Advances in Nano Research, Vol. 17, No.

5 (2024) 000-000
https://doi.org/10.12989/anr.2024.17.5.000

Green synthesis of potassium silicate nanoparticles

from biomass ashes and their antimicrobial potential

Abhishek Sharma1, Anirudh kumar1, Vikas Kumar1, Garima Sharma2,

Vini Madathil3, DVN Sudheer Pamidimari3, Beer Pal Singh1, Satendra Pal Singh4,
Ashish Ranjan Sharma5 and Sanjeev Kumar Sharma1
1
Biomaterials and Sensor Laboratory, Department of Physics, Ch. Charan Singh University, Meerut, Uttar Pradesh-250004, India
2
Department of Biomedical Science & Institute of Bioscience and Biotechnology, Kangwon National University,
Chuncheon 24341, Republic of Korea
3
Department of Molecular Biology and Genetics, Gujarat Biotechnology University, Gandhinagar, Gujarat- 382355, India
4
Department of Physics, S.S.V. College, (Affl. CCS University, Meerut), Hapur, Uttar Pradesh-245101, India
5
Institute for Skeletal Aging & Orthopedic Surgery, Hallym University, Chuncheon Sacred Heart Hospital,
Chuncheon-si 24252, Gangwon-do, Republic of Korea

(Received May 27, 2024, Revised September 28, 2024, Accepted October 16, 2024)

Abstract. Biogenic potassium silicate (K2SiO3) NPs were synthesized from the biomasses of walnut shell (w-K2Si), pinewood
stem (p-K2SiO3), and sugarcane bagasse (s-K2SiO3) by ambient fiery and KOH-assisted thermal process. The crystallite size (D)
of w-K2SiO3, p-K2SiO3, and s-K2SiO3 NPs were determined to be 73 nm, 53 nm and 47 nm using Debye-Scherrer’s formula.
The varied strain of all samples was observed in the 0.284 to 0.301 range. Microstructure showed the cubical geometry with an
irregular grain size of K2SiO3 NPs, while the SAED pattern confirmed the polycrystalline nature. The Eg of w-K2SiO3, p-K2SiO3,
and s-K2SiO3 NPs was determined from Tauc’s plot to be 3.66 eV, 3.75 eV, and 3.78 eV, which are closely matched to be 3.78
eV, 3.88 eV, and 3.79 eV estimated from the XPS core-level analysis. The antibacterial activity of w-K2SiO3, p-K2SiO3, and s-
K2SiO3 NPs was investigated against E. coli and S. aureus bacteria. Compared to K2SiO3 NPs, the s-K2SiO3 were found to be
highly toxic against E. coli and S. aureus and completely inhibited the growth of both organisms within 6 h. The findings
represent the novel low-cost development of K2SiO3 NPs with potent antibacterial activities.
Keywords: antimicrobial activity; bandgap engineering; microstructural analysis; potassium silicate (K2SiO3) nanoparticles
(NPs); residual stress from W-H model

1. Introduction 100 to 200 mm that helps plants to regulate water uptake,

enzyme activation, photosynthesis, protein synthesis,
Silicates are pioneering antimicrobial agents against the osmoregulation, stomatal movement, phloem transport,
broad spectrum of gram-positive or gram-negative microbes energy transfer, cation-anion balance, and stress resistance
due to favorable surface chemistry and amazing cell-viable (Wang et al. 2013, Danchin and Nikel 2019). Meanwhile,
nanomaterial owing to decent biocompatibility [1, 2]. phytogenic silica supports plants’ growth, strengthens
Generally, silicates [M x(SiO 2+n) 2n-] occur as inorganic against biotic/abiotic stress and health, and improves plant
compounds consisting of subunits; silicate anions (SiO2+n)2n- water/mineral uptake capacity (Deshmukh et al. 2017). It
typically associated with charge-balancing metal cations Mx also provides a defense mechanism against pests and heavy
(Mg 2+, Ca2+, Fe2+, Na+, and K +), and are found most metal toxicity, including soil salinity, and alleviates
abundant in the earth’s crust by mass (95%) (Mason 1966). immunity regarding diseases (Bhat et al. 2019). In animals,
Potassium silicate (K2SiO3) is one of the most important K+ is a critical electrolyte that assists nerves to function and
members of the silicate family, which effectively attributes muscles to contract, ensuring optimal water balance and pH
high surface functionalization, and their textural along with within the system (He and MacGregor 2008). It also helps
multimodal porosity engineering has a great potential to to move nutrients into cells and waste products out of cells.
achieve an outstanding level of maturity (Gandolfi et al. In addition, it maintains essential cardiovascular functions,
2008; Wu et al. 2015). Potassium (K) is an essential nutrient such as maintaining regular heartbeat, blood pressure, and
for plants, and the most abundant cation found consistently metabolizing carbohydrates (Tannen 1983).
with the apoplastic concentration in the cytoplasm between Similarly, silica in animals remarkably functions in
organs and connective tissue via collagen cross-linking.
Moreover, it is also well-known for strengthening bone
Corresponding author, Ph.D., tissues (Carlisle 1986). Various methods to synthesize
E-mail: [email protected] silicate micro and nanostructures and their biological
Co-corresponding author, Ph.D., activities have been studied. For example, Oliveira et al.
E-mail: [email protected] (2022) synthesized silicate microstructures and cooperative
formation of inorganic-organic interfaces. In addition, Li et
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 Abhishek Sharma et al.

