Direct nanoparticle coating using atmospheric plasma jet · 2020-06-01 · RESEARCH PAPER Direct nanoparticle coating using atmospheric plasma jet Mu Kyeom Mun & Yun Jong Jang & Dong

RESEARCH PAPER

Direct nanoparticle coating using atmospheric plasma jet

Mu Kyeom Mun & Yun Jong Jang & Dong Woo Kim &

Geun Young Yeom

Received: 27 January 2020 /Accepted: 26 April 2020# Springer Nature B.V. 2020

Abstract A new method that can simultaneously fabri-cate and deposit nanoparticles using an atmosphericpressure plasma has been investigated. To fabricateand deposit nanoparticles simultaneously on a materialsurface, a dielectric barrier-type plasma jet using noblegases such as He was used, and the material to bedeposited was used as the center power electrode forthe plasma jet. It is found that when Ag and Pd wereused as the center electrode of the pressure plasma jet,Ag and Pd nanoparticles with diameters 1–8 nm and 1–3 nm, respectively, could be successfully fabricated anddeposited onto the substrates without using any precur-sor, reducing agent, or dispersing agent. The textilesurface directly coated with Ag nanoparticles using theplasma jet also passed antibacterial, deodorization, andantifungal tests, similar to the textile coated with Agnanoparticles using conventional methods. The atmo-spheric pressure plasma jet method can be also used tofabricate and deposit nanoparticles from many different

materials simultaneously, in addition to Ag and Pd, in aneco-friendly and rapid manner.

Keywords Nanoparticles . Eco-friendly . Atmosphericpressure plasma . Silver . Palladium

Introduction

Among the nanomaterials available today, nanoparticlesare applied in various industries, such as health care andcatalysts, because of their specific properties and highsurface/volume ratios (Virkutyte and Varma 2011). Tofabricate nanoparticles, processes such as vacuum pro-cess and wet process are used (Park et al. 2007; Swihartet al. 2003). Owing to the high equipment and operatingcosts of vacuum processes such as sputtering and evap-orationmethods, most nanoparticles are fabricated usingwet processes, which are cheaper and more feasible formass production (Gromov et al. 2015; Mishra et al.2007). However, in the case of wet processing for thefabrication of nanoparticles, toxic materials such asprecursors, dispersing agents, reducing agents, and sol-vents are required, which generate byproducts duringnanoparticle fabrication, which need to be removed bytreatment, e.g., water treatment (Perelshtein et al. 2008;Le et al. 2010; Hassabo et al. 2015). Moreover, addi-tional dispersing agents and solvents could be requiredto coat the material surface, which could create addi-tional environmental problems in addition to thosecaused by the byproducts of nanoparticle fabrication(Zhang et al. 2008).

J Nanopart Res (2020) 22:136 https://doi.org/10.1007/s11051-020-04865-z

Electronic supplementary material The online version of thisarticle (https://doi.org/10.1007/s11051-020-04865-z) containssupplementary material, which is available to authorized users.

M. K. Mun :Y. J. Jang :D. W. Kim :G. Y. YeomSchool of Advanced Materials Science and Engineering,Sungkyunkwan University, Kyunggi-do, Suwon 16419, SouthKorea

G. Y. Yeom (*)SKKU Advanced Institute of Nanotechnology (SAINT),Sungkyunkwan University, Kyunggi-do, Suwon 16419, SouthKoreae-mail: [email protected]

To fabricate nanoparticles without using toxic agents,Osamu Takai, Nagahiro Satio et al. investigated a solu-tion plasma method which can reduce nanoparticles inthe solution without using a toxic reducing agent byexposing the electrodes to liquid plasmas (Nagahiroet al. 2009, Sung-Pyo et al. 2011, Kang et al. 2013,Mun et al. 2017a, b). Although this is moreenvironment-friendly method to produce nanoparticles,additional dispersing agents and solvents are still re-quired to coat the material surface. In addition, thenanoparticle surface can be made hydrophilic if thesolvent contains an OH group in the solution (Munet al., 2017a, b). In our study, nanoparticles were directlyfabricated by exposing materials as the power electrodeduring atmospheric pressure plasma generation, and thefabricated nanoparticles were coated onto the substratesurface without delay by exposing the plasma to thesubstrate.

