Talvez Interessan TiO2 Divisão Estrutura de Discussão

Progress in Organic Coatings 163 (2022) 106660
Contents lists available at ScienceDirect
Progress in Organic Coatings

journal homepage: www.elsevier.com/locate/porgcoat
Review
Titanium dioxide and other nanomaterials based antimicrobial additives in

functional paints and coatings: Review
Man Ching Chen a, Pei Wen Koh b, Vinoth Kumar Ponnusamy c, Siew Ling Lee a, d, *
a
Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 Johor Bahru, Johor, Malaysia
b
CSC Screen Process Supplies Sdn Bhd, No 14, Jalan Bertam 6, Taman Daya, 81100 Johor Bahru, Johor, Malaysia
c
Dept of Medicinal and Applied Chemistry, Research Center for Environmental Medicine, Dept of Medical Research, Kaohsiung Medical University, Kaohsiung City 807,
Taiwan
d
Centre for Sustainable Nanomaterials, Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 Johor Bahru, Johor, Malaysia
A R T I C L E I N F O A B S T R A C T
Keywords: Nanomaterials like titanium dioxide and zinc oxide are established photocatalysts that are well-known in a
Antimicrobial variety of functions. They can be applied in paint and coating as pigment while providing functionalities like
Coating antimicrobial. Antimicrobial property has been increasingly significant due to various diseases contributed by
Nanomaterials
microorganisms that cause either long term or short-term effects to humans. However, the problem with the
Photocatalyst
Inorganic binder
photodegradation of organic components within paint retards the durability and life span of paint due to the
Functional paint changing of appearance. Inorganic binders such as potassium silicate, sodium silicate, lithium silicate, and
phosphate open the opportunity to replace organic binders that ensures the well-balance of functionality and
durability. This study critically reviewed a variety of antimicrobial additives such as TiO2, Ag and ZnO nano
materials and quaternary ammonium salts used in functional paints and coatings, as well as mechanisms of
antimicrobial activities of TiO2-based materials. This paper also evaluated the strengths and drawbacks of
antimicrobial, which then leads to the existing knowledge gap and the potential way forward.
1. Introduction conditions based on needs. The raising concern on the environment has
shifted the use of solventborne coatings to waterborne, high solids,
Paint, previously used to draw cave paintings in ancient times, now powder, and radiation-curable coatings to reduce the emission of vola
has multipurpose functions as a protective coating to enhance appear tile organic compounds (VOC). Amongst them, waterborne coating owns
ance, prevent corrosion, as an antimicrobial agent with longer dura the majority hitherto thanks to its characteristics of less odour, low VOC
bility, long-lasting colour, and odourless. Titanium dioxide or titania has and viscosities, as well as easy application [3]. Dash et al. analysed the
been an established pigment since the 19th century and rose after the Indian paint consumer market and found that quality and durability of
ban of lead pigment due to its cheap, nontoxic, and high refractive index paint were the key criteria to consider when purchasing a decorative
nature. It functions well as a white pigment with hiding effects and good paint [4]. To conquer the shortcomings of waterborne coatings when
opacity from light scattering effect [1]. Additives, binders, dyes, fillers, compared to solventborne, the addition of resin has innovated corrosive
pigments, plasticisers, and solvents are the common ingredients in paint protective acrylic-based latex and chemically-resisted urethane-acrylic
that are formulated and mixed up to different functional paints like copolymer latex [3]. In order to fit in customers' need, paint manufac
protective, decorative, and signal generation paints [2]. turers innovate a variety of functional paints like weather-resistant
There are three broad market categories in the paint industry, where paint, eco-friendly paint including heat-shield and water-based paints,
the largest demand comes from decorative coatings on either interior or odourless paint, antibacterial paint and antifouling paint. Since the
exterior surfaces of commercial, industrial, institutional or residential outbreak of COVID-19 in early of 2020, antiviral paint has emerged and
buildings. The second category is industrial coatings, which are utilised it has opened up the potential of this market at least until 2025 [5–7].
on appliances, furniture, transportation or goods. The third market Apparently, COVID-19 has significantly affected people's lives, which
category is speciality coatings that are designed to undertake extreme subsequently lowered the economic performance worldwide [8]. The
* Corresponding author at: Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 Johor Bahru, Johor, Malaysia.
E-mail addresses: mcchen3@graduate.utm.my (M.C. Chen), kumar@kmu.edu.tw (V.K. Ponnusamy), lsling@utm.my (S.L. Lee).
https://doi.org/10.1016/j.porgcoat.2021.106660
Received 30 April 2021; Received in revised form 27 September 2021; Accepted 16 November 2021
Available online 10 December 2021
0300-9440/© 2021 Elsevier B.V. All rights reserved.
M.C. Chen et al. Progress in Organic Coatings 163 (2022) 106660
invasion of viruses has brought up fear and awareness against micro yet, insufficient reviews have been done for this topic. Therefore, this
organisms. In fact, bacteria, fungi, protozoa, and helminths those have review will assist to boost the discussion with the raw materials of paint,
been surrounding us all this time are tough to survive in room temper incorporation of various nanoparticles as an antimicrobial additive, the
ature or extreme conditions in a long period [9–11]. Antimicrobial usage of an inorganic binder in the attempt to solve photodegradation of
agents have thereupon elevated researchers' interest especially on nano- an organic binder by TiO2, and lastly, its antimicrobial activities with
sized particles that provide a larger contact area with bacteria, which various examples.
gives a good bactericidal effect [12].
Titanium dioxide is a well-known photocatalyst that exists in three 2. Photocatalytic paint
crystalline phases: anatase, brookite, and rutile with a bandgap energy
of 3.0 to 3.2 eV [13]. However, the large bandgap has forced it to This section discusses the common raw materials used in the
become ultraviolet-active but not visible-active. Besides, titanium di formulation of paint. It then focuses on antimicrobial as the photo
oxide photocatalyst is suffering from its high recombination rate and catalytic activities through the various examples of antimicrobial paint
low quantum yield [14–16]. Therefore, metal ions include transition or coating with the addition of nanomaterials or other antimicrobial
metal like Cr5+ and V5+ [17–21], noble metals like Ag and Au [22–24], agents.
non-metals like C, N, and S [25–29], as well as metal oxides and other
materials like ZnO, g-C3N4, and Cu2O [30–33] were doped into or onto 2.1. Titanium dioxide as pigment additive in paint
titanium dioxide to overcome the issues abovementioned. TiO2 is an
established antimicrobial agent as compared to noble metals like Ag or Paint is made up of additives, binders, extenders, pigments, plasti
Au as they are inefficient without synergetic effect with other metals, cisers, and solvents [2]. Additives provide improvements for ease of
toxic in nature, not long-lasting in paint, and expensive [34–36]. Even brushing, ease of cleaning, antimicrobial, mechanical strengths and
