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Article

Dialdehyde Cellulose Solution as Reducing Agent: Preparation of Uniform Silver Nanoparticles and In Situ Synthesis of Antibacterial Composite Films with High Barrier Properties

by
**song Zeng
1,2,
**nyi **ong
1,2,
Fugang Hu
1,2,
**peng Li
1,2 and
Pengfei Li
1,2,3,*
1
Plant Fibril Material Science Research Center, State Key Laboratory of Pulp and Paper Engineering, School of Light Industry and Engineering, South China University of Technology, Guangzhou 510640, China
2
Guangdong Provincial Key Laboratory of Plant Resources Biorefinery, Guangzhou 510006, China
3
School of Environment and Energy, South China University of Technology, Guangzhou 510640, China
*
Author to whom correspondence should be addressed.
Molecules 2023, 28(7), 2956; https://doi.org/10.3390/molecules28072956
Submission received: 25 February 2023 / Revised: 17 March 2023 / Accepted: 24 March 2023 / Published: 26 March 2023
(This article belongs to the Special Issue Carbon Nanomaterials: Design and Applications)
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Abstract

:
The demand for antimicrobial materials is gradually increasing due to the threat of infections and diseases caused by microorganisms. Silver nanoparticles (AgNPs) are widely used because of their broad-spectrum antimicrobial properties, but their synthesis methods are often environmentally harmful and AgNPs difficult to isolate, which limits their application in several fields. In this study, an aqueous solution of dialdehyde cellulose (DAC) was prepared and used as a reducing agent to synthesize AgNPs in an efficient and environmentally friendly process. The synthesized AgNPs can be easily separated from the reducing agent to expand their applications. In addition, the AgNPs were immobilized in situ on dialdehyde cellulose to form antibacterial composite films. The results showed that the prepared silver nanoparticles were mainly spherical and uniformly dispersed, with an average size of about 25 nm under optimal conditions. Moreover, the dialdehyde cellulose–nanosilver (DAC@Ag) composite films had excellent mechanical properties, positive transparency, ultraviolet-blocking properties, and effective antibacterial activity against E. coli and S. aureus. Notably, the composite films exhibited excellent oxygen and water vapor barrier properties, with WVT and ORT of 136.41 g/m2·24 h (30 °C, 75% RH) and <0.02 cm3/m2·24 h·0.1 MPa (30 °C, 75% RH), respectively, better than commercial PE films. Hence, this study not only provides an environmentally friendly method for the preparation of silver nanoparticles, but also offers a simple and novel strategy for the in situ synthesis of silver-loaded antibacterial composite films.

