321
Tekstilec, 2023, Vol. 66(4), 321–338   |    DOI: 10.14502/tekstilec.66.2023075
Brigita Tomšič, Nika Savnik, Elena Shapkova, Laura Cimperman, Lara Šoba, Marija Gorjanc, Barbara Simončič
University of Ljubljana, Faculty of Natural Sciences and Engineering, Aškerčeva 12, 1000 Ljubljana, Slovenia
Green In-situ Synthesis of TiO
2
 in Combination with 
Curcuma longa for the Tailoring of Multifunctional Cotton 
Fabric 
Zelena in situ sinteza TiO
2
 v prisotnosti ekstrakta kurkume za 
izdelavo večfunkcionalne bombažne tkanine 
Original Scientific Paper/ Izvirni znanstveni članek
Received/Prispelo 9-2023 • Accepted/Sprejeto 11-2023
Corresponding author/Korespondenčni avtorica:
Prof. dr. Barbara Simončič
E-mail: barbara.simoncic@ntf.uni-lj.si
ORCID: 0000-0002-6071-8829
Abstract
The introduction of green chemistry has become urgent in the development of innovative, high-perfor-
mance functional textiles to reduce the environmental footprint of their production. This study aims to de-
velop a new eco-friendly process for the hydrothermal in-situ synthesis of TiO
2
 in cotton fabric and dyeing 
with curcumin natural dye to produce a photocatalytically active coloured textile platform with simultaneous 
UV protection properties. Two approaches were developed: classical, which included dyeing of the cotton 
samples with Curcuma longa (turmeric) extracts at different concentrations (5 g/L, 10 g/L and 15 g/L) and 
subsequent hydrothermal in-situ synthesis of TiO
2
 in the presence of the dyed cotton samples, and greener, 
in which simultaneous dyeing with turmeric extracts and hydrothermal in-situ synthesis of TiO
2
 were carried 
out. Since increasing the turmeric concentration hindered the photocatalytic performance of TiO
2
 in the 
chemically modified cotton samples, 5 g/L was selected as the most suitable turmeric concentration. A com-
parison of the chemical modification processes shows that the simultaneous dyeing of cotton with turmeric 
extract and hydrothermal in-situ synthesis of TiO
2
 was beneficial and resulted in a UV protection factor 50+, 
which corresponds to excellent protection category. The photocatalytic activity of TiO
2
 was maintained in the 
presence of turmeric, indicating the compatibility of both players in the chemically modified cotton, but not 
the creation of a turmeric–TiO
2
 heterojunction with visible-light-driven photocatalysis. The presence of TiO
2
 
inhibited the photodegradation of the curcumin dye, further confirming the compatibility of the two players.
Keywords: cotton, TiO
2
, turmeric extract, photocatalytic activity, UV protection
Izvleček
Pri razvoju inovativnih, visokozmogljivih funkcionalnih tekstilij je za zmanjšanje okoljskega odtisa pri njihovi 
proizvodnji postala vpeljava zelene kemije nujna. Zato je bil namen raziskave razviti nov okolju prijazen postopek 
hidrotermalne in situ sinteze TiO
2
 na bombažni tkanini in barvanja z naravnim barvilom kurkume za proizvodnjo 
fotokatalitsko aktivne obarvane tekstilije s hkratnimi UV-zaščitnimi lastnostmi. Razvita sta bila dva pristopa, in sicer 

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Tekstilec, 2023, Vol. 66(4), 321–338
klasični, ki je vključeval barvanje vzorcev bombaža z izvlečki kurkume različnih koncentracij (5 g/L, 10 g/L in 15 g/L) in 
naknadno hidrotermalno in situ sintezo TiO
2
 v prisotnosti pobarvanih vzorcev bombaža, in bolj zeleni, kjer sta sočasno 
potekala barvanje z izvlečki kurkume in hidrotermalna in situ sinteza TiO
2
. Ker je povečanje koncentracije kurkume 
oviralo fotokatalitsko delovanje TiO
2
 v kemično modificiranih vzorcih, je bila kot najprimernejša koncentracija kurkume 
izbrana 5 g/L. Iz primerjave postopkov kemične modifikacije je razvidno, da sta bila sočasno barvanje bombaža z iz-
vlečkom kurkume in hidrotermalna in situ sinteza TiO
2
 zelo učinkovita, s čimer je tkanina dobila UV-zaščitni faktor 50+, 
kar je kategorizirano kot odlična zaščita. Fotokatalitska aktivnost TiO
2
 se je v prisotnosti kurkume ohranila, kar je kaže 
na združljivost obeh akterjev v kemično modificiranem bombažu, ni pa se tvoril kompozit kurkuma-TiO
2
 s povečano 
fotokatalitsko aktivnostjo pri osvetljevanju z vidno svetlobo. Prisotnost TiO
2
  je zavrla fotorazgradnjo kurkume, kar 
dodatno potrjuje združljivost obeh komponent.
Ključne besede: bombaž, TiO
2
, ekstrakt kurkume, fotokatalitska aktivnost, UV-zaščita
1 Introduction
The chemical modification of textiles is one of the 
most important textile processes to develop innova­
tive textile materials with desired multifunctional 
properties. The application of nanomaterials to 
chemically modify textiles has opened new possibili­
ties for creating new functionalities and improving 
their properties [1–4]. Among nanomaterials, 
titanium dioxide (TiO
2
) is considered as a versatile 
inorganic semiconductor material for textile func­ tionalisation with unique electronic structure and 
functional properties such as photocatalysis, UV 
protection, antimicrobial activity, thermal stability, 
biocompatibility, and non­toxicity [5, 6]. TiO
2
 is a 
wide bandgap semiconductor material with photo­ catalytic self­cleaning properties, i.e., the ability to 
degrade organic pollutants on its surface under UV 
light irradiation. Namely, when TiO
2
 is irradiated 
with UV light in the presence of water and oxygen, 
it can form reactive oxygen species (ROS) on the 
surface, which have a strong oxidation potential to 
degrade organic molecules via intermediates to wa­ ter and carbon dioxide [7, 8]. The ability to absorb 
or scatter harmful UV radiation gives TiO
2
 a strong 
UV­blocking effect, which is crucial for its UV ­pro ­ tection properties.
Growing environmental awareness dictates 
avoiding the use of conventional chemical modifica­ tion processes as they have a negative impact on the 
environment due to the consumption of significant 
amounts of water, energy and chemicals [9, 10]. 
Therefore, the adoption of eco­friendly approaches 
is crucial to reducing the environmental footprint. 
In this context, the application of green chemistry 
principles, which include the use of safer chemicals, 
minimising waste and reducing water and energy, 
plays a crucial role [11]. One of the most important 
principles of green chemistry is the green synthe­ sis of nanomaterials, which has been extensively 
studied as an alternative to conventional chemical 
synthesis processes [12–14]. This also applies to the 
green synthesis of TiO
2
 [15–22]. It can be carried 
out in various ways, but plant­mediated biological 
synthesis, in which plant extracts or phytochemicals 
can serve as stabilizers, has proven to be one of the 
most promising and well­implemented. It opens up 
unlimited resources as different plant parts such as 
roots, stems, leaves, flowers, fruits and seeds can be 
used. Since biobased materials are found in nature, 
they are considered non­toxic and safe, inexpensive, 
and readily available.
Among plants, Curcuma longa, commonly 
known as turmeric, is a flowering plant of the ginger 
family. It is known for its rhizomes, which are usually 
dried and ground into a deep orange­yellow powder 
called turmeric powder. It is used as a natural yellow 
dye for textiles and food, as a culinary spice, as a 