al. (2019) synthesized ATO/K2SiO3 film prepared by twice- Swamiappan 2020, Ghiasi Moaser et al. 2023). Distinctive
sprayed pyrolysis, and their hydrophilic, anticorrosive, topographies of biogenic K2SiO3 and its subunits, potassium
thermal conductive, and electrical resistive properties were (K+) and silicate (SiO3)2- ions, imply to attire multiple
studied. Walker and Whitehead (1966) also prepared biomedical significance, which play a pivotal role in the cell
K2SiO3 liquors of composition (SiO2/K2O) with ratios of 4:1 culture of plant and animal cells (Jones and Handreck 1967,
from aerosil, acidic washed silica-gel fines or potash glass Epstein 2009, Wang et al. 2013, Dogan et al. 2019, Pandey
and studied by (I) light scattering, (II) reaction with and Mahiwal 2020).
molybdate and (III) usage of the metachromatic effect with The KOH-assisted thermal process has recently been
pinacyanol chloridse. Mastalska-Poplawska et al. (2020) employed to produce activated carbon (Xu et al. 2017,
synthesized transparent and intumescent polymer-silicate Jawad and Abdulhameed 2020, Ao et al. 2021). Various
hydrogels by free-radical polymerization in the presence of researchers have reported the synthesis of carbon-based
cross-linking monomer (N,N′Nmethylenebisacrylamide) nanomaterials such as graphene, graphene oxide, and
with the redox initiators system (potassium persulphate/ reduced graphene oxide by KOH-assisted thermal/
sodium thiosulphate). They examined rheologically at microwave process (Deng et al. 2018, Kang et al. 2019,
different sodium acrylate concentrations to study enhanced Tamuly et al. 2022, Youssry et al. 2023). This innovative
fire-retardant properties with the development of intumescent approach of the KOH-assisted thermal process utilizes
hydrogels. Another study to synthesize K2SiO3 from biomass waste for sustainable material synthesis and
potassium carbonate and calcium silicate was reported by demonstrates the versatility of KOH-assisted thermal
Wu and Liu (2007), which also reported the rate of processes in producing advanced nanocomposite materials
releasing K2SiO3 fertilizer as a functioning superabsorbent (Tamuly et al. 2022). The synthesis of biogenic K2SiO3 NPs
and for water retention application. Menzies et al. (1992) via ambient fiery and KOH-assisted thermal processes and
have reported the foliar applications of K2SiO3 to reduce the their antimicrobial response is a novel study and has not
severity of powdery mildew on cucumber, muskmelon, and been reported to date.
zucchini squash and tested the persistence of Si foliar In this work, we have demonstrated a simple chemical-
sprays on cucumber. Conventionally, fly ashes collected free approach to synthesize biogenic K2SiO3 NPs, i.e., w-
from the molten ashes serve as one of the basic raw K2SiO3, p-K2SiO3, and s-K2SiO3, from three different types
materials for manufacturing K2SiO3 (Hongwen et al. 2015). of biomass ashes, i.e. walnut shell (WS), pinewood stem
Commercially available synthetic sources of silica, such as (PS), and sugarcane bagasse (SB), respectively. The micro-
tetraethyl orthosilicate (tetraethoxysilane or TEOS), ethyl structure of w-K2SiO3, p-K2SiO3, and s-K2SiO3 NPs could
silicate Si(OC2H5)4, and silicic acid are employed to be controlled by crushing biomass ash and subsequently
synthesize K2SiO3. However, these commercial resources varying annealing temperature at 700 °C for different time
are impractical in the industries owing to their high cost and intervals (Pascal et al. 1999, Zeng et al. 2007). The
harmful effects on health/environment. It is consequently microstructure of K2SiO3 NPs also depends on several
imperative to find a new, safer, more economical, and factors such as soil, soil microbial species, soil pH,
environmentally acceptable source of K2SiO3. Biomass geographical location, and environmental conditions of the
waste is produced abundantly every year and it has been production land of biomass (Van Horn et al. 2013). The
found that biomass waste contains a high silica concentration, microstructural, mechanical, elemental, optical, and
which can be used as an alternative raw material for the electrical properties along with the chemical bonding of
development of K2SiO3 (Permatasari et al. 2016, França et K2SiO3, were evaluated by using X-ray diffractometer
al. 2017). (XRD), field emission-scanning electron microscopy (FE-
Comparatively, biomass-derived K2SiO3 displays an SEM), high resolution-scanning electron microscopy (HR-
extraordinary advantage over synthetic potassium silicate in TEM), surface area energy dispersion (SAED) patterns, UV-
the sense of its nontoxic behavior, tuneable microstructure, Vis spectroscopy, and X-ray photoelectron spectroscopy
and cost-effectiveness, as well as eco-friendly methods of (XPS), respectively. The synthesis mechanism of K2SiO3
synthesis (Mughal et al. 2021). Furthermore, diversified NPs from biomass wastes is also discussed. Furthermore,
forms of K2SiO3 NPs can be synthesized from compositionally the antibacterial activity of w-K2SiO3, p-K2SiO3, and s-
different raw biomasses from different silicon/silica sources, K2SiO3 NPs was investigated against Escherichia coli (E.
viz. phytoliths, sponge spicules, diatoms, including radiolarian coli) and Staphylococcus aureus (S. aureus). In our study,
and potassium sources (Imran et al. 2020, Nandiyanto et al. the synthesized s-K2SiO3 NPs were highly toxic against E.
2017, Hongwen et al. 2015, de Oliveira et al. 2022, coli and S. aureus compared to p-K2SiO3 and w-K2SiO3
Kumchompoo and Puntharod 2022). Moreover, the micro- NPs. The s-K2SiO3 NPs completely inhibited the growth of
structure of synthesized K2SiO3 NPs can be further tuned by both microorganisms within 6 h of treatment. The findings
varying the physical and chemical conditions via different reveal a novel low-cost synthesis of K2SiO3 NPs with
synthesis approaches (Hu et al. 2015). Nandiyanto et al. potent antibacterial activities.
(2017) synthesized K2SiO3 NPs from rice straw ash using a
flame-assisted spray-pyrolysis method at 700 °C for 3 h
using. Consequently, biogenic K2SiO3 has a future 2. Experimental
prominent potential in versatile in-vitro/in-vivo medical
applications, such as antibacterial activity, intelligent drug 2.1 Materials and methods
delivery and release systems, bone tissue implantation,
cancer therapeutic, and bioimaging/sensing (Tallury et al. Biomass, such as pinewood stem (PS), sugarcane
2008, Jurkić et al. 2013, Zhu et al. 2017, Venkatraman and bagasse (SB), and walnut shell (WS), were collected from
 Green synthesis of potassium silicate nanoparticles from biomass ashes …