though a narrower bandgap provides visible-light action, TiO2 is still anticorrosion [76,77]. Polymeric binders or resins are used to hold
challenging to improve the redox reaction from building a more positive pigments together and provide adhesion to the wall, which influence the
valence band and more negative conduction band as compared to hy pattern and mechanical properties of dry film through their chemical
droxyl radical and oxygen [37]. Other than being a pigment [38–40], it compositions [3,78]. The most common types of binder are acrylic and
is widely applied in construction [41–43], cosmetic [44–46], environ alkyd resin. Acrylic is well-known as eco-friendly and has a wide choice
mental [47–49] and food [28,50–52] industries. in colour variety, while alkyd is more durable and provides glossiness.
Bacteria are classified into gram-positive and gram-negative bacteria The organic phase of paint coatings consists of binders and solvents,
that differentiate themselves by their cell structure. Gram-positive while the mineral phase contains binders, pigments, and extenders.
bacteria consist of a thick layer of peptidoglycan, fat, and lipid in cell Extenders or fillers are used to lower the raw material cost by replacing
walls, while gram-negative bacteria consist of lipopolysaccharide, a thin pigment or polymer such as calcium carbonate, silica, and talc that have
layer of peptidoglycan, and two layers of phospholipid in their cell wall a similar refractive index like binder and exert less scattering effect [1].
[53]. Examples of gram-positive bacteria include Bacillus subtilis, Pigments are classified into white and coloured pigments, whereby the
Enterococcus faecalis, Listeria monocytogenes, Staphylococcus aureus, former operates by scattering light away through lead, zinc oxide, and
Staphylococcus epidermidis, and Streptococcus pneumoniae; whereas gram- titanium dioxide, while the latter gives a colour that absorbs particular
negative bacteria include enterica serovar Senftenberg, Escherichia coli, wavelengths of light based on its chemical structures such as organic or
Klebsiella pneumoniae, Pseudomonas aeruginosa, and Salmonella enterica mineral compounds. The environmentally friendly titanium dioxide
subsp. enterica [54–57]. Some studies mentioned that S. aureus has a replaces toxic lead with a cheaper price while providing other func
smaller negative surface charge, which allows the penetration of nega tionalities like antimicrobial as later discussed (Section 2.3). The bi-
tively charged radicals and lower resistance from cell membranes function of titanium dioxide as a white pigment is contributed by its
[56,58–61]. However, other studies also reported that the thin layer of high refractive index, while the antimicrobial activity is activated by
peptidoglycan of E. coli allows easier penetration of ions and the nega ultraviolet light to give reactive oxygen species (ROS) that degrade
tive surface charge of lipopolysaccharide promotes cell destruction due organic compounds. Some studies examined the range from 15% to 80%
to positively charged metal nanoparticles [62,63]. Compared to bacte and found that the presence of titanium dioxide led to better photo
ria, single-cell fungi are heterotrophic, aerobic organisms that strive catalytic activity. However, it is suggested to keep the additive per
better in acidic conditions and highly concentrated heavy metal ions centage within 1% to 15% as chalking was observed when titanium
[64]. Fungi provide benefits to nutrient cycling in soil but promote dioxide exceeded this range [79]. For additives like biocides, they only
fouling and deterioration of structures [65–67]. Fungicides such as present a small amount of about 1% within the paint [1]. Theoretically,
tributyltin (TBT) and zinc pyrithione were used before but have been titanium dioxide is chemically inert, which is believed to have no
formally banned due to high toxicity, which then promotes the emer interaction with other chemical components in the paint formulation
gence of safe, non-toxic, low-cost, and self-cleaning nanocatalyst or [42]. Coloured pigments suffer from photodegradation and acid pollu
nanofungicides [68,69]. Some examples of fungi include Alternaria tion as they are organic compounds. Both plasticiser and antifreeze are
alternata, Aspergillus flavus, Aspergillus fumigatus, Aspergillus niger, co-solvents that are added to lower the glass transition temperature from
Aspergillus melleus, Aureobasidium pullulans, Candida albicans, Chaeto solid to rubbery state. This coalescent aid supports the drying of a
mium globosum, Navicula incerta, and Penicillium chrysogenu [70–73]. The continuous latex coating at normal ambient temperature through soft
virus is a genetic parasite that can multiply and interconvert between ening the polymer. Antifreeze like water-miscible, lowers the evapora
DNA and RNA, and is spherical or rod-like with a rod-like capsid protein tion rate than water, whereas a coolant like glycol is added to allow
on top of it around the nucleic acid icosahedral or helical symmetrically. water to evaporate off first before the fusion of polymer into a contin
It affects plants and human beings through diseases in which a variety of uous film [1]. Organic solvent and water are the solvents that pertain to
viruses remain undiscovered and challenging to control or prevent [74]. the solventborne and waterborne coatings, which are less popular in
A study argued that titanium dioxide could enhance the mechanical compliance with the 1990 Clean Air Act Amendments that promotes
strength of polymer binder in paint but degrade it simultaneously [40]. VOC abatement [3]. The paint components are summarised in Table 1.
A previous study on paint components found that titanium dioxide Generally, paint is mixed based on the industrial formulation
pigments would be covered with silica and hydrated alumina, which through dispersing pigments by wetting resin and additives to prevent
protected the polymer binder from the free radical attacks. Lately, sili agglomeration. It is then subjected to high-speed mixers for mill-base
cate was revealed to be the potential inorganic binder [1,75]. The po preparation to combine other materials while continuing to disperse
tential of titanium dioxide in paint application can be further developed, pigment particles and add-on elements. Ball milling, bar milling, or bead
2
Table 1 microparticles are usually applied as white pigment in paint while TiO2
Components in paint. nanoparticles which are photocatalytic active are used in air contami
Components Function Examples Ref nants removal. Arguably, a previous study claimed that the TiO2 nano
particles could easily degrade polymer matrix and the release of these
Binder Bind with pigments, Acrylic resin, alkyd resin, [3,78]
adhesion to wall, and amino resin, epoxy resin, nanoparticles to the environment could degrade the organic contami
alter mechanical polyurethanes, and silicates nants more effectively [86,89]. However, toxic VOC which was poten
properties tially harmful to paint workers or person who touched the old paint
Pigment Provides colour Organic or inorganic [1] could be released from the degradation of organic matrix by TiO2
pigments like TiO2, ZnO
Extender Replacement of pigments Calcium carbonate, silica, [79]
nanoparticles [84]. This signifies the importance of having an effective
and talc inorganic binder for these nanoparticles in order to inhibit the migration
Plasticiser Aid in coalescent of Glycol, dialkyl succinate, [1] of the TiO2 nanoparticles, and hence improving their performance as