Graphical Abstract

1. Introduction

In recent decades, with the improvement in health awareness, people have gradually recognized the hazards of illness transmission provoked by microorganisms. As a result, the usage of antimicrobial materials has risen in a variety of applications, including medical hemostatic antibacterial dressings, antimicrobial packaging materials, etc. [1,2,3]. In addition to the commonly used antibiotics, some natural or synthetic organic substances have been used as antimicrobial agents due to their excellent antimicrobial properties [4,5], such as cinnamon oil, chitosan, and quaternary ammonium salts [6,7,8]. However, the selection of appropriate antibacterial substances is still a huge challenge, due to poor heat resistance and easy-to-produce drug resistance [9]. As an antibacterial material with excellent performance, AgNPs not only exhibit broad antimicrobial activity against a wide range of pathogens such as bacteria, viruses, and fungi, but also have low cytotoxicity [10], and no microbial resistance, which has expanded their applications in medicine [11], antimicrobial packaging [12], material coatings [13], and water treatment [14]. Recently, many technologies have been developed in improving the ability to produce AgNPs as a result of great efforts devoted to thermal decomposition, UV irradiation, chemical reduction, laser etching, γ irradiation, etc. [15,16,17,18]. Among them, one of the most prevalent approaches has been the use of efficient reducing agents for chemical reduction, including borohydride, hydrazine and other substances, which have caused great damage to the environment [19]. In addition, it is hard to separate AgNPs from these added chemicals completely, limiting the applicability of generated AgNPs [20]. Therefore, it is still highly desirable to explore facile and green methods for synthesizing AgNPs with excellent antibacterial properties.
As the most abundant natural resource on Earth, cellulose has become a hot biological material with great development potential due to its biocompatibility, regeneration, biodegradability, low cytotoxicity, and environmental friendliness [21]. To date, a great deal of research has been devoted to the development of polymers containing cellulose, including nanocellulose and cellulose derivatives, and cellulose has been used in reinforcing materials, oil–water separation, food packaging, medical materials, etc. [22,23,24,25]. Antimicrobial nanoparticles combined with oxidized cellulose can reduce unwanted effects such as allergies and inflammation; moreover, the shapes and sizes of antimicrobial nanoparticles can be altered [26,27]. It has been broadly reported that a variety of oxidized celluloses can be used to prepare biocompatible products. In particular, dialdehyde cellulose, as an intriguing material, can form primary amines, secondary amines, or Schiff bases, offering a large number of possibilities for further chemical modifications, including attachment to antimicrobial units [28]. In addition, dialdehyde cellulose with a high oxidation degree (>90%) can form a homogeneous solution in hot water (>80 °C) and can be used as an environmentally friendly reducing agent [29]. The active sites at the C2 and C3 positions of the glucose unit on the surface of cellulose modified by oxidant can effectively restrict the reaction process due to the steric hindrance effect. ** of the composite film planes and cross sections. The results show a homogeneous distribution of silver in the DAC@Ag composite films, indicating that the in situ generated AgNPs were uniformly distributed throughout the films.
Figure S1a shows the XRD spectra of the DAC@Ag0-DAC@Ag5 composite films. There was only one peak in the DAC@Ag0 film, appearing at about 2θ = 20°, attributed to the diffraction peak of DAC. In contrast, a new peak at about 2θ = 38°, corresponding to the (111) crystal plane of Ag, was clearly seen in the DAC@Ag1-DAC@Ag5 composite films, and this diffraction peak was gradually enhanced with the increase in the addition of silver ammonia solution. In addition, the XRD pattern of DAC@Ag5 composite film was enlarged, as shown in Figure S1b. The diffraction peaks of AgNPs were shown at 38.12°, 44.24°, 64.54°, 77.33° and 81.46°, which corresponded to the (111), (200), (220), (311) and (222) planes, respectively. These characteristic peaks were consistent with the standard powder diffraction peak data for AgNPs (JCPDS, No. 89-3722), demonstrating the successful synthesis and immobilization of Ag NPs on DAC via this environmentally friendly method [44].
X-ray photoelectron spectroscopy was performed on the DAC@Ag0-DAC@Ag5 composite films to analyze their elemental composition. Figure S2a shows the full scan spectra (in the range of 0–1200 eV) of the DAC@Ag0-DAC@Ag5 composite films. Apparently, two peaks appeared in the XPS spectrum of DAC@Ag0, attributed to C1s and O1s, respectively, while another different peak appeared in the spectrum of DAC@Ag1-DAC@Ag5 composite films, attributed to Ag3d of nanosilver, further confirming the successful in situ generation of nanosilver in the film.
In addition, the curve fitting to the high-resolution spectrum of XPS was performed to further analyze the chemical bonding information. Figure S2b,c show the peak-fitted high-resolution spectra of C1s and O1s in the DAC@Ag composite films (the binding energies were calibrated with C1s = 284.6 eV). The binding energies with peaks at 284.89, 286.81 and 288.78 eV corresponded to C-C/C-H bond, C-O bond and C=O bond, respectively. Notably, the fitted peaks of C=O bond in DAC@Ag1-DAC@Ag5 composite films were clearly shifted to lower binding energies compared to DAC@Ag0. As shown in Figure S2c, the curve fitting of O1s in DAC@Ag0 films showed that the peaks at 530.68, 531.37 and 532.06 eV corresponded to C=O, C-O and O-H, respectively, while the O1s peak positions of the DAC@Ag1-DAC@Ag5 composite films changed, indicating that the generated AgNPs interacted with the aldehyde group of DAC. Figure S2d shows the fitted spectra of Ag3d for DAC@Ag composite films with different silver contents. It can be clearly seen that the characteristic peaks of Ag3d were double peaks located at 367 eV and 373 eV, belonging to Ag3d5/2 and Ag3d3/2, respectively. Moreover, the splitting energies of all Ag3d were about 6.0 eV, indicating that the silver ions were reduced to Ag0 by DAC [45].
