Startseite Antibacterial effect of novel dental resin composites containing rod-like zinc oxide
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Antibacterial effect of novel dental resin composites containing rod-like zinc oxide

  • Shiyu Zhou , Ruihua Liu , Xinru Ma , Yushi Xie , Xiaoling Xu EMAIL logo , Qin Du EMAIL logo und Zuowan Zhou
Veröffentlicht/Copyright: 12. März 2024
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Abstract

Dental resin composite materials are widely used as dental fillings; however, the accumulation of microbes and the resulting secondary caries often leads to filling failure. ZnO, an inorganic antibacterial material, exhibits effective antibacterial properties and is considered safe for use. In this study, rod-like ZnO was prepared by using the atmospheric-pressure hydrothermal method, and its microstructure and antibacterial effects on Streptococcus mutans were studied. Subsequently, we created modified resins by incorporating rod-like ZnO at varying mass fractions and analyzed their morphological characteristics and elemental distributions. The antibacterial effectiveness, biocompatibility, and mechanical properties of these materials were examined using in vitro experiments. The results indicated that the rod-like ZnO exhibited a complete hexagonal wurtzite structure, with columnar dimensions of approximately 2.5 μm in length, 0.8 μm in diameter, and a lattice spacing of 0.2544 nm. The growth, biofilm formation, and biofilm destruction of S. mutans were significantly inhibited at 1/4, 1/2, 3/4, and 1 times the minimum inhibitory concentration. The rod-like modified resin, with mass fractions of 2.5, 5, and 7.5 wt%, exhibited evident inhibitory effects on S. mutans biofilm formation. These modified resins demonstrated no cytotoxicity toward HGF-1 cells and exhibited enhanced compressive strength. Therefore, rod-like ZnO modified resin has promising potential for the treatment of dental caries.

1 Introduction

Dental caries is a prevalent chronic infectious disease of the oral cavity and is listed by the World Health Organization as one of the three major diseases requiring prevention and treatment, along with cancer and cardiovascular diseases [1]. Among the various treatment methods, filling treatments using dental resin composite (DRC) materials are widely used in clinical practice. These materials, which are composed of organic resin monomers, inorganic fillers, and silane coupling agents, offer aesthetic advantages, good biocompatibility, and convenient operation [2]. During the curing process, cross-linking of the C═C olefin bonds in the methacrylate monomer results in polymerization shrinkage and microleakage, leading to secondary caries and filling failure [3,4]. Similar to occlusal caries, secondary caries often occurs at the edges of repair materials. It is characterized by inorganic demineralization and organic matter decomposition. Acid-producing and acid-resistant bacteria contribute to the accumulation of acidic products, lowering the pH of the biofilm microenvironment, and causing tooth tissue demineralization [5]. Compared with silver amalgam restorations, DRC materials have been found to have a higher failure rate and increased risk of secondary caries [6]. Therefore, there is a need to develop antibacterial modified DRC materials to treat secondary caries.

One approach to reduce the failure rate of resin restorations is to incorporate antibacterial fillers into DRC. These fillers can include inorganic agents, such as silver (Ag), zinc (Zn), and other metal ions and their oxides [7,8], organic agents, such as quaternary ammonium salts [9], and natural agents, such as chitosan [10]. Zn is an essential mineral element in the human body that participates in normal growth, bone metabolism, and cell signaling pathways [11,12]. Zinc oxide (ZnO) exhibits good biocompatibility and is among the inorganic materials approved by the Food and Drug Administration (FDA) due to its favorable biosafety properties [13]. It offers aesthetic advantages and chemical stability when used as a material [14]. As an antibacterial agent, ZnO exhibits significant bactericidal potential against various bacteria and fungi, including Escherichia coli, Staphylococcus aureus, Pseudomonas aeruginosa, Klebsiella pneumoniae, and Candida albicans [15,16,17]. Submicrometer-sized ZnO particles, with a diameter of 0.1–1 μm, possess a larger specific surface area, higher surface energy, increased adsorption force and action sites, strong catalytic reaction ability, and good dispersion. This enhances the antibacterial properties of ZnO compared with regular ZnO particles [18,19]. The use of submicrometer-sized ZnO overcomes the drawbacks of poor heat resistance, short antibacterial life, and susceptibility to drug resistance observed with organic antibacterial agents [20]. Furthermore, it avoids the discoloration associated with silver metal oxides [21] and does not require light activation [22]. Submicrometer-sized ZnO is widely used as an inorganic antibacterial agent in dental restorative materials. Nano-ZnO antibacterial coatings on implant surfaces can control the adhesion and aggregation of inflammatory pathogens during the early stages of implantation, thereby significantly improving the success rate of implants [23]. Adhesives containing nano-ZnO can be used to treat demineralized dentin surfaces, enhance the immediate bonding strength with the resin, reduce the degradation of the mixed layer of collagen, and promote remineralization of the carious tissue [24]. ZnO is also employed as a temporary filling material, root canal sealer, and pulp capping agent in oral materials [25]. The possible antibacterial mechanisms of ZnO are as follows: (1) ZnO catalyzes the reduction of oxygen molecules, leading to the generation of reactive oxygen species (ROS) and causing oxidative stress and DNA damage, which results in cell death and genotoxic effects [26,27]. (2) In aqueous solution, nano-ZnO releases Zn2+ ions that enter bacterial cells, leading to cell death by disrupting Zn-dependent enzyme systems, amino acid metabolism, and altering the protein structure [14,28,29]. (3) ZnO can also cause membrane damage upon direct contact with the cell membrane, thereby affecting normal cell function [30].

ZnO particles of different shapes exhibit variations in their exposed crystal planes, specific surface areas, and surface morphologies, which affect their antibacterial activities [31,32]. By utilizing the polar surface induction of ZnO crystals in an atmospheric pressure hydrothermal method, this method enables the control of reaction conditions and synthesis of ZnO with different morphologies and exposed crystal planes [33]. Building on this principle, we synthesized rod-like ZnO by adjusting the reaction temperature, material ratio, and raw materials. In this study, we investigated the inhibitory effect of rod-like ZnO on the main cariogenic bacteria, Streptococcus mutans. We also prepared modified DRC materials with various concentrations of rod-like ZnO. This study analyzed the morphology, mechanical properties, antibacterial properties, and biocompatibility of modified DRC materials.

2 Materials and methods

2.1 Properties of rod-like ZnO

2.1.1 Preparation and physical characterization of rod-like ZnO

Rod-like ZnO was synthesized and provided by the School of Materials Science and Engineering at Southwest Jiaotong University. The detailed synthesis procedure is as follows: Zinc nitrate hexahydrate (Zn(NO3)2·6H2O) was dissolved in deionized water using the atmospheric pressure hydrothermal method. Hexamethylenetetramine (HMTA, (CH2)6N4) was gradually introduced into the Zn(NO3)2 solution with continuous magnetic stirring (JOANLAB, China) for 24 h at ambient temperature. Subsequently, the mixture was transferred to a water bath (Wiggens, Germany) and maintained at 90°C for 8 h. The resulting product was separated, filtered, precipitated, washed with deionized water and anhydrous ethanol, centrifuged three times, and finally subjected to thorough drying in an oven at 60°C for 12 h to yield rod like ZnO powder sample [31]. The rod-like ZnO was characterized by scanning electron microscopy (SEM, FEI, Netherlands), transmission electron microscopy (TEM, FEI, Netherlands), and X-ray diffraction (XRD, Phillips, Netherlands), and its crystal structure was determined using Image J software.