continuous film and texanol antimicrobial agent.
Solvent Carrier fluid Organic solvent, water [1]
Additive Fungicide, mildewcide Biocide [1]
2.3. Incorporation of nanoparticles in paint and coatings
milling is used for pigments that hardly disperse in the usual way. Af According to Jessica et al., scratch resistance agents, UV absorbers,
terwards, the mill-base will be added to mix with resin, solvent, and pigment and air purification, and biocides are the top four market needs
additives. The paint produced is tested for quality control and canned to on nanoparticle additives in coating formulation [77]. Booth et al.
release. To better regulate the technical, environmental, and safety provided a guide on the coating compositions involving titanium diox
criteria for paint and varnish, variety of European Commission (EU) ide, primary polymer, secondary polymer, and more that could reduce
Ecolabel standards including ISO 11890-2:2013 for volatile organic the amount of costly titanium dioxide needed while maintaining the
components (VOC) and semi-volatile organic components (SVOC) con light scattering effect and opacity. They proposed an optimum ratio that
tent, ISO 7783:2012 for water vapour permeability, ISO 1062-3:2008 for could provide good storage stability like viscosity and grit reduction
liquid water permeability, and ISO 13300:2002 for grinding degree or [90]. Other than the function as a pigment, titanium dioxide also acts as
particle size and wet scrub resistance have been established [56]. an additive for a variety of functions such as antimicrobial
The involvement of other paint components might affect the anti [34,38,39,91,92], improved mechanical strengths [38,91], anticorro
microbial performance of TiO2. According to Caballero et al., the mixing sion [38,91,92], and self-cleaning [39,93]. As compared to silica poly
of calcium carbonate as extender and titanium dioxide as pigment has urethane coating, the surface of nanosilica-titanium dioxide core-shell
reduced the antibacterial effect of the paint. This was attributed to the additives with polyurethane coating is rougher and has more agglom
formation of smaller pores (0.5 μm) that were unfit for bacteria to eration as observed under Scanning Electron Microscope (SEM). The
contact with the photocatalyst surface. This highlighted that the mechanical strength of nanosilica-titanium dioxide additive in paint was
bactericidal effect occurred on the surface of photocatalyst. On the tested by using Erichsen scratch hardness tester. It was understood that
contrary, different sizes of silica and talc with titanium dioxide gave the presence of silica improved the strength of coating up to 20 N load
better bactericidal performance due to larger pores produced (>3 μm, with good adhesion and impact resistance [38]. Solano et al. performed
bigger than E. coli size, 1.5 μm length × 0.9 μm diameter). Therefore, an anticorrosion test via ASTM B117:16 that coated nano-filled paint
photoinactivation could occur within the pores with the moisture cap onto carbon steel plates with 200 h of accelerated corrosion exposure.
ture [79]. This example justified the effect of extender on antimicrobial They reported that a lower concentration of 2 w/v% reduced the
activities and brought up the tendency of other components that might corrosion effect due to less substrate oxidised, less agglomeration, and
affect the exposure of titanium dioxide on the paint surface, which is pore formation that were observed under SEM with the comparison of
crucial for the contact distance killing mechanism. different w/v% [92]. Hwang et al. produced a self-cleaning hydrophobic
surface which induced by the rough surface (roughness around 1000 nm
2.2. Interest of nano-sized photocatalyst compared to micro-sized with agglomerated titanium dioxide nanoparticles, under SEM and
photocatalyst Atomic Force Microscope (AFM)) that gave lower surface energy and
thus lesser contact between water droplets and surface [39]. Conversely,
Nano-sized photocatalysts with dimension lesser than 100 nm have Sudipto et al. proposed another self-cleaning mechanism in silicate ti
gained intensive interest of researchers due to their high surface to tanium dioxide paint through the photodegradation of organic dyes.
volume ratio, high ability in generating more ROS and preventing the air They discovered that surface hydrophilicity was driven by porosity,
contaminants from agglomerate [80,81]. Microparticles have larger size which allowed better contact of organic dyes with surface, thus leading
ranging from 100 nm to less than 1 μm. The difference in size of the TiO2 to better self-cleaning performance [93]. Hwang et al. overcame this by
particles has given dissimilar effect to the mechanical properties of a proposing 1H, 1H, 2H, 2H-perfluorooctyltriethoxysilane (PFOTES) as a
coating. With the advantages of smaller size and better space distribu bridge between pigment and organic dyes. Their final result was posi
tion, nanoparticles help to build more crosslinking between the resin tive. Furthermore, there was less concern on biofilm formation as
and the additives. This could be explained by their ability to build more compared to Sudipto et al.'s. The self-cleaning mechanism involved the
Van der Waals bonding in nanocomposites which results in higher glass generation of ROS such as hydroxyl radicals and anionic superoxide
transition temperature (Tg) in nanoparticles as compared to micropar radicals from adsorbed water and oxygen that converted methylene blue
ticles. Therefore, the nanocoating could be much more brittle than that (MB) into carbon dioxide and water [92]. Besides, it was suggested that
of micro's [82,83]. the smaller the titanium dioxide's nanoparticle size (e.g. P25 ~ 25 nm),
Anatase TiO2 nanoparticles were able to generate more ROS than the larger the surface area (P25, 52.7 m2 g− 1) available for adsorption,
those in micro-size due to their lower recombination rate and higher which gives higher activity [94]. Caballero et al. proposed an optimal
surface adsorptive capacity with organic contaminants [84]. Unfortu range of 1% to 15% of titanium dioxide in the total pigment volume
nately, the cytotoxicity on human was found to be correlated with the concentration (%tPVC) as more than 30% chalking was observed. On the
increase in intracellular ROS [84–86]. Besides, as compared to micro- other hand, Alireza et al. reported that 3.5% of SSP-25 resulted in yel
sized TiO2, nano-sized TiO2 tends to migrate from its polymer matrix, lowing and chalking [79]. A recent study used a lower percentage as
thus increasing their potential of risking human health. As a result, high photocatalytic activity provided from 100% anatase and its small
majority of the life applications such as food or food packaging, and size brought better surface adsorption and light scattering effect ac
cement are made up by micro-sized TiO2 [87,88]. In industry, TiO2 cording to the Rayleigh scattering theory. It could be realised that
3
titanium dioxide alone was commonly used as a biocide additive. cheap, durable, environmental-friendly, and easy to prepare binder. It
Nevertheless, the synergy with other nanomaterials or even dyes can be found in the applications of ceramics, paint, refractory materials
allowed it to enhance its photocatalytic performance or explore in other and others. Nevertheless, limitations like low water and acid-alkali
functions. The problem became apparent when the photocatalytic per resistance as well as low cohesive strength were discovered [102].
