production and properties of carbon nanotube/cellulose

Research ArticleProduction and Properties of CarbonNanotube/Cellulose Composite Paper

Kazi Hanium Maria1,2 and Tetsu Mieno1

1Graduate School of Science and Technology, Shizuoka University, Shizuoka 422-8529, Japan2Department of Physics, University of Dhaka, Dhaka 1000, Bangladesh

Correspondence should be addressed to Kazi HaniumMaria; [email protected]

Received 14 December 2016; Accepted 5 February 2017; Published 21 February 2017

Academic Editor: Xiaolian Sun

Copyright © 2017 Kazi HaniumMaria and Tetsu Mieno. This is an open access article distributed under the Creative CommonsAttribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work isproperly cited.

Multiwalled carbon nanotube/cellulose composite papers have been prepared bymixing the cellulose withMWNT/gelatin solutionand drying at room temperature.The CNTs form an interconnected network on the cellulose paper and as a result CNT paper sheetexhibits enhanced electrical properties and thermal stabilities. It is found that both sides of CNT paper sheet have the uniformelectrical conductivities. The sheet exhibits strong microwave absorption in the microwave range of 10.5 GHz. The CNT/cellulosepaper is as flexible and mechanically tough as the pure cellulose paper. This work provides a novel and simple pathway to makeCNT/cellulose sheet as multifunctional biomaterials for electronic, magnetic, semiconducting, and biotechnological applications.

1. Introduction

Composites based on carbon nanotubes (CNTs) are verypromising for the continuous growth of telecommunicationmarket due to their many unique chemical and physicalproperties [1, 2]. Next-generation computer devices, con-sumer electronics, wireless LAN devices, wireless antennasystems, and cellular phone systems are few portable deviceapplications that require these composite materials, becausenanocomposites have the potential to significantly surpassthe physical properties of conventional bulk materials. Asheavy heat transfer materials have delayed the developmentof portable devices, it is required to develope light-weight,flexible, inexpensive, and wearable composite materials,which has high heat-conductivity [3–6].Therefore, to developthe CNT-composite materials, cellulose is considered due tobeing biosource, light-weight and biologically compatible [7,8]. The problems in developing the composites would be dis-persion of nanotubes in solvents, CNT-polymer interactions,manufacturing cost, and performance of the composite. Cel-lulose has attracted much attention with expertise in diverseareas [9, 10] as a renewable source-based biodegradablepolymer and will be medium for displaying and transmitting

information owing to its potential compostibility, mechanicalstability under atmospheric conditions, and ability to absorbliquid [11, 12]. Carbon nanotubes (CNTs) are regarded as oneof the most versatile additives of composites because it canimprove mechanical, thermal, and electrical characteristicsof cellulose [13–15]. Especially, homogeneous distribution ofCNTs in the cellulose matrix would contribute to improve itscharacteristics. However, the nonreactive surface and strongagregation properties of CNTs due to van derWaals attractiveforce have limited the effectiveness of CNTs with celluloseduring the time of mixing [16]. Previously it is found thatchemical modification of CNT is the most successful disper-sion technique which forms carboxyl functional groups onthe surfaces and the ends. This carboxyl functional groupbinds the CNTs with cellulose very tightly. On the otherhand, chemical modification would considerably alter theirdesirable properties.Therefore, CNT dispersion in solvents isprerequisite to utilize the unique multifunctional propertiesof CNTs in case of preparation of CNT/cellulose composites[17]. For this purpose, in this report, biofriendly material,gelatin is used to disperse the CNTs before mixing withcellulose. Gelatin wraps the surface of CNTs enabling theirdispersion inwater and does not affect the physical properties

HindawiJournal of NanomaterialsVolume 2017, Article ID 6745029, 11 pageshttps://doi.org/10.1155/2017/6745029

https://doi.org/10.1155/2017/6745029

2 Journal of Nanomaterials

of CNTs while enabling their dispersion in aqueous solutions[18]. CNTs form a conducting network using their electrondonating and accepting ability in the composite [19–22].

These CNT/cellulose composite materials have some out-standing properties such as mechanical toughness, electricaland thermal conductivity, and the usage of the materials thathave been investigated [17, 23–25]. In this study, CNT sheetshave been prepared by the paper making process which ison the easy, simple, and readily scalable process. Previousstudy has also not focused on sustaining the structure ofthe CNTs for making composite. Here, it is considered byusing gelatin to disperse CNT before mixing with cellulose.Besides this, we have concentrated on the good environmen-tal stability of composite and low cost combined with theeasiness of preparation. The resulting CNT/cellulose papersheets show high electrical conductivity, strong microwaveabsorbing properties, thermal stability, and wettability. Tothe best of our knowledge, no study has yet investigated theproperties of composite by increasing the amount of CNTs.This study reports that the composite properties are improvedby increasing amount of CNTs and it can be the product ofany size and shape by maintaining the CNT/cellulose ratio.The properties of the composite are reported here.