2.1.2 S. mutans culture and preparation of bacterial solution

S. mutans UA159 was inoculated into Brain Heart Infusion (BHI, BD Bacto, America) medium (14.8 g BHI medium was added to 400 mL distilled water (ddH2O)) and cultured overnight at 37°C under 5% CO2 culture conditions. The S. mutans UA159 cells were then inoculated onto BHI-A (BHI solid medium, 14.8 g BHI and 7 g agar powder were added to 400 mL of ddH2O). The plates were incubated for 48 h under the same conditions. A single colony of S. mutans UA159 was picked from the BHI-A and cultured in 10 mL of BHI medium. The cultures were incubated overnight at 37°C, 5% CO2. To obtain a logarithmic growth-phase bacterial suspension, the medium was diluted at a ratio of 1:10 and incubated in BHI medium for 2 h. The optical density (OD) value at 600 nm was adjusted to 0.5, corresponding to approximately 1 × 108 CFU/mL. The bacterial suspension obtained was then used for subsequent experiments.

2.1.3 Minimum inhibitory concentration (MIC) detection

The rod-like ZnO were ultraviolet-disinfected for 2 h (Kengewang Sanyang Electrical Equipment Co., Ltd, China) and the ZnO solution was diluted with sterile deionized water by ultrasonic dispersion for 30 min. 20 mL of gradient concentrations of rod-like ZnO suspensions were prepared and mixed with 20 mL of double concentration of BHI-A medium (29.6 g BHI and 7 g agar powder were added to 400 mL of ddH2O) in each dish. Control group was prepared using the same method but without adding rod-like ZnO. The S. mutans bacterial suspension from Section 2.1.2 was diluted ten times. Then, 100 μL of the suspension was spread onto each dish. The dishes were incubated in the dark at 37°C, 5% CO2 for 48 h. The minimum ZnO concentration without S. mutans growth in the dish was observed as the MIC of rod-like ZnO. The experiments were repeated three times independently.

2.1.4 The 6 h antibacterial rate

The rod-like ZnO was ultraviolet-disinfected for 2 h (Kengewang Sanyang Electrical Equipment Co., Ltd, China). BHI medium containing rod-like ZnO was prepared. The concentrations were adjusted to MIC, 3/4 MIC, 1/2 MIC, and 1/4 MIC. The control group was sterile BHI. 20 μL of prepared S. mutans bacterial suspension was added to each well, and the cell culture plate was incubated at 37°C, 5% CO2 in the dark for 6 h. The bacterial solution in each well was then diluted using a ten-fold gradient, and 100 μL of the diluted bacterial solution was spread onto BHI-A. The plates were then cultured at 37°C, 5% CO2 in the dark for 48 h. The colony forming units (CFU) on the plates were counted. The experiments were repeated three times independently. The antibacterial rate (%) was calculated using the equation as described before [34].

Antibacterial rate ( % ) = ( CFU control CFU ZnO ) /CFU control × 100 % ,

where CFUcontrol is the average CFU value of the control group and CFUZnO is the average CFU value of the ZnO group.

2.1.5 Effect on the growth curve of S. mutans

The growth curve assay was performed as described before [35]. Briefly, ZnO-BHI with a concentration of 1/2 MIC was prepared. The control group was sterile BHI. 500 μL of BHI were added to the wells, respectively, and then, 5 μL of prepared S. mutans bacterial suspension was added. The samples were cultured at 37°C, 5% CO2 in the dark. The OD value at a wavelength of 600 nm was measured after culturing for 2, 4, 6, 8, 10, 12, 24, and 48 h, respectively. The experiments were repeated three times independently.

2.1.6 Effect on biofilm formation

The MTT assay was used to evaluate the effect of rod-like ZnO on the biofilm formation of S. mutans. The rod-like ZnO was dispersed in BHIS medium (1% sucrose BHI medium, 14.8 g BHI and 4 g sucrose were added to 400 mL of ddH2O) at concentrations of MIC, 3/4 MIC, 1/2 MIC, and 1/4 MIC. The control group was sterile BHIS. In 96-well plates, 200 μL of ZnO-BHIS containing different concentrations of rod-like ZnO was added to the experimental group, while 200 μL of BHIS medium was added to the control group. Then, 2 μL of prepared S. mutans bacterial suspension was added. The plate was incubated in the dark at 37°C, 5% CO2 for 24 h. After incubation, the wells were washed three times with PBS buffer. After adding 200 μL of MTT (0.5 mg/mL), the plates were incubated in the dark at 37°C, 5% CO2 for 4 h. The MTT solution was then removed, and 200 μL of Dimethyl Sulfoxide (DMSO, Beijing Solebold-Technology Co, Ltd, China) was added. The OD value at a wavelength of 570 nm was measured. The experiments were repeated three times independently. The biofilm inhibition rate (%) was calculated using the equation as described below [36]:

Biofilm inhibition rate ( % ) = 1 OD ZnO /OD control × 100 % ,

where ODZnO and ODcontrol refer to the absorbance in each well with and without rod-like ZnO, respectively.

2.1.7 Effect on formed biofilms

In 96-well plates, 200 μL of BHIS and 2 μL of S. mutans bacterial suspension was added. The plates were incubated for 24 h at 37°C, 5% CO2 in the dark. After incubation, the medium in the 96-well plates was removed. Subsequently, 200 μL of ZnO-BHIS containing different concentrations (MIC, 3/4 MIC, 1/2 MIC, and 1/4 MIC) of rod-like ZnO was added to the experimental group, while 200 μL of BHIS was added to the control group. These plates were incubated for 1 h in the dark. The experiments were repeated three times independently. The inhibition rate of formed biofilm in each group was calculated using the same method as described in Section 2.1.6.

2.2 Properties of rod-like ZnO modified DRC

2.2.1 Preparation of rod-like ZnO modified DRC

Resin monomer bisphenol A glycidyl dimethacrylate (Bis-GMA, Sigma-Aldrich, USA) and diluent triethylene glycol dimethacrylate (TEGDMA, Sigma-Aldrich, USA) were weighed according to a mass ratio of 49 wt%. The photoinitiator camphorquinone (CQ, Sigma-Aldrich, USA) was measured at 0.5 wt% and the co-initiator N, N-dimethylaminoethyl methacrylate (DMAEMA, Aladdin, China) was added at 0.5 wt%, which together formed the resin mixture. Different concentrations of ZnO (2.5, 5, and 7.5 wt%) were added to the mixture, and then ultrasonically dispersed for 10 min. The modified resin composites prepolymer was filled into a stainless-steel mold with a well size of 7 mm and a thickness of 2 mm. The resin disc was then prepared by fully light-curing both sides with a light-curing lamp (Woodpecker Medical Devices Co., Ltd, China, wavelength 420–480 nm, effective area 50 mm3, light intensity 1,000–1,200 mW/cm2) for 40 s. The samples were soaked in ddH2O for 24 h to remove the soluble resin monomers. Before the experiment, the samples were washed with deionized water, dried and sterilized for 2 h.

2.2.2 Physical characterization analysis

To observe the surface physical and chemical properties of the modified DRC, SEM and energy-dispersive X-ray spectroscopy (EDS, Perkin Elmer, USA) were used.