formance was more efficient as the presence of organic components The standard from the Spanish Association for Standardisation, UNE-
would be affected by these activities, which created paint defects such as 48-083-92, could be tested for accelerated condition by using one month
chalking or yellowing [94]. at 53 ± 2 ◦ C to represent six months ageing in standard conditions, 23 ±
2 ◦ C and 50 ± 5% relative humidity [56]. Standards including ASTM
2.4. Potential of inorganic binder G154 (Standard practice for operating fluorescent ultraviolet lamp
apparatus for exposure of non-metallic materials) or ISO 11507 (Paint
Deterioration of binders and photocatalytic activities often cause and varnishes – Exposure of coatings to artificial weathering – Exposure
chalking and yellowing, but not fading in colour as it is mainly affected to fluorescent UV lamps and water) are applied to obtain desired ageing
by the colour retention of a pigment. The method used to study chalking result within a shorter period. Natural ageing based on ASTM D1435
was the black glove test that was rubbed over the paint surface after (Standard practice for outdoor weathering of plastics) or ISO 877
being exposed to sunlight for two weeks. Alireza et al. suggested that (Plastics – Methods of exposure to solar radiation) could be conducted in
STA-100 nanoparticles that modified titanium dioxide with silica and parallel to study the effect of local weathering on coatings that hardly
alumina were a better option for self-cleaning and durable paint [94]. simulated by accelerated conditions [103,104].
Braun et al. reviewed the involvement of titanium dioxide as a pigment Most of the studies using inorganic binders in the paint design do not
in paint. It was found that different combinations of stabilised or un examine durability of the resultant paints under concrete conditions
stable titanium dioxide and binder led to paint chalking either by the including time frame, weather, humidity, UV intensity, geographical,
photocatalytic activity of titanium dioxide or UV degradation of the and others, mainly due to the time-consumption of natural testing.
binder itself. Durable paint was made up of photo-stable binder and Importantly, despite the clear effective photocatalytic performance that
stabilised rutile titanium dioxide that were encapsulated in silica or is shown in prompt testing, their long-term performance is still unclear.
alumina. It was pointed out that paint degradation was influenced by
multiple events and was not time-dependent, which linked to the chal 2.5. Titanium dioxide-based antimicrobial paint
lenges of weathering simulation on both natural or accelerated weath
ering that needed to be properly designed for accurate measurements Antimicrobial includes antibacterial, antifungal, and antiviral. It is
[40]. It was proposed for both natural and accelerated weathering considered as the most applied additive in paint technology [77]. The
measurements to be combined, which was also supported by later re structures of bacteria, fungi, and virus vary, but the killing mechanism
searchers due to the difficulties in simulating real-time local weather in has some common points as discussed below.
artificial testers. Meanwhile, the parameters the artificial tester could
verify binder stability at a quicker rate [95,96]. 2.5.1. Photocatalytic antibacterial paint
Examples of inorganic binders are lithium silicate, potassium silicate, The antibacterial mechanisms of nanometals include the lipid per
sodium silicate and phosphate. Gettwert et al. reviewed the history of oxidation of ROS that are generated from photocatalyst, physical dam
silicate paint and oriented around its properties, the ratio of silicate to age contributed by sharp-edged nanomaterials, nanomaterial adhesion
potassium, curing mechanism, formulation, and applications of potas on bacterial cell walls, and release of metal ions as illustrated in Fig. 1
sium silicate. They less recommended sodium silicate as the inorganic [105,106]. The generation of ROS for titanium dioxide is described in
binder as it could provide white efflorescence with carbon dioxide the chemical equations below [107]. The photoactivated titanium di
despite that it was cheaper than potassium silicate [97]. This was sup oxide could convert oxygen and water into ROS like O2− , H2O2, and •OH
ported by Parashar et al., who explained the non-toxic, inert, available, as the bandgap of TiO2 is more negative or more positive.
and water-soluble alkali silicates such as lithium silicate, potassium
silicate and sodium silicate were good substitutions of the organic O2 + e− ➔O2 −
binder. This was because a good control of silicate to alkali ratio and
_ + H+
H2 O + h+ ➔OH
humidity in formulation could allow its curing through water evapora
tion and provided stronger adhesion through chemical reaction with
˙ + OH➔H
OH ˙ 2 O2
wall components. Strengths of potassium silicate of self-curing without
efflorescent as well as advantages of lithium silicate such as good water- _ + OH− + O2
O2 − + H2 O2 ➔OH
resistance, cure at ambient temperature, durable, considerable hardness
and abrasion resistance were highlighted. On the contrary, sodium sil ˙ + O2 + organic➔CO2 + H2 O
OH
icate was mentioned to be temperature or catalyst-dependent on curing
[78,98]. Some studies applied titanium dioxide or other nanomaterials Various antimicrobial susceptibility tests, namely Kirby-Bauer and
into lithium silicate [99], sodium silicate [75], and potassium silicate Stokes diffusion, broth microdilution, agar dilution, and E-test (that
coatings [93,100,101] for self-cleaning activities. According to Arekhi includes both diffusion and dilution), could overcome the shortcomings
et al., 5 wt% of water glass with 5 wt% of nano titanium dioxide of disk diffusion and broth dilution [108,109]. For antimicrobial paint
improved the photodegradation of organic pollutants with less effect on testing, simulation like spraying airborne bacteria on paint surface upon
discolouration and better tensile strength. They also discussed the glass slide could be done to calculate colonies grown inside the petri dish
double side effect of water glass that caused agglomeration of titanium with solid growth agar [110]. Established standards such as the Japa
dioxide yet provided better photocatalytic performance through facili nese Industrial Standard (JIS) Z 2801:2000 (Assessment of antimicrobial
tating the electron movement [75]. Krishnan et al. pointed out that the activity of hard non-porous surfaces) from the Japanese Standard As
alkaline nature of silicate coating could result in the chemisorption of sociation examines the bacteriostatic and bactericidal of plastics, metals
sulphur dioxide onto it, which contributed towards better organic ceramics or other surfaces over 24 h. This could qualify the antibacterial
pollutant reduction as compared to physisorption [100]. The porous performance of a clinical or household purpose material. To pass JIS Z
nature of silicate paint surface not only allowed easier evaporation of 2801:2000, the antibacterial efficacy must be greater or equal to 2 log10
water during application but also improved the brightness of paint. or 99% reduction in the tested microorganisms as compared to the
Coolness effect was an addition advantage due to its high solar light control surface after the contact time [111]. Later, ISO 22196:2011 was
reflectivity and emissivity [78,93]. On the other hand, phosphate is a harmonised with JIS Z 2801 to evaluate the antibacterial activity of
4
Fig. 1. Antimicrobial mechanism of metal ions.