 Green In-situ Synthesis of TiO
2
 in Combination with Curcuma longa for the Tailoring of Multifunctional Cotton Fabric 
323
cosmetic ingredient and as a medicine in traditional 
herbal medicine [23–25]. According to the literature, 
turmeric powder has not only established itself for 
textile dyeing [26–31], but also for the green synthe­ sis of TiO
2
 [32–38]. Usually, it is used as an extract 
prepared in a suitable solvent containing a natural 
polyphenolic compound called curcumin. When the 
turmeric extract was combined with the titanium 
precursor solution under suitable conditions, cur­ cumin acted as a capping agent for the synthesis of 
TiO
2
 and facilitated its formation and stabilisation 
[39]. Furthermore, when curcumin was in intrinsic 
contact with TiO
2
, the curcumin molecules could 
act as a sensitising agent that absorbed visible light, 
resulting in electron excitation in the curcumin mol­ ecule from the highest occupied molecular orbital to 
the lowest unoccupied molecu lar orbital, followed 
by electron transfer from the unoccupied molecular 
orbital to the conduction band of TiO
2
. This signifi­ cantly improved the photocatalytic efficiency of TiO
2
 
upon irradiation with visible light [32–37].
In the present work, a new sustainable approach 
for the chemical modification of cotton fabric was 
developed using hydrothermal synthesis of TiO
2
 in 
the presence of curcumin and cotton fabric to create 
photocatalytic and UV protection properties. Two 
different application procedures were investigated. 
The first was a two­step process and involved dye ­ ing of cotton fabric with turmeric extract followed 
by the in­situ synthesis of TiO
2
. The second was 
a one­step combination of dyeing with turmeric 
extract and in­situ synthesis of TiO
2
 with the aim 
of reducing water and energy consumption. In ad­ dition, the influence of turmeric extract at different 
concentrations on the functional properties of TiO
2
 
was thoroughly investigated. A newly developed 
innovative chemical modification process for the 
production of multifunctional textiles represents an 
important technological shift from conventional to 
green textile chemistry.
2 Experimental
2.1 Materials
Alkaline­soured, bleached and mercerized 100% 
cotton plain­weave fabric (Tekstina d.o.o., Aj ­ dovščina, Slovenia), with a mass per unit area of 
120 g/m
2
, was used for chemical modification. 
Turmeric powder (Maestro, Podravka d.d., Cro­ atia) was bought at a local market. Titanium(IV) 
isopropoxide (TTIP; ≥ 97.8% concentration), iso­ propanol ( ≥ 99% concentration) and acetic acid 
were procured from Sigma Aldrich (United States), 
Honeywell Research Chemicals (Seetze, Germany) 
and CARLO ERBA Reagents S.A.S (Barcelona, 
Spain), respectively.
2.2 Preparation of the turmeric extract
The extract of turmeric powder was prepared in dis­ tilled water at three different concentrations: 5 g/L, 
10 g/L and 15 g/L. A certain amount of the powder 
was covered with cold distilled water, heated and 
boiled for 5 minutes. Then, the boiled solution was 
cooled and filtered. For each concentration, 2 L of 
extract was prepared. The Curcuma longa rhizomes, 
their powder, the cooled extract solution (5 g/L) and 
the chemical structure of the natural dye curcumin 
are shown in Figure 1.
Figure 1: Curcuma longa rhizomes and their powder 
(a), the turmeric extract (b), and the chemical struc­ ture of the enol form of the curcumin natural dye in 
the turmeric extract (c).