2.2.3 Effect of modified DRC on biofilm formation

The samples of each group were placed in 48-well plates (six samples per group), and the S. mutans bacterial solution was diluted to 1 × 106 CFU/mL using BHIS medium. Each group was added to 500 μL of diluted bacterial suspension and cultured at 37°C, 5% CO2 for 48 h in the dark. The sample was transferred to a new 48-well plate and washed three times with 500 μL of sterile PBS. 500 μL of MTT (0.5 mg/mL) was added and incubated at 37°C, 5% CO2 for 1 h in the dark. The MTT solution was discarded, and 500 μL of DMSO was added and shaken for 10 min. 100 μL of the solution in the 48-well plate was transferred to another 96-well plate. The OD value at the wavelength of 570 nm was measured. The experiments were repeated three times independently. The biofilm formation rate (%) was calculated using the following equation:

Biofilm formation rate ( % ) = 1 OD DRC /OD control × 100 % ,

where ODDRC and ODcontrol refer to the absorbance in each well with and without modified DRC, respectively.

2.2.4 Cytotoxicity test of modified DRC

Cytotoxicity test was performed using Human Gingival Fibroblast-1 (HGF-1 cells, ATCC CRL-2014, USA). These cells were treated with 0.25% trypsin, counted using a hemocytometer (Shanghai Jingjing Biochemical Reagent Instrument Co., Ltd, China), and adjusted to a concentration of 5 × 104 cells/mL. In the 96-well plate, the cell suspension was added and incubated at 37°C, 5% CO2 for 24 h. The sterilized DRC was immersed in sterile deionized water and incubated at 37°C, 5% CO2 for 24 h, and the leaching solution was collected. The medium in the 96-well plate was discarded, and 100 μL of DRC leaching solution of different ZnO concentrations (2.5, 5, 7.5 wt%) was added to the experimental group, while 100 μL of deionized water was added to the control group. Six wells were set up for each group, and incubated at 37°C with 5% CO2 for 24 h. Subsequently, 10 μL of MTT (5 mg/mL) solution was added to each well and incubated at 37°C, 5% CO2 for 4 h. After incubation, the solution was discarded, and 150 μL of DMSO was added to each well. The plate was then shaked for 10 min. Following this, 100 μL of the solution from the 96-well plate was transferred to a new 96-well plate, and the OD value at a wavelength of 570 nm was measured. The experiments were repeated three times independently. The relative growth rate (RGR) (%) was calculated using the equation referenced from previous research [37]:

RGR ( % ) = OD DRC /OD control × 100 % ,

where ODDRC and ODcontrol refer to the absorbance in each well with and without modified DRC, respectively.

2.2.5 Compressive strength analysis

The test samples were prepared following the international standard ISO 4049 [38]. A stainless-steel cylindrical mold with a diameter (d) of 4 mm and a height (h) of 6 mm was placed on a glass slide, and the entire material was cured from both ends for 40 s. Six samples per group were prepared and immersed in water at 37°C for 24 h in the dark. Based on the concentration, the samples were categorized into different groups. A universal testing machine (INSTRON, USA) was utilized to place the flat end of the sample between the working plates, enabling the application of progressively increasing compressive load along the longitudinal axis of the sample. The load was applied at a compression rate of 0.5 mm/min until the specimen was fractured. After the test, the maximum failure load (Fmax) in Newtons (N) was recorded, and the compressive strength (CS) was calculated. The experiments were repeated three times independently.

CS ( MPa ) = 2 F max/ d .

2.3 Statistical analysis

All experimental quantitative data were presented as mean value ± SD (x ± s). GraphPad Prism 9.0 software was used for statistical chart drawing, and SPSS 25.0 software was used for statistical analysis. The normal distribution of the data was determined by Shapiro–Wilk test. Subsequently, the differences between adjacent groups were analyzed. T-test was used for comparisons between two independent samples. One-way ANOVA analysis of variance was applied for comparisons among multiple independent samples, Bonferroni method was used for post hoc comparison of homogeneity of variance data, and Tamheini method was used for heterogeneity of variance data. All tests were performed at the 5% significance level. P < 0.05 indicated that the difference was statistically significant. In the statistical figure, different lowercase letters indicate that there are significant differences between different groups (P < 0.05), and the same lowercase letters indicate no statistical difference.

3 Results

3.1 Physical characterization of rod-like ZnO

The morphology of the synthesized ZnO was examined using SEM and TEM (Figure 1a–d), revealing a column length of approximately 2.5 μm, a column diameter of about 0.8 μm, and a lattice spacing of 0.2544 nm. The phase composition and crystal structure of the rod-like ZnO were further analyzed by XRD. As shown in (Figure 1e), distinct diffraction peaks corresponding to the {10 1 ̅ 0}, {0002}, {10 1 ̅ 1}, {11 2 ̅ 0}, and {10 1 ̅ 3} crystal planes were observed at 2θ angles of 31.8°, 34.3°, 36.5°, 57.2°, and 63.2°, respectively. The peak positions and shapes of the rod-like ZnO are consistent with the standard spectrum of hexagonal wurtzite ZnO (JCPDS No. 36-1451). No additional diffraction peaks from intermediates or reactants were detected, indicating the successful synthesis of rod-like ZnO with complete crystallization and no impurities.

Figure 1 
                  Characterization of rod-like ZnO using SEM, TEM, and XRD. (a and b) SEM images show the overall surface morphology of the rod-like ZnO crystals. (c and d) TEM images provide detailed views of the individual rods, revealing the precise columnar dimensions and lattice structure. (e) The XRD spectra demonstrates the phase composition and crystallographic planes of the rod-like ZnO. The peak positions correlate with the standard JCPDS No. 36-1451. The scales: 10 μm, 1 μm, 500 nm, 10 nm. SEM: Scanning electron microscope, TEM: Transmission electron microscopy, XRD: X-ray diffractometer.
Figure 1

Characterization of rod-like ZnO using SEM, TEM, and XRD. (a and b) SEM images show the overall surface morphology of the rod-like ZnO crystals. (c and d) TEM images provide detailed views of the individual rods, revealing the precise columnar dimensions and lattice structure. (e) The XRD spectra demonstrates the phase composition and crystallographic planes of the rod-like ZnO. The peak positions correlate with the standard JCPDS No. 36-1451. The scales: 10 μm, 1 μm, 500 nm, 10 nm. SEM: Scanning electron microscope, TEM: Transmission electron microscopy, XRD: X-ray diffractometer.

3.2 Antibacterial effect of rod-like ZnO

The MIC of rod-like ZnO against S. mutans was detected by solid agar dilution method, and the minimum concentration of non-growing colonies was used as the MIC of the ZnO. The MIC of rod-like ZnO was 3.0 mg/mL. To further evaluate the effect of rod-like ZnO on S. mutans, we employed the CFU counting method to determine the antibacterial rate of S. mutans exposed to different concentrations of rod-like ZnO, namely, MIC, 3/4 MIC, 1/2 MIC, and 1/4 MIC, for a duration of 6 h. The data presented in Figure 2a and Table S1 indicate that as the concentration of ZnO increased, its inhibitory effect on S. mutans also increased. At MIC, rod-like ZnO exhibited excellent antibacterial activity and was able to inhibit more than 80% of S. mutans. Moreover, the growth of S. mutans was significantly inhibited at 3/4 MIC, 1/2 MIC, and 1/4 MIC. In Figure 2b and Table S2), we observed the growth curve of S. mutans in both the control group and rod-like ZnO group. In rod-like ZnO group, the presence of ZnO exhibited a bacteriostatic effect and inhibited the growth of S. mutans. From 4 to 10 h, we observed a significant increase in bacterial growth in the control group. In contrast, the growth of bacteria in ZnO group was significantly inhibited. The growth trend was slower, and the OD600 value showed only a slight increase. Between 8 to 12 h, S. mutans entered the logarithmic growth phase. During this phase, the bacterial growth of ZnO group slightly accelerated. After 12 h, the bacterial growth in ZnO group came to a halt, and the OD600 value gradually decreased. This indicates that the rod-like ZnO effectively arrested the growth of S. mutans.