2. Experimental Methods

To optimize the paper making process for CNT/cellulosecomposites and the quality of the resultant paper, it isimportant to improve the interaction between the pulpfibers, gelatin, andmultiwalled carbon nanotubes (MWNTs).MWNTs (Sigma-Aldrich, outer diameter = 10–30 nm, innerdiameter = 3–10 nm, length = 1–10 𝜇m, and purity> 90%) andgelatin (Wako 1st Grade, appearance: yellowish brown andcrystalline powder) are used as received. Cellulose fibers usedhere are made by pure paper, where cellulose is mixed well inpure water with an electric beater to get homogeneous pulpdispersion in water.

At first, Cellulose suspension is made by soaking thefibers into pure water and blended for 20 minutes. Then,10mg of MWNTs and 30mg of gelatin are sonicated with10mL of pure water by using a supersonic homogenizer(Sonic & Materials VC 130, f = 20 kHz, 6mm𝜙 probe) atan input power of 20W for 60 minutes. Different CNTdispersions are prepared by using 5, 10, 15, 20, and 30mg ofMWNTs.The concentration of the gelatin in CNT dispersionis kept fixed at 3mg/mL.Then 300mg of cellulose suspensionis added to the 10mL of CNT dispersion and blended for20 minutes. The final solution is poured into a tray dishand dried at room temperature to get a paper sheet. Thepaper making process is schematically shown in Figure 1(a).Figure 1(b) shows the photographs of pure cellulose sheet andthe CNT/cellulose sheet. The obtained paper sheets have athickness of 0.2–0.4mm.Theweight ratio of CNT to celluloseis about 1/30, 1/15, and 1/10, when 10, 20, or 30mg of CNT isadded.

Electrical resistance, R, of the sheet is measured by adigital multimeter (Iwatasu VOAC 87, Japan). Two nickelelectrodes (thickness of 0.15mm, purchased from Nilaco,Japan) of width 5mm are placed on the CNT/cellulose sheet

at a distance of 50mm and a dc voltage 𝑉in is applied bya regulated power supply (Kikusui Electronics PAB 350-0.2, Japan) between the two nickel electrodes. The image ofthe uniform distribution of MWNTs in the CNT/cellulosecomposite is taken by a SEM (JEOL JSM 6510LV) at anoperating voltage of 10 kV. Raman spectra are obtained witha Raman spectrometer (JASCO NR-1800) using a laser forexcitation (𝜆 = 532 nm). The thermal stability of the papersheet is observed by aTG/DTAanalyzer (RigakuThermoPlusTG8120). The temperature of the CNT/cellulose paper sheetis measured by using a thermometer (K type thermocouples,0.2mm in diameter, Custom CT-2000D) and an infraredcamera (FLIR i3, emissivity 0.95, focus length = 6.8mm).A gun-diode microwave transmitter and a recorder (PascoScientific WA-9314B, 𝑃𝜇 = 10mW) of 10.5 GHz with hornantenna are used to measure the microwave absorptioncharacteristics of the sheet.

3. Results and Discussion

Figure 2 shows the morphology of the CNT/cellulose papersheetswhich is observed by SEM.Thepaper surface is smoothwhen no MWNTs are coated as shown in Figure 2(a). InFigures 2(b)−2(d), CNTs cover surface of almost all fibersof the sheet. Some CNTs seem to form bridge-like structurewith paper fibers. The SEM images clearly reveal that theinterconnected networks are established by the individualCNTs so that numerous electrical paths can be formed.

In addition to the SEMobservation, Ramanmeasurementis also carried out to prove that CNTs are present in the papersheets. Raman peaks of both G-band and D-band generatedfrom CNTs are observed as shown in Figure 3.

Owing to the formation of conducting paths, the papersheet shows considerable low resistance. Resistance is mea-sured of ten randomly chosen measuring points on bothsides (A side and B side) of a CNT/cellulose paper sheetby the needle-electrodes, and the distance between needle-electrodes is kept constant at 20mm.The distributions of theresistances are shown as histograms in Figure 4. It is foundthat the electrical conductivity of the CNT/cellulose papersheets is highly uniform. In case of 5mgMWNTs added sheet,the A side has resistance, R = 2.61MΩ (standard deviations,s = ±0.08, electrical conductivity, 𝜎 = 1.91mS/m) and the Bside has resistance, R = 2.60MΩ (standard deviations, s =±0.05, electrical conductivity, 𝜎 = 1.92mS/m). When 10mgof MWNTs is added, the A side has resistance, R = 1.14MΩ(standard deviations, s = ±0.04, electrical conductivity, 𝜎= 4.38mS/m) and the B side has resistance, R = 1.103MΩ(standard deviations, s = ±0.05, electrical conductivity, 𝜎= 4.53mS/m). Therefore, it is noticed that the conductivitycan be improved by increasing the amount of CNTs addedto the cellulose. Current-voltage, I-𝑉in characteristic curveis measured by using Ni-rod-type electrodes as shown inFigure 5 and the Ohmic conduction on the paper sheet isobtained.