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2.3 Chemical modification of cotton fabric
Chemical modification of cotton fabric was carried 
out in two different processes. The first classical 
process involved two steps: the dyeing of cotton 
samples with turmeric extract followed by the in­si ­ tu synthesis of TiO
2
 on the dyed samples. For this 
purpose, 7 g cotton samples were dyed with 5 g/L, 
10 g/L and 15 g/L turmeric extracts (three samples 
for each extract concentration) by exhaustion with a 
1:20 ratio of good to liquor for 40 minutes at 40 °C 
in the Starlet laboratory dyeing machine (Daelim 
Starlet, Co., Korea). After dyeing, the samples were 
squeezed on a two­roll padder (Mathis, Switzerland) 
with a wet pickup of 100% ± 5% and air­dried. For 
the in­situ synthesis of TiO
2
, the TTIP sol (200 g) 
was previously prepared as a 4% hydrolysed dilution 
of the TTIP precursor (8 g) in isopropanol (182 g) 
by adding acetic acid (10 g) and stirred magnetically 
for about two hours until hydrolysis was completed. 
The dyed samples were immersed in the TTIP sol 
and then squeezed out on a two­roll padder with a 
wet pickup of 100% ± 5% and dried at 100 °C for 1 
minute in the laboratory drying apparatus (Mathis, 
Switzerland). Subsequently, each sample was im­ mersed in 350 g of water and hydrothermally treated 
for 90 min at 120 °C in the Starlet laboratory dyeing 
machine. Finally, the samples were squeezed with a 
wet pickup of 100% ± 5% and air­dried.
The second greener process involved the simul­ taneous dyeing of cotton samples with turmeric 
extracts and the in­situ synthesis of TiO
2
. For this 
purpose, a hydrolysed TTIP sol was applied to the 
undyed cotton samples in the same way as in the 
first procedure (immersion in the TTIP sol, squeez­ ing with a wet pickup of 100% ± 5% and drying for 
1 min at 100 °C), followed by the immersion of the 
samples in 350 g turmeric solutions of different con­ centrations (three samples for each extract concen­ tration) and hydrothermal treatment for 90 min at 
120 °C, squeezing, and drying. For comparison, the 
dyeing of cotton samples in 5 g/L turmeric extract 
solution and the in­situ synthesis of TiO
2
 were also 
performed under the same conditions as the two 
processes. The sample codes for the chemical modi­ fication processes are summarized in Table 1.
Table 1: Sample codes according to the chemical modi-
fication process
Sample code Chemical modification process
UN Untreated (no chemical modification)
C5 Dyeing of the cotton sample with 5 g/L 
turmeric extract
T Hydrothermal in-situ synthesis of TiO
2
 from 
4% TTIP in the presence of an undyed cotton 
sample
C5-T Dyeing of the cotton sample with 5 
g/L turmeric extract followed by the 
hydrothermal in-situ synthesis of TiO
2
 from 
4% TTIP in the presence of the dyed cotton 
sample
C10-T Dyeing of the cotton sample with 10 
g/L turmeric extract followed by the 
hydrothermal in-situ synthesis of TiO
2
 from 
4% TTIP in the presence of the dyed cotton 
sample
C15-T Dyeing of the cotton sample with 15 
g/L turmeric extract followed by the 
hydrothermal in-situ synthesis of TiO
2
 from 
4% TTIP in the presence of the dyed cotton 
sample
C5+T Simultaneous dyeing of the cotton sample 
with 5 g/L turmeric extract and hydrothermal 
in-situ synthesis of TiO
2
 from 4% TTIP
C10+T Simultaneous dyeing of the cotton 
sample with 10 g/L turmeric extract and 
hydrothermal in-situ synthesis of TiO
2
 from 
4% TTIP
C15+T Simultaneous dyeing of the cotton 
sample with 15 g/L turmeric extract and 
hydrothermal in-situ synthesis of TiO
2
 from 
4% TTIP
2.4 Analysis and measurements
2.4.1 Scanning electron microscopy (SEM) and 
energy-dispersive X-ray spectroscopy (EDS)
The morphological characteristics of samples UN, 
C5, T, C5­T and C5+T were determined using the 
scanning electron microscope JSM­6060 LV (JEOL, 
Japan). Each sample was imaged three times at a 
different location at 3000­ × magnification. Before 
imaging, the samples were coated with a thin layer 
of gold to ensure conductivity.