In general, atmospheric pressure plasma jets (APPJs)have been investigated by researchers to generate UVusing inert gases such as He, N2, and Ar (Schneider et al.2011; Foest et al. 2007), and produce reactive radicalsfrom molecular gases added to inert gases (Foest et al.2007) as well as heat for power melting and coatingmaterials (i.e., plasma spray coating) (Niessen andGindrat 2011, Kumar et al. 2008). In particular, atmo-spheric pressure plasmas have been used for surfacetreatment of various materials at atmospheric pressurewithout using vacuum systems. It is essential for thesurface treatment of biomaterials and can be also usefulfor large-area, in-line, and roll-to-roll processing of var-ious material surfaces (Mun et al. 2016; Mun et al.2019). Because the purpose of plasma generation usingAPPJs is to generate UV and radicals dissociated frommolecules, and heat for melting powders injected fromthe outside, the power electrode is generally made ofthermally stable materials such as tungsten (W) to min-imize melting (Wan et al. 1999).

Particle generation during APPJ generation could beused to fabricate nanoparticles if the number of gener-ated particles is sufficient and the particle sizes arewithin a certain nanoscale range. In this study, nanosizedparticles from APPJs were fabricated using low-melting-point metallic electrodes such as silver (Ag)and palladium (Pd) instead of conventional W electrodeas power electrodes for the APPJ. The feasibility ofnanoparticle generation and direct coating onto the ma-terial surface using APPJ were investigated using He asthe plasma generation gas, which requires lower voltage

to generate plasmas compared with that required by Ar(Wang et al. 2003). The nanoparticle generation mech-anism and potential applications as nanoparticle coatingon textiles for antibacterial protection, etc., were studied(Hajipour et al. 2012; El-Shishtawy et al. 2011).

Experimental

Atmospheric pressure plasma jet (APPJ) module

Figure 1 shows the dielectric barrier discharge (DBD)-type APPJ module used for the fabrication and deposi-tion of Ag nanoparticles onto various substrates.Figure 1(a) shows the assembled DBD-type APPJ mod-ule, Fig. 1(b) shows the cross section of the jet module,and Fig. 1(c) shows the roll-type coating of the APPJ ontextile. Ceramic tubing with inner diameter of 2 mm andthickness of 1.5 mmwas used as the dielectric barrier; asthe electrodes, 0.5 mm diameter Ag wire (Nilaco, AG-401385, 99.95%) or 0.5 mm diameter Pd wire (Nilaco,PD-341385, 99.95%) was located at the center of theceramic tube as the power electrode, and the outside ofthe ceramic tube was helically wound with a 0.5 mm-thick W wire (Nilaco, W-461387, 99.95%) as theground electrode. As protection from potential arcingand plasma generation on the outside of the ceramictubing, ceramic wings were installed on both the topand bottom sides of the ceramic tube. To generate theplasma, 60 kHz of pulsed AC voltage was applied to thepower electrode wire while flowing 1 slm of He gas atthe center of the ceramic tube.

Nanoparticle coating

Ag nanoparticles fabricated by APPJ were coated ontosilicon wafers and textile (Greencotage, blackout tex-tile), whereas Pd nanoparticles were coated onto anAl2O3 plate (LabCeramic, ALO, 99.8%). We coatedthe Ag nanoparticles onto the textile for antibacterialtesting using a roll-to-roll system, as shown in Fig. 1(c).Ag and Pd nanoparticles were coated onto the siliconwafer and Al2O3 plate (because Pd nanoparticles aregenerally coated onto Al2O3 for catalysis (Cargnelloet al. 2012, Heemeier et al. 2002, Valden et al. 1996,Matam et al. 2012) and their coating status was ob-served. Ag and Pd nanoparticles were also coated ontotransmission electron microscopy (TEM) grids (TED

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PELLA INC, 01824 400 mesh Cu) for particle sizemeasurement.

To observe the shape, size, and chemical compositionof Ag and Pd nanoparticles deposited onto substrates bythe DBD-type APPJ module, the AC voltage applied tothe module was varied while locating the substrates(silicon wafers for Ag and Al2O3 plate for Pd) 2 mmabove the module. The nanoparticles were depositedonto the substrates for 1 min while varying 60 kHz ofpulsed AC power from 4 to 6 kV (0 to the peak voltage)with 1 slm of He (the power was operated by a pulsedvoltage mode and the current/dissipated power were notknown). For TEM grids, Ag and Pd nanoparticles werecoated for 5 s under the same conditions.

