Superhydrophobic Surface-Assisted Preparation of Microspheres and Supraparticles and Their Applications

Pan, Mengyao; Shao, Huijuan; Fan, Yue; Yang, **long; Liu, Jiaxin; Deng, Zhongqian; Liu, Zhenda; Chen, Zhidi; Zhang, Jun; Yi, Kangfeng; Su, Yucai; Wang, Dehui; Deng, Xu; Deng, Fei

doi:10.1007/s40820-023-01284-2

Superhydrophobic Surface-Assisted Preparation of Microspheres and Supraparticles and Their Applications

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Published: 04 January 2024

Volume 16, article number 68, (2024)
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Superhydrophobic Surface-Assisted Preparation of Microspheres and Supraparticles and Their Applications

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Mengyao Pan^1,3,
Huijuan Shao¹,
Yue Fan²,
**long Yang¹,
Jiaxin Liu¹,
Zhongqian Deng¹,
Zhenda Liu¹,
Zhidi Chen¹,
Jun Zhang⁴,
Kangfeng Yi⁴,
Yucai Su⁴,
Dehui Wang¹,
Xu Deng³ &
…
Fei Deng^5,6

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Highlights

An overview of the superhydrophobic surface -assisted strategies for fabricating microspheres and supraparticles are presented.
The applications of microspheres and supraparticles fabricated using SHS-assisted strategies are discussed in detail.
NCrucial challenges facing the development of microspheres and supraparticles fabricated through SHS-assisted strategies are analysed.

Abstract

Superhydrophobic surface (SHS) has been well developed, as SHS renders the property of minimizing the water/solid contact interface. Water droplets deposited onto SHS with contact angles exceeding 150°, allow them to retain spherical shapes, and the low adhesion of SHS facilitates easy droplet collection when tilting the substrate. These characteristics make SHS suitable for a wide range of applications. One particularly promising application is the fabrication of microsphere and supraparticle materials. SHS offers a distinct advantage as a universal platform capable of providing customized services for a variety of microspheres and supraparticles. In this review, an overview of the strategies for fabricating microspheres and supraparticles with the aid of SHS, including cross-linking process, polymer melting, and droplet template evaporation methods, is first presented. Then, the applications of microspheres and supraparticles formed onto SHS are discussed in detail, for example, fabricating photonic devices with controllable structures and tunable structural colors, acting as catalysts with emerging or synergetic properties, being integrated into the biomedical field to construct the devices with different medicinal purposes, being utilized for inducing protein crystallization and detecting trace amounts of analytes. Finally, the perspective on future developments involved with this research field is given, along with some obstacles and opportunities.

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1 Introduction

Wettability, typically defined as the tendency of a liquid to spread out on a solid, has been one of the most important characteristics of a solid surface. The superhydrophobic surface (SHS) represents a specific solid surface on which a droplet of water shows a contact angle greater than 150°, thus manifesting excellent water repellency. It is found that biological surfaces, such as those of certain plants and animals, exhibit excellent superhydrophobic capabilities due to their suitable morphologies and specific surface chemistry properties [1,2,3]. Inspired by nature, superhydrophobicity has been successfully mimicked through a rational design of surface roughness and proper regulation of surface energy [4,5,6]. The extensive design and fabrication of artificial SHS have driven the potential development in many fields, such as self-cleaning [5, 7,8,9], anti-fogging [10,11,12,13,14], anti-icing [15,16,17,18,19], oil/water separation [20,21,22,23], water collection [24,25,26,27], liquid transportation [28,32,33,104]. Copyright 2019, American Chemical Society

Schematic illustration of the formation of the supraparticles via a SHS-assisted droplet template evaporation strategy. a Spherical supraparticle.

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2.3.2.1 Fabricating Supraparticles with Controllable Sizes

The size of the supraparticles primarily depends on the volume of the original droplets and the concentration of NPs within them [67]. By manipulating these two factors, it is possible to generate supraparticles with diameters ranging from a few microns to sub-millimeters [67, 102, 105,106,107]. The upper boundary of size is dictated by gravitational forces, which, in the case of drops exceeding the capillary length, will result in drop flattening. Conversely, the fundamental lower constraint depends on the inter-protrusion spacing of rough SHS, since particles smaller than this spacing are capable of permeating SHS and causing it to be wet [64].