 Green In-situ Synthesis of TiO
2
 in Combination with Curcuma longa for the Tailoring of Multifunctional Cotton Fabric 
325
In addition, the samples were examined using 
the Thermo Fischer Scientific Quattro S energy dis­ persive field emission scanning electron microscope 
(Thermo Fisher Scientific, USA), which works at an 
accelerating voltage of 1 kV in high vacuum and uses 
a concentric backscattered electron detector (CBS). 
An energy dispersive detector (Oxford Instruments 
Ultim Max 65) was used to verify the chemical 
composition of the observed particles using AZtec 
software. EDS spectra and elemental mappings of C, 
Ti and O were obtained. The samples were coated 
with a thin carbon layer before analysis.
2.4.2 Add-on
The total quantity of dry solid add­on of the samples 
UN, C5, T, C5­T and C5+T was determined using 
an electronic moisture analyser (KERN MLB­C). 
The samples were preconditioned for 24 h at 65% 
relative humidity and 20 °C. They were then dried 
at 105 °C until a constant mass was reached, i.e. until 
the change in weight within 120 s was less than 1 mg. 
The add­on value was calculated according to the 
following equation:
(1)
where m
2
 is the mass of the finished sample and 
m
1
 is the mass of the untreated sample.
2.4.3 Inductively coupled plasma-mass 
spectrometry (ICP-MS)
The concentrations of Ti in the samples T, C5­T and 
C5+T were determined via ICP­MS using a Perkin 
Elmer SCIED Elan DRC spectrophotometer. A 0.5 g  
sample was prepared in a Milestone microwave 
system via acid decomposition with 65% HNO
3
 and 
30% H
2
O
2
. Ti concentrations were reported as the 
mean values of two measurements for each sample. 
Based on the measured Ti values, the TiO
2
 concen­ tration was calculated.
2.4.4 X-ray diffraction analysis (XRD)
X­ray diffraction (XRD) patterns of the crystal phase 
of samples UN, T , C5­T and C5+T were recorded us ­ ing a Philips PW3830 X­ray diffractometer equipped 
with Cu­Kα1 1.54060 Å radiation and a secondary 
graphite monochromator. Data were recorded at  
40 kV and a current of 30 mA over a range of 10° to 
90° 2 θ at a rate of 3° per minute. Diffraction patterns 
were obtained using X’Pert HighScore Plus software 
ver. 4.8.
2.4.5 Fourier transform infrared spectroscopy 
(FTIR)
The chemical composition of the samples UN, C5, 
T, C5­T and C5+T was analysed using FTIR spec ­ trometer Spectrum 3 (Perkin Elmer, UK). Spectra 
between 4000 cm
­1
 and 600 cm
­1
 were recorded with 
a resolution of 4 cm
­1
 and an average of 120 spectra 
per sample.
2.4.6 Colour measurements
Colour measurements of the samples UN, C5­T, 
C10­T, C15­T, C5+T, C10+T and C15+T were per ­ formed using a Spectrophotometer Spectraflash 600 
PLUS CT (Datacolor, Switzerland). The reflectance, 
R, of each sample was measured five times at differ­ ent locations, and the average value was calculated. 
The colour strength, K/S value, was calculated from 
the following equation [40]:
(2) 
 
where R is the reflectance of the dyed samples at λ
max
, 
K is the absorption coefficient and S is the scattering 
coefficient of the sample.
2.4.7 UV–Vis spectroscopy and determination 
of the UV protection properties
The transmission and reflection spectra of the samples 
UN, C5­T, C10­T, C15­T, C5+T, C10+T and C15+T 
were recorded in the wavelength range 250–750 nm 
using a Lambda 850+ UV/Vis spectrophotometer 

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Tekstilec, 2023, Vol. 66(4), 321–338
(Perkin Elmer, United Kingdom) equipped with a 
reflection module—a 150 mm integration sphere—
and fully controlled by a computer running WinLab 
6 UV software. Three measurements were made for 
each sample at different angles of warp alignment, 
and the average value of transmittance, T, and reflec­ tance, R, at each wavelength was calculated. Using 
the UV transmission spectra, the UV protection 
properties of the samples were determined according 
to the standard EN 13758­1: 2001. The main values 
of T were calculated at wavelengths of 315–400 nm  
(UV A), 290–315 nm (UVB) and 290–400 nm (UVR). 
The ultraviolet protection factor, UPF, was calculated 
as follows [41]:
(3)
where E(λ) is the solar spectral irradiance, ɛ(λ) is the 
relative erythemal effectiveness, Δ(λ) is the wave­ length interval and T(λ) is the spectral transmittance 
at the wavelength λ.
UPF rating and protection categories were deter­ mined using UPF values, calculated according to the 
Australian/New Zealand Standard for Sun­Protec ­ tive Clothing—Evaluation and Classification (AS/
NZS 4399, 2020), where UPF values of 15– corre­ spond to the “minimum protection” category, UPF 
values of 30– correspond to the “good protection” 
category and UPF values of 50– correspond to the 
“excellent protection” category.
2.4.8 Photocatalytic activity
The photocatalytic activity of chemically modified 
cotton samples was investigated using the photocat­ alytic degradation of Rhodamine B (RhB) dye solu­ tion under UV and visible light illumination. For this 
purpose, the samples UN, C5­T , C10­T , C15­T , C5+T , 
C10+T and C15+T with a size of 1 cm × 3 cm were 
immersed in 5 ml of 0.025 mM RhB solution in a Pe­ tri dish and exposed to UV light for 60, 120, 180 and 
240 minutes in the Color Control Professional cham­ ber (Just Normlicht – Vertriebs GmbH, Germany).  
In addition, the samples UN, C5, T, C5­T and 
C5+T were also placed in a cuvette filled with 3 ml  
of 0.025 mM RhB solution and illuminated 
in a Xenotest Alpha instrument (Atlas, USA), 
equipped with a visible xenon arc lamp (radiation 
attitude 0.8–2.5 kVA and extended radiation range  
300–400 nm). The cuvettes were illuminated for 30, 
60, 120, 160 and 240 minutes. After each illumina­ tion time, the absorbance of the RhB solution was 
measured at λ
max
 and the corresponding concentra­ tion of RhB dye was determined using a previously 
prepared calibration curve. Measurements were 
performed using a Lambda 850+ UV/Vis spectro­ photometer (Perkin Elmer, United Kingdom). The 
RhB dye degradation efficiency was calculated as the 
percentage of dye degradation, D, as follows [42]:
(4)
where c
0 
is the concentration of the RhB dye solution 
before illumination and c
t 
is the concentration of the 
RhB dye solution after a certain time of illumina­ tion. For comparison, the photodegradation of the 
0.01 mM Methylene blue (MB) dye solution in the 
presence of the T, C5­T and C5+T samples was also 
carried out in a Xenotest Alpha instrument under 
the same conditions as in the case of the RhB dye 
solution.
2.4.9 Colour fastness to light
The colour fastness of samples C5, C5­T and C5+T 
to xenon light was tested in accordance with the stan­ dard SIST EN ISO 105­B02:2014. The samples were 
exposed to light in a Xenotest alpha apparatus (Atlas, 
USA) for a specified time (72 hours). Light fastness 
was assessed by the colour difference, . For this 
purpose, ten measurements of the colour coordinates 
L
*
, a
*
 and b
*
 in the CIELAB colour space were made 
for each sample examined using a Datacolor Spec­ tro 1050 spectrophotometer (Datacolor, USA). The 
measurements were performed with a 9 mm aper­ ture under D65 illumination and an observation 

