Research Article A Study on Toxic Acidic Vapor Removal ...Research Article A Study on Toxic Acidic Vapor Removal Behaviors of Continuously Nanostructured Copper/Nickel-Coated Nanoporous

Research ArticleA Study on Toxic Acidic Vapor Removal Behaviors ofContinuously Nanostructured Copper/Nickel-CoatedNanoporous Carbons

Byung-Joo Kim,1 Kyong-Min Bae,2 Hye-Min Lee,1 Shin-Jae Kang,1 and Soo-Jin Park2

1R&D Division, Korea Institute of Carbon Convergence Technology, Jeonju 561-844, Republic of Korea2Department of Chemistry, Inha University, Incheon 402-751, Republic of Korea

Correspondence should be addressed to Byung-Joo Kim; [email protected] and Soo-Jin Park; [email protected]

Received 31 May 2015; Accepted 13 August 2015

Academic Editor: Nguyen V. Long

Copyright © 2015 Byung-Joo Kim et al.This is an open access article distributed under the Creative Commons Attribution License,which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

Nanostructured copper (Cu)/nickel- (Ni-) coated nanoporous carbon sheets (NCS) were prepared to improve the toxic acidicvapor (hydrogen chloride, HCl) removal efficiency of NCS using a continuous bimetal electroplating method at various metalcontent ratios. The surface morphology and nanostructure of Cu/Ni-NCS were observed by scanning electron microscopy andX-ray diffraction, respectively. N

2/77 K adsorption isotherms were investigated using the Brunauer-Emmett-Teller equation. HCl

vapor removal efficiency was confirmed using two types of detection techniques: a gas detecting tube for low concentrations andgas chromatography for high concentrations. HCl removal efficiency was improved mainly in the copresence of nanostructuredCu/Ni clusters compared to the efficiencies of the as-received and single-metal-plated NCS. In particular, the removal efficiencyof Cu/Ni-3 was increased by 270% compared to that of as-received sample, but Cu/Ni-5 showed lower efficiency than Cu/Ni-3,indicating that suitable metal composition on NCS can accelerate HCl removal behaviors of the NCS.

1. Introduction

Hydrogen chloride (HCl) vapor is a by-product of variousincineration processes and a serious contributor to atmo-spheric pollution, such as smog and acid rain. HCl vapor iseasily changed to liquidHCl acid, which is very toxic, erodingmetals, inducing cancer, and acting as a precursor to dioxinin the burning of garbage (EPA’s permissible exposure limitvalue is 4.7 ppm). Therefore, there has been a strong push toremove HCl vapor from domestic and industrial combustionprocesses [1].

Nanoporous carbon sheets (NCS) are promising materialfor the removal of gas-phase pollutants [2–9], such as nitricoxides (NO

𝑥) [3, 5], sulfuric oxides (SO

𝑥) [1, 6, 8, 10], carbon

dioxide (CO2), and even HCl [1, 9–12] vapor. Normally, the

surface of neat NCS does not have strong functional groupsor catalytic active sites due to their origin. Basically, thegas-phase pollutant removal efficiency of the NCS at roomtemperature is proportional to their specific surface area andmicropore volume. The removal efficiency can be enhanced

dramatically for several pollutants by adding a small contentof active materials, such as functional groups or metal saltson the NCS [1, 2, 10–13].

This is why many researchers examine the surface modi-fication or metal salt impregnation methods on PCs [14–17].

As one of the metal-doping methods onto carbon sur-faces, electrolytic metal plating, such as copper, nickel, andsilver, of nonconducting porous carbonaceous materials hasbeen studied using a conductive-support-assistance method,such as metallic meshes [13, 16].

In a previous study [4, 13], copper (Cu), silver (Ag),and nickel (Ni) nanoparticles on carbon were found tobe so effective in HCl removal because they immediatelyformed CuCl

2, AgCl, and NiCl

2, respectively, without any

side reactions when they came in contact with HCl vapor.Several singlemetals plated by electrometal plating have beenstudied with regard to their efficacy for HCl removal. On theother hand, the effects of bimetallic cluster catalysts on HClremoval have not been reported.

Hindawi Publishing CorporationJournal of NanomaterialsVolume 2015, Article ID 546720, 7 pageshttp://dx.doi.org/10.1155/2015/546720

2 Journal of Nanomaterials

Graphite bar (no charge)

Copper salt electrolyte

Nickel salt electrolyte

Washing water

Washing water

Air dryingNanoporous carbon sheets

Nickel plate (+)Copper plate (+)

Nickel bar (−)Copper bar (−)

Figure 1: Continuous-type multimetal electroplating process on the nanoporous carbon sheets.