Thus, the binding energy shifts of C 1s, O 1s and Ag 3d in DAC@Ag films demonstrated the strong interaction between DAC and AgNPs in DAC@Ag composite films. The above results confirmed the stable deposition of AgNPs in DAC@Ag composite films, which is consistent with previous studies [26,46].
As shown in Figure 7a, the infrared characteristic peaks of the films did not vary with the addition of silver ammonia solution. In addition, the absorption peak at 1620 cm−1 was attributed to the symmetric stretching vibration of the carbonyl group [26], and the absorption peak at 879 cm−1 was attributed to the hemiacetal structure.
Mechanical properties are one of the important characteristics of composite films [47], and the stress–strain curves of the films are displayed in Figure 7b. It can be seen that the elastic modulus of the nanosilver-loaded composite films was higher than that of the DAC@Ag0 film, which was due to the loading of nanosilver increasing the stiffness of the films. As shown in Figure 7c, the tensile strength of DAC@Ag1 and DAC@Ag2 films was higher than that of the DAC@Ag0 films, due to the AgNPs enhancing the stress transfer of those films to some extent [48,49]. However, the tensile strength of DAC@Ag3-DAC@Ag5 films was lower than that of the DAC@Ag0 films, because the filling of nano-silver weakened the hydrogen bonds between fibers [50]. Moreover, the elongation at the break of the silver-loaded composite films gradually decreased compared with the DAC@Ag0 film, which was also caused by the weakening of hydrogen bonds due to nano-silver filling. In addition, Table 1 lists the elastic modulus E, tensile strength σ, and elongation at break ε of the DAC@Ag1 films, which were 2.99 GPa, 94.07 MPa and 4.17%, respectively, and better than the reported values for cellulose–nanosilver composites (E = 3.7 GPa, σ = 54.2 MPa, ε = 4.8%) [51].
Figure 7d shows the UV-vis transmittance spectra of DAC@Ag0-DAC@Ag5 films. It is clear that DAC@Ag1 film had a high transmittance (91%) between 600 nm and 800 nm, which was similar to that of DAC film and higher than that of the cellulose composite film (84.4% at 600 nm) in other study [52]. However, the transmittance gradually decreased as the nanosilver content increased, due to the scattering between DAC and AgNPs. The downward peaks of the curves around 420 nm were attributed to the surface plasmon resonance of the nanosilver, indicating the generation of nanosilver. In addition, the composite films had lower transmittance than the DAC@Ag0 films in the UV range, and the UV transmittance decreased with the increase in the nanosilver content. These indicated that the composite film had good UV-blocking properties, which is one of the important characteristics of active packaging materials [53].
The barrier is an important feature for packaging materials, being mainly manifested by water vapor transmission rate (WVT) and oxygen transmission rate (OTR). Typically, packaging film materials require lower WVT and OTR. Figure 8a and Table 1 show that the WVT values of DAC@Ag0-DAC@Ag5 films were 152.84, 140.41, 140.20, 139.91, 137.82, and 136.41 g/m2·24 h, respectively, which were lower than the values for commercial PE films (3800 g/m2·24 h) and silver-loaded composite films in existing studies (210 g/m2·24 h) [42]. In addition, the WVT of the nanosilver-loaded composite film was reduced compared to that of the DAC@Ag0 film, probably due to the filling effect of AgNPs and the increase in the zigzag path [54]. As shown in Table 1, both DAC@Ag0-DAC@Ag5 films had a very low oxygen transmission rate (OTR), being below the detection limit of the instrument (0.02 cm3/m2·24 h·0.1 MPa), and a similar situation has been reported [28]. The very low oxygen transmission rate makes the films highly attractive for packaging applications.
The water stability test was measured by the one-hour water absorption of the films. As shown in Figure 8b and Table 1, the water absorption of the DAC@Ag0 film was as high as 250%, while that of the silver-loaded composite films decreased to below 4% (Figure 8b, Table 1). The results for the water contact angle in Figure 8c indicated a slight increase in the hydrophobicity of the silver-loaded composite films compared to the DAC@Ag0 film. Therefore, the loading of silver nanoparticles is beneficial in improving the resistance of the film to water [55].
In addition, the antimicrobial properties were tested by the disc diffusion method, and each sample was tested three times. After 24 h of incubation, the antimicrobial properties were determined by detecting the inhibition zones of the films against E. coli and S. aureus. Figure 8d and Figure 9 show the inhibition behavior of the film materials against E. coli and S. aureus, in which the DAC@Ag0 films had no inhibition zones and the silver-loaded composite films showed excellent inhibition against both representative bacteria. This was the result of the destruction of the cell membranes of the bacteria by AgNPs in the silver-loaded films, causing the inactivity and death of bacteria. In addition, the width of the inhibition circle enlarged with the increase in nanosilver content, indicating that the antibacterial properties gradually improved with the increase in nanosilver content. In Figure 8d, the antibacterial activity of these films was stronger against S. aureus compared to E. coli, which was attributed to the difference in the cell wall structure of bacteria that made it easier for AgNPs to enter Gram-positive bacteria than Gram-negative bacteria [42].

