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Effect of calcination temperature on the antibacterial activity of TiO2/Ag

nanocomposite

Article in Materials Research Express · April 2019

DOI: 10.1088/2053-1591/ab155c

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Effect of calcination temperature on the antibacterial activity of TiO2/Ag

nanocomposite
To cite this article before publication: Resetiana Dwi Desiati et al 2019 Mater. Res. Express in press https://doi.org/10.1088/2053-1591/ab155c

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Page 1 of 8 AUTHOR SUBMITTED MANUSCRIPT - MRX-113416.R1

IOP Publishing Journal Title

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Effect of Calcination Temperature on the

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10 Antibacterial Activity of TiO2/Ag Nanocomposite
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Resetiana Dwi Desiati, Melda Taspika and Eni Sugiarti

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15 Research Center for Physics, Indonesian Institute of Sciences, Tangerang Selatan, Indonesia
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17 E-mail: rese001@lipi.go.id
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19 Received xxxxxx
20 Accepted for publication xxxxxx

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21 Published xxxxxx
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23 Abstract
24
TiO2/Ag nanocomposites were prepared by a sol-gel method from titanium (IV) isopropoxide
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and silver nitrate as raw materials followed by calcination at 350, 450, and 500 ºC. The
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structures and morphologies of powders were fully studied by combination of X-ray
diffraction (XRD) patterns, field emission scanning microscope (FE-SEM), and transmission
electron microscope (TEM) images. The diffraction peaks of XRD patterns confirm the
30 anatase structure of TiO2 which is applicable as an antibacterial agent. The calculation of
31 TiO2 crystallite size based on Scherrer equation suggests that sizes are 6.6, 8.9, and 10.8 nm
32 for calcination temperature 350, 450, and 500 ºC respectively. The increase of TiO2 crystallite
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33 size can be attributed to thermal-dependent crystallite growth. The higher calcination
34 temperature causes the rate of nucleation and the generation of the growth species more
35 rapidly. The band-gap energies of 2.48, 2.36, and 2.19 eV were obtained for TiO2/Ag
36 nanocomposites by calcination at temperature of 350, 450, and 500 ºC respectively. The
37 results indicate that the photoactivity of TiO2/Ag nanocomposites are feasible to active in
38 visible light. Antibacterial activity was evaluated by using Escherichia coli (E. coli) and
39 Staphylococcus aureus (S. aureus) as gram-negative and gram-positive bacteria respectively.
40 TiO2/Ag nanocomposite calcinated at 350 ºC is more active on the killing E. coli bacteria than
41 TiO2/Ag nanocomposite calcinated at 500 ºC for the same diluted concentration. On the other
42 hand, the antibacterial activity of TiO2/Ag nanocomposite calcinated at 500 ºC is higher than
43
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TiO2/Ag nanocomposite calcinated at 350 ºC for the same diluted concentration. These results
44 lead to the conclusion that the capability of TiO2/Ag nanocomposites in the killing bacteria
45 depends on their structure and morphology which are affected by their calcination
46 temperature.
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48 Keywords: sol-gel method, TiO2/Ag nanocomposite, calcination temperature-dependence, band-gap
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contaminated by E. Coli bacteria increased risk to
53 1. Introduction consumption. Therefore, antibacterial material is required to
54
enhance the shelf life and inhibit the growth of E. Coli
55 Escherichia coli (E. coli) is one of the gram-negative
bacteria. Titanium dioxide (TiO2) is widely used as
56 bacteria causing some detrimental effect on human health.
antibacterial agent because of its inert and safe material [3].
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57 This bacterium can cause diarrheal diseases, peritonitis,

58 However, pure TiO2 has a wide band gap (3.2 eV) [4] which
colitis, bacteremia, infant mortality, and urinary tract
59 restricts its antibacterial activity under visible light (400-700
infections [1]. E. Coli is a major foodborne pathogen that has
60 nm). Moreover, most of solar light is visible light. Therefore,
thermal resistance in various meets [2]. Meets that have been

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3 we need to confine TiO2 band-gap to limit electron-hole
4 recombination [5].
5 Silver is a well-known dopant metal that has prominent
6 antibacterial properties which can prevent the growth of
7 various organisms such as bacteria [6, 7], viruses [8], and
8 fungus [9, 10]. The addition of silver in TiO2 can decrease
mixed solution started to gel at room temperature. The
prepared wet gel was aged at the room temperature for 24
hours, then the gel part was washed with the mixture solution
of distilled water and ethanol with volume ratio 1:1. Finally,
the mixed solution was filtrated to get TiO2/Ag powder and
calcinated in air at various temperature (350, 450, and 500

