Malays. J. Anal. Sci. Volume 30 Number 3 (2026): 1706
Research Article
Optimizing the synthesis of silver
nanoparticle-modified Mg/Al LDH via response surface methodology for controlled
nanofiller loading in natural rubber latex
Puteri Nur Ainin Sofiya Putra Mohd Yamani,1 Mohd
Aidil Adhha Abdullah,1,2 Norhanifah Mohd Yazid,3 Ruslimie
Che Ali,3 Adila Mohamad Jaafar,4 Norhayati Hashim,5
and Mazidah Mamat,1,2*
1 Faculty
of Science and Marine Environment, Universiti Malaysia Terengganu, 21030 Kuala
Nerus, Terengganu, Malaysia
2 Advanced Nano Materials
(ANoMa) Research Group, Universiti Malaysia Terengganu, 21030 Kuala Nerus,
Terengganu, Malaysia
3 Technology
and Engineering Division, Rubber Research Institute of Malaysia, 47000, Sg.
Buloh, Selangor, Malaysia.
4 Pusat
Asasi Sains UPM, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor,
Malaysia
5 Faculty
of Science and Mathematics, Universiti Pendidikan Sultan Idris, 35900 Tanjong
Malim, Perak, Malaysia
*Corresponding
author: mazidahmamat@umt.edu.my
Received: 12 October 2025;
Revised: 27 April 2026; Accepted: 10 May 2026; Published: 30 June 2026
Abstract
The synthesis parameters for preparing silver
nanoparticle-modified Mg-Al layered double hydroxide (Mg-Al LDH/AgNP)
nanofillers were systematically optimized using Response Surface Methodology
(RSM) for natural rubber latex (NRL) applications. The co-precipitation method
performed at pH 10 to 11 was employed to ensure the synthesized layered double hydroxides (LDH)
suspension would be compatible with the basic NRL environment. Structural
analyses confirmed successful synthesis: Fourier
Transform Infrared Spectroscopy (FTIR) spectroscopy revealed
characteristic nitrate vibrations (1345 cm⁻ą), while X-ray Diffraction (XRD) patterns
showed an expanded interlayer spacing (7.9 Ĺ), confirming nitrate as the
interlayer anion. RSM with Box-Behnken Design (BBD) was applied using three independent
variables - the pH, molar ratio, and concentration of metal nitrate solutions -
to optimize LDH yield, resulting in a statistically quadratic model (R˛ >
0.95) with high predictive accuracy. Complementary Thermogravimetric analysis (TGA) and Carbon, Hydrogen, Nitrogen, and Sulfur (CHNS)
analysis provided additional structural insights, quantifying water content
(2.9 H₂O molecules per formula unit) and yielding the ideal chemical
formula [Mg0.75Al 0.25(OH)₂(NO₃)0.43·2.9H₂O].
The results demonstrate that RSM-optimized synthesis enables precise control
over LDH production, ensuring tailored nanofiller loading for NRL composites.
This approach facilitates the efficient preparation of NRL compounds
incorporating LDH nanofillers, advancing the development of high-performance
latex materials.
Keywords: latex compounding, response surface methodology, Mg-Al layered double hydroxide,
controlled loading, silver nanoparticle
References
1.
Teijido, R., Ruiz-Rubio, L., Echaide, A. G., Vilas-Vilela, J. L.,
Lanceros-Mendez, S. and Zhang, Q. (2021). State of the art and current trends
on layered inorganic-polymer nanocomposite coatings for anticorrosion and
multi-functional applications. Progress in Organic Coatings, 163: 106684.
2.
Gu, Y., Yang,
Z., Zhou, J., Fang, Q., Tan, X. and
Long, Q. (2023). Graphene/LDHs hybrid composites synthesis and application
in environmental
protection. Separation and Purification Technology, 328:
125042.
3.
Polo-Mendoza,
R., Martinez-Arguelles, G., Walubita,
L. F., Moreno-Navarro, F., Giustozzi, F., Fuentes, L. and Navarro-Donado, T.
(2022). Ultraviolet Ageing of Bituminous Materials: A Comprehensive Literature Review from 2011 to
2022. Construction and Building Materials, 350: 128889.
4.
