Colloids and Surfaces A: Physicochemical and Engineering Aspects 626 (2021) 127093

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Colloids and Surfaces A: Physicochemical and

Engineering Aspects
journal homepage: www.elsevier.com/locate/colsurfa

Fabricating Ag@MOF-5 nanoplates by the template of MOF-5 and

evaluating its antibacterial activity
Yinchun Hu a, b, *, Hui Yang b, Renhu Wang b, Menglan Duan a, **
a
College of Safety and Ocean Engineering, China University of Petroleum (Beijing), 18 Fuxue Road, Beijing 102249, China
b
Research Center for Nano-biomaterials & Regenerative Medicine, Department of Biomedical Engineering, College of Biomedical Engineering, Taiyuan University of
Technology, Taiyuan 030024, China

G R A P H I C A L A B S T R A C T

The 3–5 nm nano-Ag particles were uniformly loaded on the flaky crystals of MOF-5, and Ag@MOF-5 nanoplates were obtained. EDS showed that the content of Zn
and Ag was 18.13 wt% and 38.87 wt%, respectively. Ag@MOF-5 nanoplates are expected to be further used in tissue engineering materials, drug carriers, anti­
bacterial products and other similar fields.

A R T I C L E I N F O A B S T R A C T

Keywords: MOF-5 was prepared by hydrothermal method and Ag@MOF-5 nanoplates were obtained to improve the anti­
MOF-5 bacterial activity and dispersion of Ag nanoparticles. MOF-5 and Ag@MOF-5 were characterized by scanning
Ag nanoparticles electron microscope (SEM), high-resolution transmission electron microscope and energy spectrum (HR-
Ag@MOF-5
TEM&EDS), X-ray diffraction (XRD), infrared spectrum (FTIR) and thermal gravimetric analysis (TGA). MOF-5
Antibacterial activity
was flaky crystals accumulated and complexed to form cube-like crystalline particles with the size of 20–50
micrometers, and it was destroyed in the process of loading nano-silver particles. Ag@MOF-5 nanoplates were
nanoscale sheets, and 3–5 nm Ag nanoparticles were uniformly dispersed and loaded on nanoplates of MOF-5.
The content of silver nanoparticles reached 13 wt% of Ag@MOF-5 total weight. The results of antibacterial
experiment indicated that antibacterial ability of MOF-5 was limited, while Ag@MOF-5 showed good antibac­
terial ability to Escherichia coli and Staphylococcus aureus.

1. Introduction antibacterial spectrum and low tendency to induce bacterial resistance

The microbial variation caused by drug resistance is an extremely
serious problem due to the abuse of antibiotics, disinfectants and other
chemical drugs. The antibacterial agents can effectively kill the patho­
genic bacteria which have become a new research focus [1,2]. Silver
(Ag)-based antibacterial agents have high antibacterial activity, broad
[3,4]. The key factor of Ag-based antibacterial agents is the size and
dispersity of Ag particles. Ag nanoparticles is more than 200 times the
antibacterial performance of Ag microparticles [5,6]. Ag nanoparticles
have higher antibacterial activity, but they tend to spontaneously
aggregate into large particles and cannot be dispersed uniformly in
substrate [7,8]. Ag nanoparticles are often loaded on a suitable carrier

* Corresponding author at: College of Safety and Ocean Engineering, China University of Petroleum (Beijing), 18 Fuxue Road, Beijing 102249, China.
** Corresponding author.
E-mail addresses: huyinchun@tyut.edu.cn (Y. Hu), mlduan@cup.edu.cn (M. Duan).

