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PII: S0925-4005(17)32209-8
DOI: https://doi.org/10.1016/j.snb.2017.11.078
Reference: SNB 23572
Please cite this article as: Hongyun Xuan, Wei Dai, Yanxi Zhu, Jiaoyu Ren,
Jianhao Zhang, Liqin Ge, Self-Healing, antibacterial and sensing nanoparticle
coating and its excellent optical applications, Sensors and Actuators B:
Chemical https://doi.org/10.1016/j.snb.2017.11.078
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Self-Healing, antibacterial and sensing nanoparticle coating and its
a
National Demonstration Center for Experimental Biomedical Engineering Education,
State Key Laboratory of Bioelectronics, School of Biological Science and Medical
Engineering, School of Biological Science and Medical Engineering, Southeast
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University, Nanjing 210096, P.R. China
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b
Nanjing Center of Meat Quality and Safety Control, Key Lab of Meat Processing
and Quality Control, Ministry of Education, College of Food Science, Nanjing
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agricultural university, Nanjing 210096,P.R.China.
c
Central Laboratory of Linyi People’s Hospital, Linyi 276003, PR China.
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* E-mail: lqge@seu.edu.cn.
Prepared nanoparticle coatings can heal the damages during use and prolong the
service time.
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MoS2 is used to not only improve coatings’ antimicrobial property but also endow
them metal ions sensing property.
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Keywords: antibacterial, self-healing, LbL assembly, host-guest interactions, Co2+
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senor
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1. Introduction
Inspired by nature, self-healing materials have an attracted considerable interest
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in various fields such as biomedical engineering, [1] chemical engineering [2] and food
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[3]
engineering. Therefore, all kinds of self-healing materials, ranging from solid
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[4-5]
concrete to soft elastomers, have been introduced. In recent years, self-healing
coatings as a new type of self-healing material has become a unique and popular topic.
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Some recent studies dealt with the self-healing coatings and showed how covalent or
[4, 6-7]
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Zhu et al. [12] have reported the hydrogen bonding coatings that exhibited repeatable
self-healing and easy processability. When a supramolecular assembly approach is
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followed, the host-guest coatings exhibit not only repeatable self-healing and easy
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processability but also excellent mechanical and acid-resistant properties. [10, 13] Based
on the previous study of the self-healing host-guest coatings, [10] their antimicrobial
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and self-healed; Therefore, Molybdenum disulfide (MoS2) is first introduced to
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endow the coatings with simultaneous antimicrobial and self-healing properties, and
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other properties are also developed to expand the application fields.
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MoS2 that is a typical layered crystal like a graphene structure, has shown great
promise and has been investigated with great attention. [21] However, MoS2 nanosheets
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possess excellent biocompatibility and photoluminescence characteristics comparing
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[22-23]
with bulk MoS2. The increasingly broad application of MoS2 leads to contact
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[24]
with environmental microorganisms and photoluminescence sensors. Nilam et al.
[25]
and Marek kostecki et al. have demonstrated that MoS2 nanosheets have
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photoluminescence can emerge from MoS2 nanosheets because its band gap can reach
[26]
1.9 eV for a single monolayer. And its photoluminescence relies on the transition
from indirect band gap to direct band gap. In addition, as an attractive semiconductor
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material, MoS2 can be applied in the flexible substrate due to a large in-plane carrier
mobility of about 200-500 cm2/ (Vs) and robust mechanical properties. [27]
Goki Eda
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et al. have deposited the thin film of MoS2 on flexible PET. [28] Our work shows that
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hybrid coatings, and that, the coatings have specific response to heavy metal ions
Co2+.
Heavy metals in biological fluids and food engineering are a major source of
pollution. Excessive amounts of heavy metals could lead to chronic toxicity and
[29]
become harmful to human health. As a primary micronutrient, Co2+ is required
[30]
for the growth of plants and animals. Co2+ is also a part of vitamin B12 that human
body can’t synthesize. Humans do need to ingest this micronutrient (found in foods
[31]
such as eggs, fish, milk and green vegetables), but, large amounts of Co2+ can
[32]
generate toxicological effects in human body. Therefore, determination of Co2+
concentration is essential and significant. Up to now, several methods have been
employed to detect Co2+ concentration. [33-34]
But pretreatment steps for modification
and functionalization of a sorbent are so complicated. MoS2 nanosheets with layered
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structure and abundant sulfur groups on the edges and surfaces can greatly absorb
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Co2+ and are applied in heavy metals sensing. Only, Shemirani et al. employed MoS2
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nanosheets to defect Co2+ in vegetable and water samples. [35]
In our work, however,
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the fluorescence quenching was first investigated between Co2+ concentration and
MoS2 to successfully fabricate the sensing coatings for Co2+. Taking into account its
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damage failure, the self-healing sensing coatings were carried out.
