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Past, Present and Future Perspectives on Halloysite Clay Minerals

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Past, Present and Future Perspectives on Halloysite Clay Minerals molecules Review Past, Present and Future Perspectives on Halloysite Clay Minerals Marina Massaro * , Renato Noto and Serena Riela * Department of Biological, Chemical and Pharmaceutical Sciences and Technologies (STEBICEF), University of Palermo Viale delle Scienze, Ed. 17, 90128 Palermo, Italy; [email protected] * Correspondence: [email protected] (M.M.); [email protected] (S.R.) Academic Editor: Ali Nazemi Received: 30 September 2020; Accepted: 17 October 2020; Published: 21 October 2020 Abstract: Halloysite nanotubes (HNTs), clay minerals belonging to the kaolin groups, are emerging nanomaterials which have attracted the attention of the scientific community due to their interesting features, such as low-cost, availability and biocompatibility. In addition, their large surface area and tubular structure have led to HNTs’ application in different industrial purposes. This review reports a comprehensive overview of the historical background of HNT utilization in the last 20 years. In particular it will focus on the functionalization of the surfaces, both supramolecular and covalent, following applications in several fields, including biomedicine, environmental science and catalysis. Keywords: halloysite nanotubes; historical background; chemical modification; supramolecular functionalization 1. Introduction Halloysite nanotubes (HNTs) are clay minerals belonging to the kaolin group, which due to their interesting properties have been widely investigated in recent decades. HNTs are dioctahedral 1:1 clay minerals present in soils, discovered for the first time by Juan Baptiste Julien d’Omalius d’Halloy in Belgium, after whom they were named by Pierre Berthier in 1826. The mineral can be found worldwide, in particular in wet tropical and subtropical regions and weathered rocks. Countries such as China, France, Belgium and New Zealand are rich in this clay. It presents a chemical formula of Al Si O (OH) nH O, and according to its hydration state they 2 2 5 4· 2 can be classified as hydrated HNTs (Al Si O (OH) 2H O) with an interlayer d spacing of 10 Å, 2 2 5 4· 2 001 and dehydrated HNTs (Al2Si2O5(OH)4) with 7 Å d001 spacing. The occurrence of water molecules in the interlayer space is believed to be the reason for the different halloysite morphologies which constitute the main difference with platy kaolinite. Depending on the extraction site, geological occurrence and crystallization conditions, halloysite can be found as tubular, spheroidal or platy-like particles. Among these different morphologies, the tubular one is the most representative. Therefore, typical HNTs possess a hollow tubular structure in the sub-nanometer range with an aspect ratio of ca. 20. Structurally, HNTs are constituted by an external surface composed of siloxane (Si–O–Si) groups, an internal surface, a lumen that consists of a gibbsite-like array of aluminol (Al–OH) groups, and the presence of some Al–OH and Si–OH groups at the edges of the material or as structural defects (Figure1). HNT walls consist of 10–15 bilayers, with a spacing of approximately 0.72 nm and have a density of 2.53 g/cm3 [1,2]. Molecules 2020, 25, 4863; doi:10.3390/molecules25204863 www.mdpi.com/journal/molecules Molecules 2020, 25, 4863 2 of 44 Molecules 2020, 25, 4863 2 of 44 FigureFigure 1.1. (a,b) HNTs crystal morphology and atomic structure; (c,d) Trasmission electron microscopy (TEM)(TEM) andand (Atomic(Atomic forceforce microscopy)microscopy) AFMAFM imagesimages ofof HNTs.HNTs. AdaptedAdapted withwith permissionpermission fromfrom [1[1,2].,2]. ThanksThanks toto theirtheir didiffefferentrent chemical chemical composition, composition, the the tubes tubes undergo undergo ionization ionization in in aqueous aqueous media media in anin oppositean opposite way, way generating, generating tubes tube withs with oppositely oppositely charged charged inner andinner outer and surfacesouter surfaces [3]. This [3 charge]. This separationcharge separation occurs in occurs water in within water a widewithin pH a wide range pH from range 3 to 8from [4]. Experimentally,3 to 8 [4]. Experimentall the chargey, separationthe charge isseparation predicted is by predicted comparing by thecomparing negative the and negative positive and values positive for the values electrical for theζ—potential electrical ζ of— silicapotential and aluminaof silica and surfaces alumina in water, surfaces respectively. in water, Therespectively. tubes have The a length tubes inhave the a range length of in 0.2–1.5 the rangeµm, whileof 0.2– the1.5 innerμm, while and outer the inner diameters and outer of the diameter tubes ares inof thethe rangestubes are of 10–30 in the nm ranges and 40–70of 10– nm,30 nm respectively and 40–70 [ 5nm,–7]. Physico-chemicalrespectively [5–7]. properties Physico-chemical of HNTs properties are summarized of HNTs in Tableare summarized1. in Table 1. Table 1.1. Physico-chemicalPhysico-chemical featuresfeatures ofof halloysitehalloysite nanotubesnanotubes (HNT)s.