studies by Lotz et al. in the 1960s where they showed that block copolymers (PEO-b-PS) can crystallise into large 2D crystals in ethylbenzene.¹⁶²

4.1 Crystallisation-driven self-assembly, CDSA

Several recent reviews describe the history, opportunities and challenges of CDSA comprehensively.^163–165 CDSA involves the (controlled) crystallisation of crystalline (co)polymers, allowing for the growth of polymer particles in 1D, 2D and 3D. In particular, the use of seeds to facilitate a “seeded growth” has proven valuable in controlling the morphologies and dimensions of polymer particles: from nm to mm scale (Scheme 3). Seeded growth is typically also referred to as “living” CDSA, as it allows for the process to operate under kinetic control which bears similarities to living chain-growth polymerizations, where unimers can be added to increase the size of self-assembled structures. In this fashion, by controlling unimer addition to a system, the dimensions of particles may also be controlled. In this subchapter, we will focus on reported 2D shapes, control over their size and properties, and delve into potential applications of 2D platelets. Our aim is to provide a broader overview of this self-assembly method and the various polymer systems that have been reported to form 2D objects. We have arranged this chapter to highlight especially the crystalline components of the polymers and provided a general overview of recent (co)polymer composition and self-assembly pathways in Table 3. For polymer platelets grown by CDSA, we refrain from listing their dimensions as they are reported inconsistently (e.g., surface area vs. dimensions) and their extraction and comparison from micrographs is complicated by stark differences in platelet morphologies (e.g., squares, hexagons, diamonds, etc.). In addition, most of the CDSA platelets have been grown to micron-sized proportions, and our review has a focus on nanoscale materials. That said, most of the crystallisation-derived materials grow from the bottom-up and hence, at some stage, were nanoscale objects that most likely can be isolated.

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As CDSA is a self-assembly method driven by the crystallisation of polymers, the most used materials are therefore copolymers with a crystalline and a non-crystalline block. The crystallisation, like many crystalline materials, can be strongly influenced by temperature and solvent choice, amongst other parameters. Using a diblock copolymer as an example, the crystallisation of one block in a selective solvent leads to the formation of a micelle with a crystalline core that is stabilised by a solvated corona.¹⁶⁶ The accessible shapes of the micelles are strongly influenced by block ratio and the crystallinity of the core. BCPs with high corona-to-core block ratio typically yield cylindrical structures,¹⁶⁷ while planar platelets can be achieved at lower corona-to-core block ratios.¹⁶⁸

5. Summary and potential future applications

5.1 Discs and platelets

The synthesis strategies to achieve polymer nanodisc and platelet formation in solution abide by various key design principles, chiefly by the ability to direct block copolymers to pack into a planar morphology. While we are able to categorize disc formation into broader concepts, there are currently no universal guidelines that inform how to achieve disc formation from any (co)polymer. However, by ensuring a asymmetrical block ratio with distinctly different polarity and miscibility, it becomes possible to design polymers to maximise chances for 2D self-assembly. Whether a disc can be formed is then largely dependent on the solvent effect and the interfacial energy. Especially for direct(ed) self-assembly in solution, amphiphilic copolymers have been most used. However, self-assembly of any copolymer with distinct and segmented polarity differences should be able to self-assemble in appropriate solvent conditions, with the chance to achieve disc formation increased by incorporating segments that are either highly incompatible with their surroundings and/or prefer to strongly interact with each other. Extrinsic controls such as solvent quality and mixture, as well as intrinsic controls such as polymer type, architecture, and intramolecular interactions, present a vast playground to tailor their formation. Especially CDSA has recently become an extensively utilised approach to grow disc/platelet-like polymer (nano)particles, as crystalline−coil block copolymers favour the formation of micelles with low interfacial curvature. In addition, templates and pre-formed superstructures can assist in fabricating nanodiscs, especially with Janus character. With some of the synthetic hurdles lowered in recent years, researchers are now able to apply such 2D polymer materials in exciting areas, most notably (bio)nanotechnology and nanomedicine.

