SWCNT Supercapacitor Electrode Fabrication Methods

by Matthew H. Ervin, Benjamin S. Miller, and Brendan Hanrahan

ARL-TR-5438 February 2011

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ARL-TR-5438 February 2011

SWCNT Supercapacitor Electrode Fabrication Methods

Matthew H. Ervin, Benjamin S. Miller, and Brendan Hanrahan

Sensors and Electron Devices Directorate, ARL

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SWCNT Supercapacitor Electrode Fabrication Methods

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14. ABSTRACT

This work systematically compares various solution-based electrode fabrication methods (drop casting, air brushing, filtration, 

and electrospraying) to determine if there is an optimum method for fabricating supercapacitor electrodes out of single-wall 

carbon nanotubes (SWCNT). We have found that it is best to use SWCNT solutions free from additives that may be difficult 

to remove from the fabricated electrode. In addition, the SWCNT solution processing (e.g., dilution and sonication) has a 

small effect on the resulting specific capacitance, as did the deposition methods compared here. 

15. SUBJECT TERMS

Carbon nanotube, electrochemical capacitor, supercapacitor, cyclic voltametry, electrospray

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Matthew H. Ervin

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iii

Contents

List of Figures iv

List of Tables iv

1. Background 1

2. Capacitor Evaluation 3

3. SWCNT Solution Comparison 4

4. Fabrication Method Comparison 5

5. Conclusions and Opportunities 9

6. References 11

List of Symbols, Abbreviations, and Acronyms 12

Distribution List 13
iv

List of Figures

Figure 1. Typical 20 mV/s cyclic voltamogram for SWCNT electrodes produced in this 

study. While there are redox peaks superimposed on the approximately rectangular CV 

curve that is representative of double layer capacitance, the current for calculating the 

capacitance is measure on the reduction side (lower curve) at the open circuit potential 

which is at –88 mV in this example...........................................................................................4

Figure 2. (a) SWCNTs electrode made using a SWCNTssolution that included a surfactant 

(b) SWCNTs electrode made with a surfactant-free solution of SWCNTs resulting in a 

cleaner and more porous electrode with better electrical conductivity.....................................5

Figure 3. Pictures of the different deposition methods used (a) drop casting, (b) air brushing, 

(c) a SWCNT deposit (black) on a mixed cellulose filter paper, and (d) electrospraying.........6

Figure 4. Photographs of electrodes fabricated using the four methods (a) drop cast, (b) air 

brushed, (c) filtered/transferred, and (d) electrosprayed............................................................7

Figure 5. SEM micrographs of electrodes fabricated using the four methods (a) drop cast, 

(b) air brushed, (c) filtered/transferred, and (d) electrosprayed.................................................8

Figure 6. Specific capacitance as a function of deposition method. The diamonds are from 

samples made with the SWCNT solution merely shaken, while the “x” symbols are used 

to denote samples made from sonicated SWCNT solutions......................................................9

List of Tables

Table 1. Examples of solution processed SWCNT/graphene electrodes........................................2
1

1. Background

Supercapacitors, more properly referred to as electrochemical capacitors, have several 

advantages over conventional batteries, including higher specific power (~2 orders of magnitude 

higher), higher cycle life (millions of charge/discharge cycles), rapid charge/discharge times 

(seconds to minutes), high efficiencies (up to 98%), and unaltered performance in extreme heat 

and cold (1). Increasing supercapacitor energy and power densities will make them more useful 

for portable power applications. 

A supercapacitor consists of two solid dielectric-free electrodes, in contact with an electrolyte,

which store charge by adsorption of ions onto the electrodes. The capacitance due to the 

adsorption of ions onto the electrodes is referred to as electrochemical double-layer capacitance,

since there is a layer of ions on the electrode with a second layer of counter-ions (oppositely 

charged ions) next to the adsorbed ions. Energy can also be stored through redox reactions at the 

electrodes, whose rates are potential dependent. This type of energy storage is referred to as 

pseudocapacitance since it behaves as a capacitance, though the charge transfer reactions are 

more like that of a battery. Since there is no dielectric on the supercapacitor electrodes, the 

applied biases must remain low enough that electrochemical breakdown of the electrolyte solvent 

or charge transfer between the ions and electrodes (except when pseudocapacitance is desired)

do not occur. This limits the voltage rating on individual supercapacitor cells to about 1.2 V 

when using aqueous electrolytes, and 3.5 V when using organic electrolytes.