the surface of K2SiO3 samples to avoid the charging effect

using JEOL Auto Fine Coater (JEC-3000FC) at 30 A for 40
sec. The microstructural properties of all types K2SiO3 NPs
were investigated via Panalytical X-ray diffractometer
(XRD) (X’Pert3 Powder) using a CuKα1 radiation source
(λ = 1.5405 Å ) under a constant current of 40 mA at 40 kV
and with a scan range of 10–80°. The crystallinity of the
nanopowders were analyzed using XRD pattern (Kumar et
al. 2013, Bogireddy et al. 2017), and further justified by the
SAED pattern. A Phoibos 100 hemispherical energy
analyzer (PHOIBOS 100-63 MCD) took the typical XPS
survey of w-K2SiO3, p-K2SiO3, and s-K2SiO3 NPs in a
constant analyzer energy (CAE) mode (Specs GmbH,
Fig. 1 Schematic diagram of chemical-free (green) synthesis Berlin, Germany: Mg radiation source 1253.6 eV, and
of K2SiO3 NPs from biomass waste. 125W power). The overall resolution of 0.9 eV was
measured and calibrated using the Ag 3d5/2 (368.3 eV) and
Au 4f7/2 (84.0 eV) signals. The base pressure in an analysis
local markets in west UP, India. All chemicals and solvents chamber was kept to be 5×10-10 mbar. Before recording the
of AR grade were purchased from Merck and Sigma data, the sample was degassed in a vacuum overnight. The
Aldrich (India) and used without further purification. optical properties of K2SiO3 NPs were evaluated from the
microprocessor-controlled UV–Vis double beam
2.2 Synthesis of biogenic potassium silicate spectrophotometer (Model: IG-27DS) in the 190 -850 nm
range.
Biogenic w-K2SiO3, p-K2SiO3, and s-K2SiO3 NPs were
synthesized via a chemical-free approach through ambient 2.4 Antimicrobial studies
fiery and KOH-assisted thermal process. The synthesis of
K2SiO3 NPs from biomass wastes is shown by a schematic Two distinct pathogenic species of E. coli (gram-
representation (Fig. 1). Initially, biomasses of WS, PS, and negative) and S. aureus (gram-positive) as representative
SB, were washed with tap water to remove environmental organisms bacterial strains were used in the antibacterial
dust particles and undesired contaminations, then rinsed activity of K2SiO3 NPs. S. aureus and E. coli organisms
with deionized (DI) water to remove the tap water were cultured in a Luria-Bertani (LB) nutritional medium at
contaminations and finally dried at 80 °C for 12 h in a hot 37 °C overnight. These culture plates were filled with 0.1
air oven. Then, WS, PS, and SB were ambiently burnt using mg mL˗1 of the w-K2SiO3, p-K2SiO3, and s-K2SiO3 NPs. In
the fire-burning gas nozzle, and their ashes were obtained, order to confirm that the material’s toxicity caused the
i.e., WSA, PSA, and SBA, respectively. The burnt black decline in colony-forming units (CFU), a control sample
ashes of these three biomasses were finely crushed in DI was kept without NPs treatment and evaluated in parallel
water by ball milling at room temperature for 10 h. The with the experiment. For both E. coli and S. aureus, the
finally crushed ashes were then filtered with the help of CFU change per mL was computed via respective colony
Whatman paper of grade 1 (110 mm, 1111 µm) using the counting at an interval of 1 h and compared with the
funnels and washed with a large amount of DI water. control.
Hydro-ball-milling crushing and filtration removes heavy
metal ions such as Fe2+, Cu2+, and Al3+ from the ashes. The
obtained precipitates were dried in a hot air oven at 60 °C 3. Results and discussion
for 1 h to detach the filter paper from the funnel and then
dried at 80 °C for 2 h to separate the filtrate ashes from the 3.1 Microstructural analysis
filter papers. All three washed and filtered black ashes were
finally dried at 100 °C for 3 h. Then, the dried ashes were The crystal structure, phase formation, and crystallite
stored and sealed in the borosil vials. 1 g of each of all three size of w-K2 SiO3, p-K2 SiO 3, and s-K2 SiO3 NPs were
prepared materials was mixed with 3 g of KOH, crushed determined by the XRD. Figs. 2(a) show the XRD pattern
separately with agate mortar’s help for 5 min, and then traced between 20° and 60° at scan rate of 1° per min for all
transferred into three different alumina crucibles. All three samples of K2SiO3 NPs. Peak profile analysis of all samples
samples were annealed at 700 °C for 2 h in a muffle furnace indicates a rare combination of potassium and silica. The
at the heating ramp rate of 5 °C per minute. The synthesized observed XRD pattern has been compared with reference
biomass-derived K2SiO3 NPs were naturally cooled to room data of JCPDS file #84-0366 (Fig. 2(a)), which confirms the
temperature. polycrystalline structure of all samples (K2SiO3 NPs). The
XRD pattern with sharp peak profile of all samples was
2.3 Characterization of the K2SiO3 nanopowders observed at 25.65, 26.94, 29.52, 30.69, 32.10, 32.62, 35.20,
38.60, and 41.40 corresponding to planes (131), (130),
The surface morphology of synthesized w-K2SiO3, p- (113), (214), (140), (200), (225), (221), and (231),
K2SiO3, and s-K2SiO3 NPs was determined by FE-SEM respectively. The dominant peak (113) of K2SiO3 NPs was
(Hitachi, S-4800) and BF-TEM. The Au was sputtered on observed at 29.52 in all samples. The intensity of various
 Abhishek Sharma et al.