Modularity in surface chemistry and functionalisation are typically highlighted as major advantages of polymer-based nanomedicines. Nanoparticle delivery systems afford increased circulation and improve targeting.^227–229 More importantly, the past decade has underscored the critical importance of size and shape of nanoparticles in the context of drug delivery applications which now provides new possibilities in steering nanoparticle behaviour in vivo.²⁸ Moreover, anisotropic particles have been shown to travel through blood vessels differently compared to commonly used spherical nanomaterials,^26,230,231 preluding new opportunities in particle design. Much of the past decade had a strong focus on sphere vs. 1D (rods, cylinders) studies. But attention is shifting towards 2D materials, like synthetic nanoscale discs and platelets, as they may further improve our control to govern nanoparticle-cell interactions. The ability to reliably and uniformly produce 2D materials, such as discs and platelets, fuels further investigation into the benefits of such particles for drug delivery applications. Specifically, the possibility to improve margination, whereby high-aspect ratio particles are expected to experience flow differently in circulation and hence gravitate towards vessel walls.^232–234 The increased surface area of 2D objects may further aid development in targeted drug delivery or improve passive delivery due to altered internalisation velocity and clearance profiles.²³⁴ Discs and platelets present increased surface areas for targeted particle-cell interactions and have been found desirable over conventional spherical analogues.^235–238 Early studies by Chen and co-workers highlighted that cell uptake of micron-sized PEO-b-PCL platelets varied between cell lines.²⁰¹ While phagocytosis was shown to be dominant in macrophages (e.g. RAW264.7), micro-sized platelets were barely internalized into HUVECs and HeLa cells. Stenzel and co-workers observed that CDSA-derived platelets of polycaprolactone-block-poly(1-O-acryloyl-β-D-fructopyranose) (PCL-b-PF) were preferentially taken up by macrophages and readily processed and degraded intracellularly within a day.²²³ Glycoplatelets can be further used in drug delivery applications by functionalizing their surface with small molecules, such as drugs or fluorescent dyes (Fig. 13A).²²² It is also possible to construct stimuli-responsive polymer platelets comprising compartments that can load and release cytotoxic cargo in aqueous environments.²²⁵ Many studies using polymer platelets typically exceed desired dimensions for in vivo applications, i.e. particles should not exceed an overall size of 200 nm. However, with more reliable methods to self-assemble polymer nanodiscs and the fact that CDSA should technically be able to be stopped at any time to yield smaller platelets/discs, future studies will have the opportunity to study the potential benefits of nanoscale 2D materials in vivo more closely.

Earlier we acknowledged the vast literature around lipid-based nanodiscs. Inspiration from their use as a nanocarrier, especially in cancer treatment, will likely further inform design principles of pure polymer nanodiscs.^239,240 Beyond cancer, naturally occurring nanodiscs, such as high density lipid proteins (HDLs) for cholesterol sequestration may spark new research ideas in mimicking naturally occurring nanoparticles; more so now that synthetic difficulties are being alleviated to make polymeric analogues. Another synthetic route worth exploring has been shown by Pinkhassik and co-workers, whereby discoidal lipid aggregates can be used as a nanoreactor for polymerisation, affording polymer nanodiscs in a straightforward manner.^241,242 Many self-assembled polymer nanodiscs can be grown from clinically approved materials, such as PLA, PCL, PEG, and therefore maximise success in potential translational endeavours. The possibility to degrade polyester-containing platelets provides a favourable characteristic in the context of biomedical applications of these nanomaterials,²⁴³ as is the ability to either produce them directly in water or transfer them into aqueous environments after their fabrication.

At the same time, several biologically derived and inspired materials have been incorporated into 2D nanoparticles. From peptoids to amyloid fibrils and glyco-polymers, these materials have been copolymerised into polymers that can undergo crystallisation and form 2D particles. Platelet-like structures made from amyloid fibrils were reported by the groups of Wei, Zhang and Liu.²⁴⁴ Using amyloid fibrils, they formed nanosheets and cylinders and demonstrated that these could be used for the transduction of viruses. The lysine residues in the proteins were expressed at the surface of the sheets, giving them a strong positive charge that could carry virus particles and performed laboratorial retroviral transduction. The non-assembled, cylindrical, amyloid fibrils were also able to carry the virus particles but were not as effective as enhancers for retroviral transduction as the assembled nanosheets, despite having the same number of lysine residues. While these sheets are made from natural materials rather than synthetic polymers and therefore outside the scope of this review, this is a demonstration of the difference that the shape of particles can play in their application to technologies.