https://doi.org/10.1016/j.colsurfa.2021.127093
Received 13 April 2021; Received in revised form 16 June 2021; Accepted 27 June 2021
Available online 1 July 2021
0927-7757/© 2021 Elsevier B.V. All rights reserved.
Y. Hu et al.
which effectively prevents them aggregation and assists to develop its
antibacterial property [9].
Metal organic frameworks (MOFs) are attracting much attention due
to their smart properties, such as high surface areas, tunable pore sizes,
crystalline open structures and functionalities. There are many studies
devoted to the fabrication of MOFs nanocomposites through the appli­
cation of MOFs as templates for immobilization of metal nanoparticles
which have exhibited great potential application in gas separation,
catalytic reaction and drug carriers [10–15]. Surya et al. fabricated
Ag2O@MOF composites by the impregnation method [16]. Ganesan
et al. fabricated MOF-5(Zn) and Ag@MOF-5(Zn) in one step by hydro­
thermal process [17]. Thakare et al. used a straightforward mixture
method to prepare the silver nanoparticles loaded MOF-5 as a photo­
catalyst for water disinfection under visible light illumination [18]. Ren
et al. loaded anticancer drugs in MOF-5 and studied its vitro release
which showed good drug loading quantity and biocompatibility of
MOF-5 [19]. Wang and Deng loaded Pt and Pd nanoparticles on MIL-101
and ZIF-8 by encapsulating metal nanoparticles within their layers or
inside their channels [20,21]. Ansari-Asl fabricated Ag
nanoparticles/Zn-MOF nanocomposites through encapsulating Ag+ ions
into the framework of Zn-MOF and subsequent reduction of these ions
by a very complicated process, and the solution of AgNO3 in EtOH was
used to prepare Ag nanoparticles [22]. Akhbari et al. showed that the
antibacterial activity of three zinc-terephthalate MOFs was related to
their structural features, and activity MOF-5 showed better antibacterial
activity than MOF-5 [23]. All these studies provide many methods for
MOFs as the carrier of metal nanoparticles or drugs which also indicate
the potential application of MOF-5 in antibacterial agents of Ag
nanoparticles.
Water molecules attack the weak metal-organic coordination bonds
of MOF-5 in humid environment which results in the phase transition or
structural collapse which provides a potential chance for loading Ag
nanoparticles on the chips of collapsed MOF-5 [24–26]. In this paper,
the flaky crystalline MOF-5 was synthesized by hydrothermal method.
Ag nanoparticles were loaded on the chips of MOF-5 with AgNO3 solu­
tion as the reaction solution and glucose as reducer, which was named as
Ag@MOF-5. The structures and properties of MOF-5 and Ag@MOF-5
were characterized by X-ray powder diffraction (XRD), scanning elec­
tron microscope (SEM), high-resolution transmission electron micro­
scope and energy spectrum (HR-TEM&EDS), infrared spectrum (FTIR)
and thermal gravimetric analysis (TGA). The antibacterial activity was
tested by the method of bacteriostatic circle which provided the basis for
their application in biomedicine, antibacterial products and other
related fields.
2. Experimental
2.1. Materials
Zinc nitrate hexahydrate (Zn (NO3)2.6H2O, AR), 1,4-benzenedicar­
boxylic acid (H2BDC, AR), N, N-dimethyl formamide (DMF), silver ni­
trate, β-D-glucose are analytical pure, purchased from Aladdin reagent
company; All experimental water was deionized water.
2.2. Preparation of MOF-5 and Ag@MOF-5
MOF-5 was synthesized according to the reported procedures with
some modification [27]. The difference between the reported synthesis
and ours was that we used a hydrothermal reactor (100 mL), while a
glass vial was used by the former. 1.5 × more starting materials were
used in this study. A mixture of 0.528 g H2BDC, 2.496 g Zn (NO3)2.6H2O
and DMF was added in a hydrothermal reactor at 130 ◦ C under autog­
enous pressure for 4 h. Then, the reaction system was cooled slowly to
room temperature. The resulting black products were filtered off and