 Green In-situ Synthesis of TiO
2
 in Combination with Curcuma longa for the Tailoring of Multifunctional Cotton Fabric 
327
angle of 10°. The value of 
 
was calculated using 
the following equation [40]:
(5)
where ΔL
*
, Δa
*
 and Δb
*
 are the differences in the 
lightness, green–red, and blue–yellow colour coor­ dinates, respectively, calculated between the illumi­ nated and non­illuminated samples.
3 Results and discussion
The influence of the concentration of turmeric ex­ tract and the process of chemical modification on 
the colour yield of the cotton samples is shown in 
Figure 2. From both the photographs (Figure 2a) 
and the K/S values (Figure 2b), it can be seen that in­ creasing the concentration of turmeric extract from 
5 g/L to 10 g/L significantly increased the colour 
yield of the samples in both modification processes. 
Accordingly, the K/S values increased from 0.4 for 
sample C5­T to 0.68 for sample C10­T and from 0.73 
for sample C5+T to 1.71 for sample C10+T. In con­ trast, the additional increase in concentration from 
10 g/L to 15 g/L turmeric extract did not contribute 
to colouration of the samples and even resulted in a 
slight decrease in colour yield. It is also clearly seen 
that at the same concentration of turmeric extract, 
the K/S values of samples C5+T, C10+T and C15+T 
are significantly higher compared to samples C5­T, 
C10­T and C15­T. This indicates that the chemical 
modification process strongly influenced the inten­ sity of the colouration of the samples. Definitely, 
the colour strength of curcumin dye was higher in 
the chemical modification process involving the 
simultaneous dyeing of the cotton samples with 
turmeric extract and hydrothermal in­situ synthesis 
of TiO
2
 than in the process where the samples were 
previously dyed with the turmeric extract followed 
by the hydrothermal in­situ synthesis of TiO
2
 in the 
presence of the dyed cotton samples.
Figure 2: Photos of the chemically modified cotton samples (a); K/S values of untreated and chemically modified 
cotton samples (b)
To gain insight into the influence of the curcum­ in dye and TiO
2
 on the functional properties of the 
chemically modified cotton samples, the UPF values 
and the efficiency of degradation of the RhB dye were 
determined (Figure 3). The results in Figure 3a show 
that the chemical modification of the cotton samples 
resulted in a dramatic improvement in UV protection 
properties, as reflected by an increase in UPF values 
from 4.1 for sample UN to 42.2, 47.5 and 40.1 for 
samples C5­T, C10­T and C15­T, respectively, and 
to 53.2, 58.0 and 77.9 for samples C5+T, C10+T 
and C15+T. The UPF values of all three samples 

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Tekstilec, 2023, Vol. 66(4), 321–338
C5­T, C10­T and C15­T correspond to the “good 
protection” category, and the UPF values of all three 
samples C5+T, C10+T and C15+T correspond to 
the “excellent protection” category. These results 
clearly show that simultaneous dyeing with turmeric 
extract and hydrothermal in­situ synthesis of TiO
2
 
is beneficial to achieving maximum protection of 
cotton fabric against UV radiation. The highest UPF 
value was obtained for sample C15+T, in which the 
highest concentration of turmeric extract was used.
The efficiency of the chemically modified cotton 
samples for the degradation of the RhB dye solution 
was investigated under UV illumination, which is 
crucial for the photocatalytic activity of TiO
2
. The 
results in Figure 2b clearly show that the photocata­ lytic degradation of the RhB dye solution was more 
efficient in the presence of samples C5­T, C10­T and 
C15­T than in the presence of samples C5+T , C10+T 
and C15+T, which is contrary to the results obtained 
for the UV protection properties. In terms of pho­ tocatalytic performance, it is reasonable to conclude 
that the chemically modified cotton samples pre­ pared via the process in which TiO
2
 synthesis was 
carried out in the presence of the previously dyed 
samples provided a more efficient photocatalytic 
platform for RhB dye degradation than the cotton 
samples prepared via simultaneous dyeing and TiO
2
 
synthesis. Moreover, increasing the concentration 
of curcumin dye on the cotton samples hindered 
the photocatalytic efficiency of TiO
2
, as the cotton 
samples dyed with 5 g/L turmeric extract exhibited 
the highest percentage of photodegraded RhB dye at 
all degradation time intervals. This phenomenon is 
particularly evident in the C5+T, C10+T and C15+T 
samples, where the TiO
2
 was synthesised in the tur­ meric extract. This suggests that the curcumin dye 
forms the composites with TiO
2 
in which it covers 
the TiO
2
 particles and hinders the TiO
2
 photocata­ lytic activity at higher dye concentrations. After con­ sidering both results, i.e., UPF and photocatalytic 
efficiency, samples C5­T and C5+T were selected as 
representative samples with the optimal multifunc­ tional properties tailored with the combination of 
curcumin dye and TiO
2
 in both chemical modifica­ tion processes and were therefore used for further 
investigations in comparison to the chemically mod­ ified samples with solei TiO
2
 or curcumin dye.
Figure 3: UPF of untreated and chemically modified cotton samples (a), photocatalytic degradation of the RhB 
dye solution without and in the presence of chemically modified cotton samples after different illumination 
times under UV light (b)
The SEM images of samples UN, C5, T , C5­T and 
C5+T are shown in Figure 4. As can be seen in the 
SEM image of sample UN, the untreated cellulose 
fibres have a typical ribbon­like structure with a 
smooth and even surface, showing some natural im­ purities. Dyeing of the cotton samples with turmeric 