3. Experimental Section

3.1. Materials and Chemicals

Microcrystalline cellulose (MCC) was purchased from Sinopharm Chemical Reagent Co., Ltd. (Shanghai, China), sodium periodate (NaIO4, purity ≥ 99%) was purchased from Aladdin Biochemical Science and Technology Co., Ltd. (Shanghai, China), and ethylene glycol (purity ≥ 98%) was purchased from Shanghai Runjie Chemical Reagent Co. Silver nitrate (AgNO3, purity ≥ 99%) and aqueous ammonia (purity ≥ 25%) were provided by Guangzhou Chemical Reagent Factory (Guangzhou, China), and all chemicals were used as is without further purification. The water used in the experiments was deionized.

3.2. Periodate Oxidation and Hydrothermal Dissolution of Cellulose

Twelve grams of MCC and 500 mL of deionized water were added to a 1000 mL blue-capped bottle to form a suspension. Then, 19.0125 g of sodium periodate (molar ratio of NaIO4 to dehydrated glucose units AGU of 1.2) was weighed and dissolved in 242 mL of deionized water. Finally, the sodium periodate solution was added to the above suspension, and the bottle was completely wrapped with aluminum foil to prevent exposure of sodium periodate to light. The bottle was placed in an oil bath at 48 °C and stirred at 800 rpm. After 19 h, an excess of ethylene glycol was added to terminate the reaction. Then, the suspensions were left to stratify, and the supernatant was poured off. The lower solid was washed and dispersed in deionized water to obtain suspensions with a concentration of 5 wt%. The suspensions were then heated for 45–60 min with magnetic stirring (1000 rpm) at 100 °C. After the solid was dissolved, the hot solution was cooled and centrifuged to remove a small amount of insoluble material to obtain dialdehyde cellulose aqueous solution (DAC).