washed with DMF for three times. And then the remaining solid was
dried in vacuum oven at 60 ◦ C for 24 h. The resulted white crystals were
2
Colloids and Surfaces A: Physicochemical and Engineering Aspects 626 (2021) 127093
MOF-5.
Ag@MOF-5 was fabricated by a green and mild method according to
the reported procedures with some modification [21,22,28]. MOF-5
powder was evenly dispersed in deionized water. The 0.1 mol/L silver
nitrate solution was added in the solution while it was stirring, and then
stirred for more than 6 h away from light. Finally, the pink precipitation
was formed. The supernatant was poured out and the precipitation was
activated in a vacuum oven at 60 ◦ C for 12 h. The solution of β-D-glucose
(molar ratio of glucose to silver ion is 1:2) was used to reduce silver ion
for 1 h [29,30]. The supernatant was poured out and the Ag@MOF-5
was dried in a vacuum oven at 60 ◦ C for 24 h.
2.3. Characterizations and antibacterial activity assay of MOF-5 and
Ag@MOF-5
The morphologies of MOF-5 and Ag@MOF-5 were characterized by
scanning electron microscope (SEM, JSM-7100F, JEOL), high-resolution
transmission electron microscope and energy spectrum (HR-TEM&EDS,
F20, FEI). The crystal structures of MOF-5 and Ag@MOF-5 were deter­
mined by X-ray diffraction (XRD, XRD-1730, Philips) with Cu Ka radi­
ation. The diffractometer was operated at 40 kV and 35 mÅ . Scanning
was performed with the 2θ values ranging from 5◦ to 50◦ . Fourier
transformed infrared spectrometer (FTIR, Perkin Elmer) was used within
the range of 4000–800 cm-1 to identify the functional groups. MOF-5
and Ag@MOF-5 were mixed with KBr pellet to prepare the specimens
for FTIR, and transmission mode was used at room temperature. Ther­
mal gravimetric analysis (TGA, STA-449C, Netzsch) was used for weight
loss process analysis, and temperature range is 20–600 ◦ C.
The bacterial strains used were Gram-positive Staphylococcus aureus
(S. aureus) and Gram-negative Escherichia coli (E. coli). These strains
were provided by the Shanxi Medical University, China. Nutrient agar
plates were inoculated using 100 microliters of bacterial suspension
containing 1 × 106 cfu/mL, where the cfu is the colony forming unit, by
using the paper disc diffusion method. Sterile filter paper discs with a
diameter of 6 mm were immersed in 10 mL of MOF-5, Ag@MOF-5
aqueous solution with a concentration of 0.5 mg/mL. Then, the paper
discs were placed on the agar plates inoculated with bacteria. These
plates were incubated at 37 ◦ C for 24 h, and the diameters of the inhi­
bition zone around the samples were measured.
2.4. Statistical analysis
All experiments were performed in triplicates. The data were
expressed as the means ± standard deviations. Statistical significance
was assessed using Student’s t - test, and the values were considered
significant at p < 0.05.
3. Results and discussion
3.1. Microstructure and crystal structure
MOF-5 is one of the most classic MOFs is Zn4O13C24H12 framework
which was invented in1999 [15]. It has been recognized that MOF-5
occupies either cubic or tetragonal structure related to the synthetic
conditions. MOF-5 of cubic structure shows more intense (200)
diffraction peak than (220), and it is more stable than tetragonal
structure [31–34]. The microstructure of MOF-5 synthesized by hydro­
thermal method is shown in Fig. 1. The flaky crystals of MOF-5 accu­
mulated and complexed to form cube-like crystalline particles with the
size of 20–50 micrometers. There were many cracks on the surface of
cube-like crystalline particles obviously. The SEM morphology of
Ag@MOF-5 obtained by loading nano-Ag particles on MOF-5 is shown in
Fig. 2. Ag@MOF-5 was nanocrystalline particles with thickness of tens
nanometers, and nanoscale granular matters attached on the surface of
MOF-5 nanoplates. This indicated that the cube-like crystalline particles
of MOF-5 was collapsed in the loading nano-Ag process and nano-Ag
Y. Hu et al. Colloids and Surfaces A: Physicochemical and Engineering Aspects 626 (2021) 127093