Figure 2 
                  Antibacterial effects of rod-like ZnO. (a) The antibacterial rate of rod-like ZnO on S. mutans after 6 h of treatment at MIC and sub-MIC concentrations. Rod-like ZnO exhibited a significant antibacterial effect. (b) The growth curve of S. mutans was significantly inhibited at 1/2MIC concentration. (c) Biofilm formation was significantly inhibited at MIC and sub-MIC concentrations. (d) The formed biofilm was destroyed by rod-like ZnO. MIC represents the concentration adjusted according to the MIC value of rod-like ZnO.
Figure 2

Antibacterial effects of rod-like ZnO. (a) The antibacterial rate of rod-like ZnO on S. mutans after 6 h of treatment at MIC and sub-MIC concentrations. Rod-like ZnO exhibited a significant antibacterial effect. (b) The growth curve of S. mutans was significantly inhibited at 1/2MIC concentration. (c) Biofilm formation was significantly inhibited at MIC and sub-MIC concentrations. (d) The formed biofilm was destroyed by rod-like ZnO. MIC represents the concentration adjusted according to the MIC value of rod-like ZnO.

To assess the impact of rod-like ZnO on biofilm formation, we conducted an MTT assay to measure the survival of bacteria within S. mutans biofilms. In Figure 2c and Table S3), we observed that rod-like ZnO significantly inhibited biofilm formation at both MIC and sub-MIC concentrations. The inhibition rate of biofilm formation was more than 30% compared to the blank control. Furthermore, as the concentration of ZnO increased, its inhibitory effect on biofilm metabolic activity gradually intensified. At the MIC concentration, the inhibition rate of biofilm formation reached approximately 70%. In addition, we employed the MTT assay to evaluate the impact of different MIC concentrations of rod-like ZnO on the survival of bacteria within the formed S. mutans biofilms. The results are shown in Figure 2d and Table S4), indicating that rod-like ZnO significantly disrupted S. mutans biofilm at both MIC and sub-MIC concentrations. At 1/4 MIC concentration, the inhibition rate of biofilm formation was approximately 30%. As the concentration of ZnO increased, the inhibition rate reached about 80% at the MIC concentration.

3.3 Physical characterization of modified DRC

To examine the modified DRC, we used SEM to observe randomly selected samples from different ZnO concentration groups. Representative images were chosen to present the results. Specifically, we observed the surface of the rod-like ZnO modified DRC under the SEM, as depicted in Figure 3a–c and Figure S1). No apparent agglomeration was observed, indicating a uniform distribution of the ZnO particles within the modified DRC material. To further characterize the presence of Zn on the surface of the modified material, we employed EDS to obtain the elemental composition. The EDS spectrum of the modified DRC is presented in (Figure 3d–f). It clearly demonstrates that the Zn element is evenly distributed on the surface of the DRC. This reinforces the notion that the rod-like ZnO particles are uniformly dispersed throughout the modified DRC.

Figure 3 
                  Physical characterization of modified DRCs using SEM and EDS. (a–c) SEM images depict the surface morphology of the 5 wt% ZnO modified DRC, showcasing a uniform distribution of rod-like ZnO particles within the material. (d–f) EDS spectra reveal the elemental composition of Zn on the surface of the modified DRCs. The spectra represent 2.5 wt% (d), 5 wt% (e), and 7.5 wt% (f) ZnO modified DRC. The scales: 50, 10, and 3 μm.
Figure 3

Physical characterization of modified DRCs using SEM and EDS. (a–c) SEM images depict the surface morphology of the 5 wt% ZnO modified DRC, showcasing a uniform distribution of rod-like ZnO particles within the material. (d–f) EDS spectra reveal the elemental composition of Zn on the surface of the modified DRCs. The spectra represent 2.5 wt% (d), 5 wt% (e), and 7.5 wt% (f) ZnO modified DRC. The scales: 50, 10, and 3 μm.

3.4 Effect of modified DRC on biofilm formation

From Figure 4a and b, Tables S5 and S6), it is evident that the modified DRC with different ZnO concentrations have an inhibitory effect on S. mutans biofilm. Figure 4a and Table S5 show that 2.5 and 5 wt% ZnO modified DRC could significantly inhibit biofilm activity. Figure 4b and Table S6) show that the concentrations of 2.5, 5, 7.5 wt% ZnO had an inhibitory effect on S. mutans biofilm. Notably, the most significant biofilm inhibition effect is observed with the 5 wt% ZnO modified DRC, achieving approximately 40% inhibition.

Figure 4 
                  Antibacterial effect, cytotoxicity and compressive strength of modified DRC. (a) The modified DRC with different ZnO concentrations has an inhibitory effect on S. mutans biofilm. (b) The concentrations of 2.5, 5, and 7.5 wt% ZnO had a significant inhibitory effect on S. mutans biofilm. (c) The relative growth rate of HGF-1 cells treated with ZnO modified DRC indicates the absence of cytotoxic effects. (d) The compressive strength of modified DRC increases with the increase in the ZnO concentration, especially with 5 wt% ZnO showing the best anti-compression effect.
Figure 4

Antibacterial effect, cytotoxicity and compressive strength of modified DRC. (a) The modified DRC with different ZnO concentrations has an inhibitory effect on S. mutans biofilm. (b) The concentrations of 2.5, 5, and 7.5 wt% ZnO had a significant inhibitory effect on S. mutans biofilm. (c) The relative growth rate of HGF-1 cells treated with ZnO modified DRC indicates the absence of cytotoxic effects. (d) The compressive strength of modified DRC increases with the increase in the ZnO concentration, especially with 5 wt% ZnO showing the best anti-compression effect.

3.5 Cytotoxicity test of modified DRC

The MTT assay was employed to assess the cytotoxicity of rod-like ZnO modified DRC after direct contact with HGF-1 cells for 24 h. As shown in Figure 4c and Table S7, the RGR of HGF-1 cells treated with 2.5, 5, 7.5 wt% ZnO modified DRC was greater than 75%, indicating no cytotoxic effects. In comparison to the control group, no significant differences were observed between the three concentrations of the modified DRC. However, as the concentration increased, the relative growth rate of cells treated with 7.5 wt% ZnO decreased to approximately 90% with no statistical difference. These results indicate that the ZnO modified DRC exhibit good biocompatibility with HGF-1 cells, as evidenced by the high relative growth rates and lack of cytotoxic effects. This suggests their potential applicability in dental and medical fields where biocompatible materials are crucial.

3.6 Compression strength of modified DRC

Figure 4d and Table S8 show that the compressive strength of the modified DRC with 2.5 and 5 wt% ZnO concentration increased with the increase in concentration, especially the 5 wt% ZnO had the best anti-compression effect.