3.3. Preparation of AgNPs

First, 50 g of 0.5 wt% aqueous silver nitrate solution was prepared, and then roughly 0.75 g of 25 wt% ammonia was added to the prepared 50 g of aqueous silver nitrate solution to obtain silver ammonia solution ([Ag(NH3)2]OH). Next, a portion of the aqueous DAC solution was diluted to 0.1 wt% and then mixed with the silver ammonia solution and reacted under heating and stirring in an oil bath. The reaction originated from the classical Tollens reaction. After the reaction, the mixture was dialyzed off the unreacted DAC solution with a dialysis bag (cut-off molecular weight, 3500) to obtain pure silver nanoparticle colloid. A portion of the silver nanoparticle colloid was lyophilized at −40 °C for subsequent assay characterization. During the reaction process, the optimal conditions for the preparation of nanosilver were explored by controlling different mass ratios of DAC to silver ammonia solution, reaction temperature, heating time and different silver ion contents.

3.4. In Situ Synthesis of DAC@Ag Composite Films

Silver ammonia solutions of 0, 200 μL, 400 μL, 600 μL, 800 μL, and 1000 μL were added to 10 mL of 5 wt% DAC aqueous solution, respectively, then stirred magnetically at 50 °C for 60 min. The obtained solutions were each transferred to a Petri dish (diameter of 9 cm), air-dried naturally, and the obtained films were named DAC@Ag0, DAC@Ag1, DAC@Ag2, DAC@Ag3, DAC@Ag4, and DAC@Ag5, respectively.

3.5. Analytical Characterization

3.5.1. Determination of DAC Oxidation

The degree of oxidation of DAC was calculated indirectly by the absorbance of sodium periodate consumption [28]. Briefly, after 19 h of oxidation (before the addition of ethylene glycol), an appropriate amount of liquid was removed from the mixture and diluted 40-fold, and then its absorbance at 290 nm was measured by UV spectrophotometer. The degree of oxidation (DO) was calculated by the following equation [56]:
DO(%) = B/A × 100
where A = moles of periodate consumed per dehydrated glucose unit (162) (1.00), and B = moles of periodate actually consumed per dehydrated glucose unit (162).

3.5.2. Analytical Characterization of Nanosilver and Cellulose

The nanosilver was spectroscopically scanned with a UV spectrophotometer (UV-2600, Shimadzu, China, scanning range 800–300 nm, interval 0.5 nm, speed fast). The average size of nanosilver was examined by a Malvern laser particle sizer (3000HSA, Malvern, UK). The FTIR spectra of MCC and lyophilized DAC were obtained by the potassium bromide press method on a Fourier infrared spectrometer (FT-IR 4700, JASCO, Japan) with a scan range of 4000–400 cm−1 and a resolution of 2 cm−1. The nanosilver colloids were dropped on ultrathin carbon film copper grids, and the morphological characteristics of the nanosilver were observed by transmission electron microscopy (TEMJEM-1400 Plus, Japan) after it was air-dried. The X-ray photoelectron spectra (XPS) of the samples were recorded by an AXIS Ultra DLD spectrometer (Kratos, UK) with Mg Kα radiation (hγ = 1253.6 eV) as the excitation source in steps of 0.1 eV. The crystal structure of the samples was studied by a D8 advanced X-ray diffractometer (Bruker, Germany), where the Cu Kα filtered radiation (λ = 0.15418 nm) was generated at 40 kV and 40 mA current density. The samples were scanned at a scan rate of 2 °/s in steps of 0.0195° over a range of (2θ) from 5 to 90°. The data were then processed using Jade 6.5 software to obtain an approximate crystallinity of AgNPs, and the crystallinity of cellulose was calculated using the following equation [57]:
CI (%) = [(I200 − Iam)/I200] × 100
where I200 is the maximum intensity corresponding to the main peak in plane (200) at 2θ = 22.6°, and Iam is the diffraction intensity in the amorphous region at 2θ = 18.5°. The average particle size of nanosilver (D) was calculated using the Debye–Scherrer equation [46]:
D = Kλ/(βcosθ)
where λ is the wavelength of X-ray diffraction (Cu Kα = 0.15418 nm), K is a constant, taken here as 0.89, β is the half-peak width, and θ is the diffraction angle.