Moreover, nanoparticle shape can induce a range of immune responses.²⁴⁵ Using CDSA of various block copolymers with a glycopolymer corona block and a PLA core block, a range of nano-sized carbohydrate-coated platelets could be designed and tested for their shape-dependent immune-stimulation (Fig. 13A).²⁰⁸ Interestingly, platelet-like glyconanoparticles were more efficient in inducing inflammatory responses when compared to cylinders. Similarly, smaller platelets demonstrated a more effective stimulation of the immune system. The size also played a role when polymer platelets with a quaternized PDMAEMA shell were tested for their antimicrobial activity, with smaller platelets exhibiting increased activity.²⁰⁷ When polymer platelets were added to hydrogels, they improved the mechanical properties.²²¹ Platelets enhanced the hydrogel resistance to breaking under strain compared to their spherical and cylindrical counterparts.

Aside from health-related applications, 2D materials are interesting components in Pickering emulsions or as particle-based surfactants more generally. Control over the size of the platelets is an added advantage when stabilizing water-in-water emulsions, where smaller platelets increase droplet stability compared to their larger analogues.²⁰⁶ The ability to generate Janus character in polymer nanodiscs will increase their potency in interfacial applications and may allow them to be used to structure emulsions and dispersions via dialling in interface stabilisation.²³⁹ Some examples mentioned prior by Yang and Gröschel already demonstrate the preliminary use of Janus-type discs in this manner, with stabilisation of cyclohexane–water and toluene–water emulsions with PEO/PS and PMMA/PSS amphiphilic discs respectively.^74,87 Janus-type nanodiscs may also find applications in polymer blends where their customisable size and surface chemistry will allow for tuning blend composition, domain sizes and hence mechanical properties, more universally.²⁴⁶ Moreover, the ability to control the surface chemistry of nanodiscs may render them useful in template chemistry and allow 2D inorganic and hybrid materials fabrication that is not based on traditional crystal growth methods. Some examples have already shown the possibility of hybridising nanodiscs with inorganic matter.^70,74,83,87 Long et al. for example demonstrated organic/inorganic nano-patterning by selectively localising silver into defined regions within a nanodisc, generating unique, functional domains within a single particle (Fig. 13B).⁷⁰ Such patterning might be useful for catalytic nano-platforms with broad solvent compatibility. The anisotropic shape of polymer platelets was exploited for the formation of nanomotors.²⁴⁷ Gold, platinum and iron oxide nanoparticles were deposited onto a PCL single crystal platelet. Using optical microscopy, the platelet motors were observed to rotate and move when an external magnetic field was applied. Hydrogen peroxide could also be used as a fuel for stimulating nanomotor movement.

5.2 Toroids

The precision synthesis of toroids remains a knowledge gap. While several core principles of their formation seem to emerge, like the end-to-end closure of cylindrical micelles with tailored stiffness, overall toroid formation is still rather sporadically reported. Therefore, their application potential is rarely tested. Inspiration can however be taken by other systems that are not based on macromolecules. Supramolecular toroids made of molecules rather than macromolecules have already demonstrated their potential usefulness in various areas.^248–250 With enhanced synthetic avenues to produce uniform polymer toroids, their applications are set to grow in future years. Especially with their use in nanomedicine, template chemistry, and as building blocks for hierarchical superstructures, their diverse applications are emerging.

Toroidal nanostructures may hold untapped potential in nanomedicine. Aside from the fact that naturally occurring DNA is also able to pack into distinct toroidal structures,²⁵¹ several studies attest the ring-shaped arrangement of genetic materials enhanced rates of transfection into cells.^252,253 Kataoka and colleagues demonstrated that packaging pDNA (akin to viral genomic packaging) into toroid-shaped micelles boosted transcription efficiency and showed higher in vivo gene transfer efficacy, when compared to rod-like analogues.²⁵⁴ Similar advantages have been ascribed to nanoscale polymer rings for drug delivery.^255,256