4 Discussion

Inorganic antibacterial materials such as ZnO can effectively exhibit antibacterial properties in the form of micro-nano particles. Micro-nano ZnO materials offer significant potential for diverse applications owing to their cost-effectiveness, abundance of resources, and environmental friendliness. Although the precise mechanism underlying the antibacterial effect of ZnO remains to be fully elucidated, the current understanding suggests that it primarily operates via the following mechanisms: (1) Oxygen vacancies on the surface of light or crystals catalyze the reduction of oxygen molecules to water. Incompletely reduced oxygen leads to the formation of superoxide anion radicals, which enhance the production of ROS [39,40,41] and induce oxidative stress and DNA damage, rendering cells unable to maintain normal physiological redox regulation, leading to cell death and genotoxic effects [26,27]. (2) Zn2+ released in an aqueous solution can bind to the fat and proteins of bacteria, change the osmotic balance of the cell membrane, reduce the permeability of the cell membrane, and penetrate the bacterial cell membrane. Disruption of the zinc-dependent enzyme system, amino acid metabolism, changes in protein structure, and destruction of the electron transport system lead to the destruction of intracellular homeostasis, damage to lysosomes and mitochondria, and induction of cell death [14,28,29]. (3) The slowly released Zn2+ into the aqueous medium binds to the surface of negatively charged bacteria owing to the mutual attraction between heterogeneous charges. It reacts with some groups or anions on the cell membrane proteins, causing the cell membrane to lose its original biological function and structure and causing membrane damage through direct contact [30]. In this study, rod-like ZnO structures were synthesized using an atmospheric pressure hydrothermal system. The reaction conditions were adjusted to promote electrostatic adsorption between different ions and the ZnO nuclei in the solution [31]. SEM and TEM morphology characterization analyses (Figure 1a–d) revealed that the length of these rod-like ZnO structures is approximately 2.5 μm, with a column diameter of about 0.8 μm. The lattice spacing was measured to be 0.2544 nm. The microstructures were submicron in size, with diameters ranging from 0.1 to 1 μm. The XRD pattern (Figure 1e) confirmed that rod-like ZnO crystals were well formed, exhibiting a smooth surface with no impurities. Low-dimensional ZnO can be prepared using various solid-, gas-, and liquid-phase methods [42]. Among these, the hydrothermal method stands out because it can successfully synthesize microns and nanomaterials at the three-phase contact surface of liquids, solids, and solvents. This synthesis was achieved via phase transfer and separation mechanisms [43]. The atmospheric pressure hydrothermal method offers several advantages, including a simple process, easy control, and low cost. By adjusting the reaction temperature, material ratio, and raw reaction materials, researchers can obtain ZnO crystals with multiple morphologies [44,45]. Overall, the hydrothermal method proved effective in synthesizing rod-like ZnO structures, highlighting the potential of this approach for producing ZnO materials with the desired characteristics for various applications. The ZnO crystals synthesized in this study with multiple morphologies exhibited different exposed crystal planes, which contributed to their varied antibacterial activities. The surfaces of low-dimensional ZnO crystals are characterized by an abundance of oxygen vacancies and positive charges. These features enable interactions with negatively charged bacterial cell walls, resulting in bacterial rupture and death [46]. Common low-index crystal planes of ZnO include the {000 1 ̅ }, {10 1 ̅ 0}, {0001}, {2 1 ̅ 1 ̅ 0}, {0001}, and {000 1 ̅ }, and so on. Each crystal plane provides distinct active sites for different reactions and their oxygen vacancies and oxygen absorption capacities differ. Theoretical calculations suggested that the {0001} crystal plane exhibited the highest catalytic activity, followed by the {2 1 ̅ 1 ̅ 0} crystal plane [47,48]. Previous research [31] has found that rod-like ZnO primarily exposes the {0001} and {101̅0} crystal planes. Therefore, the antibacterial properties of rod-like ZnO crystals against S. mutans, a key cariogenic bacterium of the oral cavity, were investigated in this study.

S. mutans is a primary cariogenic bacterium found in the oral cavity that primarily synthesizes extracellular polymeric substances (EPS) through a sucrose-dependent pathway, allowing it to colonize tooth surfaces [49]. The EPS composition acts as a barrier that restricts the diffusion of acidic byproducts. It not only lowers the local pH and establishes a specific microenvironment, but also enables S. mutans to adapt to acidic stress, allowing it to survive under low pH conditions [50]. The plaque biofilm formed by S. mutans possesses a dense structure, making it challenging to physically remove, preventing effective penetration of antibiotics [49]. Studies have indicated that biofilms are a resistance to antimicrobial agents that is at least 500 times stronger than that observed in planktonic bacterial cells [51]. In this study, we examined the inhibitory effects of rod-like ZnO on both S. mutans and S. mutans biofilms to explore its antibacterial activity against major oral cariogenic bacteria. Rod-like ZnO exhibited significant antibacterial properties against S. mutans at MIC and sub-MIC levels. Furthermore, the antibacterial efficacy increased with the increase in the concentrations of rod-like ZnO (Figure 2a and Table S1). Remarkably, even at a low concentration (1/4 MIC), rod-like ZnO inhibited more than 50% of S. mutans, demonstrating excellent antibacterial activity. The results of this study demonstrate that both the MIC and sub-MIC of rod-like ZnO were effective in inhibiting the adhesion of S. mutans on repair materials and preventing biofilm formation (Figure 2c and Table S3). Moreover, rod-like ZnO exhibited a significant inhibitory effect on mature biofilm formation at both MIC and sub-MIC levels (Figure 2d and Table S4). These findings suggest that rod-like ZnO has great potential for preventing secondary caries. In the growth curve experiment depicted in (Figure 2b), rod-like ZnO significantly inhibited the growth of S. mutans at 1/2 MIC. The OD value of S. mutans treated with rod-like ZnO increased notably at 10–12 h but decreased significantly after 24 h. This indicates that rod-like ZnO not only suppressed the growth of S. mutans after 12 h but also caused the death of some bacterial cells. Conversely, the control group exhibited the most vigorous growth and proliferation of S. mutans at 24 h, whereas the rod-like ZnO reached its peak inhibition after 12 h. These results suggest that rod-like ZnO shortens the growth cycle of S. mutans and significantly inhibits the growth of all bacteria. Examination of the inhibitory effect of rod-like ZnO on S. mutans at sub-MIC levels is particularly beneficial for reducing the cytotoxicity associated with high concentrations of ZnO. This finding is of positive significance for minimizing the amount of ZnO required for oral materials. The inhibitory effect of rod-like ZnO on the biofilm and viable bacteria within the biofilm might be attributed to the fact that ZnO readily precipitates and makes direct contact with the S. mutans biofilm. This contact killing mechanism likely disrupts the bacterial cell wall [52].

In this study, we prepared modified DRC with varying concentrations of rod-like ZnO. Their antibacterial properties as well as physical and chemical characteristics were assessed. The SEM images (Figure 3a–c) and EDS results (Figure 3d–f) revealed that Zn was evenly distributed in the modified DRC samples with 2.5, 5, and 7.5 wt% ZnO. The ZnO on the surface of the modified DRC appeared to be evenly distributed without apparent agglomeration. The antibacterial properties of the modified DRC were evaluated as shown in (Figure 4a and b). The modified DRC with 5 wt% ZnO exhibited the most effective inhibition of biofilm formation, whereas the inhibitory effect decreased for the modified DRC with 7.5 wt% ZnO. One explanation for this observation is that an increase in the amount of ZnO increased the surface roughness of the modified DRC. Consequently, cariogenic bacteria may be more likely to attach to rough surfaces, resulting in a decrease in the inhibition rate. Bacterial adhesion is a crucial factor in the formation of dental plaque biofilms, and surface roughness is known to influence the nonspecific adhesion of oral microorganisms [53]. Hong and He [54] found that excessive levels of nano-ZnO can cause aggregation, leading to an increase in the surface roughness of the film and a decrease in its antibacterial properties. Consistent with these findings, our study demonstrated a decrease in the antibacterial properties of the resin as the ZnO concentration increased. Overall, it can be concluded that although the addition of ZnO can enhance the antibacterial properties of resin materials, an optimal concentration of ZnO is required to maintain the desired effect. Higher concentrations may lead to an increased surface roughness and decreased antibacterial efficacy.