This paper reports the effects of bimetallic catalystscomposed of Cu and Ni clusters on porous carbon sheetsin the removal of HCl vapor. Bimetallic catalysts were pre-pared using a continuous metal electroplating technique fornonconducting carbonaceous materials at different currentdensities.

2. Experiments

2.1. Materials and Methods. The NCS used in this study arenonwoven type sheets (specific surface area is 1350m2/g andthickness is 3mm) supplied by Korea ACF Co. Prior to use,the impurities in the PCswere removed via Soxhlet extractionby boiling with acetone at 80∘C for 2 h. The PCs were thenwashed several times with distilled water and dried in avacuum oven at 120∘C for 12 h.

For the electroplating of copper (Cu) and nickel (Ni)metals, the NCS were electroplated continuously using ahome-made device, as shown in Figure 1. Prior to platingthe NCS, each sample was immersed in 10wt.% HNO

3for

5min at room temperature in order to remove the impuritieson the carbon surfaces and rinsed with distilled water. Thepurified NCS were activated in an aqueous solution of 0.38MK2Cr2O7/4.5M H

2SO4and refluxed in a water bath and

maintained at 60∘C for 2 h to enhance the interfacial adhesionbetween the nickel particles and the NCS surfaces. Anelectroplating device that can plate nanostructured metallicCu and Ni continuously onto the NCS surfaces was con-structed.Themetal plating rate was controlled by the currentdensity with a fixed collecting speed of 0.1m/min [4, 13]. Amechanical sample collecting winder which can collect thesample sheet with fixed tension is placed at the right end.In order to avoid excessive tension load on the sample sheet,each bar (graphite and metals) is free to rotate.

Table 1 lists the formulation of the Cu and Ni electroplat-ing bath and operation conditions [16, 18]. Cu and Ni sulfateswere the main salts used in the electroplating solution, andCu and Ni plates were used as the anode. The Cu and Nimesh rolls were used as the cathode. The NCS were closelyattached to the rolls to enhance the electric conductivity ofthe sheets, resulting in good Cu and Ni electroplating onthe NCS. The current densities were fixed to 30A/m2 for

Table 1: Formulation of the copper and nickel electroplating bathand operation conditions.

Cu plating Ni plating

CompositionCuSO

4⋅5H2O 10 g/L NiSO

4⋅6H2O 280 g/L

H2SO420mL/L NiCl

2⋅6H2O 40 g/L

H3BO330 g/L

pH 3.0∼3.5 4.5∼5.0Temperature (∘C) 25 45Current density (A/m2) 30 10∼50

Cu plating and were in the range of 10 to 50A/m2 for Niplating.The samples were namedCu/Ni-1 (10 A/m2), Cu/Ni-2(20A/m2), Cu/Ni-3 (30A/m2), and Cu/Ni-5 (50A/m2) withthe current densities for Ni plating. pH was controlled bydiluted sulfuric acid solution with automatic pH meter. Thetemperature was controlled by heating coils placed underplating baths. The current density of each plating batchwas controlled by a power supply which can give fixedelectric current. The metal content was measured by atomicabsorption spectrophotometry (AAS).

2.2. Surface Nanostructures and Morphologies. To examinethe change in the nanostructures of the metal-coated NCS,X-ray diffraction (XRD, Rigaku Model D/MAX-III B) wascarried out using a rotation anode with CuK𝛼 radiation.

Scanning electron microscopy (SEM, JEOL JSM-840A)was used to observe the surface morphology of the Cu/Ni-coated NCS as well as the distribution of metal particlesbefore and after HCl vapor removal tests. Energy-dispersiveX-ray spectrometry (EDS, LINK system AN-10000/85S) wasused to observe the formation of metal chlorides after HClvapor removal tests.

The nitrogen (N2) adsorption isotherms at 77K were

measured using BELSORP-max (BEL Japan). Prior to anal-ysis, the samples were degassed at 573K for 9 h to obtaina residual pressure of

Journal of Nanomaterials 3

0

3

6

9

12

15

62%

38%72%

Cu/Ni-5Cu/Ni-3Cu/Ni-2

Met

al q

uant

ifica

tion

(wt.%

)

Nickel

Cu/Ni-1

28%

60%

40%

51%

49%0.99

1.13

2.56

Copper (3.7wt.%)

Figure 2: Metal quantification of Cu/Ni-coated nanoporous carbonsheets as a function of current densities.