(HNT)s. ChemicalChemical Formula Formula Al2Si Al22OSi5(OH)2O5(OH)4·nH42On H2O · LengthLength 0.2–2 0.2–2 μm µm OuterOuter diameter diameter 40–70 40–70 nm nm InnerInner diameter diameter 10–40 10–40 nm nm AspectAspect ratio ratio (L/D) (L/D) 10–50 10–50 ElasticElastic modulus modulus (theoretical (theoretical value) value) 140 GPa 140 GPa(130– (130–340340 GPa) GPa) MeanMean particle particle size insize aqueous in aqueous solution solution 143 nm 143 nm 2 ParticleParticle size size range range in aqueous in aqueous solution solution 22.1–22.1–81.681.6 m2/g m [8/]g [8] BETBET surface surfac areae area 50–400 50–400 nm nm Pore space 22.1–46.8% Pore space 22.1–46.8% Lumen space 11–395 Lumen space 11–395 Density 2.14–2.59 g/cm3 Density 2.14–2.59 g/cm3 Average pore size 79.7–100.2 Å Average pore size 79.7–100.2 Å Structural water release temperature 400–600 ◦C Structural water release temperature 400–600 °C Currently,Currently, HNTsHNTs priceprice rangesranges fromfrom USUS $600$600 perper tonton forfor applicationapplication inin fracking,fracking, toto USUS $3000$3000 perper tonton forfor finefine chemicalchemical applications.applications. It is easy to imagine that in the near future HNTs could replacereplace thethe muchmuch moremore expensiveexpensive carboncarbon nanotubesnanotubes ($500($500 perper kg)kg) andand inin many cases HNTs couldcould bebe usedused inin high technologicaltechnological applicationsapplications wherewhere carboncarbon nanotubesnanotubes areare notnot suitable.suitable. Furthermore,Furthermore, HNTs areare availableavailable atat thethe scalescale ofof thousandsthousands ofof tons,tons, comparedcompared toto gram-scalegram-scale forfor CNTs,CNTs, andand converselyconversely toto thethe latterlatter theythey areare biocompatiblebiocompatible materialsmaterials [[99].]. ComparedCompared withwith imogoliteimogolite nanotubes,nanotubes, whichwhich are are also also naturally naturally occurring, occurring, the pore the sizepor ofe size HNTs of is HNTs much larger;is much whereas larger; conversely whereas toconversely boron nitride, to boron which nitride, is chemically which is inert,chemical HNTsly inert, can be HNTs modified can be on modified their surfaces on their by surfaces the grafting by the of suitablegrafting groupsof suitable [10]. groups [10]. TheThe developmentdevelopment andand broadbroad application application of of HNTs HNT baseds based nanomaterials nanomaterial haves have rapidly rapidly advanced advanced in recentin recent years years as as indicated indicated by by the the large large number number of of publications publications from from their their advent advent as as cheapcheap andand widewide available nanocontainers in 2001 to the present day. This trend clearly reveals the global significance of HNTs and the intense interest of scientific research in this field (Figure 2). Molecules 2020, 25, 4863 3 of 44 availableMolecules 2020 nanocontainers, 25, 4863 in 2001 to the present day. This trend clearly reveals the global significance3 of of44 HNTs and the intense interest of scientific research in this field (Figure2). (a) (b) Figure 2.2. ((aa)) AA brief brief timeline timeline for for the the development development of HNTs;of HNTs; (b) Number(b) Number of publications of publications on HNTs on sortedHNTs bysorted year by and year for and application. for application Data. wereData collectedwere collected from “Scopus”.from “Scopus The”. word The word “halloysite” “halloysite is keyed” is key intoed theinto “topic” the “topic” search search box(date box (date of search: of search: 22 September 22 September 2020). 20 Adapted20). Adapted with permissionwith permission from [from11–15 [11]. – 15]. Until 2001 the research on halloysite clay was only focused on the geological and mineralogical aspectsUntil of these2001 the clay research minerals on and halloysite their main clay use was was only in focused ceramic on manufacturing. the geological and mineralogical aspectsThen, of th Priceese clay et al.minerals proposed and their the usemain of use HNTs was asin ceramic a low-cost manufacturing. alternative to more traditional microencapsulationThen, Price et systemsal. proposed for the the delivery use of of hydrophobicHNTs as a low compounds-cost alternative [16]. Their to idea more was traditional the result ofmicroencapsulation previous studies on systems lipid tubules for the formed delivery from of polymerizable hydrophobic phospholipids,compounds [16 used]. Their as nanocontainers idea was the forresult several of previous hydrophilic studies and hydrophobicon lipid tubules
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