(Reproduced from [113].)
antibacterial-treated plastics or non-porous surfaces except their prop generation of ROS like •OH, O2− • and HO2• [79]. Hwang et al. used
agation of bacteria, prevention of biodeterioration, and odour [56]. A Degussa P25 as an additive with white-light activated antimicrobial
recent review discussed the effect of parameters like pH, temperature, agents (WLAAA), toluidine blue O (TBO), and crystal violet (CV) to
particle size, dopants, and active light region with the intensity on create white (without WLAAA), blue, and violet paints. These were
antimicrobial activities of nanoparticles [112]. subjected onto double side tapes to create a superhydrophobic surface
NanoAg is an established antimicrobial agent that provides complete (water contact angle = 160◦ ). Amongst the coloured paints, WLAAA
bactericidal effects overnight or within 48 h. Its mechanisms involve exhibited intrinsic bactericidal effect even in the dark and co-created
direct contact with negatively charge bacterium surface through disso ROS with titanium dioxide. Therefore, it functioned better than the
ciation of functional groups, oxidative stress arising from ROS, affinity white paint. The best performer was the violet paint that created more
to phosphorus and sulphur groups in DNA and proteins in cell mem free radical species. The superhydrophobicity property was created by
branes that affect the replication capacity, and enhance the membrane reducing adhesion force between water and surface as affected by lower
permeability through soft acid characteristics [110,114,115]. NanoZnO surface energy and greater surface roughness. Prevention of biofilm by
also provided complete bactericidal effects within hours with higher superhydrophobic surface is illustrated in Fig. 2. As bacterial was not
dopant percentage as compared to nanoAg. In fact, the synergetic effect contacted with nanomaterials, hydrophobic nanomaterials showed no
of both nanoZnO and nanoAg in antibacterial make lower dopant con or weak bactericidal activity. Hence, the addition of per
centration for good performance was possible [56,59]. However, Ag+ fluorooctyltriethoxysilane (PFOTES) was proposed as a bridge between
from nanoAg could be washed out and might lost its antimicrobial bacterial and dye adsorbed titanium dioxide [39].
protection within a year, while nanoZnO is quite soluble and might A later study by Verma et al. suggested that structure of silica
release toxic Zn2+ ions to the surrounding above the concentration of modified titanium dioxide where silica as the core and titanium dioxide
0.2 μg/mL. From the formal study, the incorporation of nanoAg had as the shell could improve the mechanical strength. The authors pro
caused colour change due to the presence of pinkish Ag+ [56]. Impor posed an optimum bactericidal of 4 wt% in paint coating that oxidised
tantly, both of them are classified under “extremely toxic” with L(E)C50 negatively charged bacteria through the attraction from positively
< 0.1 μg/mL [36]. As a result, the usage of nanoAg and nanoZnO pho charged metal and coordination with electron-donating groups within
tocatalysts in the paint design is less popular. cellular enzymes and DNA that attributed to enzyme deactivation and
Silver is expensive, thus the cheaper, less toxic, and white colour cell death [38]. Nawarat et al. formulated antibacterial primers for Thai
TiO2 could be a better option. TiO2 would not leach out and hence it Mural Arts by using commercial-grade rutile titanium dioxide as white
would not cause a reduction in antimicrobial activities [28]. Caballero pigment, nanoAg as antimicrobial agent, binder, additives, and
et al. substituted rutile titanium dioxide pigments with 100% anatase aluminium silicate as extender together with 1-inch blade mixer to
PC105 nanoTiO2 (80% tPVC, size 15–25 nm) that showed complete ensure good mixing and dispersion. Their results proved that nanoAg or
killing of bacteria E. coli within 96 h. This study suggested that the tPVC aluminium silicate alone provided no or poor antibacterial activity.
% should not exceed 20% for the sake of paint film durability. It was Meanwhile, the rutile titanium dioxide pigments showed positive inhi
noted that all tested tPVC% ranging from 15% to 80% provided fairly bition towards all Bacillus bacterial tested and could be further enhanced
well bactericidal effects in 48 h and then a complete killing in 96 h. by the addition of silver nanoparticles and aluminium silicate [116].
Consequently, this signified the importance of nanoTiO2 dispersion on Despite the fact that a previous study had highlighted that anatase
paint surface that optimised the photocatalytic activity, especially when portrayed better antibacterial activity [79], the study by Nawarat el al.
extenders were applied. Therefore, good control over the percentage of that applied commercial-grade rutile titanium dioxide also portrayed
extenders that allowed more exposure of nanoTiO2 would be favoured. It fair antibacterial activity through the generation of ROS due to the de
was proposed for the antibacterial mechanism to be driven by the fects that allowed it to absorb both UV and visible light [116]. The
5
Fig. 2. Influence of surface hydrophobicity on reducing bacterial attachment.