Jing, G.,
Yang, L., Wang, H., Niu, J., Li, Y. and Wang, S. (2022). Interference of
layered double hydroxide nanoparticles with pathways for biomedical applications. Advanced
Drug Delivery Reviews, 188:
114451.
5.
Yılmaz,
G. E., Göktürk, I., Ovezova, M., Yılmaz, F.,
Kılıç, S. and Denizli, A. (2023). Antimicrobial Nanomaterials: A Review.
Hygiene, 3(3):
269–290.
6.
Joudeh, N.
and Linke, D. (2022). Nanoparticle classification,
physicochemical properties, characterization,
and applications: A comprehensive review
for biologists. Journal of Nanobiotechnology, 20(1): 1–15.
7.
Mekuye, B.
and Abera, B. (2023).Nanomaterials: An overview of synthesis, classification,
characterization, and applications. Nano Select, 4(8): 486–501.
8.
Baig, N.,
Kammakakam, I. and Falath, W. (2021). Nanomaterials: A review of
synthesis methods, properties, recent
progress, and challenges.
Materials Advances, 2(6): 1821–1871.
9.
El-Khawaga,
A. M., Zidan, A. and El-Mageed, A. I. A.
A. (2023). Preparation methods of different nanomaterials for
various potential applications: A
review. Journal of Molecular Structure,
1281: 135148.
10.
Baig, N.
(2022). Two-dimensional nanomaterials: a
critical review of recent progress, properties,
applications, and future directions.
Composites Part A: Applied Science and Manufacturing, 165: 107362.
11.
Zhang, Y.,
Xu, H. and Lu, S. (2021). Preparation and
application of layered double hydroxide
nanosheets. RSC Advances, 11(39): 24254–24281.
12.
Ambegoda, V.
T., Egodage, S. M., Blum, F. D. and
Maddumaarachchi, M. (2020). Enhancement of
hydrophobicity of natural rubber latex films using diatomaceous earth. Journal
of Applied Polymer Science, 138(12):
50096.
13.
Van Tonder,
L. and Labuschagné, F. J. W. J. (2021).
Systematic literature review of the effect of layered double hydroxides on the
mechanical properties of rubber. Polymers, 13(21): 3716.
14.
Wang, X.,
Zhang, Y., Ren, S., Xu, Z., Li, K., Hao, X. and He, Q. (2023). Effect of zinc
oxide/layered double hydroxide on the mechanics of silicone rubber at low temperature. European
Polymer Journal, 200: 112478.
15.
Zhang, P.,
You, P., Feng, J., Xie, R., Chen, L., Xiong, Y. and Song, P. (2023).
Vitrimer-like, mechanically
robust, healable and recyclable biobased
elastomers based on epoxy natural rubbers, polylactide and layered
double hydroxide. Composites
Part A: Applied Science and Manufacturing, 171: 107575.
16.
Assadakorn,
D., Liu, G., Hao, K., Bai, L., Liu, F.,
Xu, Y., Guo, L. and Liu, H. (2024). Effects of BET surface area and silica
hydrophobicity on natural rubber
latex foam using the dunlop process.
Polymers, 16(21): 3076.
17.
Hou, Z.,
Zhou, D., Chen, Q. and Xin, Z. (2023). Effect of different silane coupling
agents in-situ modified sepiolite on the structure and properties of natural
rubber composites prepared by latex compounding method. Polymers, 15(7):
1620.
18.
Patil, S. and
Jagadale, S. (2023). Co-precipita tion
methods for the synthesis of metal oxide nanostructures. Elsevier eBooks,
pp. 39–60.
19.
Ba-Abbad, M.
M., Benamour, A., Ewis, D., Mohammad,
A. W. and Mahmoudi, E. (2022). Synthesis
of Fe3O4 nanoparticles with different shapes through a
co-precipitation method and their application. JOM, 74(9): 3531–3539.
20.
Breig, S. J.
M. and Luti, K. J. K. (2021). Response surface methodology:
A review on its applications and challenges in microbial cultures. Materials Today:
Proceedings, 42: 2277–2284.
