- Nano Express
- Open Access
Influence of Mg Doping on ZnO Nanoparticles for Enhanced Photocatalytic Evaluation and Antibacterial Analysis
© The Author(s). 2018
- Received: 29 May 2018
- Accepted: 26 July 2018
- Published: 3 August 2018
In this research, a facile co-precipitation method was used to synthesize pure and Mg-doped ZnO nanoparticles (NPs). The structure, morphology, chemical composition, and optical and antibacterial activity of the synthesized nanoparticles (NPs) were studied with respect to pure and Mg-doped ZnO concentrations (0–7.5 molar (M) %). X-ray diffraction pattern confirmed the presence of crystalline, hexagonal wurtzite phase of ZnO. Scanning electron microscope (SEM) images revealed that pure and Mg-doped ZnO NPs were in the nanoscale regime with hexagonal crystalline morphology around 30–110 nm. Optical characterization of the sample revealed that the band gap energy (Eg) decreased from 3.36 to 3.04 eV with an increase in Mg2+ doping concentration. Optical absorption spectrum of ZnO redshifted as the Mg concentration varied from 2.5 to 7.5 M. Photoluminescence (PL) spectra showed UV emission peak around 400 nm. Enhanced visible emission between 430 and 600 nm with Mg2+ doping indicated the defect density in ZnO by occupying Zn2+ vacancies with Mg2+ ions. Photocatalytic studies revealed that 7.5% Mg-doped ZnO NPs exhibited maximum degradation (78%) for Rhodamine B (RhB) dye under UV-Vis irradiation. Antibacterial studies were conducted using Gram-positive and Gram-negative bacteria. The results demonstrated that doping with Mg ions inside the ZnO matrix had enhanced the antibacterial activity against all types of bacteria and its performance was improved with successive increment in Mg ion concentration inside ZnO NPs.
- Mg-doped ZnO nanoparticles
- Structural study
- Optical study
- Photocatalytic evaluation
- Antibacterial study
Nanoparticles exhibit novel properties which depend on their size, shape, and morphology which enable them to interact with plants, animals, and microbes . Nanoparticles of commercial importance are being synthesized directly from metal or metal salts, in the presence of some organic material or plant extract. The creepers and many other plants exude an organic material, probably a polysaccharide with some resin, which helps plants to climb vertically or through adventitious roots to produce nanoparticles of the trace elements present, so that they may be absorbed . Nanosize inorganic compounds have shown remarkable antibacterial activity at very low concentration due to their high surface area to volume ratio and unique chemical and physical features . In addition, these particles are also more stable at high temperature and pressure . Some of them are recognized as non-toxic and even contain mineral elements which are vital for the human body . It has been reported that the most antibacterial inorganic materials are metallic nanoparticles and metal oxide nanoparticles such as silver, gold, copper, titanium oxide, and zinc oxide [6, 7]. Zinc is an essential trace element for the human system without which many enzymes such as carbonic anhydrase, carboxypeptidase, and alcohol dehydrogenase become inactive, while the other two members, cadmium and mercury belonging to the same group of elements having the same electronic configuration, are toxic . For biosynthesis of nanoparticles, different parts of a plant are used as they contain metabolites such as alkaloids, flavonoids, phenols, terpenoids, alcohols, sugars, and proteins which act as reducing agents to produce nanoparticles. They also act as capping agent and stabilizer for them. They are used in medicine, agriculture, and many other fields as well as technologies. The attention is therefore focused on all plant species which have either aroma or color in their leaves, flowers, or roots for the synthesis of nanoparticles because they all contain such chemicals as will reduce the metal ions to metal nanoparticles . Recently, nanoparticles have started gaining interest because of their unique mechanical, optical, magnetic, electrical, and other properties . These emergent characteristics make them a promising candidate for use in electronics, medicine, and other fields. It has been observed that nanomaterials have a greater surface to volume ratio compared with their conventional forms . This is the reason why nanomaterials show greater chemical reactivity. Basically at nanoscale, the quantum effect is more pronounced to determine their end characteristics leading to novel optical, magnetic, and electrical behavior. Among the various metal oxide semiconductor nanostructures, ZnO nanostructures have attracted considerable interest because of their low cost, high chemical stability, and mass production . ZnO research only makes up a reasonable bit of the current nano-look into; however, all factors considered it is one of the important materials which will presume an expanding part of the nanotechnology without bounds. ZnO is one of the most generally connected topical drugs ever. It is utilized in most sunscreens and discovers its way into numerous treatments for anguish and itching alleviation . It will be seen on the function of photocatalysis, essentially on ZnO and doped ZnO; there is a large cluster of potential chemical, photochemical, and electrochemical responses that can happen on the photocatalyst surface . ZnO has won much consideration in the degradation and total mineralization of environmental contaminations . The best-preferred point of view of ZnO is the capacity to attract an extensive variety of solar-powered light range and more light quanta than some semiconducting metal oxides. ZnO has developed as the main material and a proficient and promising candidate in green ecology management structure due to its novel attributes .