2.3. HCl Vapor Removal Tests. Two types of detecting meth-ods were used as a highly accurate HCl removal test. A gasdetection tube techniquewas employed at low concentrations(30 ppm) [3, 10, 14].

A gas detecting tube (GASTECNo.; 14L, range 1–40 ppm)was used to measure HCl vapor removal efficiency. BeforeHCl removal experiment, all samples and the reactor werepurged with high purity N

2gas (99.9%) at room temperature

for 1 h to remove the residual moisture. Approximately 0.1 gof the samples was packed with a cylindrical quartz tube andHCl vapor with a concentration of 1013 ppm and N

2balance

was injected at 298K. The gas flow rate was maintained at50mL/min using a mass flow controller. HCl vapor removalefficiency was determined from HCl concentration at theoutlet reactor.

A gas chromatograph (DS 6200 model, Donam Co.,Korea) with a thermal conductivity detector was used. Thesamples (0.1 g of each sample) were packed into a cylindricalquartz tube and HCl vapor (1013 ppm of N

2balance) was

injected. The gas-feeding rate was maintained at 50mL/minusing a mass flow controller. HCl vapor removal efficiencywas determined fromHCl concentration at the outlet reactor.Before each analysis, HCl vapor adsorption curves weregained by using 300, 600, and 1000 ppm HCl standard gas.

3. Results and Discussion

3.1. Cu/Ni Bimetal Plating. Figure 2 shows the metal contentobtained from the AAS results for the Cu/Ni-coated NCS(Cu content was fixed at 3.7 wt.%). Ni content on the NCSsurfaces increased steadily to 6.12 wt.% with increasing cur-rent density. The specific content ratio of Ni in the bimetalliccluster increased from 28% at Cu/Ni-1 to 62% at Cu/Ni-5.Cu/Ni-3 showed a similar content ratio of both metals. Asmentioned above, the collecting speed for metal plating inthe continuous electroplating process was fixed. Therefore,

Nanoporous carbon sheets Copper nanoparticles Nickel nanoparticles

(a) (b) (c)

Figure 3: A schematic of metal deposition mechanism onnanoporous carbon sheets. (a) Initial plating state. (b) Mediumplating state. (c) Final plating state.

10 20 30 40 50 60

As-received

Cu/Ni-1

Cu/Ni-3

Cu/Ni-5Ni(200)Cu(200)

Ni(111)Cu(111)

2𝜃 (deg)

Figure 4: XRD spectra of Cu/Ni-coated nanoporous carbon sheetsas a function of current densities.

Ni plating rate is obviously dependent on the input currentdensity. Ni content of Cu/Ni-2 was 0.99wt.% higher thanthat of Cu/Ni-1. Ni content of Cu/Ni-3 was 1.12 wt.% higherthan that of Cu/Ni-2. A similar behavior was also observed atCu/Ni-5 (1.28 wt.% per 10A/m2). This increase suggests thatthe increase in Ni content enhances the specific conductivityof the metal-coated NCS, resulting in an acceleration of themetal plating rate.

Figure 3 exhibits the mechanism of metal deposition oncarbon surfaces. In the initial plating state, newly coatednickel nanoparticles are placed separately or near coppernanoparticles due to the highermetal-metal interactionwhencompared to carbon-metal interaction. In the medium state,nickel nanoparticles make clusters with copper nanoparticlesbecause metal-metal interaction is much higher than metal-carbon interaction. This sate can be seen Ni/Cu copresencestate. In the final state, rich nickel nanoparticles mainlycover the surfaces of copper nanoparticles, so that effectiveremoval behaviors by Ni/Cu copresence can be diminished.This schematic can have good correlation with XRD data.

3.2. Surface Morphology and Nanostructure. Figure 4 showsthe XRD patterns of the Cu/Ni-coated NCS. Cu peaks wereobserved at 43∘ 2𝜃 (111) and 49∘ 2𝜃 (200), and Ni peaks


(a) (b)

(c)

Ni

Ni

Cu

C

ClCu

0

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

10.00

11.00

12.00

13.00

14.00

(d)

Figure 5: SEM images and EDS result of Cu/Ni-coated nanoporous carbon sheets before and after HCl removal test. (a) As-received porouscarbon. (b) SEM image of Cu/Ni-3 before HCl test. (c) SEM image of Cu/Ni-3 after HCl test. (d) EDS result of Cu/Ni-3 after HCl test.

were observed at 44∘ 2𝜃 (111) and 51∘ 2𝜃 (200). The intensityof Cu peaks was almost regular due to the fixed currentdensity under the plating condition.Ni peaks at 44∘ and 51∘ 2𝜃increased proportionally with increasing current density forNi plating, indicating that the content of Ni in Cu/Ni clustershad increased steadily. These results show good agreementwith Figures 2 and 3.