Nano- and meso-porous materials are crucial in many applications, ranging from membranes and adsorbents to catalyst supports and storage systems.²⁵⁷ Building on the pioneering work of Huang et al.¹¹⁸ in making uniform toroids via the direct self-assembly of diblock copolymers, Qiu and co-workers have made excellent progress in further understanding the self-assembly of PI₁₀₄₀-b-P2VP₂₀₀.¹⁵⁹ Also using THF:ethanol (1:4 w/w) solvent mixtures, they investigated ways to manipulate the toroidal assemblies as building blocks to form superstructures. Aggregation of the toroids did not occur when the solution was concentrated, however the addition of a second diblock copolymer, poly(ferrocenyldimethylsilane)-b-P2VP (namely PFS₅-b-P2VP₇₀ and PFS₂₀-b-P2VP₁₄₀), caused the toroids to interact and coalesce into a planar network (Fig. 14A). The smaller diblock copolymers were found to create small, oligomeric supermicelles consisting of 2 to 10 toroids bound together. The larger diblock copolymers resulted in planar arrays with areas exceeding 100 μm². The PFS block was necessary, as the P2VP homopolymer did not cause any aggregation of toroids. The hydrophobic nature of the PFS block was thought to rapidly precipitate on the PI cores. By further increasing the hydrogen bonding of these diblock copolymers by including hydroxyl groups that can hydrogen bond with the P2VP coronas, 3D toroidal sponge arrays were formed. This work showed how toroidal assemblies can be used as hierarchical building blocks. In this context, Guerin and co-workers used crystallisation-driven self-assembly to form 2D and 3D multi-tori mesostructures from the interplay of two diblock copolymers (Fig. 14B).¹⁶⁰ PFS₂₆-b-PS₃₀₆ self-assembled into micrometre-large raspberry-like vesicles. In the presence of crystalline seed micelles form by PFS₅₅-b-PI₅₀₀, the PFS₂₆-b-PS₃₀₆ formed cylindrical core–shell micelles within the vesicle, forcing them to grow concentrically around the droplet to become toroids. Polymer toroid networks have also been seen by Förster and co-workers who studied the self-assembly of poly(ethylethylene)-block-poly(styrenesulfonic acid) (PEE-b-PSS) in varying salt concentrations.¹⁵⁶ Charge, salt concentration and polymer concentration were found to impact the rigidity of the formed micelles, and hence played a role in toroid structure formation and their assembly into fractal networks. Supramolecular toroids have recently been shown to undergo an autonomous helical propagation to form 1D spring-like nanomaterials.^258,259 Uniform polymer toroids may be adapted to act similarly, generating nanomaterials that may interact with light. Notably, rod-coil block copolymers have already demonstrated sizable similarity to small molecule self-assembly.²⁶⁰

The interior cavity in toroids has been used as a confined nanoreactor to control the growth of inorganic nanomaterials.^261–264 The use of polymers in templated synthesis of hybrid, composite and inorganic materials is well document and explored.²⁶⁵ Ring-shaped nanomaterials however remain difficult to fabricate and toroidal templates offer a promising synthetic strategy.^118,147,266 Yang and co-workers used a symmetric ABA triblock copolymer PVP₄₃-b-PS₂₆₀-b-PVP₄₃ to generate toroidal template particles where the polyelectrolyte shell could be further used to incorporate inorganic precursors (Fig. 14C).¹⁵⁸ This acts as a general example for core–shell templating, the likes of which can be found using other core–shell structures, such as filomicelles and MPBs.^267–271 Pathways to controllably access metal nanorings may provide new materials with unique optical and superconducting properties.^272,273 A rather unusual way of using a polymer toroid was recently described by Qiu and co-workers, whereby the toroid acted as a “micellar rubber band” to wrap around an inorganic colloid, generating an intriguing hybrid material that was likened to a colloidal version of “Saturn”.¹⁶¹ These polymer rubber bands could also be used to grow silica discs within their cavity. Earlier, Chen and co-workers had also used uniform polymer toroids based in PEG-b-P4PVP to wrap around negatively charged colloids.¹⁴⁹

6. Conclusions and outlook

The ability to produce tailor-made and uniform polymer nanomaterials in the shape of discs, rings and platelets has significantly improved over the past decade. Much of the gained control is owed to an in-depth understanding and deliberate manipulation of key design principles that govern polymer self-assembly in solution. Precisely controlling important factors, such as chain rigidity and solvent conditions, has become fundamental in accessing complex polymer self-assemblies directly from solution. The use of crystallisation or rod-coil-like copolymers has endowed some of these processes with ‘living’-like kinetic control that allow growth and composition to be tailored like never before. With access to advanced functional nanomaterials, the potential of these exquisite polymer nanoparticles can now be assessed in more applied research. Advances have also been made in the generation of nanoparticles that are able to degrade and decompose, an attribute especially important to biomedical applications. Looking ahead, the production of these nanomaterials in larger quantities will need to be addressed. Opportunities to alter processing parameters such a shear rates may aid this endeavour.¹³³ Establishing protocols that make use of the advantages of heterophase systems, such as PISA, may hold promise in achieving complex architectures at high solid content.⁷³ Emulsion-confined self-assembly has demonstrated its potential to produce nanodiscs and toroids, but exhibits further untapped potential, especially in using discrete nanoparticles in conjunction with (co)polymers.²⁷⁴ Similarly, the use of pre-segmented polymer particles, like MPBs, adds another feature to this type of self-assembly as MPBs are both a nanoparticle as well as a giant copolymer-like macromolecule.²⁶⁷