2.3.2.2 Constructing Supraparticles with Diverse Morphologies

The morphology of supraparticles is mainly governed by the initial morphology of droplets and the dynamic behavior of the TPCL) during the evaporation process [68]. These two factors, in turn, typically depend on the surface utilized and the characteristics of the NP suspension. Employing appropriately designed surfaces is one of the methods to achieve diverse supraparticle morphologies [99,100,101], but this study focuses solely on low-adhesion SHS. When a droplet of NP suspension is deposited on SHS, it initially maintains a spherical shape with a contact angle of more than 150°. Consequently, the motion behavior of TPCL is regarded as the crucial factor in determining the morphologies of supraparticles. In general, the TPCL freely moves over the SHS during evaporation, forming a spherical supraparticle (Fig. 5a) [67, 102, 105,106,107]. Substituting NPs with different types of colloids, such as nano-cubes, nano-plates, and nano-sheets, has no effect on supraparticle morphology [108].

Numerous approaches have been reported to regulate the dynamic behavior of TPCL for the purpose of morphology manipulation, which can be broadly categorized into two main categories. One approach involves altering the properties of NP suspensions, while the other involves introducing magnetic components into suspensions and applying an external magnetic field. For example, when adjusting the concentration of the original NP suspension to a low critical value, the TPCL remains continuously receding at the beginning, leading to a reduction in droplet size. With the further extension of evaporation time, the NPs become confined in the vicinity of the TPCL, resulting in TPCL pinning. In the final phase of evaporation, there is a notable decrease in the height of the droplet in relation to the meridian radius, causing a curvature at the center. This phenomenon becomes more pronounced as the concentration decreases (Fig. 5b) [109]. Therefore, as the concentration continuously decreases below the threshold, the in-folded or concave sphere [103, 109]、doughnut-like [103, 110], or even coffee ring [103, 111] shaped supraparticles can be realized successively. By introducing sucrose into a colloidal dispersion with varying concentration, the supraparticle morphology can be further altered, resulting in a series of new forms on SHS, such as a three-quarter sphere with a dimpled bottom, a three-quarter sphere with a flat bottom, a bagel shape with a dimpled bottom, and a pizza shape with a dimpled bottom [112]. The emergence of these morphologies is due to sucrose acting as a shape-preservative during evaporation. Additionally, by utilizing suspensions containing NPs with specific forms and properties, such as CdSe/CdS nanorod suspension or 26 vol% alumina powder suspension, a hollow dome-shaped structure, also known as an inverted bowl shape, were successfully fabricated onto SHS [113, 114]. The formation of a hollow dome-shape can be attributed to the fact that the TPCL of the drop gets pinned and increased solute concentration induces a residue solidification, while the air pockets below the droplet remain throughout the evaporation process.

By adjusting both the concentration of superparamagnetic NPs in the suspension and the intensity of the applied magnetic field, various supraparticle morphologies such as barrel-like, cone-like, and two-tower-like structures were achieved on the SHS (Fig. 5c) [104].

Furthermore, anisometric-shaped supraparticles can also be produced by modifying the specific properties of the original NP solution, such as ion strength [115,116,117], NP density [108], NP mono-dispersity [102, 108], and even adding volatile solvent composition [118]. For example, anisometric boat-like and ellipsoidal supraparticles can be obtained by adding salt (e.g., NaCl) beyond a threshold into fumed silica NP suspensions and subsequently drying the suspension droplets on a flat or curved V-shaped SHS (Fig. 5d) [115,116,117].

In summary, the dynamic behaviors of the TPCL during the evaporation process have the following effects on droplet morphology: continuous and homogeneous receding of the TPCL promotes the formation of spherical or nearly spherical supraparticles, while the pinning of the TPCL during evaporation tends to result in symmetrical non-spherical structures. Asymmetric receding of the TPCL, with pinning in one direction and homogeneous receding in the perpendicular direction, facilitates the formation of anisotropic-shaped supraparticles [119].

2.3.2.3 Creating Supraparticles with Various Structures

Supraparticles with diverse structures can be obtained by SHS-assisted droplet template evaporation strategy. All supraparticles show mesoporous structures since they are formed by an aggregation of NPs [67, 120,121,11b) [173]. Furthermore, by combining this structure with a fluorescence device, DNA can be detected at concentrations as low as 10^–18 mol L⁻¹ [173].