Fig. 2 (a) XRD pattern, and (b) Crystallite size, lattice strain and dislocation density determination of w-K2SiO3, p-
K2SiO3, and s-K2SiO3 NPs using Debye-Scherrer’s formula

peaks deteriorated due to the partial amorphization and (Fig. 2(b)). The positive value of the observed strain
formation of grain boundaries. The crystallite size (d) of w- indicates the identical distance of relevant crystal planes,
K2SiO3, p-K2SiO3, and s-K2SiO3 NPs were calculated as 73 which might be possible due to the presence of defects and
nm, 53 nm, and 47 nm, respectively, using Debye- stresses. The following expression was used to estimate the
Scherrer’s formula, which is as follows: stress along the plane (113):
𝑘𝜆 𝜎 = 𝑌𝜀 (3)
𝑑= (1)
𝛽ℎ𝑘𝑙 𝑐𝑜𝑠 𝜃
where Y is the Young’s modulus (75 GPa) for SiO2 (Chen et
where k is denoted as the material’s constant (k=0.89), hkl al. 2014), and σ is presented as the stress of the material.
is the FWHM of the diffraction peak at angle θ, and λ is the The strain and stress values of K2SiO3 NPs extracted from
wavelength of X-ray corresponding to CuK1 (λ=0.1540 WSA, PSA, and SBA are tabulated in Table 1. The
nm) radiation under a constant current of 40 mA at a dislocation density () of the samples was calculated by
potential difference of 40 kV. The diffraction patterns of Williamson Smallman’s equation:
these three samples were achieved equally in structure.
Compared to w-K2SiO3 NPs, a slight decrease in the peak 𝛿 = 𝑛⁄𝑑 2 (4)
intensity was observed for p-K2SiO3 and s-K2SiO3 NPs,
Here, n is a fraction of unity, and d is the crystallite size.
which is inappropriate for distinguishing d-spacing of
As per Scherrer’s equation, peak broadening for the
silicate molecules because of different distributions of
moisture content in materials. The decrease in peak crystallite size of the materials generally depends on 1/cos,
intensity of the XRD pattern at 29.59° indicates the whereas the strain of materials depends on tan as shown in
absorption of water molecules by the silicate molecules Eqs. (1) and (2). The contribution of crystallite size and
(Billingham et al. 1997). Decreasing the peak intensity of p- strain in the peak broadening are independent and exhibit a
K2SiO3 and s-K2SiO3 NPs, the value of βhkl increased, Cauchy-like profile. Therefore, the following relationship
signifying a decrease in the crystallinity, which is correlated can be established by the sum of peak broadening
to Scherrer’s Eq. (1). responsible for crystallite size and strain.
The development of lattice strain (ɛ) in all samples was 𝛽ℎ𝑘𝑙 = [𝛽𝑑 + 𝛽𝑠 ] (5)
calculated from the following equation:
By substituting eq. (1) and (2) put in eq. (5) the value of
𝛽𝑠
𝜀= (2) peak broadening is given by
4 𝑡𝑎𝑛 𝜃ℎ𝑘𝑙
𝑘𝜆
In the XRD section, specify how peak shifts and 𝛽ℎ𝑘𝑙 = [ + 4𝜀 𝑡𝑎𝑛 𝜃] (6)
𝑑 𝑐𝑜𝑠 𝜃
broadening correlate with particle size and crystallinity
changes, particularly in relation to the Debye-Scherrer Now rearrange the above equation, and we get,
calculations.
The lattice strain of w-K2SiO3, p-K2SiO3, and s-K2SiO3 𝑘𝜆
𝛽ℎ𝑘𝑙 𝑐𝑜𝑠 𝜃 = + 4𝜀 𝑠𝑖𝑛 𝜃 (7)
NPs was observed as 0.195, 0.269, and 0.302, respectively 𝑑
 Green synthesis of potassium silicate nanoparticles from biomass ashes …