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Herein, to achieve antibacterial and self-healing coatings, the
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MoS2/β-CD-PEI/AD-PAA coatings were successfully fabricated on the substrate via
LbL self-assembly technique (Scheme 1). Besides, the photocatalytic disinfection
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activity of MoS2 nanosheets was introduced to achieve better disinfection effect. And,
the photoluminescence property was firstly applied in Co2+ sensor. Then,
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between the fluorescence intensity and the Co2+ concentration was demonstrated by
fluorescence spectra.
2. EXPERIMENTAL SECTION
2.1 Materials
poly ( acrylic acid ) ( PAA ) ( Mw ≈ 450000 g.mol-1 ), Poly ( ethylenimine ) ( PEI )
( Mw ≈ 25000 g.mol-1 ), 1-rthyl-3-( 3 ( dimethylamino ) propyl ) carbodiimide,
ammonium polyphosphate, hydrochloride ( EDC ) and N-hydroxysuccinimide ( NHS )
were purchased from Sigma-Aldrich. Adamantanamine (AD) and Carboxymethyl
beta-cyclodextrin (β-CD) were respectively obtained from Shanghai mindray
chemical technology co., LTD and Shandong binzhou wisdom source biotechnology
co., LTD. Cobalt ions and dialysis bag was bought from Nanjing yat sen villa glass
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instrument co., LTD. The emerald-green solution of Molybdenum disulfide (MoS2)
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flakes (100-400 nm, 18 mg/ mL) was bought from Graphene Supermarket.
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Dihydrogen phosphate and disodium hydrogenorthophosphate were all purchased
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from Nanjing yat sen villa glass instrument co., LTD to perpetrate pH 8.0 phosphate
buffered saline (PBS). Fetal bovine serum (FBS), Dulbecco’s modified eagle’s
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medium (DMEM), and L929 cells were bought from Biotechnology Center (Nanjing,
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Ge man).
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2.2 Characterization
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the prepared samples. The self-healing process of the samples on the substrate
was observed with SEM and Microscope (OLYMPUS BX51). Fluorescence
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typical current−voltage (I−V) measurements and imaging were carried out using
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2.3 Fabrication self-healing, antibacterial and metal-ion sensing coatings via LbL
assembly technique
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[36]
plates . Then, the L929 cells were cultured in 6-well cell culture plates at 5x105
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cells per well in 90% DMEM and 10% FBS and incubated at 37 ℃ in a 5% CO2 / 95%
O2 atmosphere for 48 h. Finally, the L929 cells on the coatings were observed by the
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inverted microscope to evaluate the cell viability.
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2.5 Antibacterial Activity
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As a model bacterial strain, gram-negative Escherichia coli aw1.7 (E.coli) was
employed to evaluate the antimicrobial properties of the coatings. E.coli were
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incubated in nutrient broth at 37 ℃ for 24 h to yield a cell count of approximately 109
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colony forming units (CFU) / mL. Then 50 μL bacterial solution was respectively
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coatings. They were incubated at 37 ℃ for 1 h after irradiated by UV light for 30 mins.
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Then the coatings with the bacterial solution were cleaned with 5 mL of sterile 0.85%
(wt / vol) saline solution. The cleanout fluid was carefully pipette out, and bacteria
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concentrations were determined by the standard plate count method. The plates were
incubated at 37 ℃ for 24 h. The number of colonies was enumerated through visual
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MoS2/(PAA-AD/PEI-β-CD) coatings, which exhibited the emission characteristic
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peak at ~500 nm (Figure 6c). What’s more, their contact angle was about 98.02 ℃ as
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shown in Figure 1d, which describes that the coatings possess an excellent
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hydrophobic surface. The data above clearly indicates the MoS2/(PAA-AD/PEI-β-CD)
interfaces are then joined with each other and the host–guest interaction is
formed again. The self-healing process is thus completed. Figure 2a shows that
the width of the scar was 20 μm after scratching. Then, host-guest complexes were
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formed again when the scar interface was more closely contacted for 30 mins
with the evaporation of water. Finally, the scar healed successfully, recovering the
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initial coatings (Figure 2b). In order to further investigate the self-healing process of
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ITO substrate, as per the samples. In Figure 2c, their typical I−V curves of the
self-healing process showed the linear (ohmic) characteristics. The ohmic value of the
initial coatings was 48.9 Ω. Due to the ITO surface exposed to air after scratching, the
current obviously increased and the ohmic value was 40.2 Ω. However, the I−V curve
after the self-healing process was almost restored to the initial state and its ohmic
value was 49.5 Ω. This shows that the scar healed successfully and the
MoS2/(PAA-AD/PEI-β-CD) 15 coatings exhibited their admirable self-healing
capacity.