The crystalline size of Cu andNi particles on theNCSwascalculated as a function of the coating time from the XRDresults using Scherrer equation [20]:

𝐿

𝑐=

𝐾𝜆

𝛽 cos 𝜃, (1)

where 𝐿𝑐is the crystalline size (nm), 𝐾 is the Scherrer con-

stant (=0.9), 𝜆 is the X-ray wave length (CuK𝛼 = 0.154 nm), 𝜃is the Bragg angle, and 𝛽 is full width at half max.

Table 2 shows XRD results and crystal size of Cu(111) andNi(111) with Ni content. It was found that Cu nanoparticlesshowed very uniform size of 10.5 nm at each sample. How-ever, the crystal size of Ni(111) was decreased with currentdensity, indicating that surface resistivity of Cu-precoatedNCS affected Ni deposition. In our previous work [16], highcurrent density formetal plating can cause finemetal particlesdue to the change of surface resistivity.

SEM analysis was used to observe the morphology ofCu/Ni clusters introduced on the NCS before and after HCl

Table 2: XRD results and metal crystal size (𝐿𝑐) of Cu/Ni-plated

nanoporous carbon sheets as a function of the Ni content.

Samples Brag angle (𝜃) 𝑑(111)

(Å) FWHM 𝐿𝑐(nm)

Cu(111)Cu/Ni-1 21.64 2.09 0.80 10.7Cu/Ni-3 21.64 2.09 0.81 10.6Cu/Ni-5 21.64 2.09 0.81 10.6

Ni(111)Cu/Ni-1 22.10 2.05 — —Cu/Ni-3 22.11 2.05 0.80 10.7Cu/Ni-5 22.11 2.05 0.98 8.8

removal tests (Figure 5). The nickel particles grew graduallyand formed island-like metallic clusters that were well coatedover the surface, as shown in Figure 5(b), whereas the surfaceof the as-received NCS was quite clean.

Figures 5(c) and 5(d) show SEM image and EDS resultof Cu/Ni-3 sample after HCl test, respectively. The size ofCu/Ni clusters increased afterHCl removal.This suggests thatCu/Ni clusters reacted chemically with HCl vapor and mightform metal chlorides. Figure 5(d) can be obvious evidencefor the formation of metal chlorides after HCl removaltest. As shown in Figure 5(d), Cu, Ni, and Cl atoms were


0 20 40 60 80

10

100

1000

K2

K3

As-receivedCu/Ni-1Cu/Ni-2

Cu/Ni-3Cu/Ni-5

Out

let c

once

ntra

tion

(ppm

)

Reaction time (min)

K1

Figure 6: HCl removal results of Cu/Ni-coated nanoporous carbonsheets as a function of current densities at 298K/100 kPa (EPA’spermissible exposure limit value: 4.7 ppm).

observed together, meaning that Cu𝑥Cl𝑦and Ni

𝑥Cl𝑦were

newly formed by a reaction with HCl vapor [4, 13, 17].

3.3. Hydrogen Chloride Vapor Removal. Figure 6 shows HClvapor removal efficiency of Cu/Ni-coated NCS. The as-received NCS showed good HCl removal efficiency for aremoval time up to 20min and then HCl concentration atthe outlet reactor increased rapidly. This suggests that HClremoval behavior of the as-received NCS occurred mainlyvia physisorption mechanism due to the sharp breakthroughcurve (K1). On the other hand, the gradient between 25 and35min (K3) decreased slightly, meaning that a mild chemicalreaction could have occurred by the PCs themselves.

In the case of Cu/Ni-coated NCS, all Cu/Ni samplesshowed a significantly higher HCl removal efficiency thanthe as-received NCS, and the total removal time (up tobreakthrough concentration) was proportional to the metalcontent. On the other hand, the removal efficiency of Cu/Ni-5 sample was lower. This can be explained by the fact thatexcessive metal plating of over Ni 6.1 wt.% (total 9.8 wt.%)can cause a decrease in HCl removal efficiency because of thesevere pore filling behavior.

Interestingly, the gradient of the removal efficiency curvesfor Cu/Ni-2,3,5 has “K2” region, and the “K3” gradient issignificantly lower than that of the as-received and Cu/Ni-1 PCs, even though the “K1” gradient was almost the samein all samples in this work. These results clearly mean thatCu/Ni introduction enhanced the physisorption capacity ofthe samples dramatically, and the chemisorption capacity alsoincreased. Moreover, the patterns of the removal efficiencycurve between Cu/Ni-3 and 5 were quite similar, indicatingthat the chemisorption behaviors of the two samples weresimilar, but the excessive metal content of Cu/Ni-5 caused adecrease in the physisorption capacity of the PCs.