Table 1 The crystallite size, lattice strain, and dislocation density estimated from the Scherrer and W-H equations
of K2SiO3 NPs derived from PSA, SBA, and WSA biomass ashes
Debye-Scherrer’s formula W-H method (UDM)
Samples Dislocation Dislocation
Crystallite Lattice Strain Lattice Stress Crystallite Lattice Strain
density density 
Size (nm) ɛ (×10-2)  (×103) Size (nm) ɛ (×10 )
-2
 (×1011) cm-2 (×1011) cm-2
w-K2SiO3 73 0.195 14.62 0.187 138 0.087 0.052
p-K2SiO3 53 0.269 20.17 0.356 125 0.155 0.064
s-K2SiO3 47 0.302 22.65 0.452 78 0.166 0.164

Fig. 3 (a-c) Williamson-Hall equation plot, and (d) crystallite size, lattice strain of w-K2SiO3, p-K2SiO3, and s-K2SiO3
NPs, respectively

The above equation is a straight-line equation known as Figs. 4(a-c) show the digital images of WS, PS, and SB
the Williamson-Hall equation. Figs. 3(a-c) demonstrates the biomasses and snapshots of their ashes in the corresponding
W-H plot of all samples. The crystallite size, strain, and inset, respectively. Figs. 4(d-f) show the FE-SEM images of
dislocation density of w-K2SiO3, p-K2SiO3, and s-K2SiO3 synthesized w-K 2 SiO 3 , p-K 2 SiO 3 , and s-K 2 SiO 3 NPs,
NPs are shown in Fig. 3(d). According to the result, the respectively. The microstructure of p-K 2 SiO 3 was
crystallite size of all samples of K2SiO3 was determined to agglomerated NPs. The other two synthesized nanomaterials
be 138 nm, 125 nm, and 78 nm, respectively, and the strain (s-K2SiO3, and w-K2SiO3) showed non-uniform, asymmetrical,
was observed to be 0.087, 0.155, and 0.166, for w-K2SiO3, and agglomerated NPs that moderately/ highly adhered with
p-K2SiO3, and s-K2SiO3 NPs, respectively. The crystallite each other. The average crystallite size of w-K2SiO3, p-
size estimated from the W-H plot analysis was higher than K2SiO3, and s-K2SiO3 NPs decreased from 138 nm to 78
the crystallite size calculated from Debye-Scherrer’s nm, respectively. BF-TEM images of w-K2SiO3, p-K2SiO3,
formula, which is possible because the W-H equation and s-K2SiO3 NPs are shown in Figs. 4(g-i), respectively.
considers the broadening phenomenon caused by the The p-K2SiO3 showed an agglomerated and asymmetrical
internal strain, while Scherrer’s method does not (Gong and geometry with a wide size distribution similar to cubical
Kim 2013). Dislocation density () indicates the shapes of approximately 125 nm. Every primary particle
malformation of the lattice sight compared to the well- was interconnected and adhered to each other. The s-
arranged crystal lattice of the material. The dislocation K2SiO3 and w-K2SiO3 NPs clearly showed moderately and
density values of w-K2SiO3, p-K2SiO3, and s-K2SiO3 NPs, highly combined NPs with an average crystallite size of 78
are shown in Fig. 2(b). The dislocation density of the nm and 138 nm, respectively. Comparatively, s-K2SiO3 NPs
material can occur due to unlike vacancies, interstitial were observed to be the most minor and non-uniform size
defects, and point defects, among other things. Table 1 distribution of NPs. The SAED pattern of w-K2SiO3, p-
summarises the computed  for all biomasses. K2SiO3, and s-K2SiO3 NPs are shown in the inset of Figs.
 Abhishek Sharma et al.

Fig. 4 Surface morphology analysis by biomasses (a, b & c), FE-SEM (d, e & f), BE-TEM, (g, h & i) and SAED
patterns (j, k & l) of w-K2SiO3, p-K2SiO3, and s-K2SiO3 NPs