Supercapacitors achieve large capacitances by using electrodes with very large surface areas. 

Carbon electrodes are desirable because they are conductive and have high surface area, good 

corrosion resistance, and good thermal stability (1). Carbon materials with improved surface 

area may increase the capacitance of supercapacitors. Two materials being studied for this are 

carbon nanotubes (CNTs) and graphene. Graphene is a single atomic layer of graphite. 

Similarly, a single-wall CNT (SWCNT) is a single atomic layer of graphite that curve back on 

itself to form a tube. Multi-wall carbon nanotubes (MWCNTs) are carbon nanotubes that are 

more than one atomic layer thick; they were not used in this study. This study focused on 

SWCNTs since they have the largest surface area-to-mass ratio given that any interior walls in a 

MWCNT contribute mass but not surface area. Extremely large capacitances may be obtainable 

if these materials can be assembled in a manner that optimizes the electrode surface area that is 

accessible to the electrolyte. 

This report details investigations into various solution-based electrode fabrication methods that

are compared to determine if there is an optimum method for fabricating SWCNT electrodes. 

Solution-based processing was chosen, as it is manufacturable and does not impose significant 

thermal and chemical constraints on the underlying current collector as direct growth on the 

current collector would. When SWCNTs are deposited from solution, they typically do so in 
2

bundles. It is not yet clear if this bundling is detrimental to the resulting accessible surface area 

and, therefore, the resulting capacitance. In addition, the deposition method may also affect the 

porosity of the electrode, which will affect how easily the electrolyte ions can move into and out 

of the electrode (the Warburg impedance) during the charge/discharge process.

Many solution-based processing approaches have been demonstrated with measured specific 

capacitances of 23–200 F/g, as shown by the representative works listed in table 1 (2–9). Since 

these papers use different CNT sources, solution compositions/processing, deposition methods, 

and characterization protocols, it is difficult to draw meaningful conclusions about the electrode 

fabrication methods from a comparison of these works. In addition, many of the higher specific 

capacitances, reported in table 1, likely include pseudocapacitive contributions to the measured

specific capacitance. Such pseudocapacitance contributions may overwhelm the double-layer 

capacitance, which is the focus of this work, as the double-layer capacitance is related to the 

realized accessible electrode surface area. Here we have systematically investigated the 

individual contributions of the solution preparation and the deposition methods to achieved 

double-layer capacitance. 

Table 1. Examples of solution processed CNT/graphene electrodes.

Fabrication 

method

CNT solution F/g Comments Reference

Spray Deposition SWCNT 38 SWCNTs not functionalized X Zhao Nanotech 

2009 (2)

Spray Deposition SWCNT-COOH 155 Functionalization results in clear 

redox pseudocapacitance

X Zhao Nanotech 

2009(2)

Spray Deposition MWCNT 23 MWCNTs not functionalized X Zhao Nanotech 

2009(2)

Spray Deposition MWCNT-COOH 77 Functionalization results in clear 

redox pseudocapacitance

X Zhao Nanotech 

2009(2)

Spray Deposition SWCNT 90–120 SWCNTs possibly functionalized 

during purification

Kaempgen NL 09

(3)

Layer by Layer MWCNT-COOH

MWCNT-NH2

150 Pseudocapacitance contribution S W Lee JACS 08

(4)

Filtration DWCNT 67 DNA dispersed double walled CNTs Cooper APL 2009

(5)

Filtration DWCNT 32 Double walled CNTs Chou Electrochem 

Comms 08 (6)

Electrospray MWCNT-COOH 108 Pseudocapacitance contribution J H Kim Carbon 06

(7)

Meyer Rod -

Adsorb on Paper

SWCNT 200 Measurements indicate at least some 

pseudocapaitance

Hu PNAS 09 (8)