As shown in Figure 3a-c, the MoS2/(PAA-AD/PEI-β-CD) 15 coatings were able
to kill E.coli with more than 65.7% reduction in bacterial counts. Moreover, the
MoS2/(PAA-AD/PEI-β-CD) 15 coatings displayed the good biocompatibility in
Figure S2. [40] These indicate that MoS2 nanosheets had the antibacterial effect in the
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[41]
dark, which was in accordance with Na Wu’s results. The coatings displayed a
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mild direct cytotoxicity because of its excellent hydrophobic surface, [42-43] which
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shown in Figure 1d. MoS2 nanosheets had a larger surface area than bulk MoS2.
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Furthermore, MoS2 nanosheets could penetrate cell walls to damage the cell
membranes and increase the reactive oxygen species that reduces membrane stability.
[44-45]
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In order to further research, SEM was utilized to observe the E. coli morphology
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on the coatings’ surface (Figure S3). Some E. coli changed in structure (i.e., they
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shrunk) and their membranes appeared to be broken. These results were similar to the
observations reported for other nanomaterials. [41, 46-47]
As a result, without UV
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The h+, HO·, H2O2, and O2- were usually considered to be the reactive oxidative
[48]
species responsible for the bactericidal activity. Understanding which species
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played the most remarkable role was important in affecting the microbial environment.
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The related photocatalytic reactions about the MoS2 could be summarized by the
following: [49-50]
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MoS2/β-CD-PEI/AD-PAA coatings vastly improved their antibacterial property,
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which was able to reach 100% (Figure 4d). Because the MoS2 surface increased the
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more reactive oxygen species (h+, HO·, H2O2, and O2-) under UV light irradiation,
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particularly, the HO·, H2O2 and O2- would reduce membrane stability and damage the
membrane. Therefore, the MoS2/(PAA-AD/PEI-β-CD) 15 coatings have the
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completely antibacterial property under UV light irradiation. Taking into account its
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high antibacterial activity, the coatings are ideal for advanced pathogenic bacteria
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wastewater treatment and fresh storage of fresh fruits and vegetables.
To investigate the quenching ability of Co2+ towards the
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MoS2/(PAA-AD/PEI-β-CD) 15 coatings and acquire the best sensing for Co2+, the
Co2+ analysis is recorded by fluorescence spectrophotometer. In order to absorb more
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Co2+, the pH value and contact time were investigated. Recently, Shemirani et al.
have found that MoS2 nanosheets had the best adsorption capacity of Co2+ when they
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were immersed in the Co2+ solution (pH 8.0) for 20 mins. [35, 38]
Therefore, according
to the above conditions, the experiment exploring the hypothesis that the coatings
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could detect Co2+ by the fluorescence quenching method had been completed for the
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first time. The results were shown in Figure 5. By adding the different Co2+
concentration, the fluorescent intensity of the coatings exhibited a decreasing process
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as shown in Figure 5a. Co2+ ions were absorbed on the surface of the
MoS2/(PAA-AD/PEI-β-CD) 15 coatings to induce energy transition. The quenching
efficiency E was calculated according to the formula blow: [51-52]
F0 − F
E= × 100%
F0
where F0 and F were the fluorescence intensities in the absence and the presence
of Co2+. The ultimate quenching efficiency of the MoS2/(PAA-AD/PEI-β-CD) 15
coatings reached 77.4% when the final Co2+ concentration was 0.1 μg/mL. Along with
the increase of the Co2+ concentration from 0 to 0.1 μg/mL, a gradual reduction of the
fluorescence peak centered at 500 nm could be observed in Figure 5a. Figure 5b
shows the curve obtained with the fluorescence intensity versus the Co2+
concentration. A high correlation (R2 = 0.993) was achieved in the Co2+ concentration.
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The Co2+ sensing system demonstrated a limit of detection of 0.018 mg/mL and a
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dynamic range over 0 ~ 0.1 μg/mL. The results clearly demonstrate that the
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MoS2/(PAA-AD/PEI-β-CD) 15 coatings could be applied as a sensing platform for the
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detection of Co2+.