Table 2 Optical band gap, Urbach Energy (eV), and

Refractive Index (η) of w-K2SiO3, p-K2SiO3, and s-K2SiO3 (𝛼ℎ𝜈)𝑛 = 𝐶𝑚 (ℎ𝜈 − 𝐸𝑔 ) (8)
NPs
on the y-axis. The Tauc’s relation is given in the following
Bandgap energy Urbach Tail Refractive
Samples equation.
(Eg) (eV) (EU) (eV) Index (η)
Where Eg is the optical energy bandgap, hν is the energy
w-K2SiO3 3.66 0.3108 1.8148 of the incident photon, α is the optical absorption
p-K2SiO3 3.75 0.3003 1.7528 coefficient, and Cm is the material constant. The value of
s-K2SiO3 3.78 0.2601 1.7404 “n” in the Tauc’s relation depends on the transmission
phenomenon. The Eg of biomass-derived K2SiO3 NPs has
been treated as the direct bandgap by applying factor “n” as
4(j-l), respectively. The electron diffraction rings with tiny 2. The Eg of w-K2SiO3, p-K2SiO3, and s-K2SiO3 NPs was
dots in all SAED images also indicated the polycrystalline calculated to be 3.66 eV, 3.75 eV, and 3.78 eV,
nature of all K2SiO3 NPs samples. respectively. The size of particles could significantly
influence the Eg of silicates. The higher values of Eg are
3.2 Optical Properties responsible for the smaller particle size of silicates (Asyikin
et al. 2020). Fig. 5(c) illustrates the EU, which was created
The optical properties such as Urbach tail (EU), bandgap by the straight line of the natural logarithm of the
(Eg), and refractive index (η) were determined from the absorption coefficient ln(α) against (h). The EU of the
transmittance spectra of WSA, PSA, and SBA-derived materials is computed as the inverse slope of a straight line.
K2SiO3 NPs from UV-Vis spectroscopy. Fig. 5(a) shows the The EU informs us about the scale of disorder in amorphous
absorption and transmission spectra of biomass-derived materials (Dousti et al. 2013). Materials with high EU levels
K2SiO3 NPs in the 200 - 850 nm range. The broadened are more prone to introduce weak bonds, such as defects
edges of the absorption spectra were observed in the 300- (Halimah et al. 2010). The EU of w-K2SiO3, p-K2SiO3, and
375 nm range. The absorption spectrum of biomass is s-K2SiO3 NPs were estimated to be 0.3108 eV, 0.3003 eV,
primarily affected by the roughness, scattering from the and 0.2601 eV, respectively (Table 2). The η of the
surface, oxygen deficit, and impurity centers (Kumar and materials is another substantial parameter for optical
Mohanty 2014). It is clear from the inset of Fig. 5(a) that properties that directly depends on the degree of the
the observed average transmittance percentage of w- crystallinity (Sommer et al. 2016). The values of η are used
K2SiO3, p-K2SiO3, and s-K2SiO3 NPs is 22%, 45%, and as the potential of the material for utilization as optical
43%, respectively. The optical energy bandgap (Eg) was devices (Azlan et al. 2014). Using the Eg, we have
determined from Tauc’s plot. The trend of Eg of silicate determined the η of w-K2SiO3, p-K2SiO3, and s-K2SiO3 NPs
samples is shown in Fig. 5(b). The optimization of Eg for by applying the following equation (Reddy et al. 1998).
these three biomasses was determined by the intercept value
of the plot at the x-axis as photon energy h (eV) vs. (h)n 𝑛 = 4.084 − 0.62𝐸𝑔 (9)
 Green synthesis of potassium silicate nanoparticles from biomass ashes …

Fig. 5 (a) UV-visible absorption, where the inset shows the transmission spectra, (b) direct bandgap, (c) Urbach energy
tail plot, and (d) full survey of XPS spectra of w-K2SiO3 NPs, p-K2SiO3 NPs, and s-K2SiO3 NPs.

Where Eg is the optical bandgap value and η is the 378.2 eV and 293.1eV due to spin-orbital interaction,
refractive index. The calculated values of η with Eg for w- respectively. Figs. 6(B1-B3) show the sub-signals of K2p at
K2SiO3, p-K2SiO3, and s-K2SiO3 NPs are given in Table 2. 292.5 eV, and 295.5 eV characteristic for K2p3/2 and K2p1/2,
It was observed that η of all three samples (K2SiO3 NPs) respectively, where silica ironically coordinated the
decreased in the order from 1.8148 to 1.7404. potassium (Tolj et al. 2021). The intensity and the area
under the curve of Si2p peak for s-K2SiO3 NPs is relatively
3.3 Elemental analysis and binding energy increased from other p-K2SiO3 and w-K2SiO3 NPs, which
implies that the concentration of related silica in SBA is
The chemical composition of p-K2SiO3, s-K2SiO3, and higher, as shown in Figs. 6(C1-C3). From Fig. 6(C2), the
w-K2SiO3 NPs was investigated using XPS analysis. The Si2p peak of s-K2SiO3 is broader because of the variation in
concentration, chemical valence, microstructure, and electron density at the silicon atom by changing the
elemental composition of the top of the surface of the chemical environment (Simonsen et al. 2009). Here Si2p1/2
materials could be determined because of the usual sample and Si2p3/2 signal peaks are overleaped due to the Si-OH
depth for XPS, which was up to 10 nm. The XPS peak group being detected as the broadening of the signal of
fitting software “XPSPEAK4.1” was used to observe the Si2p, which makes it hard to separate the Si-OH group from
core-level analysis of p-K2SiO3, s-K2SiO3, and w-K2SiO3 the Si-O-Si bond for the network of bulk silica (Simonsen et
NPs. The XPS complete survey shows the existence of Si, al. 2009). By the calculation, the elemental composition for
K, fraction part of Na and O atoms in p-K2SiO3, s-K2SiO3, O1s, C1s, Si2p, and K2p of s-K2SiO3 NPs was found to be
and w-K2SiO3 NPs, as shown in Fig. 5(d). According to the 37.02%, 20.18%, 7.79%, and 31.80%, respectively (Table
full scanned spectra, the binding energies of silica, carbon, 3).
potassium, oxygen, and sodium were found in all three A fraction of 3.18% of Na1s was present in all samples,
samples, which are centered at around 101.3 eV, 287.5 eV, possibly due to the chemical process. Meanwhile, we have
293.2 eV, 531.2 eV, and 976.7eV, respectively. Two signals calculated the direct energy bandgap, Eg by XPS O1s data
were obtained for silica as Si2p and Si2s situated at 102.2 of p-K2SiO3, s-K2SiO3, and w-K2SiO3 NPs shown in the
eV and 153.6 eV, respectively. The deconvolution of the Figs. 6(D1-D3). Many scientists have reported direct
Si2p spectrum of all these three biomass is shown in Figs. bandgap by XPS O1s data (Kamimura et al. 2014, Nichols
6(A1-A3). Three sub-signals of Si-O-Si, C-O-H, and C=O et al. 2014, Zhang et al. 2014). The values of Eg were
corresponding to the binding energy centered at 532.01 eV, determined as 3.88 eV, 3.79 eV, and 3.78 eV for p-K2SiO3,
530.01 eV, and 529.01 eV, respectively, confirmed the s-K2SiO3, and w-K2SiO3 NPs, respectively. The estimated
presence of hybrid silica. As per the XPS analysis, K has a direct bandgap from XPS was observed in close agreement
similar asymmetry. The signals of potassium were found to with the calculated values from Tauc’s plot. (Ma et al.
be split into two peaks K2s and K2p, at a binding energy of 2019).
 Abhishek Sharma et al.