 Green In-situ Synthesis of TiO
2
 in Combination with Curcuma longa for the Tailoring of Multifunctional Cotton Fabric 
329
extract did not cause any visible morphological sur­ face changes in the cellulose fibres (sample C5). In 
contrast, in­situ synthesis of TiO
2
 particles resulted 
in an increase in the roughness of the cellulose fibres 
with a clearly visible thin TiO
2
 coating containing 
many small and larger TiO
2 
agglomerates (samples 
T, C5­T and C5+T). This phenomenon is most pro ­ nounced in sample C5+T.
The successful in­situ synthesis of TiO
2
 on the 
cellulose fibres was confirmed by the EDS analysis, 
which is shown in Figure 5 for the representative 
sample T. From the EDS spectrum in Figure 5b, 
obtained from the part of Figure 5a marked with a 
yellow frame, and from the element mapping images 
in Figure 5c, it is clear that sample T contains Ti, O 
and C elements in the structure. The EDS analysis 
also confirms that the white spots in Figure 5a repre­ sent TiO
2
 particles.
Figure 4: SEM images of the untreated and chemically modified cotton samples at 3000x magnification
Figure 5: SEM/BSE image of the sample T with the position of the EDS analysis (a), EDS spectrum (b) and 
element mapping images of C, O, and Ti (c) in the sample T

330
Tekstilec, 2023, Vol. 66(4), 321–338
The total content of TiO
2
 in samples T, C5­T 
and C5+T was determined by calculating the dry 
solid add­on and using ICP ­MS analysis (Table 2). 
From Table 2, the amount of TiO
2
 synthesised with 
the same 4% TTIP sol was highest in sample C5+T, 
followed by sample T, and the lowest amount was 
obtained in sample C5­T. This indicates that the hy ­ drothermal in­situ synthesis of TiO
2
 was promoted 
in turmeric extract (sample C5+T) compared to wa­ ter (sample T). In contrast, the presence of curcumin 
dye in the previously dyed cotton samples slightly 
decreased the amount of TiO
2
 synthesised (sample 
C5­T). Based on these results, the simultaneous 
dyeing of cotton samples with turmeric extract and 
hydrothermal in­situ synthesis of TiO
2
 is favourable 
for the production of chemically modified cotton 
fabric.
Table 2: Dry solid add-on and the concentration of 
TiO
2
 in the chemically modified samples included TiO
2
Sample m (g) Add-on (%) c TiO
2
 (mg/kg)
UN 0.287 / /
T 0.291 1.39 8600
C5-T 0.289 0.70 8000
C5+T 0.295 2.79 8900
The XRD analysis of the samples UN, T, C5­T 
and C5+T shown in Figure 6 provided valuable 
information about the crystal phases of the in­situ 
synthesised TiO
2
 in the cotton samples. The XRD 
pattern of sample UN shows well­defined diffrac ­ tion peaks at 2θ = 15.0°, 16.8°, 22.7° and 34.5°, 
corresponding to the (110), (
110
_
), (200) and (400) 
crystallographic planes of the crystalline structure of 
cellulose, respectively [43]. As expected, these peaks 
are also clearly visible in samples T, C5­T and C5+T. 
The prominent diffraction peaks at 2θ = 25.3°, 37.8° 
and 48°, corresponding to the (101), (220) and (022) 
crystallographic planes of the anatase crystalline 
phase of TiO
2
 [44], could not be detected in samples 
T, C5­T and C5+T, suggesting that the in­situ syn ­ thesised TiO
2
 has an amorphous structure. This is 
plausible, since the hydrothermal in­situ synthesis of 
TiO
2
 was carried out at 120 °C, which is too low for 
the calcination of TiO
2
 to produce crystalline phases. 
The same results have been reported in the literature 
[44–46].
Figure 6: XRD patterns of the samples UN, T, C5-T 
and C+T
The influence of curcumin dye and TiO
2
 on the 
chemical properties of the chemically modified 
cotton samples was determined by FTIR analysis 
(Figure 7). The IR ATR spectrum of the sample 
UN showed the absorption bands characteristic 
of the cellulose fingerprint in the 1500–800 cm
­1
 
region, corresponding to C–H, C–O, C–C C–O–C 
and O–H vibrations [47]. A comparison of the IR 
ATR spectrum of sample C5 with that of sample 
UN revealed no significant changes. This suggests 
that the characteristic bands of turmeric occur­ ring at 1740–1680 cm
­1
 due to C=O absorption, at  
~1510 cm
­1
 due to aromatic skeletal stretching vi­ bration and at ~1030 cm
­1
 due to C–OH stretching 
vibration were blurred by the strong vibrational 
bands of cellulose [48]. In addition, the character­ istic bands of TiO
2
 in samples T, C5­T and C5+T, 
which appear at 700–600 cm
­1
, could not be detect­ ed by FTIR analysis due to the low concentration of 
TiO
2
 [47]. The TiO
2
 vibrations that appear at wave­ numbers below 600 cm
­1
 could not be analysed.
T ransmission and reflection spectra were recorded 
to determine the influence of the curcumin dye and 
TiO
2
 on the UV protection properties of the chem­ ically modified cotton samples (Figure 8, Table 3). 
From Figure 8a, it can be seen that the transmission 