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9 recombination rate of electron and hole so that photoexcited ⁰C) for 2 hours with heating rate 5 ⁰C/minute.
10 electron-hole pair recombination was delayed [6]. Kubacka
11 et al. reported that the presence of silver on the anatase 2.3 Characterization of TiO2/Ag nanocomposite
12
surface TiO2 could improve antibacterial properties of TiO2
13 The X-ray diffraction (XRD) patterns of TiO2/Ag powders
against bacteria [11]. In order to damage bacteria cell

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14 were recorded using CuKα radiation (Rigaku instrument)
membrane, silver nanoparticles will release silver ions
15 with the wavelength 1.541862 Å. The morphological
followed by increased membrane permeability of bacteria
16 analysis was carried out using field emission scanning
that induces loss of proton motive force, causing de-
17 electron microscope (FE-SEM) (JEOL JIB 4610f) to observe
18 energization of the cells and efflux of phosphate, leakage of
the effect of calcination temperature on the morphology of
19 cellular content, and disruption DNA replication [12].
TiO2/Ag powders. The transmission electron microscope
20 Up to date, many works on antibacterial activity of
(TEM) was performed (TECNAI Twin G2) to confirm

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21 TiO2/Ag nanocomposite have been reported. Zhang et al.
investigated the effect of various Ag-to-TiO2 weight ratio on TiO2/Ag structure and to observe the distribution of Ag
22
particles in the as-prepared sample. The UV-visible
23 the antibacterial activity of TiO2/Ag nanocomposite powder
absorption spectrum was measured by a HITACHI UH5300
24 synthesized at calcination temperature 550 ºC [13]. Jing et al.
spectrometer to observe the absorbance spectra of the
25 synthesized TiO2/Ag aerogel powder by sol-gel method with
26 calcination temperature 270 ºC [14]. Zheng et al. investigated samples. The FTIR spectra were recorded by
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the effect of various annealing temperatures on the
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photocatalytic activity of TiO2 [15]. However, to the best of
our knowledge, none of the reported research has been
ThermoscientificNicolet to analyze the effect of calcination
temperature on chemical bonding.
The antibacterial activities of powders were evaluated by
30 focused on studying the effect of calcination temperature on using a colony-counting method based on the effects of
31 TiO2/Ag antibacterial activity. Because of that, this research bacterial growth on the nutrient agar plate. Firstly, E. coli
32 will be focused on the effect of various calcination (BTCCB614) and S. aureus (BTCCB611) bacteria were
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33 temperatures on the antibacterial activity of sol-gel cultivated in nutrient broth at 35 ºC for 24 hours in shaking
34 synthesized TiO2/Ag nanocomposite to further analyze the table. Bacteria concentration of nutrient broth incubated was
35 ability of TiO2/Ag nanocomposite in destructing E. coli and about 106 cfu (colony forming units)/ml. After that, 2.5 ml of
36 Staphylococcus aureus (S. aureus) cell membranes. diluted bacteria was added to various concentration (0, 5, 10,
37 15, 20, 25, and 30%) of TiO2/Ag composite solutions that
38 2. Experimental were named as S0, S5, S10, S20, S25, and S30, respectively.
39 Each mixture solution was put into the shaking table at
40 2.1 Materials temperature 35 ºC for 0 and 24 hours. Observation of the
41 samples was carried out by total plate count (TCP) on time 0
42 Titanium (IV) isopropoxide (TIP, 97%, Sigma Aldrich), and 24 hours, which counted the number of growth bacteria
43 nitric acid (HNO3), and silver nitrate (AgNO3, 0.1 mol/L,
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in each sample. For easily and correctly counting the grown

44 Merck) were used without further purification. The mixing of bacterial colonies, 0.5 ml of the treated solution was diluted
45 distilled water and ethanol was used to wash the as-prepared in bacto peptone water to suitable concentration. After that,
46 gel. the diluted solution was spread on a nutrient agar plate and
47 incubated at 35 ºC for one until two days for counting the
48 2.2 Synthesis of TiO2/Ag nanocomposites bacterial colonies.
49
The sol-gel method was used to fabricate the composite
50 3. Results and Discussions
powders. TiO2/Ag sol was prepared according to the
51
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52 following steps. Firstly, deionized water (5 ml) and ethanol