3.5.3. Analytical Characterization of the Composite Films

The surface and cross-sectional morphology of the composite films were observed with a field emission scanning electron microscope (SU5000, HITACHI, Japan) at an accelerating voltage of 3 kV, and were analyzed by energy dispersive X-ray spectroscopy (EDS) for elemental map** (the cross-sectional samples were obtained by liquid nitrogen embrittlement). The infrared spectra of the composite films were obtained with a Fourier infrared spectrometer (FT-IR 4700, JASCO, Japan), setting a scan range of 4000–400 cm−1 and a resolution of 2 cm−1. To characterize the transmittance of the composite films, a UV spectrophotometer (UV-2600, Shimadzu, China) was used to determine the UV transmittance of the samples, setting the scan range from 800–300 nm with an interval of 0.5 nm and a fast speed.
The mechanical properties of the films were obtained by a universal testing machine (INSTRON 5565, USA) at a constant displacement rate of 5 mm/min at room temperature. The water vapor transmission rate (WVR) and oxygen transmission rate (OTR) of the films were tested by a water vapor transmission rate tester (W413 2.0, China) and an oxygen transmission rate tester (Y310 2.0, China), respectively, at a temperature of 30 °C and relative humidity of 75%. The water contact angle was measured and calculated on a contact angle analyzer (ZJ-7000, China): a drop of water (2 μL) was placed on the film surface using an automatic piston syringe and subsequently photographed to capture its side-view image, then the contact angle was calculated. The water stability of the films was measured by immersing the film materials in water for 1 h to measure the water absorption rate and recording the weight change of the sample before and after water immersion [58]. Water absorption rate = (W2 − W1)/W1, where W1 is the film mass before water immersion, and W2 is the film mass after water immersion. Each sample was tested three times and averaged.
In addition, the antibacterial performance of DAC-AgNP composite films was evaluated by disc diffusion method using E. coli and S. aureus as representative Gram-negative and Gram-positive bacteria, respectively. The strain and 0.9 wt% physiological saline were used to prepare an active bacterial suspension with a concentration of approximately 5 × 105 cfu/mL. Subsequently, the film samples were sterilized with UV light for 30 min (samples were cut to 10 mm in diameter). About 10 mL of sterilized nutrient agar medium was poured into sterile Petri dishes. The medium was solidified and inoculated with 50 μL of bacterial suspension, then the samples were affixed to the medium and incubated at 37 °C for 24 h. After incubation, the Petri dishes were removed to measure the inhibition circle. The assay was repeated three times for all samples.

4. Conclusions

To sum up, in this study, silver nanoparticles were successfully prepared in a homogeneous aqueous solution of dialdehyde cellulose without adding other reducing and stabilizing agents. The prepared silver nanoparticles were mainly spherical in shape with an average size of about 25 nm under optimal conditions. Moreover, in situ-synthesized DAC@Ag composite films were also prepared. The obtained films were smooth and dense. The AgNPs were uniformly distributed on the surface and the inside of the films. Upon the increase in AgNP content, the tensile strength of the composite films rose to 94.6 MPa and then gradually decreased. The obtained composite films not only had good transparency but also had good UV-blocking properties. In addition, the composite films also had excellent oxygen and water vapor barrier, water stability, and outstanding antibacterial ability against E. coli as well as S. aureus. Therefore, this study not only developed a green and simple method for the preparation of metal nanoparticles but also provided a novel route for the in situ synthesis of antibacterial composite films. The synthesized nanosilver can be isolated for use in other fields, and the synthesized silver-loaded composite films can be further used in antimicrobial packaging materials.