Freeze Dry graphene 120 200 °C anneal of graphene oxide 

may not remove all oxide functional 

groups

J. Wang ECS 

Trans. 09 (9)
3

2. Capacitor Evaluation

When characterizing capacitors, one needs to be careful to distinguish between double-layer 

capacitance and any pseudocapacitance contributions. In addition, measurement methodologies 

can contribute to significant differences in measured capacitances. Therefore, standard test 

conditions of 20 mV/s have been used for cyclic voltametry (CV) measurements made using one 

molar potassium hydroxide (KOH) electrolyte. To avoid inclusion of any reduction and 

oxidation (redox) (pseudocapacitive) contributions, the capacitance has been calculated for each 

electrode using the current measured at the open circuit potential on the reduction side of the CV 

loop. In figure 1, this would correspond to measuring the CV current on the lower portion of the 

curve at approximately –0.1 V, which avoids the redox peak(s) that starts at about –0.2 V as the 

potential is scanned more negatively. At the open circuit potential, any redox reactions should 

be in equilibrium and make no contribution to the measured current. Electrochemical impedance 

spectroscopy was also performed at the open circuit potential. In order to compare the 

capacitances generated by the different fabrication methods, we calculated specific capacitance 

(F/g) using only the mass of the SWCNTs after subtracting the capacitance of the metal foil 

current collector. It became apparent during the experiments that there was excessive error in the 

measured SWCNT masses. This error was tracked down to magnetic field effects while 

measuring our nickel current collector-based electrodes. Therefore, the reported results will rely 

on masses calculated from the solution concentrations/volumes used. Since this is not wholly 

accurate, due to mass loss from overspray or incomplete filtering, some experiments have been 

repeated using nonmagnetic tungsten current collectors in order to verify the trends.
4

Figure 1. Typical 20 mV/s cyclic voltamogram for SWCNT electrodes produced in this study. 

While there are redox peaks superimposed on the approximately rectangular CV 

curve that is representative of double layer capacitance, the current for calculating 

the capacitance is measure on the reduction side (lower curve) at the open circuit 

potential which is at –88 mV in this example. 

3. SWCNT Solution Comparison

Both SWCNT and graphene materials are frequently processed as suspensions/solutions. In 

order to get stable dispersions, the SWCNTs/graphene are either chemically functionalized 

and/or dispersed with a surfactant. Both approaches have drawbacks. Chemical 

functionalization can make the material more soluble, but the addition of these functional groups 

introduces defects that can decrease conductivity. Functional groups can also be redox active 

and produce undesirable decomposition byproducts over time. Surfactants can be used in place 

of functionalization to help solubilize SWCNTs or graphene, but since they are generally 

nonconductive, they typically degrade performance. Therefore, further processing is required to 

wash them off, which may remove SWCNTs/graphene from the substrate or alter the electrode 

morphology. We have made numerous electrodes using SWCNT solutions obtained from 

commercial sources. The first solutions used were of functionalized or unfunctionalized 

SWCNTs suspended in acetone, using surfactants and/or dispersants containing: a-

(nonylphenyl)-hydroxy-,branched poly(oxy-1,2-ethanediyl)(20% - 50%); 2,4,7,9-Tetramethyl-5-

decyne-4,7-diol (2% - 10%); and 2-Butoxyethanol (<1%); and other proprietary components. 

These electrodes were examined in a scanning electron microscope (SEM) and little porosity was 

seen. The anticipated porosity between the SWCNTs was filled with surfactant/dispersant 

additives, as is shown in figure 2a. Attempts to remove these additives through thermal 
5

annealing, acid washing, or solvent extraction were largely unsuccessful. As a result, the 

electrodes had poor capacitances due to low accessible surface area and high resistivity due to 

poor tube-to-tube electrical contact.

Subsequent electrodes were made using SWCNTs functionalized with carboxyl groups by 

refluxing in strong acids. These SWCNTs are somewhat soluble in water without the aid of 

surfactants/dispersants, and they yield much better-looking (figure 2b) and higher performing 

electrodes. The SWCNT mat made without surfactants in figure 2b has six times the 

conductivity and four times less contact resistance, when probed with an ohmmeter, as the 

surfactant containing mat shown in figure 2a. While the differences in conductivity between 

surfactant-free and surfactant-containing mats is highly variable, the surfactant-free mats 

consistently produce better properties, as we have observed in other work in our lab (10). We 

concluded that using surfactant/dispersant free solutions of SWCNTs is the better approach, even 

though it requires the use of less concentrated solutions.