(95 ml) were mixed. The mixture was stirred vigorously to 3.1 Crystalline structure of TiO2/Ag nanocomposites
53
54 form homogeneous solution. Secondly, TIP (25 ml) and The XRD patterns of TiO2/Ag nanocomposites with
55 AgNO3 (220 ml) were slowly added dropwise with stirring, different calcination temperature are presented in Fig. 1.
56 respectively. The pH of the mixed solution was measured. If TiO2/Ag nanocomposite diffraction peaks at 25.42, 37.96,
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57 the pH value is not 2 or 3, a desired amount of HNO 3 was 47.99, 54.06, and 62.89º correspond to (101), (103), (200),
58 added to the mixture. After stirring about 24 hours, the
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3 (105), and (204) crystal planes, respectively [14]. Among
4 these peaks which belong to TiO2 crystal planes, diffraction
5 peak at 25.42º confirms the anatase structure of TiO2 [16].
6 Compare to rutile TiO2, the photocatalytic activity of the
7 anatase TiO2 is higher. It would generate the charge carriers
8 in anatase TiO2 can be excited deeper than in the rutile
small size. The size of particles depends on their calcination
temperature. With the increase of calcination temperature,
TiO2 particle size is larger. Nucleation is a process to form a
crystal which has a crucial role in the growth of particles and
crystallites. The rate of nucleation is affected by temperature.
The particle size and its distribution depend on the rates of

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9 structure [17]. Furthermore, anatase TiO2 is more applicable nucleation and growth species. The major steps of the
10 as an antibacterial agent. nucleation process are (i) generation of the growth species,
11 (ii) diffusion of the growth species, (iii) adsorption of the
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growth species, and (iv) surface growth to produce
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crystallite. The nucleation rate at the lower temperature is

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much higher than the rate of the growth species, so that
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nucleation is not able to co-occur with the growth species,
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and then the narrow size distribution can be obtained. In the
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18 higher temperature, the nucleation rate is lower than the rate
19 of the growth species which generates the nucleation and
20 growth species is simultaneous. Because of that, the older

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21 nuclei will grow to be larger than the younger ones, resulting
22 in a broad grain-size distribution [21-23].
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30 Fig. 1. XRD patterns of TiO2/Ag nanocomposites with
31 different calcination temperature
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In another report, TiO2 diffraction peak at 37.96º also
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correlates to (004) crystal plane [13]. Besides, diffraction
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peak at 37.96º is (111) crystal plane of face-center cubic
36
silver [18]. Because of that, the diffraction peak of the TiO2
37
38 (004) crystal plane and the Ag (111) plane overlap each other
39 as they are very adjoining. The XRD measurement of Ag
40 particles is unseen clearly because its particle size is small.
41 This result appropriates with TEM result that indicates the
42 nano-size of Ag particles. Calculations based on the Scherrer
43 equation suggest that the anatase crystallite sizes are 6.6, 8.9,
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44 and 10.8 nm in TiO2/Ag with calcination temperature 350,

45 450, and 500 ºC, respectively. The anatase crystallites
46 increase from 6.6 to 10.8 when the calcination temperature is
47 raised from 350 to 500 ºC. The increase of crystallite size can
48 be attributed to the crystallite growth is promoted by thermal
49 treatment, which means that titania grains are crystallized
50 and diameter of titania grain increases [19, 20].
51
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52 3.2 Morphology and microstructure of TiO2/Ag

53 nanocomposites
54
55 The as-produced TiO2/Ag powders with various
56 calcination temperatures were characterized by FE-SEM and
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57 their results are revealed in Fig. 2. All samples have spherical Fig. 2. FE-SEM images of TiO2/Ag nanocomposites
58 particle shape, with Ag particles are undetected due to their synthesized at various temperatures
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3 TEM images of TiO2/Ag nanocomposites calcinated at
4 350 ºC are revealed in Fig. 3(a). Ag clusters are dispersed
5 over the larger TiO2 nanoparticles, that is indicated by the
6 dark spots. The size of Ag particles is much smaller than
7 TiO2 particles which induce Ag particles are undetected on
8 the FE-SEM images and XRD patterns. Fig. 3(b) is high-

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9 resolution TEM image of TiO2/Ag nanocomposite. The
10 image shows some clear lattice fringes. The inter-planar
11 crystal spacing is calculated to be about 0.35 , 0.18 , and 0.17
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nm, correlating to the crystal plane of (101), (200), and
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(105), respectively. In addition, the lattice plane of Ag