general antibacterial mechanism is illustrated in Fig. 3 while the per were reported by studies, therefore, it is mostly accompanied by
formance of antibacterial paint or coatings is outlined in Table 2. In nanoAg, chitosan, or bentonite clay and surface wettability modification
short, nanoAg, nanoZnO, and nanoTiO2 all showed antibacterial prop for fungistatic effect [56,71,122]. Interestingly, the cationic bentonite
erties with a majority of the size lesser than 50 nm. Nevertheless, clay was a natural antibacterial agent that could damage the bacterial
nanoTiO2 is even better as it does not bring up any health concern due to physically, chemically poison it, or deprive their nutrition [123,124]. As
less toxicity and more long-lasting as well as no leaching concern. discussed previously, nanoAg would cause colour variation, leaching,
Meanwhile, the white pigment within the paint had a double role as an and a higher dosage is always required for effective antifungal activity.
antibacterial agent. Thus, combination of nanoAg with other materials such as nanoZnO and
nanoTiO2 is necessary for good antifungal activity through surface en
2.5.2. Photocatalytic antifungal paint gineering [36,72,73]. Snežana et al. developed a coating with 3% w/w
Antifungal activities include inhibition of mycelium growth, reduc of titanium dioxide to spray on white façade paint for antifungal pur
tion in sporulation, and retardation of droplet formation [117]. The poses as direct involvement in paint formulation might result in lower
mechanism of an antifungal is quite similar to antibacterial, which in photocatalytic efficiency and photodegradation of organic components
cludes the generation of ROS and toxic ions that could be supported by a in the paint. They pointed out the issue of subjective data collection from
study on Ag-TiO2 to inhibit C. albicans [118]. To test for the antifungal previous reports on antifungal activity, which motivated them to self-
activity in paint, the American Society for Testing and Materials (ASTM) code a program to calculate antifungal surface area in the agar plate.
D 5590-00 (Standard test method for determining the resistance of paint Their study reported the durability of titanium dioxide coating on paint
films and related coatings to fungal defacement by accelerated four- based on hydrophilicity assessment and photocatalytic activity before
week agar plate assay) could be conducted. ASTM D 5590-00 allows and after UV/VIS irradiation for 210 min. Between paint coated with
the testing for the relative resistance of two or more paint films to fungal biocides, titanium dioxide, and the mixture of titanium dioxide and
growth within the high humidity chamber. There are four ratings based biocides, the mixture took advantages of biocides that allowed it to leach
on this standard: 0, none; 1, traces of growth (<10%); 2, light growth out from the paint for antifungal, while the ROS generated by titanium
(10–30%); 3, moderate growth (30–60%); and 4, heavy growth dioxide could kill fungi in contact distance [125]. Auyeung et al. eval
(60–100%) [119]. Furthermore, ISO 16869 (Plastic assessment of the uated a mixture of nanoparticles including titanium dioxide and nano
effectiveness of fungistatic compounds in plastics formulations) could ZnO as additives in water or acrylic-based paint. This justified that
visualise the fungistatic effect by covering the test film (thickness < 10 mixed metallic nanoparticles (Cu, Ag and others) were able to inhibit
mm) onto a layer of test agar with spores. Sufficient water must be fungal growth under fluorescent light through the synergetic effect of
provided to germinate spore to compensate for the hydrophobic effect of ROS generated from metallic [34]. On the other hand, large surface area
the plastic surface. nanosilica‑titanium dioxide core-shell was incorporated into coatings
It was previously reported that both nanoAg and nanoTiO2 showed through binding with polyurethane or polyacrylic binder to prevent the
better antifungal properties as compared to nanoZnO [103]. For growth of Acremonium kiliense, Acremonium strictum, and Fusarium solani
nanoAg, most of the studies ran their simulation under high humidity that brought diseases to plants and humans. Through the toxicity study
conditions and attempted in using polydimethylsiloxane (PDMS) or a of UV–Vis spectrum over nano core-shell, water, and water of coating
combination of gelatine, urea, and formaldehyde as a trapping agent to sample, it was observed that binders served to trap the nanoparticles
prevent leaching [120,121]. For nanoZnO, weak antifungal properties from releasing toxic ion to the surrounding [91]. Suélen et al. innovated
mesoporous titanium dioxide microsphere as a paint additive that
balanced between good photocatalytic efficiency and durability of paint.
The authors mixed 10 w/v% mesoporous titanium dioxide microsphere
into acrylic paint by using the high-speed disperser aids with high shear
impeller for an hour to distribute the additive evenly within the coating.
They reported that P25 provided good antifungal activity but greater
film degradation as observed while the degradation of μTiO2 micro
sphere and commercial paint was similar. μTiO2 microsphere (pore size
13 nm) exhibited better photocatalytic activity on pollutants due to their
porous structure exposed after paint degradation that could be observed
under SEM (Fig. 4) [126,127]. However, the pore size here was too small
to capture bacterial with μm sizes, therefore, the porosity was likely to
Fig. 3. General antibacterial mechanism of TiO2. serve for more surface areas exposed for the generation of ROS. Studies
6
Table 2
Summary of antibacterial paint activities.
Nanoadditives Shape Size Species Active Photocatalytic activity Method Efficiency Kinetic study Ref
light
region
Ag Nanoparticles 12- – – Antibacterial of E. coli, Agar diffusion MIC: 50–150 μg/ Generation of ROS [72]
80 K. granulomatis, and method, 48 h mL ZOI: 12-30
nm P. aeruginosa nm
Ag Nanoparticles 12- Ag+, – Antibacterial of E. coli Aerosol spraying Complete killing Physical destruction of [110]
14 Ag0 and S. aureus bacteria on a glass for S. aureus, the bacterial cell
nm slide (2.5 × 7.5 cm), partial killing for membrane
overnight E. coli
Ag Nanoparticles 5-40 – – Antibacterial of CLSI microdilution MIC: 1.00–5.00 Physical destruction of [57]
nm E. faecalis, E. coli, assay, 48 h μg/mL MBC: the bacterial cell
S. aureus, and S. enterica 1.00–69.00 5.00 membrane, generation
μg/mL of ROS, DNA and
enzyme destruction
ZnO-Ag Hybrid of rod 35 ZnO, – Antibacterial of ISO 22196:2011 Complete killing Release of toxic ions [56]
and sphere nm Ag L. monocytogenes, in 24 h
P. aeruginosa, and
S. senftenberg
ZnO Nanoparticles 9 nm – – Antibacterial of E. coli JIS Z 2801:2000 Complete killing – [59]
and S. aureus for S. aureus (2 h)
and E. coli (6 h)
TiO2 Nanoparticles 15- – UV and Antibacterial of E. coli JIS Z 2801:2000 Complete killing Generation of ROS: •OH, [79]
25 Vis in 96 h O2−
nm
TiO2 Nanoparticles 21 Vis Antibacterial of E. coli Agar diffusion CFU/mL E. coli Generation of ROS: OH− [39]
nm and S. aureus method, 3–4 h in
dark, 3–4 h under
white light White: 58
Blue: 35
Violet: 0
CFU/mL
S. aureus
White: 45
Blue: 20
Violet: 0
SiO2-TiO2 Core-shell 144 – UV Antibacterial of E. coli CFU 100% in 24 h Attraction of oppositely [38]
nm charged NPs and
bacterial, enzyme
deactivation through
EDG
Commercial – – – UV Antibacterial of Bacillus Agar diffusion 14.7 ± 0.6 mm Generation of ROS: [116]
rutile TiO2 mycoides D3 method OH− , H2O2 and O2
Fig. 4. Interaction of paint film consisting of mesoporous titanium dioxide microspheres photocatalyst.
regarding antifungal paint or coatings are tabulated under Table 3. It 2.5.3. Photocatalytic antiviral paint
was noted that nanoparticles alone did not give good antifungal activ The general mechanism of antiviral included surface oxidation, the
ities while surface engineer and synergy between few nanoparticles release of free radicals, binding prevention, and viral membrane disso
could provide better antifungal properties that were applied with a lution [128]. Antiviral paint testing could be conducted via modification
lower dosage to prevent toxicity concerns. of ISO 27447:2009(E) (Fine ceramics – test method for antibacterial
activity of semiconducting photocatalytic materials) and JIS R 1702
(Fine ceramics – test method for antibacterial activity of photocatalytic
7
Table 3
Summary of antifungal paint activities.
Compound Shape Size (nm) Species Active Photocatalytic Method Efficiency Kinetic study Ref
light activity
region
Ag Nanoparticle – – UV Antifungal of Agar well diffusion No activity – [55]