Fig. 1. SEM images of MOF-5.

Fig. 2. SEM images of Ag@MOF-5.

particles were loaded on the surface of the wafer from collapsed MOF-5.
Further analysis by TEM and energy spectrum were performed on
Ag@MOF-5 nanoplates, as shown in Fig. 3. A large number of irregular
nanoparticles with a diameter of 3–5 nm were uniformly attached on the
nanoplates. The lattice fringe spacing of nanospheres in high-resolution
images was 0.235 nm, which was consistent with the lattice spacing of
silver (111) crystal faces. EDS of nanoplates in Fig. 3 showed that the
content of Zn and Ag was 18.13% and 38.87%, respectively. Fig. 5 was
XRD spectra of MOF-5 and Ag@MOF-5. MOF-5 and Ag@MOF-5 both
showed the strongest characteristic diffraction peak at 2θ = 9.6◦ which
was assigned to lattice plane (220), and the much weaker peak at
2θ = 7◦ of MOF-5 was assigned to the lattice plane (200). Thus, the flaky
crystalline MOF-5 was tetragonal crystal structure, and this result was
connected with DMF as solvent in the process of vacuumed drying and
the collapsing of cube-like crystalline particles in the loading nano-Ag
process [35]. While the diffraction peaks of Ag nanoparticles (111)
and (200) crystal planes appeared at 2θ = 37.5◦ and 43.5◦ on the XRD
spectra of Ag@MOF-5. These results showed that 3–5 nm Ag nano­
particles were loaded on MOF-5 nanoplates which formed Ag@MOF-5
nanoplates (Fig. 4).

3.2. Thermogravimetic analysis

Fig. 4. XRD patterns of MOF-5 and Ag@MOF-5.
The thermogravimetic (TG) curves of MOF-5 and Ag@MOF-5 are

Fig. 3. HR-TEM images and EDS analysis of Ag@MOF-5 nanoplates.

3
Y. Hu et al.
shown in Fig. 5. MOF-5 has two weight loss processes. First one is about
20 wt% weight loss between 100 and 250 ◦ C which is the weight loss of
residual solvents and guest molecules in the channel of MOF-5. Second is
a rapid weight loss process between 500 and 525 ◦ C (35 wt%) which is
the decomposition process of MOF-5, and MOF-5 is completely decom­
posed at 560 ◦ C with a residual of 45 wt% [29]. The weight loss process
of Ag@MOF-5 is also divided into two steps. About 15 wt% weight loss
between 100 and 300 ◦ C which is the weight loss of glucose and solvent
molecules adhered to Ag@MOF-5. Then a platform appears at
300–400 ◦ C which indicates the Ag@MOF-5 can exist stably in this
temperature region. The weight loss between 380 and 550 ◦ C is about
30 wt% which is the decomposition process of Ag@MOF-5. By
comparing the residual after completely decomposition of MOF-5 and
Ag@MOF-5, it can be seen that the amount of loaded Ag nanoparticles is
about 13 wt% of the total mass. It is about 28.9 wt% of the mass of Zn of
MOF-5.
3.3. FTIR analysis
The FTIR spectra of MOF-5 and Ag@MOF-5 were shown in Fig. 6.
The position and numner of strong absorption peaks of them were all
similar which indicated that only the shape of MOF-5 was destroyed in
the process of loading silver while the molecular structure did not
change significantly. There were two strong infrared absorption peaks in
the range of 1400–1700 cm-1. 1585 cm-1 was the absorption peak of
COO asymmetric stretching vibration, and 1392 cm-1 was the absorption
peak of COO symmetric stretching vibration, which indicated that C– –O
bond of the carboxyl group on terephthalic acid had not been broken
and carboxyl group may be combined with the bridge mono-oxygen
mono-tooth coordination mode [36]. The absorption peaks in the
fingerprint area were mainly caused by the extrareal vibration of ter­
ephthalic acid. 752 cm-1 was the characteristic absorption peak caused
by the stretching vibration of Zn–O in the tetrahedral Zn4O crystal
cluster in MOF-5 [37]. The wide peak around 3427 cm-1 was the
stretching vibration peak of O–H and the absorption peak of water in
the sample [26]. According to the literature [38], 3650–3580 cm-1 was
the absorption peak of weakly bound water. In this infrared spectrum,
there was no obvious absorption peak in this region, which indicated
that there was no large amount of weakly bound water in the framework
of MOF-5 and Ag@MOF-5. In the infrared spectrum of MOF-5, C–H
vibration absorption peaks of benzene ring in aromatic group and
aliphatic group were found at 2930–2875 cm-1 [39], which indicated
the presence of guest molecules in MOF-5. This is consistent with TG
analysis results.
Fig. 5. TG curves of MOF-5 and Ag@MOF-5.
4
Colloids and Surfaces A: Physicochemical and Engineering Aspects 626 (2021) 127093
Fig. 6. FTIR spectra of MOF-5 and Ag@MOF-5.
3.4. Antibacterial activity
The antibacterial properties of silver nanoparticles have received
extensive attention and research. At present, there are three main views
on their bactericidal mechanism: silver ions hinder bacterial DNA
replication, nano-silver destroys cell membrane, and nano-silver pro­
duces reactive oxygen species to interfere with the activity of its internal
substances. Silver nanoparticles mainly achieve antibacterial functions
by destroying the cell membrane of Escherichia coli and inhibiting the
cell division of Staphylococcus aureus [40].
The antibacterial property test results of MOF-5 and Ag@MOF-5
were shown in Figs. 7 and 8. The average diameters of inhibition
zones of MOF-5 and Ag@MOF-5 on Escherichia coli were 11.44 mm and
16.05 mm, respectively. The average diameters of inhibition zones of
MOF-5 and Ag@MOF-5 on Staphylococcus aureus were 13.36 mm and
14.62 mm, respectively. It could be concluded that Staphylococcus au­
reuses were more sensitive to MOF-5 than Escherichia coli, and this
result was similar to the study of Akhbari [41]. It is due to the fact that
Gram-negative bacteria consists of a lipopolysaccharide outer mem­
brane and plasma inner membrane which makes it difficult for Zn2+ to
cross the cell wall of Escherichia coli [42,43]. However, the inhibition
zones of Zn-MOF and Ag NPs/Zn-MOFs nanocomposites report by
literature were only 8–9 mm and 9 − 12 mm [22]. So, this flaky crys­
talline MOF-5 had certain antibacterial properties, and it was due the
fact that Zn2+ and flaky crystal morphology of MOF-5 lead to certain
antibacterial properties of MOF-5. Meanwhile, Zn2+ was located in the
skeleton of MOF-5 and could not be released, and its antibacterial
properties were limited [44]. Ag@MOF-5 had good antibacterial prop­
erties against both bacteria, and its antibacterial activity against
Escherichia coli was obviously much better than that of Staphylococcus
aureus. Ag@MOF-5 showed more excellent broad spectrum antibacte­
rial properties than MOF-5 which indicated that Ag nanoparticles loaded
on the nanoplates of MOF-5 could be released in the medium and cross
the cell wall of bacteria.
4. Conclusion
The tetragonal crystal structured MOF-5 was synthesized by hydro­
thermal method. The flaky crystals of MOF-5 accumulated and com­
plexed to form cube-like crystalline particles with the size of 20–50
micrometers. Nano-Ag was successfully loaded on the nanoplates of
MOF-5, and we gained Ag@MOF-5 nanoplates antibacterial agent. By
Y. Hu et al. Colloids and Surfaces A: Physicochemical and Engineering Aspects 626 (2021) 127093