Analysis and measurements

The shapes of the Ag and Pd nanoparticles fabricated byAPPJ and coated onto the silicon and Al2O3 substrates,respectively, were observed using a field emission scan-ning electron microscope (FE-SEM, Hitachi, S-4700).The chemical composition of the nanoparticles coatedonto the substrates was measured using X-ray photo-electron spectroscopy (XPS, thermo VG SIGMAPROBE). The size of nanoparticles was measured byhigh-resolution TEM (HR-TEM, JEM-2100F). To mea-sure the functionality of Ag nanoparticles coated ontothe textile using the DBD-type APPJ module, antibac-terial activity test, antifungal test, and deodorization ratetest were carried out using the textile coated with Agnanoparticles. For the antibacterial activity test, KS K0693 (2016 Korean standards) was used (Son et al.2007). For the antibacterial activity test, Staphylococcusaureus (ATCC6538) with initial concentration of 3.3 ×105 CFU/ml and Klebsiella pneumoniae (ATCC4352)with initial concentration of 2.9 × 105 CFU/ml wereused (Oh et al. 2006). The antifungal test was carried

out using the method approved by the American Asso-ciation of Textile Chemists and Colorists (AATCC30)with Aspergillus niger (ATCC6275) (Usha et al. 2010).For the deodorization rate test, the KS I 2218 methodwas used, which measures the deodorization rate withacetic acid using a detector tube-type gas measuringinstrument (Moon et al. 2014).

Results and discussion

To observe the nanoparticles deposited directly onto thesubstrates after fabrication by APPJ, Ag and Pd nano-particles deposited on the silicon substrates and Al2O3

substrates, respectively, were observed using SEM; theresults are shown in Figs. 2b–d for Ag nanoparticles onsilicon substrates, and Fig. 2f–h for Pd nanoparticles onAl2O3 substrates. The deposition was carried out using60 kHz AC voltage from 4 to 6 kV to the Ag (Pd)electrode for 1 min while flowing 1 slm of He. Asshown in Fig. 2, after exposure to APPJ, nanoparticlesdeposited onto the substrates could be observed. As thevoltage to the Ag and Pd increased, the number ofparticles also increased for both silicon substrates forAg nanoparticles and Al2O3 substrates for Pdnanoparticles.

To investigate whether the nanoparticles depositedonto the substrates are Ag and Pd nanoparticles, thecomposition of materials on the silicon and Al2O3 sur-faces deposited at different AC voltages were observedusing XPS; the results are shown in Fig. 3. The figureshows that after exposure to APPJ, the peaks related toAg and Pd were observed on the substrates. Increaseddeposition voltage increased the XPS peak intensities onthe substrate surfaces for both Ag and Pd, indicating theincreased surface coverage of nanoparticles (Brun et al.1999; Sharma et al. 2018). In the case of Ag, Ag peaks at

Fig. 1 DBD-type APPJ moduleused for the deposition of Agnanoparticles onto the substrates:(a) the assembled DBD-typeAPPJ module, (b) cross-section ofthe jet module, and (c) roll-to-rolltype coating of the APPJ ontextile

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368.3 eV (Ag 3d5/) and 374.2 eV (Ag 3d3/2) wereobserved. In the case of Pd, peak positions at 336.6 eV(Pd 3d5/2, 335.4 eV) and 341.6 eV (Pd 3d3/2, 340.9 eV)were observed (Voogt et al. 1996). (In fact, Ag and Pdparticles could be partially oxidized during the deposi-tion and, for oxidized Ag, Ag2O 3d5/2 is observed at367.9 eVand, for oxidized Pd, PdO 3d5/2 is observed at367.9 eV. From more peak shift to a higher bindingenergy for Pd compared to Ag, it appears that Pd ispartially oxidized more compared to Ag. In fact, Pd ismore easily oxidized under atmospheric condition andthese Pd particles are used as catalyst for the decompo-sition of toxic gases such as NOx, and are reduced as Pdunder high temperature conditions, such as inside anautomobile engine (Álvarez-Galván et al. 2004.) Whenthe surface percentage after 60s deposition was

measured, as shown in Figs. 3(a) and (b), Ag nanopar-ticle surface coverage percentage increased from 4.6%for 4 kV to 11.5% for 6 kV on silicon substrate; Pdnanoparticle surface coverage percentage increasedfrom 1.2% for 4 kV to 7.8% for 6 kV, respectively.(Even though the XPS provides atomic concentrationof the elements on the surface within a few nanometer inthickness, because the deposited atoms do not react withsubstrate and the size of the deposited atoms is largerthan a few nanometer, the XPS composition of thedeposited atoms was used as the surface coverage per-centage of the deposited materials on the substrate.)