Figure 2. (a) SWCNT electrode made using a SWCNT solution that included a surfactant (b) SWCNT

electrode made with a surfactant-free solution of SWCNTs resulting in a cleaner and more 

porous electrode with better electrical conductivity.

4. Fabrication Method Comparison

At the outset of this work, it was assumed that the amount of SWCNT bundling would be a 

significant factor in the capacitance that could be achieved. It may also affect the power 

performance due to the electrolyte resistance to reach the interior electrode surfaces. Therefore, 

methods for producing solutions of unbundled SWCNTs and deposition methods that prevent rebundling as the solution dried would be critical. In light of this, four methods for depositing the 

SWCNT solutions that might yield different amounts of re-bundling were selected for 

comparison. All four methods were used to deposit 1ml of SWCNT solution of ~70 ug/1 ml 

water concentration onto nickel current collectors, which were heated on a 175 °C hot plate 

during the deposition (except for the filter and transfer method). 
6

The easiest method, drop casting, consists of depositing droplets of solution onto the current 

collector and evaporating the droplets over 1–2 min, with the total deposition taking about 

20 min. The second method, air brushing, sprays much smaller droplets onto the current 

collector; the droplets dry in 1–3 s, with the total deposition time being about 30 min. The third 

method, vacuum filtration, takes a few seconds total, and is followed by transferring the dry 

SWCNT mat to the current collector by placing the filter face down onto the current collector 

and dissolving the mixed cellulose filter (0.22 micron) with acetone. The last method 

investigated is electrospraying (11), which required a dilution of the solution with ethanol 

(1:0.43 v/v water:ethanol) to decrease its surface tension. This method produces extremely small

droplets, on the order of 4 microns in diameter, and they may dry before reaching the current 

collector. In addition, as the droplets dry in transit, the charge density on the droplets may 

increase enough that columbic repulsion within the droplets cause the droplets to explode, 

perhaps preventing or reducing SWCNT bundling. Pictures of the four deposition methods are 

shown in figure 3. 

Figure 3. Pictures of the different deposition methods used (a) drop 

casting, (b) air brushing, (c) a SWCNT deposit (black) 

on a mixed cellulose filter paper, and (d) electrospraying.

The resulting electrodes were characterized photographically and through SEM imaging. Figure 

4 is a photograph showing electrodes made with the four different methods. The area that the 

SWCNTs were deposited over was roughly the same for the four methods. The filtration and 

transfer method produced the most uniform deposit, while drop casting yielded the most nonhomogenous deposit. SEM images of the four electrodes are shown in figure 5. At a 

microscopic scale, the four electrodes look very much the same, with SWCNT bundles on the 

order of ~5–50 nm in diameter being typical, and with the filtered electrode distribution, perhaps,

being skewed somewhat to the larger bundles and the electrosprayed electrode to the smaller 
7

bundles. The microscopic similarity between these electrodes would seem to indicate that the 

deposition methods investigated are having little effect on the resulting electrode topography.

Figure 4. Photographs of electrodes fabricated using the four methods (a) drop 

cast, (b) air brushed, (c) filtered/transferred, and (d) electrosprayed.
8

Figure 5. SEM micrographs of electrodes fabricated using the four methods (a) drop cast,

(b) air brushed, (c) filtered/transferred, and (d) electrosprayed.

Figure 6 shows the specific capacitances that result from these electrode fabrication methods. 

Focusing on the diamond symbols in the graph, which are electrodes generated with the solution 

used as is, it appears that these different methods do not result in greatly different capacitances. 

In fact, the differences may be less than they appear since the lower specific capacitances of the 

air-brushed, filtered, and, perhaps, electrosprayed methods may be due in part to a loss of 

SWCNTs due to overspray, or incomplete filtration of the SWCNTs. (Remember that the 

SWCNT masses were calculated from the solution used and not measured due to difficulty in 

getting accurate masses at the tens of microgram level used here.) The “x” symbols in the figure 

represent electrodes made from SWCNT solutions sonicated with added ethanol, water, or no 

added solvent. Again, it appears that the SWCNT solution preparation (sonication and dilution 

with ethanol) may be at least as significant as the fabrication methods used here. 
9

Figure 6. Specific capacitance as a function of deposition method. The diamonds are from 

samples made with the SWCNT solution merely shaken, while the “x” symbols are 

used to denote samples made from sonicated SWCNT solutions.