Basically two factors, namely surface area and surface defects, are the most important variables to determine the photocatalytic activity of semiconductor metal oxides. Due to its high surface activity, crystalline nature, morphological features, and texture; ZnO nanoparticles are considered as the most favorable catalyst for the degradation of organic pollutants . Recent literature reported that Mg-doped ZnO nanostructures can exhibit excellent properties for device application . Investigation on doping Group II elements with ZnO showed that the dopants can alter the band gap energy (Eg) with an increase in the UV-Visible luminescence intensity .
Doping of Mg into ZnO is expected to modify the absorption, physical, and chemical properties of ZnO . Metal ion-doped ZnO nanostructures are the most promising catalyst for the degradation of various pollutants because of its enhancement in its optical properties . Different types of infectious diseases caused by bacteria pose a severe menace towards the public health worldwide. To enhance the antibacterial activity of ZnO, different types of physiochemical properties such as particle size, crystallinity index, and optical properties should be modified by doping with metal or non-metal .
By inducing more defects over the surface of ZnO, the optical adsorption properties can be enhanced. Basically minute amounts of dopants are sufficient to act as donors or acceptors inside the semiconductor crystal lattice which will significantly alter the properties of the semiconductor up to a greater extent. The size quantization makes variation in the energy gap between the conduction band electrons and valence band holes which result in change in optical properties of the doped metal oxide nanostructures . Earlier literature reported that ZnO nanoparticles can resist bacterium and they have the ability to shield ultraviolet radiations . Zinc oxide NPs have the ability to disrupt the gram-negative cell membrane structure of Escherichia coli [25, 26]. It was reported also that nanoparticles with a positive charge could bind the gram-negative cell membrane using electrostatic attraction . ZnO NPs doped with different metal ions were evaluated against E. coli, and Staphylococcus aureus showed the antibacterial activity increasing with crystallite size .Various physical and chemical techniques have been adopted by researchers to synthesize pure and doped ZnO NPs like the vapor transport process , spray pyrolysis , thermal decomposition , electrochemical method , sol-gel method , hydrolysis , chemical precipitation , and hydrothermal method  in order to tailor its morphology and size. Among all these methods, co-precipitation method is relatively simple and inexpensive. Furthermore, it can give high yield at room temperature for the synthesis of pure and doped ZnO NPs .
Here, we have investigated the preparation and characterization of ZnO nanoparticles with different concentrations of Mg dopants by using a simple chemical co-precipitation method. The effects of Mg2+ ion concentration inside the ZnO lattice have been evaluated in terms of structural, morphological, optical, and photocatalytic studies. Further, the effect of Mg2+ ions on the antibacterial activity were studied against (Gram-positive and Gram-negative) S. aureus, E. coli, and Proteus cultures.
In the electrochemical series, Mg is more reactive than Zn and hence it undergoes reduction to occupy the Zn lattice.
The crystal structures of the samples were investigated by X-ray diffraction (XRD) Bruker D8 advanced X-ray diffractometer) with Cukα radiation (λ = 1.54 Å) and surface morphology features were studied by field emission scanning electron microscope (FESEM, ZEISS). Optical absorption spectra of the samples were recorded with a double beam UV-Visible spectrophotometer using Hitachi U-3900H in the range 200–1200 nm. Photoluminescence (PL) emission studies were carried out by means of a spectrometer (JOB HR800 IN Yoon Horbe) using a He-Cd laser source with a wavelength of 325 nm. The antibacterial activity of the synthesized samples was tested towards different organisms by agar disc diffusion technique.