Biomaterials must exhibit excellent biocompatibility to ensure safety in clinical applications. In this study, the MTT assay was employed to assess the cytotoxicity of the rod-like ZnO modified DRC upon direct contact with HGF-1 cells for 24 h. According to the cell viability classification outlined in the United States Pharmacopoeia, a cytotoxicity rating of grade 0 or 1 is considered qualified when the RGR is ≥75% [55]. The results depicted in Figure 4c and Table S3 indicate that the modified DRC with 2.5, 5, and 7.5 wt% ZnO exhibited no cytotoxicity, signifying their excellent biological safety. However, it should be noted that the modified DRC, even with different concentrations of ZnO, displayed a certain degree of inhibition of the growth of HGF-1 cells. A previous study by Pengyu et al. [56] suggested that the growth inhibition observed in HGF-1 cells owing to nano-ZnO may be attributed to various factors, including the release of Zn2+ ions, generation of ROS, and DNA damage. Małkiewicz et al. [57] emphasized that incompletely polymerized resin composites may release considerable amounts of residual monomers into the oral environment. Among these monomers, TEGDMA has been reported to have cytotoxic effects and to inhibit cellular growth.

In addition to their effective antibacterial activity, clinical filling materials should possess sufficient mechanical properties to withstand the pressure exerted on the occlusal surface. Based on the compression strength test results presented in Figure 4d and Table S4, different concentrations of ZnO increased the compression strength of the modified DRC, with the 5 wt% ZnO concentration exhibiting the best results. Regarding the relatively decreased compressive strength observed with 7.5 wt% ZnO (with no statistical difference), it is speculated that the increase in compressive strength at low ZnO content is due to its relatively good dispersion. However, at higher ZnO mass fractions, bundles and agglomerates may form, resulting in defects and consequently degrading the mechanical properties of the composites [58]. One of the main antibacterial mechanisms of ZnO is the photocatalytic production of ROS [29]. However, because the oral environment lacks light, this mechanism cannot be employed for antibacterial action. Therefore, to simulate the dark environment of the oral cavity, this experiment was conducted under light-free conditions to explore the antibacterial ability of rod-like ZnO in the absence of light. Studies have demonstrated that ROS generated by nano-ZnO under dark conditions is the primary reason for its antibacterial activity. The increased production of ROS by ZnO induces oxidative stress in bacterial cells, ultimately leading to bacterial death [59]. Zhou et al. [40] also confirmed that ZnO can produce H2O2 in the absence of light, owing to the presence of oxygen vacancies on the crystal surface. Therefore, further experimental research is required to elucidate the specific antibacterial mechanisms of rod-like ZnO modified DRC. Overall, the addition of ZnO not only enhanced the antibacterial properties, but also improved the mechanical strength of the modified DRC. Antibacterial activity in dark environments is primarily attributed to the generation of ROS, which exert oxidative stress on bacterial cells. However, additional studies are required to fully understand the precise antibacterial mechanisms of the rod-like ZnO modified DRC.

5 Conclusion

Rod-like ZnO has a significant inhibitory effect on the growth, adhesion, and aggregation of S. mutans, which is the main cariogenic bacterium in the oral cavity. The modified DRC prepared using hexagonal prism ZnO exhibited good antibacterial effects, biofilm inhibition, biosafety, and mechanical strength. This finding provides a basis for the prevention of secondary caries in the oral cavity. As the oral cavity is a complex microecological environment composed of a variety of microorganisms, it is necessary to further study the antibacterial mechanism of rod-like ZnO and conduct more in vivo experiments to evaluate its biosafety in clinical treatment.


# These authors contributed equally to this work and should be considered first co-authors.


Acknowledgments

The authors are grateful for the reviewer’s valuable comments that improved the manuscript.

  1. Funding information: This work was supported by the Sichuan Provincial Natural Science Foundation (Project No.: 2023NSFSC1998).

  2. Author contributions: Zhou Shiyu is responsible for the preparation and physical characterization of rod-like ZnO. Liu Ruihua is responsible for experimental data processing and article writing. Shiyu Zhou and Ruihua Liu contributed equally. Xinru Ma is responsible for the bacterial experiment. Yushi Xie is responsible for assisting with material preparation. Xiaoling Xu is responsible for reviewing and editing. Du Qin is responsible for experimental design and management. Zuowan Zhou is responsible for experimental design and management. All authors have accepted responsibility for the entire content of this manuscript and approved its submission.

  3. Conflict of interest: The authors state no conflict of interest.

  4. Ethical approval: The conducted research is not related to either human or animals use.

  5. Data availability statement: The datasets generated during and/or analyzed during the current study are available from the corresponding author on reasonable request.

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Received: 2023-07-10
Revised: 2023-12-22
Accepted: 2023-12-31
Published Online: 2024-03-12