Fig. 7. Inhibition zone tests of MOF-5 and Ag@MOF-5 against Escherichia coli (a1 and a2) and Staphylococcus aureus (b1 and b2).

means of SEM, TEM, EDS, XRD, IR, TG analysis, it was shown that the
3–5 nm nano-Ag particles were uniformly loaded on the nanoplates of
MOF-5. The dispersion and solid loading of Ag nanoparticles was real­
ized by the flaky crystal MOF-5, and nano-Ag loading amount was up to
13 wt% of Ag@MOF-5 total weight. MOF-5 had certain antibacterial
activity, and its antibacterial activity was limited because Zn2+ was
located in the skeleton of MOF-5. Ag@MOF-5 nanoplates showed good
antibacterial activity against Escherichia coli and Staphylococcus
aureus. Ag@MOF-5 nanoplates are expected to be further used in tissue
engineering materials, drug carriers, antibacterial products and other
similar fields.

CRediT authorship contribution statement

Yinchun Hu, Renhu Wang: Data curation, Writing - original draft.

Hui Yang: Visualization, Investigation. Menglan Duan: Supervision.
Yinchun Hu, Hui Yang: Writing - review & editing.

Declaration of Competing Interest

Fig. 8. Inhibition zone tests of MOF-5 and Ag@MOF-5 against Escherichia coli
and Staphylococcus aureus.
The authors declare that they have no known competing financial

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Y. Hu et al. Colloids and Surfaces A: Physicochemical and Engineering Aspects 626 (2021) 127093

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