Measurement of Photocatalytic Activity
where C0 represents the initial time of absorption and Ct represents the absorption after various intervals of time (0, 30, 60, 90, and 120 min).
E. coli (Gram-negative), S. aureus (Gram-positive), and Proteus (Gram-negative strains) were maintained at 4 °C on broth media before use. Nutrient agar medium was prepared and sterilized at 121 °C for 15 min. Twenty-five milliliters of nutrient agar was poured into sterile Petri dishes and setting was allowed. In each Petri dish was spread 0.2 ml of different bacterial species (E. coli, S. aureus, and Proteus). A disc was prepared and placed in the plates with the help of a sterile loop, and two discs per plates were made into the set agar containing the bacterial culture.
Lattice parameters of pure and Mg-ZnO NPs
Crystallite size (D)
Atomic packing fraction (APF) %
1.995 × 10− 3
2.5% Mg-ZnO NPs
1.552 × 10− 3
5% Mg-ZnO NPs
1.201 × 10−3
7.5% Mg-ZnO NPs
1.043 × 10−3
Effect of Doping on Lattice Parameters
The crystallite size, lattice parameters, atomic packing fraction (APF), lattice strain, and volume show the physical properties of pure and doped ZnO NPs . For a wurtzite phase, the lattice parameters are calculated by using the Eq. (7–9) where, a = b, and c are the lattice parameters, dhkl is the interplanar distance corresponding to its Miller indices (hkl).
The calculated lattice parameters are listed in Table 1. It is observed from Table 1 that there is an alteration in its lattice parameter values as Mg2+ ion substitutes Zn2+ ion in the lattice. As the doping concentration increases, the dopant atom incorporated occupies the substitutional lattice site. It is also observed from Table 1 that the crystallite size (D) varies inversely with the atomic packing fraction (APF) as shown in Eq. (10).
Furthermore, it is noted that there is a decrease in its lattice strain due to Mg2+ ions doping inside the ZnO matrix (Table 1), which causes the local distortion of the crystal structure. This is evident and noted earlier also in the literature for the difference in their atomic radii as well as in their doping concentration .
Field Emission Scanning Electron Microscope (FESEM) and EDS Analysis
From Fig. 5b, it is found that the band gap energy (Eg) for pure ZnO NPs is around 3.36 eV and decreases with Mg dopant (3.36 to 3.04 eV). The band gap is decreased due to strong quantum confinements and enhancement in their surface area to volume ratio . Enhancement of redshift and decrease in band gap energy (Eg) confirm the presence of Mg2+ inside the Zn2+ site of the ZnO lattice.
Catalytic degradation with band gap energy:(pure and Mg-doped ZnO NPs)
Band gap (Eg) eV
Degradation (%) at 120 min
Degradation rate constant (k)
1.09 × 10−3
2.5% Mg-ZnO NPs
2.76 × 10− 3
5% Mg-ZnO NPs
5.72 × 10− 3
7.5% Mg-ZnO NPs
1.26 × 10−2
It seems that Mg-doped ZnO NPs act similar to electron sink, which consequently can enhance significantly the separation of the photo-generated electron−hole pairs and inhibit their recombination resulting in improved photocatalytic activity .
Thus, it is necessary to prevent the recombination of electron–hole pairs to have better photocatalytic activity of semiconductor based NPs. Controlled doping of Mg over the ZnO NPs up to a certain limit can enhance the photocatalytic activities. All the Mg-doped ZnO NPs show a significant enhancement of the photo-degradation of RhB dye compared with the pure ZnO NPs. In this research, 7.5% Mg-doped ZnO NPs show better photocatalytic properties after 120 min compared with pure ZnO sample. This might be due to the change in their particle size and band gap effects .