Further inspiration and design principles may be taken directly from nature, who is able to pack DNA into well-defined objects. DNA origami is a very powerful tool in the precision fabrication of nanoscale functional soft matter. Structuring DNA into modular 3D nano-objects has allowed it to be applied in drug/gene delivery, photonics, nanoreactors, in catalysis or as membrane nanopores.^275–277 While some of the complexity may not be matched yet by synthetic polymer chemistry, our review has shown that intricate, functional nano-objects can be synthesized of relatively simple, cost-effective, and stable polymeric materials; potentially overcoming some inherent challenges of working with DNA.²⁷⁸ For example, membrane nanopores enabled with DNA may well be realised using functional polymer toroids in the future.^249,279,280 Specifically for toroids, or ring-shaped polymer particles, the use of MPBs seems obvious. While this review focuses on self-assembly strategies, polymer nanorings can also be produced uniformly by grafting cyclic backbones with polymer sidechains.²⁸¹ Overall, the past decade has significantly advanced our ability to generate complex polymer nanoparticle morphologies. With more generalisable design principles now established, the next decade will likely be focused on endowing these materials with functionality and function. Establishing the true potential of nanodiscs, toroids and platelets is just in its beginnings, and we hope this review motivates researchers beyond synthetic chemistry to work with these fascinating nanomaterials.