Fig. 6 Core-level analysis of (A, 1-3) O1s, (B, 1-3) K2p, and (C, 1-3) Si2p, (D, 1-3) the determination of Eg through the
O1s peak analysis by XPS measurement for w-K2SiO3, p-K2SiO3, and s-K2SiO3 NPs

Table 3: Elemental (atomic) percentage of O, C, Na, Si, and K in s-K2SiO3 NPs (as per XPS analysis)
Peak Intensity (I) Sensitivity (S) I/S Concentration Concentration (%)
O 1s 440,000 0.63 698,412 0.3702 37.02
C 1s 78,048 0.205 380,721 0.2018 20.18
Na 1s 150,747 2.51 60,058 0. 0318 3.18
Si 2p 25,000 0.17 147,058 0.0779 7.79
K 2p 329,895 0.55 600,000 0.3180 31.80
𝐼
∑ = 1,886,258
𝑆

3.4 Antibacterial activity toxic against E. coli and S. aureus and efficiently inhibit the
growth of both organisms. In this study, s-K2SiO3 NPs
The antibacterial activity of w-K2SiO3, p-K2SiO3, and s- displayed the best antibacterial activity compared to p-
K2SiO3 NPs was performed on Gram-negative E. coli and K2SiO3 NPs and w-K2SiO3 NPs (Figs. 7(a) and (b)). A semi-
Gram-positive S. aureus bacteria. The antibacterial activity logarithmic graph of the viable cell counts of s-K2SiO3 NPs
of three synthesized samples of K2SiO3 was studied through in E. coli and S. aureus displayed the complete eradication
a time-dependent test, as reported by Sharma et al. (2015). in the viable cell counts after 6 h of the treatment. However,
All three synthesized K2SiO3 NPs are found to be highly the p-K 2 SiO 3 and w-K 2 SiO 3 NPs did not completely
 Green synthesis of potassium silicate nanoparticles from biomass ashes …

Fig. 7 Time-dependent bacterial cell viability compared with control (without treatment) for (a) E. coli and (b) S.
aureus, and semi-logarithmic graph of the viable cell counts of (c) E. coli and (d) S. aureus under the treatment of p-
K2SiO3, w-K2SiO3, and s-K2SiO3 NPs

Fig. 8 Culture plates exposed with 0.1 mg of s-K2SiO3, nanoparticles for 6 h were plated on Luria-Bertani (LB) agar
plates for E. coli and S. aureus

eradicate the bacterial cell viability for both organisms known to have larger surface areas that result in direct and
(Figs. 7(c) and (d)). Fig. 8 shows the culture plates, which increased contact with bacterial cell walls. This interaction
confirmed the reduction of colony numbers with time for further results in increased cellular permeability and
both E. coli and S. aureus under the influence of s-K2SiO3 membrane dysfunction, significantly inhibiting bacterial
NPs. growth via triggering reactive oxygen species (ROS)
Previous studies demonstrated that the inhibition of generation, enzyme inactivation, and damaging proteins and
bacterial growth was observed to be varied and size- nucleic acids (Wang et al. 2017). Although it is well-known
dependent (Balaz et al. 2019). The smaller crystallite size that smaller nanoparticles are more toxic to bacterial cells,
leads to direct interactions with microorganisms, which some studies claim that larger nanoparticles have more
showed more significant effects on both microbes (Ohira antimicrobial potential, which could be due to other factors,
and Yamamoto 2012, Li, Wu et al. 2016). Compared to the such as surface charge and functional modifications (El
p-K2SiO3 (53 nm) and w-K2SiO3 (73 nm), s-K2SiO3 NPs Badawy et al. 2011) (Fig. 9a). Nevertheless, in this study,
(47 nm) showed a significantly higher inhibitory effect since the biogenically as-synthesized small-sized K2SiO3
against both Gram-negative and Gram-positive bacteria due NPs showed high antimicrobial activity, it can be assumed
to the smallest crystallite size. Smaller nanoparticles are that small-sized K2SiO3 NPs might possess more interactive
 Abhishek Sharma et al.