For the measurement of nanoparticle size distribu-tion, the Ag and Pd nanoparticles were observed usingTEM after deposition onto TEM Cu grids for 5 s usingAC voltage from 4 to 6 kV. Figures 4 (a)–(c) and (d)–(f)

Fig. 2 SEM images of Agnanoparticles coated onto siliconwafers by He APPJ with Agelectrode at the different ACvoltages: (a) as-is, (b) 4 kV, (c)5 kV, and (d) 6 kV; and those ofPd nanoparticles coated on Al2O3

substrates: (d) as-is, (e) 4 kV, (f)5 kV, and (g) 6 kV. The nanopar-ticles were coated on the substratewith He 1 slm for 1 min

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Fig. 3 XPS narrow scan data of (a) Ag on the silicon surfaces and (b) Pd on Al2O3 surfaces deposited at different AC voltages. Surfacepercentages of Ag and Pd on the substrates for different AC voltages are also shown

Fig. 4 TEM images of Ag nanoparticles and Pd nanoparticles on TEM Cu grids deposited for 5 s with different AC voltages: (a) 4 kV, (b)5 kV, (c) 6 kV for Ag nanoparticles; and (d) 4 kV, (e) 5 kV, (f) 6 kV for Pd nanoparticles

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show the TEM images for Ag and Pd nanoparticles,respectively, with different AC voltages of 4, 5, and6 kV. As shown in Fig. 4, in addition to the increasednanoparticle surface coverage, the increase in the ACvoltage of APPJ increased the size of both Ag and Pdnanoparticles. The size distributions of Ag and Pd nano-particles observed by TEM were measured, as shown inFigs. 5(a), (b), and (c) for 4, 5, and 6 kV, respectively. Asshown in Fig. 5, for Pd nanoparticles, 70% of particleswere in the range 0–1 nm for 4 kV; at 6 kV, the particlesize in the range 0–1 nm decreased to 50% with theincrease of particle size. However, the size of Pd nano-particles was generally in the range 0–3 nm; Pd nano-particles larger than 3 nm were not observed. Similartrends were observed for Ag nanoparticles; however, theaverage nanoparticle size was much larger comparedwith Pd nanoparticles for the same AC voltage, asshown by the peak particle distribution at 2–3 nm for4 kV and 4–5 nm for 6 kV. Finally, using energy-dispersive X-ray spectroscopy (EDS) in HR-TEM, theparticle composition was observed and the results areshown in Fig. S1 for both Ag and Pd nanoparticlesdeposited at 6 kV. Ag and Pd are color red in EDSand, as shown in Fig. S1, only particles in TEM wereidentified as Ag or Pd.

To further investigate the nanoparticle formationmechanism in APPJ, the surfaces of APPJ Ag and Pdelectrodes operated at different AC voltages wereobserved by SEM; the results are shown in Figs. 6(a)–(d) for Ag and (e)–(h) for Pd. The surfaces of Agand Pd electrodes were observed after operating theAPPJ under the same conditions in Fig. 2 for 1 min.As shown in Fig. 6, the surfaces of Ag and Pdelectrodes became rough after plasma generation.The increase in AC voltage to the electrodes in-creased the surface roughness. The use of Pd insteadof Ag at the same AC voltage decreased the surfaceroughness. The change in surface roughness for dif-ferent AC voltage and electrode materials is attribut-ed to the lower local melting of the electrode surfaceduring APPJ operation using He. (The melting tem-peratures of bulk Ag and Pd are 1235 K and 1828 K,respectively; and melting temperatures of 10 nm Agnanoparticles and Pd nanoparticles are ~760 K and ~873 K, respectively (Little et al. 2012, Lai et al.2008).) The increase in nanoparticle size and densitywith increasing AC voltage of APPJ, and the differ-ences in nanoparticle size and density between Agand Pd during the nanoparticle deposition with APPJ

at the same AC voltage shown in Figs. 2 and 5 arealso believed to be related to the differences in localmelting of Ag and Pd electrodes. It is believed thatthe nanoparticles are formed by the melting of theelectrode surface by local melting sources such asstreamers in the plasma during APPJ operation eventhough the streamers could not be visually identifiedunder the experimental conditions (Fig. S2).