 Green In-situ Synthesis of TiO
2
 in Combination with Curcuma longa for the Tailoring of Multifunctional Cotton Fabric 
331
Figure 7: IR ATR spectra of the samples UN, C5, T, C5-T and C+T
Figure 8: Transmission (a) and reflection (b) spectra of the samples UN, C5, T, C5-T and C5+T. 
of UV rays (250–400 nm) through the sample UN was 
between 15% and 35%, which was too high to provide 
UV protection properties. Accordingly, the UPF of 
the sample UN was very low (3.86 in Table 3). The 
presence of curcumin dye reduced the transmission 
of UV rays through sample C5 compared to sample 
UN with T values of 9.52% for the UVA region and 
11.41% for the UVB region (Table 3). However, the T 
values of about 10% were too high to provide minimal 
UV protection. In contrast to the curcumin dye, the 
presence of TiO
2
 drastically reduced the transmis­ sion of UV rays in the UVB (290–315 nm) region, 
but in the UVA (315–400 nm) region, the transmis­ sion increased significantly and even exceeded that 
of sample C5 (Figure 8a). This resulted in a UPF 
value of 34.29, which is categorized as good pro­ tection. The combination of the curcumin dye with 
TiO
2
 in samples C5­T and C5+T improved their UV 

332
Tekstilec, 2023, Vol. 66(4), 321–338
protection properties. In particular, at UV A, the syn­ ergism between the curcumin dye and TiO
2
 led to a 
significant reduction in T values to 6.04 and 3.15 for 
samples C5­T and C5+T, respectively. This resulted 
in a UPF value of 42.17 for sample C5­T and 53.24 
for sample C5+T. The latter is in the 50+ category, 
which corresponds to excellent protection. Since the 
reflection spectra of samples C5, T, C5­T and C5+T 
(Figure 8b) are lower than the spectrum of sample 
UN, this suggests that the UV blocking mechanism 
of TiO
2
 is based on the absorption of UV light. As 
expected, the same phenomenon was observed for 
the curcumin dye due to the absorption capacity of 
the conjugated system in its aromatic structure.
Table 3: The arithmetic mean of transmittance, T, in the UVA, UVB and UVR ranges and the UVR protection 
categories for the untreated and functionalised cotton samples according to the Australian/New Zealand Stan-
dard Sun-Protective Clothing—Evaluation and Classification
Sample T (UVA) (%) T (UVB) (%) T (UVR) (%) UPF
UVR protection 
category 
a)
UN 31.28 23.71 29.53 3.86 NR
C5 9.52 11.41 9.96 8.75 NR
T 12.43 1.91 9.98 34.29 G
C5-T 6.04 1.87 5.07 42.17 G
C5+T 3.15 1.64 2.80 53.24 E
a)
 NR – non rateable, G – good protection, E – excellent protection
The photocatalytic activity of TiO
2
 in the cotton 
samples without and with the presence of the curcum­ in dye was investigated using the rate of degradation 
of RhB and MB dyes under visible light illumination 
(Figure 9). Visible light illumination was chosen to 
determine whether the presence of the curcumin 
dye in samples C5­T and C5+T could act as a sen ­ sitizer and have a photosensitisation effect on the 
visible­light­induced photocatalytic performance of 
TiO
2
. The results in Figure 9a clearly show that, as 
expected, samples UN and C5 did not exhibit photo­
catalytic activity, resulting in insignificant photo­
degradation of the RhB dye solution, which was still 
coloured after 4 hours of illumination, very similar 
to the blank solution without a sample (Figure 9c). 
In contrast, the photodegradation of the RhB dye so­ lution in the presence of samples T, C5­T and C5+T 
was very efficient, with the percentage of dye deg­ radation being over 95% in 2 hours of illumination 
and almost 100% in 4 hours of illumination, result­ ing in the complete decolourisation of the RhB dye 
solution (Figure 9c). A close inspection of Figure 9a 
reveals that the presence of the curcumin dye slight­ ly hindered the photodegradation performance of 
TiO
2
 at the beginning of the illumination compared 
to sample T. However, the photodegradation perfor­ mance of samples C5­T and C5+T was comparable 
to that of sample T at longer illumination times. In 
the experiment on the photodegradation of the MB 
dye (Figure 9b), the C5+T sample showed slightly 
higher photocatalytic activity than the T and C5­T 
samples after 1 hour of illumination; however, this 
phenomenon did not occur at longer illumination 
times, when the photodegradation efficiency of the 
T, C5­T and C5+T samples was very similar (Figure 
9b). Comparison of the results in Figure 9a and 
Figure 9b also shows that the photodegradation ef­ ficiency of the T, C5­T and C5+T samples is slightly 
higher for the RhB dye than for the MB dye, result­ ing in a photodegradation of more than 98% for the 
RhB dye and about 95% for the MB dye after 4 hours 
of illumination. This indicates that the chemical 
structure of the dye influences the photodegradation 
efficiency of the photocatalyst, which is consistent 
with literature data [49].
The results in Figure 9 clearly indicate that the 
photocatalytic activity of TiO
2
 was maintained in 
the presence of the curcumin dye but was not en­