In order to investigate whether the lower specific capacitances resulting from air brushing and 

filtering were due to loss of SWCNTs during the deposition, two more electrodes were made. 

One was air-brushed onto a current collector with upturned edges to minimize the amount of 

SWCNT solution droplets that were blown off the substrate during deposition. This electrode 

clearly showed an additional deposit of SWCNTs at the bent up edges of the current collector. 

The other was made by triple-filtering the SWCNT solution through the same filter paper prior to 

transferring the SWCNTs onto the current collector. In both cases, the more carefully prepared 

electrodes reproduce the highest specific capacitances seen for those methods in figure 6.

The electrochemical impedance spectroscopic characterization, of all of the electrodes fabricated, 

did not show significant qualitative differences between the electrodes. However, the one 

difference that we noticed was that the air-brushed electrodes retained more of their initial 

capacitance at higher frequencies. Since these electrodes started with lower capacitance and,

therefore, likely contain fewer SWCNTs, it would appear that they are thinner electrodes, which 

could explain why they perform slightly better at higher frequencies. More work would be 

required to determine if these frequency response differences are significant.

5. Conclusions and Opportunities

In the present work, a systematic comparison of different SWCNT solution compositions and 

deposition methods has been undertaken to determine the important factors in electrode 

fabrication. We have found that it is best to use SWCNT solutions free from additives that may 
10

be difficult to remove from the fabricated electrode. The SWCNT solution composition and

processing (e.g., sonication or dilution) are more important than the choice of the SWCNT

deposition methods used here. In the end, the choice of fabrication method may be determined 

by other factors such as manufactuability or the efficiency with which the SWCNTs are used.

Continuing work will focus on the fundamental capacitance limits of SWCNTs/graphene

electrodes to determine if further fabrication method development is warranted. We are 

currently attempting to address this issue by investigating the capacitance achievable with welldefined single-layer graphene electrodes.

Even if SWCNTs/graphene electrodes do not yield specific capacitances in excess of activated 

carbon, they may still yield improvements in power due to increased electrode conductance and 

optimized porosity. There may also be important supercapacitor improvements due to the 

mechanical properties of SWCNTs/graphene. For instance, SWCNTs/graphene may lend 

themselves to flexible, conformal, or integrated supercapacitors that would be useful for 

applications where there is little available space.

While the different electrode fabrication methods investigated here appear to yield similar 

capacitances, the SEM images appear to show potential differences in bundle size distributions. 

In the end, there may be an optimum bundle size that is small enough to allow easy electrolyte 

penetration and large enough to enhance conductivity.
11

6. References

1. Pandolfo, A. G.; Hollenkamp, A. F. J. Power Sources 2006, 157, 11–27.

2. Zhao, X.; et al. Nanotech. 2009, 20, 065605.

3. Kaempgen, M.; et al. Nano Lett 2009, 9, 1872–1876.

4. Lee, S. W.; et al. J. Amer. Chem. Soc. 2009, 131, 671–679.

5. Cooper, L.; et al. Appl. Phys. Lett. 2009, 95, 233104.

6. Chou, S.-L.; et al. Electrochem. Comm. 2008, 10, 1724–1727.

7. Kim, J. H.; Nam, K.-W.; Ma, S. B.; Kim, K. B. Carbon 2006, 44, 1963–1968.

8. Hu, L.; et al. Proc. Nat. Acad. Sci. 2009, 106, 21490–21494.

9. Wang, J.; Ellsworth, M. W. Electrochem. Soc. Trans. 2009, 19, 241–247.

10. Anton, C. M.; Ervin, M. H. Electrochem. Soc. Trans., in press.

11. Jaworek, A. J. Mater. Sci. 2007, 42, 266–297.
12

List of Symbols, Abbreviations, and Acronyms

CNTs carbon nanotubes

CV cyclic voltametry

KOH potassium hydroxide

MWCNTs Multi-wall carbon nanotubes

Redox reduction and oxidation

SEM scanning electron microscope

SWCNT single-wall CNT
13

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