Specific surface areaBreakthrough time

0800

900

1000

1100

1200

1300

1400

Cu/Ni-1 Cu/Ni-2 Cu/Ni-3 Cu/Ni-5As-received020

30

40

50

60

70

Brea

kthr

ough

tim

e (m

in)

Spec

ific s

urfa

ce ar

ea (m

2/g

)

Figure 7: Specific surface area and breakthrough time for HClremoval of Cu/Ni-coated nanoporous carbon sheets as a functionof current densities.

Figure 7 shows the relationship between the specificsurface area and breakthrough time of the samples. Thespecific surface area of all Cu/Ni samples ranged from 900to 1,000m2/g (10% margin of error). On the other hand, thebreakthrough time increased by 250% at Cu/Ni-3 comparedto the as-received NCS. This suggests that the physisorptioncapacity of theNCS is controlled not only by the large specificsurface area but also by the removal effects of themetal clusterloading [21–25].

To observe the effect of the total metal content on HClremoval capacity, single Cu or Ni-coated samples with asimilar total metal content of Cu/Ni-3 and -5 were prepared,and their HCl removal results are listed in Table 3. The singleCu or Ni-plated NCS showedmuch lower breakthrough timeat a similar total metal content than that of Cu/Ni-3 sample.This suggests that the copresence of Cu/Ni on the NCS caneffectively improve HCl vapor removal ability. It is probablydue to the synergetic effects on HCl dissociation by thepresence of bimetal particles on NCS surfaces.

In order to confirm reusability of Cu/Ni/PCs, the sameHCl removal tests were repeated five times, and results wereshown in Table 4. Before the reusability tests, all sampleswere degassed for 4 h at 120∘C. It was found that as-receivedsample showed almost constant breakthrough time.However,the breakthrough time of Cu/Ni-3 decreased rapidly andthen showed stable state after 3rd repeating tests. This resultindicates that the as-received sample removesHCl gasmainlyby physisorptionmechanism, butCu/Ni-3 hasmixed removalmechanisms, such as physisorption/chemisorption.

4. Conclusions

Cu/Ni-coated NCS with various content ratios were preparedusing a continuous electroplating technique as a functionof the inputted current densities. Ni content increased withincreasing current density, and HCl removal capacity was inproportion to Ni content up to Cu/Ni-3 sample. HCl removalbehavior of Cu/Ni-coated samples was improved effectivelyby the enhanced physisorption and chemisorption to form


Table 3: Breakthrough time results for HCl vapor removal of nanoporous carbon sheets as a function of the metal species and content.

Samples Cu content on porouscarbons (wt.%)Ni content on porous

carbons (wt.%)Total content on porous

carbons (wt.%)Breaking time at

298K/100 kPa (min)Cu/Ni-3 3.70 3.56 7.26 60Cu/Ni-5 3.70 6.12 9.82 49Cu #11 7.32 0 7.32 42Cu #22 9.90 0 9.90 28Ni #13 0 7.23 7.23 46Ni #24 0 10.04 10.04 441,2Single Cu-electroplated porous carbon as the same method with Cu/Ni-coated samples.3,4Single Ni-electroplated porous carbon as the same method with Cu/Ni-coated samples.

Table 4: Reusability test of as-received and Cu/Ni-5 at 298K and100 kPa.

Samples Breaking time at 298K/100 kPa (min)1st 2nd 3rd 4th 5th

As-received 20 20 18 19 18Cu/Ni-3 54 44 42 39 39

metal chlorides. A comparison of the single metal loadingshowed that the copresence of Cu and Ni on the PCs resultedin excellent HCl removal abilities compared to single Cu orNi samples with a similar metal content.

Conflict of Interests

The authors declare that there is no conflict of interestsregarding the publication of this paper.

Acknowledgments

This study was supported by a grant from the “Carbon ValleyR&D Project (Project no. R0002651) and Material &Component Technology Development Project (Project no.10050391)” funded by the Ministry of Trade, Industry &Energy (MOTIE), Republic of Korea.

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Research Article A Study on Toxic Acidic Vapor Removal ...Research Article A Study on Toxic Acidic Vapor Removal Behaviors of Continuously Nanostructured Copper/Nickel-Coated Nanoporous