A. niger and method observed
C. albicans
AgA Quasi- 10 Ag+, UV Antifungal of ASTM D5590-00, 1 <10–30% fungi Release of toxic ions [73]
spherical Ag0 A. alternata and month growth in 4th
C. globosum week
Ag Nanosphere 12–80 Ag – Antifungal of Inoculation of paint Complete Generation of ROS [72]
A. flavus, and fungi in inhibition
A. fumigatus, and McCartney bottles
A. niger then pour plate
method, 48 h
Ag-PDMS Nanoparticle <10 – – Antifouling Field trial in Red Sea No biofouling on – [120]
water, 12 months the surface at
12th month
ZnO Quasi- 40–50 – UV Antifungal of ASTM D5590-00, 1 No growth – [73]
spherical A. alternata and month inhibition in 4th
C. globosum week
ZnO-chitosan Nanoparticle 35–45 – – Antifungal of Mesocosm experiment Low biofilm Bacteriostatic action of [71]
N. incerta in small aquaria with formation chitosan, release of toxic
natural seawater, 4 compared to ions, physical destruction
weeks others of cell wall and generation
of ROS
ZnO Nanoparticle 56 ± 8 – – Antifungi of Modification of Bauer- Spore inhibition Release of toxic ion [122]
A. niger Kirby disk diffusion diameter: 16-18
assay, 24 h mm
TiO2 and – – – UV Antifungal of Agar method with 19.9% of the Generation of hydroxyl [125]
biocides A. niger assist of Matlab surface without radicals, leaching of
R2012a, 5 days fungi biocides
Metallic Nanoparticle 7 – UV Antifungal of Disk diffusion method, 100 μg/mL Generation of superoxide [34]
A. flavus MIC and hydroxyl radicals
SiO2-TiO2 Core-shell 144 – UV Antifungal of Agar method, % fungi 80% More surface area for [91]
F. solani reduction, 10 days fungicidal activity
Mesoporous Microsphere 600–1300 – UV Antifungi of Agar method, 3 days Halo formed Generation of hydroxyl [126]
TiO2 Monascus Ruber around paint radicals, superoxide anion
film; no exact and hydrogen peroxide
data provided
materials and efficacy) that measure the antibacterial activity of pho virus as it had a similar virion structure like SARS-CoV-2. They tested the
tocatalytic film like flat sheet, board, plate shape or textiles except for antiviral coating with different UV intensity and humidity. They
powder, granular or porous photocatalytic materials [129]. ASTM concluded that the merit of titanium dioxide brought about oxidative
E1052-11 (Standard test method to assess the activity of microbicides damage and rendered HCoV-NL63 virus to non-infectious even under
against viruses in suspension) examines the virucidal effect in the sus low UV intensity or high humidity that simulated the living conditions of
pensions that will be diluted and plated in quadruplicate to host cell the various viruses [133]. Although the study from FDA and others
monolayers in a 24-well tray. The tested sample will be considered as mentioned that the consumable quantity of titanium dioxide should not
effective virucidal if at least 4-log10 infectious units per 0.1 mL recov exceed 1 wt% because of free radicals to the respiratory system, it was
ered from the virus recovery control, complete inactivation of the test reported that nanoTiO2 that had been incorporated within paint film
virus at all assay dilutions or considered as cytotoxicity if at least 3-log10 portrayed no risk to the consumers [36,134,135]. Results of the antiviral
is reduced as compared to the previous level of cytotoxicity observed coatings are summarised in Table 4.
[130].
Fewer papers reported about metal nanoparticles-based antiviral 2.5.4. Properties of photocatalytic antimicrobial paint
paint. Antiviral additives like quarternary ammonium salt, a patent on The properties of photocatalyst affected its antimicrobial perfor
the antiviral coating with 99.99% effectiveness and silver, were reported mance. Studies had been arguing between the efficiency of hydropho
due to their promising bactericidal effect [131,132]. The virucidal bicity and hydrophilicity of the paint surface. Surface hydrophobicity
mechanism was similar to the bactericidal mechanism, therefore, the could be induced by metals like nanoAg, nanoCu, and nanoSiO2 and
potential of nanoTiO2 in antiviral paint could be further discovered. provided benefits like preventing biofouling or fungi and bacterial
Nakano et al. spin-coated titanium dioxide onto glass. It was observed attachment [39,120]. Conversely, hydrophilicity promoted better con
that under low level of UVA intensity that simulated indoor light con tact with bacteria to exhibit bactericidal effect and better trapping of
dition, a complete killing of H1N1 within 16 h was obtained through moisture, which was the key element in generating ROS [71,93,125].
generating ROS to attack influenza virus protein. Then, the RNA could Studies attempted to create a rough surface for inducing surface hy
reduce infectability [129]. The modification of 1 wt% Ag into titanium drophobicity. Nevertheless, they are theoretically indirectly relatable as
dioxide released silver ions and generated ROS that subsequently led to surface roughness was linked to surface area and surface energy in
the cell death of H1N1 virus and enterovirus type 71 strain under UVA which the latter was related to surface wettability [120,136,137].
and visible light. The presence of Ag formed a Schottky barrier that Roughness in micro or nanoscale could trap air within the valley,
reduced the electron-hole pair recombination and enhanced photo lowering the surface energy, and hence avoiding water from entering the
catalytic efficiency [130]. Svetlana et al. researched on the virucidal valley and staying on the surface (Fig. 2) [138]. Also, rough surface