© 2024 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  21. Cementitious composites modified by nanocarbon fillers with cooperation effect possessing excellent self-sensing properties
  22. Confinement size effect on dielectric properties, antimicrobial activity, and recycling of TiO2 quantum dots via photodegradation processes of Congo red dye and real industrial textile wastewater
  23. Biogenic silver nanoparticles of Moringa oleifera leaf extract: Characterization and photocatalytic application
  24. Novel integrated structure and function of Mg–Gd neutron shielding materials
  25. Impact of multiple slips on thermally radiative peristaltic transport of Sisko nanofluid with double diffusion convection, viscous dissipation, and induced magnetic field
  26. Magnetized water-based hybrid nanofluid flow over an exponentially stretching sheet with thermal convective and mass flux conditions: HAM solution
  27. A numerical investigation of the two-dimensional magnetohydrodynamic water-based hybrid nanofluid flow composed of Fe3O4 and Au nanoparticles over a heated surface
  28. Development and modeling of an ultra-robust TPU-MWCNT foam with high flexibility and compressibility
  29. Effects of nanofillers on the physical, mechanical, and tribological behavior of carbon/kenaf fiber–reinforced phenolic composites
  30. Polymer nanocomposite for protecting photovoltaic cells from solar ultraviolet in space
  31. Study on the mechanical properties and microstructure of recycled concrete reinforced with basalt fibers and nano-silica in early low-temperature environments
  32. Synergistic effect of carbon nanotubes and polyvinyl alcohol on the mechanical performance and microstructure of cement mortar
  33. CFD analysis of paraffin-based hybrid (Co–Au) and trihybrid (Co–Au–ZrO2) nanofluid flow through a porous medium
  34. Forced convective tangent hyperbolic nanofluid flow subject to heat source/sink and Lorentz force over a permeable wedge: Numerical exploration
  35. Physiochemical and electrical activities of nano copper oxides synthesised via hydrothermal method utilising natural reduction agents for solar cell application
  36. A homotopic analysis of the blood-based bioconvection Carreau–Yasuda hybrid nanofluid flow over a stretching sheet with convective conditions
  37. In situ synthesis of reduced graphene oxide/SnIn4S8 nanocomposites with enhanced photocatalytic performance for pollutant degradation
  38. A coarse-grained Poisson–Nernst–Planck model for polyelectrolyte-modified nanofluidic diodes
  39. A numerical investigation of the magnetized water-based hybrid nanofluid flow over an extending sheet with a convective condition: Active and passive controls of nanoparticles
  40. The LyP-1 cyclic peptide modified mesoporous polydopamine nanospheres for targeted delivery of triptolide regulate the macrophage repolarization in atherosclerosis
  41. Synergistic effect of hydroxyapatite-magnetite nanocomposites in magnetic hyperthermia for bone cancer treatment
  42. The significance of quadratic thermal radiative scrutinization of a nanofluid flow across a microchannel with thermophoretic particle deposition effects
  43. Ferromagnetic effect on Casson nanofluid flow and transport phenomena across a bi-directional Riga sensor device: Darcy–Forchheimer model
  44. Performance of carbon nanomaterials incorporated with concrete exposed to high temperature
  45. Multicriteria-based optimization of roller compacted concrete pavement containing crumb rubber and nano-silica
  46. Revisiting hydrotalcite synthesis: Efficient combined mechanochemical/coprecipitation synthesis to design advanced tunable basic catalysts
  47. Exploration of irreversibility process and thermal energy of a tetra hybrid radiative binary nanofluid focusing on solar implementations
  48. Effect of graphene oxide on the properties of ternary limestone clay cement paste
  49. Improved mechanical properties of graphene-modified basalt fibre–epoxy composites
  50. Sodium titanate nanostructured modified by green synthesis of iron oxide for highly efficient photodegradation of dye contaminants
  51. Green synthesis of Vitis vinifera extract-appended magnesium oxide NPs for biomedical applications
  52. Differential study on the thermal–physical properties of metal and its oxide nanoparticle-formed nanofluids: Molecular dynamics simulation investigation of argon-based nanofluids
  53. Heat convection and irreversibility of magneto-micropolar hybrid nanofluids within a porous hexagonal-shaped enclosure having heated obstacle
  54. Numerical simulation and optimization of biological nanocomposite system for enhanced oil recovery
  55. Laser ablation and chemical vapor deposition to prepare a nanostructured PPy layer on the Ti surface
  56. Cilostazol niosomes-loaded transdermal gels: An in vitro and in vivo anti-aggregant and skin permeation activity investigations towards preparing an efficient nanoscale formulation
  57. Linear and nonlinear optical studies on successfully mixed vanadium oxide and zinc oxide nanoparticles synthesized by sol–gel technique
  58. Analytical investigation of convective phenomena with nonlinearity characteristics in nanostratified liquid film above an inclined extended sheet
  59. Optimization method for low-velocity impact identification in nanocomposite using genetic algorithm
  60. Analyzing the 3D-MHD flow of a sodium alginate-based nanofluid flow containing alumina nanoparticles over a bi-directional extending sheet using variable porous medium and slip conditions
  61. A comprehensive study of laser irradiated hydrothermally synthesized 2D layered heterostructure V2O5(1−x)MoS2(x) (X = 1–5%) nanocomposites for photocatalytic application
  62. Computational analysis of water-based silver, copper, and alumina hybrid nanoparticles over a stretchable sheet embedded in a porous medium with thermophoretic particle deposition effects
  63. A deep dive into AI integration and advanced nanobiosensor technologies for enhanced bacterial infection monitoring
  64. Effects of normal strain on pyramidal I and II 〈c + a〉 screw dislocation mobility and structure in single-crystal magnesium
  65. Computational study of cross-flow in entropy-optimized nanofluids
  66. Significance of nanoparticle aggregation for thermal transport over magnetized sensor surface
  67. A green and facile synthesis route of nanosize cupric oxide at room temperature
  68. Effect of annealing time on bending performance and microstructure of C19400 alloy strip
  69. Chitosan-based Mupirocin and Alkanna tinctoria extract nanoparticles for the management of burn wound: In vitro and in vivo characterization
  70. Electrospinning of MNZ/PLGA/SF nanofibers for periodontitis
  71. Photocatalytic degradation of methylene blue by Nd-doped titanium dioxide thin films
  72. Shell-core-structured electrospinning film with sequential anti-inflammatory and pro-neurogenic effects for peripheral nerve repairment
  73. Flow and heat transfer insights into a chemically reactive micropolar Williamson ternary hybrid nanofluid with cross-diffusion theory
  74. One-pot fabrication of open-spherical shapes based on the decoration of copper sulfide/poly-O-amino benzenethiol on copper oxide as a promising photocathode for hydrogen generation from the natural source of Red Sea water
  75. A penta-hybrid approach for modeling the nanofluid flow in a spatially dependent magnetic field
  76. Advancing sustainable agriculture: Metal-doped urea–hydroxyapatite hybrid nanofertilizer for agro-industry
  77. Utilizing Ziziphus spina-christi for eco-friendly synthesis of silver nanoparticles: Antimicrobial activity and promising application in wound healing
  78. Plant-mediated synthesis, characterization, and evaluation of a copper oxide/silicon dioxide nanocomposite by an antimicrobial study
  79. Effects of PVA fibers and nano-SiO2 on rheological properties of geopolymer mortar
  80. Investigating silver and alumina nanoparticles’ impact on fluid behavior over porous stretching surface
  81. Potential pharmaceutical applications and molecular docking study for green fabricated ZnO nanoparticles mediated Raphanus sativus: In vitro and in vivo study
  82. Effect of temperature and nanoparticle size on the interfacial layer thickness of TiO2–water nanofluids using molecular dynamics
  83. Characteristics of induced magnetic field on the time-dependent MHD nanofluid flow through parallel plates
  84. Flexural and vibration behaviours of novel covered CFRP composite joints with an MWCNT-modified adhesive
  85. Experimental research on mechanically and thermally activation of nano-kaolin to improve the properties of ultra-high-performance fiber-reinforced concrete
  86. Analysis of variable fluid properties for three-dimensional flow of ternary hybrid nanofluid on a stretching sheet with MHD effects
  87. Biodegradability of corn starch films containing nanocellulose fiber and thymol
  88. Toxicity assessment of copper oxide nanoparticles: In vivo study
  89. Some measures to enhance the energy output performances of triboelectric nanogenerators
  90. Reinforcement of graphene nanoplatelets on water uptake and thermomechanical behaviour of epoxy adhesive subjected to water ageing conditions
  91. Optimization of preparation parameters and testing verification of carbon nanotube suspensions used in concrete
  92. Max-phase Ti3SiC2 and diverse nanoparticle reinforcements for enhancement of the mechanical, dynamic, and microstructural properties of AA5083 aluminum alloy via FSP
  93. Advancing drug delivery: Neural network perspectives on nanoparticle-mediated treatments for cancerous tissues