 Green In-situ Synthesis of TiO
2
 in Combination with Curcuma longa for the Tailoring of Multifunctional Cotton Fabric 
333
hanced under visible light. The curcumin dye defi ­ nitely did not act as a sensitizer for TiO
2
 in samples 
C5­T and C5+T. It can be concluded that the two 
chemical modification processes investigated do 
not provide the conditions for the creation of a cur­ cumin­TiO
2
 heterojunction with visible­light­driv ­ en photocatalysis.
Figure 9: Photocatalytic degradation of RhB (a) and MB (b) dyes solution without sample (blank) and in the 
presence of samples UN, C5, T, C5-T, and C5+T after different illumination times under visible light; photos of 
RhB dye solution after 4 hours of radiation without and in the presence of the samples (c)
To verify whether the photocatalytic effect of 
TiO
2
 causes photodegradation of the curcumin dye 
in samples C5­T and C5+T, the colour fastness of 
these samples was determined in comparison to 
sample C5 without TiO
2
 and the results are shown 
in Table 4. It can be seen that the colour of all sam­ ples faded during illumination, resulting in high 
values of . This phenomenon was expected as 
it is known that most natural dyes have poor colour 
fastness to light, which is also true for curcumin 
[50]. However, the results in Table 4 show that the 
highest value of 
 
was obtained for sample C5 
and that this value was much higher than the 
 
values of samples C5­T and C5+T, indicating that 
the presence of TiO
2
 did not promote but rather 
inhibited the photodegradation of the curcumin 
dye, confirming the compatibility of the curcumin 
and TiO
2
 in the chemically modified cotton samples. 
This phenomenon may be surprising, as cotton 
samples loaded with TiO
2
 efficiently photodegrade 
both RhB and MB dyes. However, it should be em­ phasised that the photodegradation of the RhB and 

334
Tekstilec, 2023, Vol. 66(4), 321–338
MB dyes was carried out in the dye solutions, the 
colour fastness of the curcumin dye was investigat­ ed on dry cotton samples. It is evident that for the 
photocatalytic activity of TiO
2
, a sufficient amount 
of water must be absorbed at the surface of the TiO
2
 
particles to generate reactive hydroxyl radicals. At 
the same time, TiO
2
 acted as a UV absorber on the 
textile surface, which significantly reduced the dose 
of UV rays reaching the curcumin dye and causing 
its photodegradation.
Table 4: Colour fastness to light of the chemically modified cotton samples
Sample Illumination time (h) L
*
a
*
b
*
∆E
*
ab
C5
0 89.87 -5.73 76.24
74.90
72 93.54 -0.25 1.63
C5-T
0 90.16 -5.97 50.75
51.14
72 94.03 -0.33 0.07
C5+T
0 73.94 10.11 44.95
47.68
72 93.24 -0.34 2.62
4 Conclusion
A novel green process for the chemical modifi­ cation of cotton fabric was developed using the 
combination of curcumin dye and TiO
2
 to adjust 
the simultaneous photocatalytic activity and UV 
protection properties. During development, the 
influence of concentration of the turmeric extract 
and the two application processes on the functional 
properties of the chemically modified cotton fabric 
was thoroughly investigated. It was found that the 
optimum functional properties of the cotton fabric 
were achieved when the lowest concentration (5 g/L) 
of turmeric extract was applied and that the greener 
process including the simultaneous dyeing of cotton 
samples with turmeric extract and in­situ synthesis 
of TiO
2
 was more beneficial than the classical pro­ cess in which the cotton sample was first dyed with 
turmeric extract and then in­situ synthesis of TiO
2
 
was performed on the dyed sample.
It was found that the presence of the curcumin 
dye did not cause any visible morphological changes 
in the cellulose fibres, while the in­situ synthesis of 
TiO
2
 particles resulted in an increase in the rough­ ness of the cellulose fibres with a clearly visible thin 
TiO
2
 coating containing many small and larger TiO
2 
agglomerates. The application of both the curcumin 
dye and TiO
2
 did not lead to significant changes in 
the chemical structure of the cellulose fibres. Hydro­ thermal in­situ synthesis of TiO
2
 was promoted in 
turmeric extract compared to water, resulting in a 
higher total TiO
2
 content in the sample compared to 
that chemically modified in the absence of turmeric 
extract. As the hydrothermal in­situ synthesis of 
TiO
2
 was carried out at 120 °C, an amorphous struc­ ture of TiO
2
 was obtained in the chemically modified 
cotton sample.
The combination of the curcumin dye and TiO
2
 
in the chemically modified cotton sample drastically 
improved the UV protection properties, resulting in 
a UPF value of 53.24, which corresponds to excellent 
protection. While TiO
2
 alone provided excellent UV 
protection in the UVB region, the curcumin dye sig­ nificantly reduced the transmission of the sample in 
the UV A region, representing a synergistic effect be­ tween the two players. The presence of curcumin did 
not hinder the photocatalytic activity of TiO
2
 under 
visible light, but it also did not act as a sensitizer for 
TiO
2
. This indicates that the chemical modification 
process developed did not create a curcumin­TiO
2
 
heterojunction with visible­light­driven photocatal ­ ysis. The inhibition of the photodegradation of the 
curcumin dye in the presence of TiO
2
 also confirmed 
the compatibility of the two players in the chemically 
modified cotton samples.

 Green In-situ Synthesis of TiO
2
 in Combination with Curcuma longa for the Tailoring of Multifunctional Cotton Fabric 
335
Acknowledgments
This research was carried out within the framework 
of the courses on Advanced Finishing Processes and 
Chemical Functionalisation of Textiles in the Master 
Study Programme for Textile and Clothing Planning. 
The research was co-funded by the Slovenian Research 
and Innovation Agency (Programme P2-0213 Textiles 
and Ecology, Infrastructural Centre RIC UL-NTF).
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