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nanoparticle is 0.23 nm, which contributes to the crystal
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plane of (111). The result of the diffraction pattern in Fig.
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3(c) is appropriate to crystal planes on the XRD spectra.
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18
3.3 Chemical bonds and optical properties of TiO2/Ag
19
20 nanocomposites

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21 The FTIR spectra image of the prepared TiO2/Ag
22 nanocomposites are depicted in Fig. 4. The broad peak
23
centered about 3439 cm-1 is associated with the stretching
24
vibration of the hydroxyl group (-OH) that absorbs water
25
molecules and CO2 in the air, and at 1618 cm-1 is originated
26
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an from the bending vibrations of the water molecules [24]. The
-OH group becomes much weaker when the calcination
temperature is higher. This indicates the more -OH group
30 will be broken in the higher calcination temperature. The
31 photocatalytic activity of TiO2/Ag depends on the number of
32 the -OH groups. The more -OH groups, the more hydroxyl
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33 radicals and the photocatalytic activity will be higher [25].
34 The wavenumber of 1384 cm-1 indicates the bonding of
35 TiO2-Ag, which confirms that Ag molecules are successfully
36 deposited in TiO2 particles [26, 27]. With increasing the
37 calcination temperature, the intensities of TiO2-Ag peaks are
38 decreased, implying the breaking of TiO2-Ag bonding in
39 forming a crystalline structure [28]. The peaks in the range
40 500-1000 cm-1 are contributed from the anatase phase of Ti-
41 O [29].
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55 Fig. 3. (a) TEM image, (b) HRTEM image, and (c)
56 diffraction pattern of TiO2/Ag nanocomposite calcinated at Fig. 4. FTIR spectra of TiO2/Ag nanocomposites with
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57 temperature 350 ºC different calcination temperatures

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3 recorded from 295 to 800 nm that presents the as-prepared
4 TiO2/Ag nanocomposites can absorb UV and visible light
5 spectra. The increase of calcination temperatures causes the
6 slight red-shift of the peak center to the higher wavelength.
7 The shifting is related to the particle size of TiO2/Ag
8 nanocomposites, the higher calcination temperature will

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9 decrease TiO2/Ag particle size [30]. The broader of the
10 absorbance spectra and the higher the peak amplitude
11 because of the higher calcination temperature implies that the
12
higher calcination temperature causes the broader particle
13
size distribution [31].

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The band-gap energy plots are shown in Fig. 5(b-d). The
15
estimation of an indirect band-gap of TiO2/Ag
16
nanocomposites were obtained around 2.48, 2.36, and 2.19
17
18 eV for calcination temperatures 350, 450, and 500 ºC
19 respectively. It is found that the optical band-gap decreases
20 as the calcination temperature is increased. This implies that

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21 the calcination temperature can modify the gap between
22 valence band and conduction band. The increase temperature
23 will increase the grain size of TiO2/Ag particles that induces
24 the quantum size effect [32, 33]. The band-gap energies < 3
25 eV associates with the possibility to activation TiO2/Ag
26 nanocomposites in visible light [34].
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an 3.4 Antibacterial activity of TiO2/Ag nanocomposites
The antibacterial activity of TiO2/Ag nanocomposites
30
calcinated at temperature 350 and 500 ⁰C were investigated
31
32 against gram-negative (E. coli) and gram-positive (S. aureus)
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33 bacteria, as presented in Fig. 6(a) and 6(b), respectively. It is
34 seen that the number of viable bacteria reduced with time.
35 The increase of diluted TiO2/Ag concentration can suppress
36 the growth of bacteria more potentially, lots of bacteria are
37 killed within 24 hours. Antibacterial activity against E. coli
38 of TiO2/Ag nanocomposite calcinated at temperature 350 ⁰C
39 is higher than the antibacterial activity of TiO2/Ag
40 nanocomposite calcinated at temperature 500 ⁰C for the same
41 concentration. It is depicted on the graph in Fig. 6(a) which
42 TiO2/Ag nanocomposite calcinated at temperature 350 ºC can
43
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inhibit the growth of E. coli bacteria more effective than

44 TiO2/Ag nanocomposite calcinated at temperature 500 ºC. In
45 contrary, antibacterial activity against S. aureus of TiO2/Ag
46 nanocomposite calcinated at temperature 500 ºC is higher
47 than the antibacterial activity of TiO2/Ag nanocomposite
48 calcinated at temperature 350 ⁰C for the same concentration.
49 It is shown on the graph in Fig. 6(b) that TiO2/Ag
50 nanocomposite calcinated at temperature 500 ºC can kill S.
51
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aureus bacteria more adequately than TiO2/Ag