While the above dual-functional structure can enhance detection sensitivity, there is an inevitable migration of droplets onto SHS during the evaporation process, leading to uncertain deposition sites. Hence, when performing SERS analysis, the surface should be completely examined unless the target is fluorescently labeled. To address this issue, Shin-Hyun Kim and colleagues proposed a structure with uneven density [174]. This structure was composed of the micropillar array with a radial density gradient, where the nanotip array was located on the top surface of each micropillar and Ag NPs were deposited on the nanotips. Since a radial density gradient of micropillar causes a radial gradient of contact angle onto the structure surface, the droplets can spontaneously move towards the central region with the highest density [174]. Consequently, the analyte dissolved in the droplets can be enriched at the central surface of the structure during the evaporation process (Fig. 11c) [174]. The analyte can be detected at predetermined positions using Raman spectra without requiring a complete scan of the substrate, thus significantly saving the detection time [174]. This makes it a general structure to promote the enrichment of the solute [175].

In summary, the SHS-assisted droplet template evaporation strategy plays a significant role in molecular detection, particularly for molecules with concentrations as low as the attomolar scale. Additionally, this approach has the potential to be integrated with various spectral analysis techniques (e.g., SERS spectra, fluorescence, and Raman), and is fully compatible with existing biological and medical protocols. Consequently, it is of great significance for the analysis of rare or hazardous chemicals involved in biomedical, food safety and ecological pollution.

4 Summary and Future Perspective

In this review, we have presented a comprehensive overview of the recent advancements in the field of SHS-assisted preparation of microspheres and supraparticles, as well as their applications. Firstly, the strategies for fabricating microspheres and supraparticles, including SHS-assisted cross-linking curing, SHS-assisted polymer melting, and SHS-assisted droplet template evaporation, have been presented. Especially, the preparation processes of supraparticles have been described in detail in terms of morphology, structure and properties. In addition, we also summarized the influence of the dynamic TPCL behavior of droplets during the evaporation process on the resulting shapes of supraparticles. Then, we demonstrated the wide range of applications for microspheres and supraparticles fabricated through the SHS-assisted strategies. These applications encompass advanced optical devices, catalysts with superior catalytic efficiency, drug delivery systems with controlled release rates, cell encapsulation materials with improved encapsulation efficiency, Polymer crystallization, and molecular trace detection.

Although significant progress has been made, there are still challenges and potential outcomes that need to be addressed. These difficulties and potential outcomes are outlined below:

(1)
Size and Shape Control: Achieving precise control over the size and shape of microspheres and supraparticles remains a challenge. While SHS-assisted methods offer some level of control, further optimization is needed to achieve mono-dispersity and uniformity in size and shape. Exploring the impact of original droplet size and solute concentration on the resulting particle size, as well as conducting systematic investigations into the factors influencing different supraparticle morphologies, will offer significant benefits for fine-tuning fabrication parameters in SHS-assisted methods. This exploration will lead to improved control over size and shape, ultimately enhancing reproducibility in the process.
(2)
Scalability and Production Efficiency: Scaling up the production of microspheres and supraparticles while maintaining their desired properties is an ongoing challenge in the field. SHS-assisted methods often involve complex fabrication processes that can be time-consuming and require specialized equipment to ensure uniform manufacturing. Additionally, these specialized equipment often have limited throughput, typically ranging from 100 to 1,000 droplets per second [64]. Develo** strategies to improve production efficiency, such as modifying microfluidic devices by integrating multiple channels and sprinklers, may be expected to enable the fast fabrication of microdroplets.
(3)
Reproducibility, Stability, and Durability: Ensuring the good reproducibility of the SHS-assisted methods, the long-term stability and durability of microspheres and supraparticles is essential for their practical applications. The reproducibility of the SHS-assisted methods mainly depends on the durability of SHS. Thus, investigating the impacts of various nano-microstructures and modification techniques on the durability of SHS, with the aim of finding a robust SHS, assumes significant importance in maintaining consistent production of supraparticles and microspheres. Concerning the stability and durability of microspheres and supraparticles, multiple factors come into play, including structural integrity, resistance to degradation, and stability under various environmental conditions. Exploring the factors holds promise for advancing the practical utility of microspheres and supraparticles.
(4)
Functionalization and Integration: Expanding the functionality and integration of microspheres and supraparticles is a promising direction for future research. SHS-assisted methods can potentially enable the incorporation of functional elements or materials within the microspheres or on their surfaces. Develo** strategies for precise functionalization and integration will enhance their capabilities and enable new applications. One example is the combination of catalytic performance with controlled self-propelled motion features, which holds significant potential across various domains, including oil cleanup, pollutant decomposition, agitation and mixing, and selective chemical reactions. Another area of interest is the development of multiple-compartment microspheres that enable the sequential release of multiple drugs. Although multi-compartment structures and drug delivery systems with controlled release rates have been developed, the diffusion of drugs between chambers and the external environment remains an unavoidable issue, which leads to the failure of sequential delivery. To address this problem, it is important to select drug delivery systems with large release rate differences. The integration of these systems into a single drug delivery system holds significant potential for achieving sequential drug release. In summary, the functionalization and integration of microspheres and supraparticles offer exciting prospects for future research.
(5)
Characterization and Understanding: Comprehensive characterization techniques and an in-depth understanding of the formation mechanisms are essential for further advancements in microspheres and supraparticles fabricated by SHS-assisted methods. Efforts should be made to develop advanced characterization techniques that provide detailed information about their structural, optical, mechanical, and chemical properties. This knowledge will contribute to the optimization of fabrication processes and the development of tailored microspheres and supraparticles.