Finally, to investigate the potential application ofnanoparticles directly deposited by APPJ onto vari-ous areas, Ag nanoparticles were directly coated onthe textile by He APPJ. The effects of Ag nanoparti-cles on antibacterial, deodorization, antifungal prop-erties were investigated, and the results are shown inFig. S3. Ag nanoparticles were coated on the textileusing He APPJ at 6 kVand speed of 125.6 cm/min bya roll-to-roll system. Figures 7(a)–(d) show the textilesurfaces (a) before and after coating with Ag nano-particles for (b) two times, (c) four times, and (d) sixtimes. As shown in the figure, with the increase incoating times, increased Ag nanoparticles on thetextile surface could be observed. Using XPS, thesurface percentage of Ag on the textile for differentnumber of coatings was measured and, as shown inFig. 7(e), ~0.87% was observed on the surface afterthe six times coating. After the coating for six times,the effect of the Ag nanoparticle coating on the textilewas investigated by carrying out the deodorizationrate and antibacterial tests; the results are shown inFigs. 7(f) and Table 1, respectively. As shown in Fig.7(f), the textile coated with Ag nanoparticles(AgNPs) showed higher deodorization rate, that is,30% higher deodorization percentage compared withthat without Ag nanoparticles (blank) after 120 min.In the antibacterial test, as shown in Table 1, theAgNPs showed 99.9% removal percentage of bacte-ria such as Staphylococcus aureu and Klebsiellapneumonia, and 0% removal percentage for the blankafter 18 h. The antifungal test was also carried outand showed that the AgNPs had no fungal growthwhile the blank had significant fungal growth (Fig.S3). These results suggest that the nanoparticles fab-ricated by the APPJ module and directly coated ontothe material surface can be applied to various indus-tries that use nanoparticle coatings. Moreover, it isbelieved that using this method, nanoparticles forother metallic materials with low melting tempera-tures can be fabricated and directly coated onto thematerial surface.

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Fig. 5 Size distribution of the Agnanoparticles (red) and Pd nano-particles (black) observed byTEM in Fig. 4: (a) 4 kV, (b) 5 kV,and (c) 6 kVof AC voltage

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Conclusion

In this study, a new method that can directly fabricateand apply nanoparticles as coating onto substratesusing a He APPJ module was investigated using Agand Pd nanoparticles. It was found that the size anddensity of nanoparticles coated onto the substrateincreased with the increase in AC voltage to theelectrode used for nanoparticle formation. For thesame AC voltage, the size distribution of Pd nano-particles was lower than that of Ag nanoparticleswith particle sizes in the range of 0–3 nm and 1–8 nm for Pd and Ag, respectively. The size distribu-tion and coverage of nanoparticles on the substrate

surface were related to the local melting of the elec-trode surface. Higher AC voltage and lower meltingtemperature of the electrode material resulted in larg-er size distribution and higher surface coverage ofnanomaterials on the substrate. The textile coatedwith Ag nanoparticles showed 30% higher deodori-zation percentage after 120 min compared with thetextile without coating. The antifungal test alsoshowed 99.9% bacterial removal percentage and nofungus growth after 18 h. It is believed that variousnanoparticles with low melting point materials can beeasily fabricated and coated by the He APPJ modulefor applications in various industries that use nano-particle coatings.

Fig. 6 SEM images on thesurfaces of APPJ Ag and Pdelectrodes operated at differentAC voltages. For Ag electrodes:(a) as-is, (b) 4 kV, (c) 5 kV, and (d)6 kV); for Pd electrodes: (e) as-is,(f) 4 kV, (g) 5 kV, and (h) 6 kV.The surfaces of Ag and Pd elec-trodes were observed after theoperation of the APPJ under thesame conditions as in Fig. 2 for1 min

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Fig. 7 Textile surfaces before (a)and after the coating with Agnanoparticles for (b) two times,(c) four times, and (d) six times.(e) Surface percentage of Ag onthe textile for different number ofcoatings, Effect of Ag nanoparti-cle coating (coating six times) tothe textile on (f) the deodorizationrate

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Acknowledgements This work was supported by the NationalResearch Foundation of Korea (NRF) grant funded by the Koreagovernment (MSIT) (2018R1A2A3074950).

Compliance with ethical standards

Conflict of interest There are no conflicts to declare

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Test bacteria Sample Start CFU/ml After 18 h Removal Rate (%)

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Ag NPs ND 99.9

Klebsiella pneumonia Blank 2.9 X 105 2.2 X 108 0.0

Ag NPs ND 99.9

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