Moreover, the effect of the Co2+ concentration on the self-healing ability was
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investigated. These results found that the MoS2/(PAA-AD/PEI-β-CD) 15 coatings had
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good self-healing properties and recovered the original plain coatings in the different
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Co2+ concentration, as shown in Figure S4 (a, b,…f). It could be inferred that the
host-guest interaction between PEI-β-CD and AD-PAA improved the assembled
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ability to make the film more stable. According to the result shown in Figure S4, the
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In pathogenic bacteria wastewater, fruits and vegetables, Co2+ was the common
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coexistence of other heavy metals, such as Ca2+, Fe2+, Mg2+, Li+ and so on. In
our research, the MoS2/(PAA-AD/PEI-β-CD) 15 coatings were provided with
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could be found that the coatings exhibited so admirable self-healing capacity;
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meanwhile their antibacterial property was investigated. Under UV light irradiation,
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the self-healing coatings exhibited the superior antibacterial efficiency, which was due
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to the unique heterojunction in the MoS2 nanosheets. Their antibacterial properties
are able to reach 100%. Besides, the self-healing coatings first applied the
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fluorescence quenching for detecting the heavy metals. A Co2+ detection platform was
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established with a limit of 0.018 mg/mL and a dynamic range over 0 μg/mL to 0.1
μg/mL. This simple and easy approach to preparing the self-healing coatings with
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field of highly engineered materials, such as food packaging, for which safety,
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ACKNOWLEDGEMENTS
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support from 12th five-year national science and technology support plan corpus
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Southeast University. Prof. Dr. Ge also thanks for the support from Prof. Dr. Gu
Zhongze's group.
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Author biographies
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Liqin Ge
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Title: Pro.
Affiliation, Country: State Key Laboratory of Bioelectronics, School of Biological
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Science and Medical Engineering, Southeast University, Nanjing, P.R. China
Phone: +86-025-83795632 Fax: +86-025-83795632-809 E-mail: lqge@seu.edu.cn
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Prof. Ge is currently a professor in southeast university and mainly researches
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polymer and self-assembly functional materials. She graduated from Chinese
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Academy of Sciences Institute of Chemistry in 2003 year and received a doctorate
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that was the jointly training of the two institutes of Chinese Academy of Sciences and
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Germany Mapu collogen and interface. She went to McGill University in Canada for
postdoctoral research. Moreover, she has received the following projects:
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In recently years, prof. Ge has published many articles about the self-healing
multi-functional coatings in SCI journal.
[1] H. Y. Xuan, J. Y. Ren, X. Z. Wang, J.H. Zhang, L. Q. Ge. Flame-retardant, non-irritating and
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on intermolecular hydrogen bonding and metal–ligand coordination[J]. RSC Advances, 2016,
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6(92): 89757-89763.
[9] J. Y. Ren, H. Y. Xuan, Y. X. Zhu, X. F. Liu, L. Q. Ge. Beta-glucan quantification by
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fluorescence analysis using photonic crystals. RSC Adv, 2016, 6, 32286-322895.
[10] J. Y. Ren, H. Y. Xuan, C. H. Liu, C. Yao, Y. X. Zhu, X. F. Liu, L. Q. Ge. Graphene oxide
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hydrogel improved sensitivity in one-dimensional photonic crystals for detection of beta-glucan.
RSC Adv, 2015, 5, 77211-77216.
[11] J. Y. Ren, H. Y. Xuan, L. Q. Ge. Colorful self-healing polyelectrolyte nano-film based on
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Schiff base linkage capable of sensing. European Polymer Journal, 2017, 93, 521–529.
[12] Y. X. Zhu, C. Yao, J. Y. Ren, C. H. Liu, L. Q. Ge. Graphene improved electrochemical
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property in self-healing multilayer polyelectrolyte film [J]. Colloids and Surfaces A:
Physicochemical and Engineering Aspects, 2015, 465: 26-31.
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Figure 1. (a, b) SEM images of the MoS2 nanosheets coated on the
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(PAA-AD/PEI-β-CD) 15 coatings; (c) UV-vis absorption spectrum of the
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coatings via LbL self-assembly: (a, b) SEM ; c) I−V curves of the
MoS2/(PAA-AD/PEI-β-CD) 15 coatings during the self-healing process
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Figure 3. (a, b) Images of E.coli colonies on agar plates (a) the glass substrate (b)
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Figure 4. (a, b) Images of E.coli colonies on agar plates (a) the glass substrate (b)
the MoS2/(PAA-AD/PEI-β-CD) 15 coatings; (c) Photoluminescence spectra of the
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after the addition of 0 ~ 0.1 μg/mL Co2+ (pH 8.0); b) calibration curve achieved with
the fluorescence intensity versus the Co2+ concentration
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Figure 6. The effect of various metal ions on the self-healing coatings sensors
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fluorescence intensity shift. (0.1 μg/mL for Co2+ and 15 μg/mL for Ca2+, Fe2+,
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Mg2+, Li+)
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Scheme 1. Schematic of the
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preparation of the self-healing
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MoS2/β-CD-PEI/AD-PAA antibacterial coatings via LbL assembly, with dynamic
cross-linked formation generated based on guest–host complexation of β-CD
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and AD.
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