52
Fig. 5. TiO2/Ag nanocomposites with different calcination nanocomposite calcinated at temperature 350 ºC.
53
The cell wall of bacteria is complex, has a crucial role in
54 temperature: (a) absorbance spectra, (c-e) band gap energy
protecting their lives. The cell wall of gram-positive bacteria
55 plot
is thicker than that of gram-negative [18]. Gram-negative
56 The UV-vis spectra of TiO2/Ag nanocomposites with
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57 different calcination temperatures are shown in Fig. 5(a). The bacteria are enveloped by a thin peptidoglycan cell wall
58 broad spectra with the long tail absorbance peaks were surrounded by an outer membrane that contains
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3 lipopolysaccharide. However, gram-positive bacteria are
4 enclosed by a layer of peptidoglycan much thicker, but lack
5 of the outer membrane [35]. Because of that, we propose the
6 smaller particle of TiO2/Ag can penetrate and destruct
7 bacteria cell wall more easily than the larger particles. TiO2
8 can decrease coenzyme-independent respiratory chains of
smaller particles, the fraction of the atoms at low-
coordination and high energy site is more abundant than in
the larger particles. Because of that, the smaller particles are
more active than the larger particles [13, 37]. The cell wall of
E. coli will be damaged by Ag particles when they
accumulate in E. coli membrane, the increase of membrane

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9 bacteria rapidly which leads the cell respiratory of bacteria permeability resulting in death of the cell [38]. These are the
10 will be passive [36]. reasons why TiO2/Ag calcinated at 350 ºC is better in
11 suppressing the growth of E. coli bacteria, due to their
12
particle size is smaller.
13
On the hydrophilic surface, S. aureus bacteria is easier to

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attach than E. Coli bacteria. On the other hand, E. coli
15
bacteria is more adhesive on the hydrophobic surface [39].
16
The higher calcination temperature can increase the
17
18 hydrophilicity of TiO2 so that TiO2/Ag calcinated at 500 ºC
19 is more hydrophilic than TiO2/Ag calcinated at 350 ºC [40].
20 The number of TiO2/Ag particles calcinated at 500 ºC on S.

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21 aureus cell wall is greater than TiO2/Ag particles calcinated
22 at 350 ºC. Therefore, TiO2/Ag calcinated at 500 ºC can
23 inhibit the growth of S. aureus bacteria better than TiO2/Ag
24 calcinated at 350 ºC. Anatase TiO2 has an abundance of
25 hydroxyl groups on its surface that contribute in making a
26 strong binding between TiO2/Ag nanocomposite and cell
27
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an membrane, leading to increasing cellular membrane rigidity
[41, 42].

30 Conclusions
31
In summary, TiO2/Ag nanocomposites have been
32
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successfully synthesized by sol-gel method using titanium
33
34 (IV) isopropoxide and silver nitrate as raw materials follow
35 by calcinated at temperature 350, 450, and 500 ºC,
36 respectively. Antibacterial activity of anatase TiO2/Ag
37 nanocomposites depends on their calcination temperature.
38 The ability of TiO2/Ag nanocomposite calcinated at
39 temperature 350 ⁰C is higher on killing E. coli bacteria
40 because of the smaller particle size. In another hand, the
41 capability of TiO2/Ag nanocomposite calcinated at
42 temperature 500 ⁰C is better on inhibiting the growth of S.
43
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aureus bacteria because it is more hydrophilic than TiO2/Ag

44 nanocomposite calcinated at temperature 350 ⁰C. Overall, the
45 as-prepared TiO2/Ag nanocomposites are potential as an
46 antibacterial agent.
47
Fig. 6. The growth of (a) E. coli and (b) S. aureus in nutrient
48 Acknowledgements
broth with various concentration of diluted TiO2/Ag
49
nanocomposites (0, 5, 10, 15, 20, 25, and 30%) which are
50 This work was supported by INSINAS IRPI Grant
51 named as S0, S5, S10, S15, S20, S25, and S30, respectively. No.056/P/RPL-LIPI/INSINAS-1/III/2018 for entirely
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52 The colony of bacteria were calculated at 0 and 24 hours in funding this research.
53 time
54 References
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56 the killing of E. coli bacteria depends on their particle size.
economic impact of extraintestinal infections due to
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57 Smaller particles have more surface area that will be active

58 when TiO2/Ag particles contact with E. coli cell. In the
59
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