  94. PEG-PLGA core–shell nanoparticles for the controlled delivery of picoplatin–hydroxypropyl β-cyclodextrin inclusion complex in triple-negative breast cancer: In vitro and in vivo study
  95. Conduction transportation from graphene to an insulative polymer medium: A novel approach for the conductivity of nanocomposites
  96. Review Articles
  97. Developments of terahertz metasurface biosensors: A literature review
  98. Overview of amorphous carbon memristor device, modeling, and applications for neuromorphic computing
  99. Advances in the synthesis of gold nanoclusters (AuNCs) of proteins extracted from nature
  100. A review of ternary polymer nanocomposites containing clay and calcium carbonate and their biomedical applications
  101. Recent advancements in polyoxometalate-functionalized fiber materials: A review
  102. Special contribution of atomic force microscopy in cell death research
  103. A comprehensive review of oral chitosan drug delivery systems: Applications for oral insulin delivery
  104. Cellular senescence and nanoparticle-based therapies: Current developments and perspectives
  105. Cyclodextrins-block copolymer drug delivery systems: From design and development to preclinical studies
  106. Micelle-based nanoparticles with stimuli-responsive properties for drug delivery
  107. Critical assessment of the thermal stability and degradation of chemically functionalized nanocellulose-based polymer nanocomposites
  108. Research progress in preparation technology of micro and nano titanium alloy powder
  109. Nanoformulations for lysozyme-based additives in animal feed: An alternative to fight antibiotic resistance spread
  110. Incorporation of organic photochromic molecules in mesoporous silica materials: Synthesis and applications
  111. A review on modeling of graphene and associated nanostructures reinforced concrete
  112. A review on strengthening mechanisms of carbon quantum dots-reinforced Cu-matrix nanocomposites
  113. Review on nanocellulose composites and CNFs assembled microfiber toward automotive applications
  114. Nanomaterial coating for layered lithium rich transition metal oxide cathode for lithium-ion battery
  115. Application of AgNPs in biomedicine: An overview and current trends
  116. Nanobiotechnology and microbial influence on cold adaptation in plants
  117. Hepatotoxicity of nanomaterials: From mechanism to therapeutic strategy
  118. Applications of micro-nanobubble and its influence on concrete properties: An in-depth review
  119. A comprehensive systematic literature review of ML in nanotechnology for sustainable development
  120. Exploiting the nanotechnological approaches for traditional Chinese medicine in childhood rhinitis: A review of future perspectives
  121. Twisto-photonics in two-dimensional materials: A comprehensive review
  122. Current advances of anticancer drugs based on solubilization technology
  123. Recent process of using nanoparticles in the T cell-based immunometabolic therapy
  124. Future prospects of gold nanoclusters in hydrogen storage systems and sustainable environmental treatment applications
  125. Preparation, types, and applications of one- and two-dimensional nanochannels and their transport properties for water and ions
  126. Microstructural, mechanical, and corrosion characteristics of Mg–Gd–x systems: A review of recent advancements
  127. Functionalized nanostructures and targeted delivery systems with a focus on plant-derived natural agents for COVID-19 therapy: A review and outlook
  128. Mapping evolution and trends of cell membrane-coated nanoparticles: A bibliometric analysis and scoping review
  129. Nanoparticles and their application in the diagnosis of hepatocellular carcinoma
  130. In situ growth of carbon nanotubes on fly ash substrates
  131. Structural performance of boards through nanoparticle reinforcement: An advance review
  132. Reinforcing mechanisms review of the graphene oxide on cement composites
  133. Seed regeneration aided by nanomaterials in a climate change scenario: A comprehensive review
  134. Surface-engineered quantum dot nanocomposites for neurodegenerative disorder remediation and avenue for neuroimaging
  135. Graphitic carbon nitride hybrid thin films for energy conversion: A mini-review on defect activation with different materials
  136. Nanoparticles and the treatment of hepatocellular carcinoma
  137. Special Issue on Advanced Nanomaterials and Composites for Energy Conversion and Storage - Part II
  138. Highly safe lithium vanadium oxide anode for fast-charging dendrite-free lithium-ion batteries
  139. Recent progress in nanomaterials of battery energy storage: A patent landscape analysis, technology updates, and future prospects
  140. Special Issue on Advanced Nanomaterials for Carbon Capture, Environment and Utilization for Energy Sustainability - Part II
  141. Calcium-, magnesium-, and yttrium-doped lithium nickel phosphate nanomaterials as high-performance catalysts for electrochemical water oxidation reaction
  142. Low alkaline vegetation concrete with silica fume and nano-fly ash composites to improve the planting properties and soil ecology
  143. Mesoporous silica-grafted deep eutectic solvent-based mixed matrix membranes for wastewater treatment: Synthesis and emerging pollutant removal performance
  144. Electrochemically prepared ultrathin two-dimensional graphitic nanosheets as cathodes for advanced Zn-based energy storage devices
  145. Enhanced catalytic degradation of amoxicillin by phyto-mediated synthesised ZnO NPs and ZnO-rGO hybrid nanocomposite: Assessment of antioxidant activity, adsorption, and thermodynamic analysis
  146. Incorporating GO in PI matrix to advance nanocomposite coating: An enhancing strategy to prevent corrosion
  147. Synthesis, characterization, thermal stability, and application of microporous hyper cross-linked polyphosphazenes with naphthylamine group for CO2 uptake
  148. Engineering in ceramic albite morphology by the addition of additives: Carbon nanotubes and graphene oxide for energy applications
  149. Nanoscale synergy: Optimizing energy storage with SnO2 quantum dots on ZnO hexagonal prisms for advanced supercapacitors
  150. Aging assessment of silicone rubber materials under corona discharge accompanied by humidity and UV radiation
  151. Tuning structural and electrical properties of Co-precipitated and Cu-incorporated nickel ferrite for energy applications
  152. Sodium alginate-supported AgSr nanoparticles for catalytic degradation of malachite green and methyl orange in aqueous medium
  153. An environmentally greener and reusability approach for bioenergy production using Mallotus philippensis (Kamala) seed oil feedstock via phytonanotechnology
  154. Micro-/nano-alumina trihydrate and -magnesium hydroxide fillers in RTV-SR composites under electrical and environmental stresses
  155. Mechanism exploration of ion-implanted epoxy on surface trap distribution: An approach to augment the vacuum flashover voltages
  156. Nanoscale engineering of semiconductor photocatalysts boosting charge separation for solar-driven H2 production: Recent advances and future perspective
  157. Excellent catalytic performance over reduced graphene-boosted novel nanoparticles for oxidative desulfurization of fuel oil
  158. Special Issue on Advances in Nanotechnology for Agriculture
  159. Deciphering the synergistic potential of mycogenic zinc oxide nanoparticles and bio-slurry formulation on phenology and physiology of Vigna radiata
  160. Nanomaterials: Cross-disciplinary applications in ornamental plants
  161. Special Issue on Catechol Based Nano and Microstructures
  162. Polydopamine films: Versatile but interface-dependent coatings
  163. In vitro anticancer activity of melanin-like nanoparticles for multimodal therapy of glioblastoma
  164. Poly-3,4-dihydroxybenzylidenhydrazine, a different analogue of polydopamine
  165. Chirality and self-assembly of structures derived from optically active 1,2-diaminocyclohexane and catecholamines
  166. Advancing resource sustainability with green photothermal materials: Insights from organic waste-derived and bioderived sources
  167. Bioinspired neuromelanin-like Pt(iv) polymeric nanoparticles for cancer treatment
  168. Special Issue on Implementing Nanotechnology for Smart Healthcare System
  169. Intelligent explainable optical sensing on Internet of nanorobots for disease detection
  170. Special Issue on Green Mono, Bi and Tri Metallic Nanoparticles for Biological and Environmental Applications
  171. Tracking success of interaction of green-synthesized Carbopol nanoemulgel (neomycin-decorated Ag/ZnO nanocomposite) with wound-based MDR bacteria
  172. Green synthesis of copper oxide nanoparticles using genus Inula and evaluation of biological therapeutics and environmental applications
  173. Biogenic fabrication and multifunctional therapeutic applications of silver nanoparticles synthesized from rose petal extract
  174. Metal oxides on the frontlines: Antimicrobial activity in plant-derived biometallic nanoparticles
  175. Controlling pore size during the synthesis of hydroxyapatite nanoparticles using CTAB by the sol–gel hydrothermal method and their biological activities
  176. Special Issue on State-of-Art Advanced Nanotechnology for Healthcare
  177. Applications of nanomedicine-integrated phototherapeutic agents in cancer theranostics: A comprehensive review of the current state of research
  178. Smart bionanomaterials for treatment and diagnosis of inflammatory bowel disease
  179. Beyond conventional therapy: Synthesis of multifunctional nanoparticles for rheumatoid arthritis therapy
Heruntergeladen am 22.9.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ntrev-2023-0195/html?lang=de
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