effect of titanium dioxide nanoparticles in the coating with HCoV-NL63 inhibits the adhesion of bacteria when the pores size attributed by
8
Table 4
Summary of antiviral paint activities.
Compound Shape Size Active Photocatalytic Method Efficiency Kinetic study Ref
light activity
region
TiO2 Thin film – UV Antiviral of Modification of ISO Completely inactivated ROS: •OH, [129]
influenza virus 27447:2009(E) and JIS R after 16 h, reduce 4-log10 of O2−
1702, TCID50/mL virus
TiO2 (P25) Nanoparticles – UV Antiviral of HCoV- Virus infectivity assay 100% in 1 min ROS: OH− , [133]
NL63 virus O2−
Ag-TiO2 Nanocrystalline Major axes: UV Antiviral of H1N1 ASTM E1052-11, % virucidal 99.99% in 20 min ROS, release [130]
12–32 nm of metal ions
Minor axes:
3–8 nm
surface roughness smaller than bacteria's [139]. Between surface hy microbes including virus, bacteria and fungus. Since a good additive in
drophobicity and hydrophilicity, hydrophobic was proven to have no or paint and coating should not lead to colour variation, thus the usage of
weak bactericidal activity and needed to be accompanied with a binding nanoparticles of TiO2 and ZnO is always highlighted. The effect of
agent for bactericidal effect [39]. Despite more bacteria can contact the various structural and morphological properties of the additive such as
photocatalyst surface, hydrophilicity would lead to the deposition of size, shape, crystallinity, and surface wettability should be further
waste product and dead bacterial cells upon photocatalyst's surface. This investigated in order to improve the antimicrobial performance of the
would hinder their antimicrobial performance and hence it is necessary desired functional paints and coatings. To protect human being, synergy
to remove the unwanted waste product from the photocatalyst's surface effect between different nanomaterials that gives good antimicrobial
(Fig. 5) [57]. effect and not exceeding regulated dosages should be discovered. With
Although most of the studies pointed anatase as the most effective the evolving theories about the photocatalytic mechanism of the
crystallinity phase of TiO2, commercial-grade rutile TiO2 could portray different nanomaterials in antimicrobial, it allows the researchers to
fairly well antimicrobial performance too as these studies co-agreed understand the role of different nanomaterials in degrading different
with particle sizes as part of the contributing factor for a larger sur microbes under UV, visible light and solar light. A verifiable durability
face area exposed for photocatalytic activities [12,79,116]. The porosity testing that symbolises the functionality of paint in a long-term
of TiO2 could bring in moisture and exposed larger surface area for more perspective is necessary especially after loading a new antimicrobial
efficient bactericidal effect even it could not trap the bacterial due to agent and other inorganic binder in the paint. Besides, the incorporation
unfit criterion of large bacterial size into comparatively smaller pores of new additive in the paint formulation would lead to a change in its
[79,126]. To improve performance of TiO2, doping with metals could physical properties. Thus, more efforts should be made to optimise the
help to reduce recombination rates that were attributed to a better additive input, minimise the additive's influence towards other paint
photocatalytic activity [130]. A variety of additive percentages were components and lastly to further enhance antimicrobial effectiveness of
studied and most of them mentioned about higher percentage and better the resultant paint or coating materials under different environments.
antimicrobial activities. Dispersion of TiO2 on coating surface is more Further investigations should include broader perspective from the
essential than that especially involving extenders with a similar size as design of nanomaterial, incorporation between nanomaterial to other
extenders might hide TiO2 from bacterial, moisture, and sunlight. In a components and long-term durability testing to produce an effective and
lower percentage and well-dispersed of TiO2, a lesser photodegradation durable antimicrobial paint. Taking into consideration the principal of
of organic components and a better antimicrobial performance were green chemistry, the use of safer chemicals, workers safety and envi
observed [79,122]. ronmental issues, the search for a high effective and cheap antimicrobial
additive in functional paints and coatings design is highly demanded
3. Future perspective and in progress.
The quest for antimicrobial paint is dramatically increase especially 4. Conclusion

after the outbreak of COVID-19 pandemic in early 2020. Nanomaterials
are undeniable good choice as antimicrobial agent in paint and coating In general, it has been proven that Ag, ZnO and TiO2 nanomaterials
due to their low toxicity and high catalytic activity in denaturing the are functioning well as antimicrobial additives in paint and coating.
Fig. 5. Schematic diagram showing close contact between bacterial and a hydrophilic surface.
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Progress in Organic Coatings 163 (2022) 106660

Contents lists available at ScienceDirect

Progress in Organic Coatings

Titanium dioxide and other nanomaterials based antimicrobial additives in

Fig. 1. Antimicrobial mechanism of metal ions.

Fig. 2. Influence of surface hydrophobicity on reducing bacterial attachment.

Ag Nanoparticle – – UV Antifungal of Agar well diffusion No activity – [55]

The quest for antimicrobial paint is dramatically increase especially 4. Conclusion

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