Average diameter values of Zones of Inhibition (ZOI) for pure and Mg-doped ZnO NPs (2.5–7.5 M %)
Zone of inhibition (mm)
6 ± 0.7
9 ± 0.7
9 ± 0.6
2.5% Mg-ZnO NPs
9 ± 0.4
10 ± 0.4
13 ± 0.4
5% Mg-ZnO NPs
12 ± 0.3
14 ± 0.5
16 ± 0.3
7.5% Mg-ZnO NPs
15 ± 0.4
16 ± 0.5
19 ± 0.3
The interaction between the NPs and the cell wall of bacteria was changed due to doping of Mg. The growth of S. aureus and the other two bacteria was more commendably affected by Mg2+-doped ZnO nanostructures compared with pure ZnO NPs. From Table 3, it is noted that Gram-negative and Gram-positive have different inhibition zones. This difference in the antibacterial activity of Mg-doped ZnO nanostructures against Gram-negative and Gram-positive bacterial strains may be due to the difference in cell wall structure of those respective bacteria. It was also reported earlier that various bacterial strains had considerably different infectivity and tolerance levels towards the different agents including antibiotics . Also differences in the antibacterial activity might be due to different particle dissolution.
Basically, the antibacterial efficiency of pure and Mg-doped ZnO NPs is mainly dependent on the increased levels of reactive oxygen species (ROS), mostly hydroxyl radicals (OH) and singlet oxygen . This is mainly due to the enlarged surface area which causes increase in oxygen vacancies as well as the diffusion capacity of the reactant molecules inside the NPs . The reactive oxygen group contains superoxide radical and hydrogen peroxide. Both of them can damage the DNA and cellular protein leading to cell death . Moreover, the presence or addition of the nanostructures on the surface or cytoplasm of the bacteria can cause the disruption of cellular function as well as disorganization of the cell membranes . The doping of Mg with ZnO may lead to the variation in grain size, morphology, and solubility of Zn2+ ions. All these factors combined together have a robust impact on the antibacterial activity of ZnO [71, 72]. The results have revealed that Mg-doped ZnO nanostructures will be a promising candidate to be used for potential drug delivery systems to cure some significant infections in the near future.
To conclude, pure and Mg-doped ZnO structures were successfully synthesized by co-precipitation method. The XRD patterns revealed the wurtzite structure for all the nanosamples and no impurity phase was noted. The maximum crystallite size obtained from XRD was less than 100 nm. FE-SEM studies confirmed that the crystallite size increased with increase in Mg content. The UV-Visible results revealed that absorption underwent a redshift with Mg into ZnO as compared to pure ZnO exhibiting strong quantum confinement effects. Optical band gap energy was found to decrease from 3.36 to 3.04 eV with Mg doping, resulting in the increment in their crystallite size as a result of Mg doping. PL results confirmed the enhanced visible emissions with Mg-doped ZnO leading to the increase in delocalization of electron-hole pairs. Photocatalytic measurements revealed the increase in Mg doping in the ZnO nanoparticles that caused higher photocatalytic activity. The antibacterial activities of the synthesized nanosamples were tested against E. coli (Gram-negative), S. aureus (Gram-positive bacteria), and Proteus (Gram-negative strains).
The authors are also grateful to the authorities concerned for providing them the testing facilities of IIT Madras-Chennai, India, Anna University, and Department of Chemistry, L.R.G. Govt Arts College, Tiruppur, TN, India. One of the authors (Suresh Sagadevan) acknowledges the honor, namely the “Visiting fellow” at the Department of Physics, Center for Defence Foundation Studies, National Defence University of Malaysia, Kem Sg. Besi, 57000 Kuala Lumpur, Malaysia. The author wishes to place on record his heartfelt thanks that are due to the authorities concerned.
The authors are thankful to the authorities concerned for the funding provided from the Grant No. RP044C-17AET and RP044D-17AET from the University of Malaya, Malaysia.
Availability of Data and Materials
All relevant data are within the paper.
KPr, KS, and AK conceived and designed the experiments; KPr had performed the experiments; SS, ZZC, MRBJ, FAA, and RFR analyzed the data; KS, AK, RTS, and RRb had contributed reagents/materials/analysis tools. KPr, SS, and ZZC had written the paper. All authors read and approved the final manuscript.
The authors declare that they have no competing interests.
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