List of abbreviations

Å	Ångstrom
AA	Acrylic acid
AC60−	Anionic(C60-Ih)[5,6]fullerene
AFM	Atomic force microscopy
C18TAB	Trimethyloctadecylammonium bromide
C3M	Coacervate core micelle
CDSA	Crystallisation-driven self-assembly
Cryo-TEM	Cryogenic transmission electron microscopy
CTA	Chain transfer agent
CTAB	Cetyltrimethyl ammonium bromide
DGEBA	Diglycidylether of bisphenol A
DLS	Dynamic light scattering
DMAEMA	2-(Dimethylamino)ethyl methacrylate
DMF	Dimethyl formamide
DNA	Deoxyribonucleic acid
DSC	Differential scanning calorimetry
EDDA	Ethylenediaminediacetic acid
EGCD	Ethylene glycol cyclodextrin
EHMA	2-Ethylhexyl methacrylate
FIPA	Fusion-induced particle assembly
FPOSS	Fluorinated polyhedral oligomeric silsesquioxane
HRP	Horseradish peroxidase
iPS	Isotactic polystyrene
LC	Liquid crystalline
LC	Liquid crystalline
LCSM	Laser confocal scanning microscopy
LCST	Lower critical solution temperature
LPE	Linear polyethylene
MAA	Methacrylic acid
macro-CTA	Macro chain transfer agent
Mb	Myoglobin
MeOx	2-Methyl-2-oxazoline
METAC	(2(Methacryloyloxy)ethyl)trimethylammonium chloride
MPBs	Molecular polymer bottlebrushes
mPEG	Poly(ethylene glycol) monomethyl ether
MTC-Chol	2-(5-Methyl-2-oxo-1,3-dioxane-5-carboxyloyloxy)ethyl carbamate
NaSS	Sodium styrene sulfonate
NC60+	Neutral (C60-Ih)[5,6]fullerene
NOESY	Nuclear Overhauser effect spectroscopy
OPBA	Oligo (p-benzamide)
P[CE][AOT]	Poly(cobaltoceniumethylene)[bis(2-ethylhexyl) sulfosuccinate]
P2MVP	Poly(2-methylvinylpyridinium iodide)
P2VP	Poly(2-vinylpyridine)
P3HT	Poly(3-hexylthiophene)
P4VP	Poly(4-vinylpyridine)
PAA	Poly(acrylic acid)
PAAm	Polyacrylamide
PAGE	Poly(allyl glycidyl ether)
PB	Polybutadiene
PBLG	Poly(γ-benzyl-L-glutamate)
PBPyAA	Poly(N-(2,2′-bipyridyl)-4-acrylamide)
PCEMA	Poly(2-cinnamoyloxylethyl methacrylate)
PCL	Poly(ε-caprolactone)
PCoAEMA	Poly(cobaltocenium amidoethyl methacrylate)
PCPTM	Polymerized camptothecin prodrug monomer
PCPV	Poly(cyclopentenylene-vinylene)
PDDL	Poly(λ-dodecanolactone)
PDLA	Poly(D-lactide)
PDLLA	Poly(D,L-lactide)
PDMA	Poly(N,N-dimethylacrylamide)
PDMAEMA	Poly(2-(dimethylamino)ethyl methacrylate)
PDMS	Polydimethylsiloxane
PDP	Pentadecylphenol
PDPA	Poly(2-(diisopropylamino)ethyl methacrylate)
PE	Polyethylene
PEG	Poly(ethylene glycol)
PEO	Poly(ethylene oxide)
PEP	Poly(ethylene propylene)
PF	Poly(1-O-acryloyl-D-fructopyranose)
P[F-co-BMDO]	Poly[(1-O-acryloyl-D-fructopyranose)-co-(5,6-benzo-2-meth-ylene-1,3-dioxepane)]
PFluoro	Poly(hexafluoroethane)
PFDMG	Poly(ferrocenyldimethylgermane)
PFMA	Poly(perfluoro octylethyl methacrylate)
PFPO	Poly(hexafluoropropylene oxide)
PFS	Poly(ferrocenyldimethylsilane)
PGMA	Poly(glycidyl methacrylate)
PHEA	Poly(2-hydroxyethyl acrylate)
PHEMA	Poly(2-hydroxyethyl methacrylate)
PHIC	Poly(n-hexylisocyanate)
PHL	Poly(heptalactone)
PHNA	Poly[2-hydroxy-3-(naphthalen-1-ylamino)propyl methacrylate]
PHOS	Poly(p-hydroxylstyrene)
PHOVE	Poly(2-hydroxyethyl vinyl ether)
PhOX	2-Phenyl-2-oxazoline
PI	Polyisoprene
PISA	Polymerisation-induced self-assembly
PLA	Polylactide
PLys	Poly(L-lysine)
PM	Polymethylene
PMA	Poly(methyl acrylate)
PMAStbn	Poly(11-(4-((E)-4-butylstyryl)phenoxy)undecyl methacrylate)
PMBPS	Poly{(+)-2,5-bis[4′-((S)-2-methylbutoxy)phenyl]styrene}
PMMA	Poly(methyl methacrylate)
PMPC	Poly(2-(methacryloyloxy)ethyl phosphorylcholine)
PnBA	Poly(n-butyl acrylate)
PNDG	Poly(N-decyl glycine)
PNEHG	Poly(N-2-ethyl-1-hexylglycine)
PNIPAM	Poly(N-isopropylacrylamide)
PNMEP	Poly(N-(2-methacryloyloxyethyl)pyrrolidone)
PNMG	Poly(N-methyl glycine)
PNOG	Poly(N-octyl glycine)
PNPE	Poly(N-(2-phenylethyl)glycine)
POM	Polyoxometalate
PPEGMA	Poly[poly(ethylene glycol) methyl ether methacrylate]
PPO	Poly(propylene oxide)
PS	Polystyrene
PSS	Poly(styrene sulfonate)
PTFEP	Poly[bis(trifluoroethoxy)phosphazene]
RAFT	Reversible addition–fragmentation chain-transfer
ROMP	Ring opening metathesis polymerisation
ROPI-CDSA	Ring opening polymerisation-induced crystallisation driven self-assembly
SANS	Small-angle neutron scattering
SAXS	Small-angle X-ray scattering
SEM	Scanning electron microscopy
SLS	Static light scattering
SSP	Supramolecular star polymers
SSSR	Superstrong segregation regime
tBMA	tert-Butyl methacrylate
TDMT	Temperature-directed morphology transformation
TEM	Transmission electron microscopy
TPE	Tetraphenylethene
WAXS	Wide-angle X-ray scattering

Author contributions

E. R. L. B. and M. J. H. W. contributed equally. M. M. conceived the proposal and synopsis. E. R. L. B. prepared the initial draft, and all co-authors contributed to literature revision and the writing of the final version.

Conflicts of interest

There are no conflicts to declare.

Acknowledgements

M. M. acknowledges the Australian Research Council for a DECRA (DE180100007, supporting E. R. L. B.), Future Fellowship (FT200100185, supporting M. J. H. W. and S. K.) and Discovery Project (DP220100452), respectively. M. M. is a grateful recipient of a University of Sydney Research Accelerator (SOAR) Prize.

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