By addressing these challenges and exploring their potential outcomes, further advancements can be achieved in the SHS-assisted preparations of microspheres and supraparticles, as well as their applications. Overcoming these challenges will bring new opportunities for their use in various fields, including materials science, biotechnology, medicine, and environmental applications.

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Acknowledgements

We acknowledge the financial support from Shenzhen Science and Technology Program (JCYJ20210324142210027, X.D.), the National Natural Science Foundation of China (52103136, 22275028, U22A20153, 22102017, 22302033, and 52106194), the Sichuan Outstanding Young Scholars Foundation (2021JDJQ0013), Natural Science Foundation of Sichuan Province (2022NSFSC1271) and Sichuan Science and Technology Program (2023JDRC0082); “Oncology Medical Engineering Innovation Foundation” project of University of Electronic Science and Technology of China and Sichuan Cancer Hospital (ZYGX2021YGCX009); “Medical and Industrial Cross Foundation” of University of Electronic Science and Technology of China and Sichuan Provincial People’s Hospital (ZYGX2021YGLH207). Shandong Key R&D grant (2022CXGC010509)

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Institute of Fundamental and Frontier Sciences, University of Electronic Science and Technology of China, Chengdu, 611731, People’s Republic of China
Mengyao Pan, Huijuan Shao, **long Yang, Jiaxin Liu, Zhongqian Deng, Zhenda Liu, Zhidi Chen & Dehui Wang
School of Materials Science and Engineering, Sun Yat-Sen University, Guangzhou, 510275, People’s Republic of China
Yue Fan
Shenzhen Institute for Advanced Study, University of Electronic Science and Technology of China, Shenzhen, 518110, People’s Republic of China
Mengyao Pan & Xu Deng
Pharmaceutical Glass Co. Ltd, Zibo, 256100, People’s Republic of China
Jun Zhang, Kangfeng Yi & Yucai Su
Department of Nephropathy, School of Medicine, Sichuan Provincial People’s Hospital, University of Electronic Science and Technology of China, Chengdu, People’s Republic of China
Fei Deng
Department of Nephrology, Sichuan Provincial People’s Hospital **niu Hospital, Chengdu **niu District People’s Hospital, Chengdu, People’s Republic of China
Fei Deng

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Mengyao Pan
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Huijuan Shao
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Yue Fan
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**long Yang
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Jiaxin Liu
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Zhenda Liu
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Zhidi Chen
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Jun Zhang
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Kangfeng Yi
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Yucai Su
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Dehui Wang
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Xu Deng
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Fei Deng
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Correspondence to Dehui Wang, Xu Deng or Fei Deng.

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Pan, M., Shao, H., Fan, Y. et al. Superhydrophobic Surface-Assisted Preparation of Microspheres and Supraparticles and Their Applications. Nano-Micro Lett. 16, 68 (2024). https://doi.org/10.1007/s40820-023-01284-2

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Received: 14 July 2023
Accepted: 09 November 2023
Published: 04 January 2024
DOI: https://doi.org/10.1007/s40820-023-01284-2

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Superhydrophobic Surface-Assisted Preparation of Microspheres and Supraparticles and Their Applications