21.
Chelladurai,
S. J. S., K, M., Ray, A. P., Upadhyaya, M., and Narasimharaj,
V. S. G. (2020). Optimization of
process parameters using
response surface methodology: A review. Materials Today: Proceedings,
37: 1301–1304.
22.
Lee, S., Lee,
S. and Roh, J. (2021). Analysis of activation
process of carbon black based on structural parameters obtained by
xrd analysis. Crystals, 11(2):
153.
23.
Fatimah, S.,
Ragadhita, R., Husaeni, D. F. A. and
Nandiyanto, A. B. D. (2021). How to calculate crystallite size from X-ray
diffraction (XRD) using Scherrer method.
ASEAN Journal of Science and
Engineering, 2(1): 65–76.
24.
Tkachenko, Y.
and Niedzielski, P. (2022). FTIR as a method for qualitative assessment of
solid samples in geochemical
research: A review. Molecules,
27(24): 8846.
25.
Bhattacharya,
S. (2021). Central composite design
for response surface methodology and its application in pharmacy. IntechOpen
eBooks, pp. 1–15.
26.
Njoku, C. N.
and Otisi, S. K. (2023). Application of
central composite design with design
expert v13 in process optimization. IntechOpen eBooks, pp.
1–20.
27.
Dargahi, A.,
Samarghandi, M. R., Shabanloo, A.,
Mahmoudi, M. M. and Nasab, H. Z. (2021). Statistical modeling of phenolic
compounds adsorption onto
low-cost adsorbent prepared from
aloe vera leaves wastes using CCD-RSM optimization: Effect of Parameters,
Isotherm, and Kinetic Studies. Biomass
Conversion and Biorefinery, 13(9):
7859–7873.
28.
Araújo, L. K.
F., Albuquerque, A. A., Ramos, W. C.
O., Santos, A. T., Carvalho, S. H. V., Soletti, J. I. and Bispo, M. D.
(2021). Elaeis guineensis-activated
carbon for methylene blue removal:
Adsorption capacity and optimization using
CCD-RSM. Environment, Development and
Sustainability, 23(8): 11732–11750.
29.
Nivedhitha,
K., Venkatesh, R., Banapurmath, N.,
Ramesh, K., Sajjan, A. M. and Subramanian, K. (2024). Enhancing hydrogen
storage capacity: MWCNT-infused Mg–Ti alloy synthesized via mechanical
alloying. International Journal of Hydrogen Energy, 67: 351–360.
30.
Hameed, S. E.
A., El-Maaty, W. M. A., Gomaa, E. A. and Awad, F. S. (2026). PAR-intercalated
Mg/Al layered double hydroxide for efficient adsorption of acid fuchsin: experimental
study and molecular docking insights.
RSC Advances, 16(7): 6408–6420.
31.
Al-Rawajfeh,
A. E., Alrawashdeh, A. I., Etiwi, M. T., Mainali, B., Shahid, M. K., Al-Itawi,
H., Al-Shamaileh, E., Al-E’bayat, M. and Al-Sahary, A. (2025).
Fabrication of silver-incorporated ZN-AL
Layered Double Hydroxide: Characterization and Bromide-Adsorption Performance. Water,
17(11): 1578.
32.
Hassan, M.
A., Wahdain, S. F. and Onaizi, S. A. (2025). Recent advances in CO2 capture
and mineralization using layered double hydroxide-based materials: a review. Environmental
Science and Pollution Research,
32: 27368–27412.
33.
Gao, M.,
Khalkhali, M., Beck, S., Choi, P. and Zhang,
H. (2018). Study of thermal stability of hydrotalcite and carbon dioxide adsorption behavior on hydrotalcite-derived
mixed oxides using atomistic
simulations. ACS Omega, 3(9): 12041–12051.
34.
Kaur, H.,
Singh, S. and Pal, B. (2022). Effect of plasmonic metal (Cu, Ag, and Au) loading
over the physicochemical and
photocatalytic properties
of Mg-Al LDH towards degradation of tetracycline
under LED light. Applied Surface Science, 609: 155455.