Fig. 9 (a) Schematic diagram of the antibacterial effect of s-K2SiO3 NPs against bacteria, (b) possible mechanism of
antibacterial activity with K2SiO3 NPs

properties with the bacterial cell wall that facilitates K2SiO3 NPs, respectively. Electron diffraction rings of the
enhanced cellular penetration of the K2SiO3 NPs to initiate SEAD pattern also confirmed the polycrystalline nature of
the antibacterial activity and the destruction of the cell wall, samples of K2SiO3 NPs. Agglomerated species of w-
via intercellular ROS generation, inactivation of cellular K2SiO3, p-K2SiO3, and s-K2SiO3 NPs were confirmed from
enzymes, mitochondrial damage, and denaturation of DNA SEM images. The optical bandgap of w-K2SiO3, p-K2SiO3,
and protein. Consequently, the synthesized s-K2SiO3 NPs and s-K2SiO3 NPs was calculated to be 3.66 eV, 3.75 eV,
show promising results for their biological applications, and 3.78 eV, respectively. The higher optical bandgap
primarily as antibacterial agents. The possible mechanism values are responsible for the smaller particle size of
of bacterial destruction by K2SiO3 NPs is shown in Fig. potassium silicates. The core-level XPS spectra of Si2p
9(b). The factors contributing to the remarkable anti- deconvolution peaks were observed in the hybrid silica.
bacterial activity of K2SiO3 NPs are the significant K2p3/2 (292.5 eV) and K2p1/2 (295.5 eV) peaks overlap and
adhesion to the bacterial cell walls and the release of K+ make the K2p signal because the K is ironically coordinated
ions, which results in the formation of hydroxyl ions that by silica. The coordination K2p confirms the presence of
cause toxicity to the bacteria and cell membrane. However, potassium silicate in all samples. The antibacterial activity
further research is needed to fully understand the of w-K2SiO3, p-K2SiO3, and s-K2SiO3 NPs was investigated
antibacterial mechanisms of K2SiO3 NPs synthesized from against E. coli and S. aureus. In our study, the synthesized
biomass wastes with underlying effects for enhanced s-K2SiO3 NPs are found to be highly toxic against E. coli
antibacterial capabilities. and S. aureus compared to p-K2SiO3 NPs and w-K2SiO3
NPs were able to eradicate both microorganisms within 6 h
of treatment entirely. The findings revealed the novel low-
4. Conclusions cost development of K2SiO3 NPs with potent antibacterial
activities.
Biogenic w-K2SiO3, p-K2SiO3, and s-K2SiO3 NPs were
synthesized by ambient fiery and KOH-assisted thermal
process at a precise temperature of 700 °C in a muffle Acknowledgement
furnace. The dominant peak (113) in the XRD pattern of
potassium silicate NPs indicated the breakage of the Anirudh Kumar acknowledges the CSIR-SRF (08/096-
potassium and silica components regardless of activation 0012/2020/EMR-I) provided for the Ph.D. dissertation
temperature. W-H method reveals the micro-strain increased work. Vikas Kumar acknowledges the Centre of Excellence
from 0.087 to 0.166 MPa as the crystalline size decreased Project to provide the Research Associate fellowship.
from 138 to 78 nm for samples varied from w-K2SiO3 to s- Sanjeev K. Sharma (SKS) acknowledges the financial
 Green synthesis of potassium silicate nanoparticles from biomass ashes …

support from the Department of Higher Education, potassium”, J. Mol. Evol., 87(9-10), 271-288.
Government of Uttar Pradesh, India for sanctioning the https://doi.org/10.1007/s00239-019-09915-2
projects (108/2021/2585/Sattar-4-2021-4(28)/2021/20) under de Oliveira, K.G., de Lima, R.R.S., de Longe, C., Bicudo, T.d.C.,
the Research & Development program and (78/2022/1984/ Sales, R.V. and de Carvalho, L.S. (2022), “Sodium and
potassium silicate-based catalysts prepared using sand silica
Sattar-4-2022-003-70-4099/7/022/19) under Centre of concerning biodiesel production from waste oil”, Arab. J.
Excellence for Research and innovation of smart materials Chem., 15(2), 103603.
for Sensor applications. SKS also acknowledges the financial https://doi.org/10.1016/j.arabjc.2021.103603
support from the sanctioned project, CST/D-1524, by CST- Deng, W., Kang, T., Liu, H., Zhang, J., Wang, N., Lu, N., Ma, Y.,
UP, and C.C.S. University-funded project (Ref. No. Dev./ Umar, A. and Guo, Z. (2018), “Potassium hydroxide activated
1043/29.06.2022) to implement research and innovation. and nitrogen doped graphene with enhanced supercapacitive
Ashish R. Sharma: This study was supported by the Basic behavior”, Sci. Adv. Mater., 10(7), 937-949.
Science Research Program through the National Research https://doi.org/10.1166/sam.2018.3279
Foundation of Korea (NRF) funded by the Ministry of Deshmukh, R.K., Ma, J.F. and Bélanger, R.R. (2017), “Role of
silicon in plants”, Front. Plant Sci., 8, 1858.
Education (NRF-2020R1C1C1008694). https://doi.org/10.3389/fpls.2017.01858
Dogan, M.F., Yildiz, O., Arslan, S.O. and Ulusoy, K.G. (2019),
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