Supplementary Materials

The following supporting information can be downloaded at: https://mdpi.longhoe.net/article/10.3390/molecules28072956/s1, Figure S1: (a) XRD spectra of DAC@Ag0-DAC@Ag5 composite films and (b) enlarged view of the spectra of DAC@Ag5 composite film; Figure S2. XPS spectra of DAC@Ag0-DAC@Ag5 composite films: (a) full scan spectrum, (b) C1s region, (c) O1s region and (d) Ag3d region.

Author Contributions

Conceptualization, J.Z. and Pengfei Li; Methodology, J.Z., X.X., F.H. and J.L.; Software, J.Z. and X.X.; Validation, X.X.; Formal analysis, J.Z., F.H. and P.L.; Investigation, X.X.; Resources, P.L.; Data curation, J.Z. and X.X.; Writing – original draft, X.X.; Writing – review & editing, J.Z., X.X., F.H. and P.L.; Supervision, F.H.; Project administration, P.L.; Funding acquisition, J.Z., J.L. and P.L. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by Guangdong Provincial Key Laboratory of Plant Resources Biorefinery (2021GDKLPRB-K03), “Pioneer” R&D program of Zhejiang (2022C01234), Shandong **ing Key R&D Program (2022JBZP003), Characterization and Instrument of cross-scale nanofiber based on micro-fluidic technology (2020ZD01), Sichuan Yibin “Jie bang gua shuai” Program (2022JB014), the Foundation of State Key Laboratory of Biobased Material and Green Papermaking, Qilu Univer-sity of Technology, Shandong Academy of Sciences (No. GZKF202230), Guangzhou Basic and Applied Basic Research Program (2023A04J1575), Science and technology project of Guangzhou (202102020713), Project of Jiangxi Provincial Technological Innovation Center (20222BCD43021).

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

The data presented in this study are available on request from the corresponding author.

Conflicts of Interest

The authors declare no conflict of interest.

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Molecules 28 02956 g001 550
Figure 1. Results for different DAC to silver ammonia solution mass ratios: (a) UV-vis spectra and (inset) average size histogram; (b–f) TEM images of DAC to silver ammonia solution mass ratios of 0.25–4, respectively.
Figure 1. Results for different DAC to silver ammonia solution mass ratios: (a) UV-vis spectra and (inset) average size histogram; (b–f) TEM images of DAC to silver ammonia solution mass ratios of 0.25–4, respectively.
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Molecules 28 02956 g002 550
Figure 2. Results for different reaction times: (a) UV-vis spectra and (inset) average size histogram; (b–f) TEM images for reaction times of 20–100 min, respectively.
Figure 2. Results for different reaction times: (a) UV-vis spectra and (inset) average size histogram; (b–f) TEM images for reaction times of 20–100 min, respectively.
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Molecules 28 02956 g003 550
Figure 3. Results for different reaction temperatures: (a) UV-vis spectra and (inset) average size histogram; (b–f) TEM images for reaction temperatures of 50–90 °C, respectively.
Figure 3. Results for different reaction temperatures: (a) UV-vis spectra and (inset) average size histogram; (b–f) TEM images for reaction temperatures of 50–90 °C, respectively.
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Figure 4. Results for different Ag+ contents: (a) UV-vis spectra; (b) average size histogram; (c–e) TEM images for Ag+ contents of 0.05 wt%–0.1 wt%, respectively.
Figure 4. Results for different Ag+ contents: (a) UV-vis spectra; (b) average size histogram; (c–e) TEM images for Ag+ contents of 0.05 wt%–0.1 wt%, respectively.
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Figure 5. FT-IR spectra (a) and XRD spectra (b) of MCC and DAC, (c) in high resolution, (c, inset) selected area electron diffraction of AgNPs, (d) XRD spectra of AgNPs, (e) XPS spectra of DAC and AgNPs.
Figure 5. FT-IR spectra (a) and XRD spectra (b) of MCC and DAC, (c) in high resolution, (c, inset) selected area electron diffraction of AgNPs, (d) XRD spectra of AgNPs, (e) XPS spectra of DAC and AgNPs.
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Molecules 28 02956 g006 550
Figure 6. Optical photograph of DAC@Ag0-DAC@Ag5 films (a), SEM images of the plane and cross section of DAC@Ag0 film (b,c) and DAC@Ag1 film (d,e), EDS element map** of composite film planes (f) and cross sections (g).
Figure 6. Optical photograph of DAC@Ag0-DAC@Ag5 films (a), SEM images of the plane and cross section of DAC@Ag0 film (b,c) and DAC@Ag1 film (d,e), EDS element map** of composite film planes (f) and cross sections (g).
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Figure 7. FT-IR spectra (a), mechanical properties (b,c) and UV transmission spectra (d) of DAC@Ag0-DAC@Ag5 films.
Figure 7. FT-IR spectra (a), mechanical properties (b,c) and UV transmission spectra (d) of DAC@Ag0-DAC@Ag5 films.
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Figure 8. Water vapor transmission rate (WRT) (a), water absorption (b), water contact angle (c), and bacterial inhibition zone (d) of DAC@Ag0-DAC@Ag5 films.
Figure 8. Water vapor transmission rate (WRT) (a), water absorption (b), water contact angle (c), and bacterial inhibition zone (d) of DAC@Ag0-DAC@Ag5 films.
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Figure 9. Antibacterial test of DAC@Ag0-DAC@Ag5 films. Inhibition images of the DAC@Ag0-DAC@Ag5 films against E. coli (a–f) and S. aureus (g–l).
Figure 9. Antibacterial test of DAC@Ag0-DAC@Ag5 films. Inhibition images of the DAC@Ag0-DAC@Ag5 films against E. coli (a–f) and S. aureus (g–l).
Molecules 28 02956 g009
Table
Table 1. Tensile testing, antimicrobial properties, barrier and water stability results for DAC@Ag films.
Table 1. Tensile testing, antimicrobial properties, barrier and water stability results for DAC@Ag films.
SampleTensile TestingAw
(°)		Inhibition Zone (mm)WVT
(g/m2·24 h)		ORT
(cm3/m2·24 h·0.1 MPa)		Water Absorption
(%)
E
(GPa)		σ
(MPa)		ε
(%)		E. coliS. aureus
DAC@Ag02.2677.384.3162.1200152.84<0.02254.12
DAC@Ag12.9994.074.1766.633.12.8140.41<0.023.31
DAC@Ag23.1683.133.2366.903.94.8140.20<0.023.24
DAC@Ag33.0869.152.6766.934.45.1139.91<0.023.05
DAC@Ag44.5956.011.5766.854.95.4137.82<0.022.83
DAC@Ag53.8836.991.4366.945.36.3136.41<0.020.81
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Zeng, J.; **ong, X.; Hu, F.; Li, J.; Li, P. Dialdehyde Cellulose Solution as Reducing Agent: Preparation of Uniform Silver Nanoparticles and In Situ Synthesis of Antibacterial Composite Films with High Barrier Properties. Molecules 2023, 28, 2956. https://doi.org/10.3390/molecules28072956

AMA Style

Zeng J, **ong X, Hu F, Li J, Li P. Dialdehyde Cellulose Solution as Reducing Agent: Preparation of Uniform Silver Nanoparticles and In Situ Synthesis of Antibacterial Composite Films with High Barrier Properties. Molecules. 2023; 28(7):2956. https://doi.org/10.3390/molecules28072956

Chicago/Turabian Style

Zeng, **song, **nyi **ong, Fugang Hu, **peng Li, and Pengfei Li. 2023. "Dialdehyde Cellulose Solution as Reducing Agent: Preparation of Uniform Silver Nanoparticles and In Situ Synthesis of Antibacterial Composite Films with High Barrier Properties" Molecules 28, no. 7: 2956. https://doi.org/10.3390/molecules28072956

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