TG/DTA experiments for the cellulose sheet and theCNT/cellulose sheet are carried out at a heating rate of10∘C/min from room temperature to 800∘C and the curvesare shown in Figure 6. DTA curves show that the thermal

Journal of Nanomaterials 3

Dispersed CNTs ingelatin water solution

Cellulose pulpin pure water

+Mixing

Homogeneouscellulose, CNTs,gelatin solutionin water

CNTCellulose pulp

CNT/cellulose sheet Drying in a tray

(a)

100mm100mm

100mm

(b)

Figure 1: (a) A schematic of the paper making process for the fabrication of CNT/cellulose composite sheets. (b) Photographs of a purecellulose sheet (left) and a CNT/cellulose sheet (right).

degradation of both sheets occurs in two different steps in airatmosphere. In the first step of degradation, the pure cellulosesheet and the CNT/cellulose sheet begin to lose weight at332 and 355∘C, respectively, and the final combustion in thesecond step occurs at 409 and 507∘C, respectively. The finalcombustion of the CNT/cellulose sheet delayed by ca. 100∘Cis clearly observed from the DTA curves, which indicates thatthe cellulose sheet loses weight faster than the CNT/cellulosesheet. From the TG curves, it is observed that the combustionof CNT/cellulose sheet is 22% less than that of the purecellulose sheet. This result signifies that the thermal stabilityof the sheet is improved by adding MWNTs [26, 27]. There isalso a hump shape peak at 463∘C on the CNT/cellulose curvebefore the final combination peak which corresponds to thecombustion of the gelatin [18].

The flame retardancy test is carried out for both the cellu-lose and CNT/cellulose sheets. The image of the combustion

process is shown in Figure 7. Both sheets with same thicknessare hanged on a metal supporter and ignited simultaneouslyby a gas flame. It is observed that the cellulose sheetburns quickly to be ash completely within 20 s, while theCNT/cellulose takes more than 30 s to burn and turns tocharcoal sheet, which indicates that added MWNTs improvethe flame retardancy of the sheet. It is conjectured thatthe flame retardancy of the nanocomposites is stronglyaffected by MWNTs network structures on the cellulose [28].The flame retardancy is attractive for the use in industrialapplications.

The sheet could be used as a flat-type electric heater.The heating test is carried out by measuring the changein the temperature under the applied voltage, 𝑉in = 80–220V. The schematics of the measurement are shown inFigure 8(a).Three layers of CNT/cellulose sheets (d = 1.2mm)have been used to reduce resistance lowly enough by which


1𝜇m

×10,000

(a)

1𝜇m

×10,000

(b)

1𝜇m

×20,000

(c)

1𝜇m

×30,000

(d)

Figure 2: SEM images of (a) the pure cellulose sheet and (b)–(d) the CNT/cellulose sheet at different magnifications taken at an operatingvoltage of 10 kV.

I (ar

b. u

nits)

k (cm−1)1350 1400 1450 1500 1550 1600 1650

D

GID/IG = 0.53

460

465

470

475

480

485

490

Figure 3: Raman spectrum of the CNT/cellulose paper sheet. TheG and D bands show the quality of CNTs.

the electric current through a CNT/cellulose sheet releasesheat due to the Joule heating process [29, 30]. Heating andcooling temperatures of the sheet are measured at the centreof the sheet. Figures 8(b) and 8(c) show the time variationof temperature of the CNT/cellulose sheet measured by athermocouple and by an IR camera during heating andcooling process. It is observed that surface temperature startsto increase with time by applying a dc voltage, and the IRemission from the sheet increases. The surface temperatureof the CNT/cellulose sheet reached a maximum temperatureof 120∘C within 5 minutes depending on the applied voltage.By increasing the number of layers of the CNT/cellulosesheets more, the sheet resistance can be decreased. Thecooling rate of the sheets is also measured. During thetest, all the samples are heated to 35 minutes and thencooled naturally. It is observed that the temperature decreasesexponentially to the room temperature within few minutes.The thermocouple-based measurement shows a little lowervalue of temperature than the infrared-based measurement.


Num

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s

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Figure 4: Histograms of measured resistance on the both sides of the CNT/cellulose paper sheet. Resistances are decreased with the increaseof MWNTs content.

This difference would arise from the slow response of thethermocouple due to the slow heat propagation [31]. The IRimage of the CNT/cellulose sheet is shown in Figure 8(d),which indicates the uniformity of the surface temperature ofthe area (50mm × 50mm). It is clearly shown that the highesttemperature area is located at the centre of the sheet. To studythe flexibility of the CNT/cellulose sheets, the temperatureand current are alsomeasured during bending the sheetmorethan 90∘ for 20 times, and the total time elapsed for thewhole process is 80 minutes. Figure 8(e) shows the flexiblenature of the paper sheet, because repeated bending of papersheet does not make any significant change of the currentconduction through the paper sheet, and temperature alsoremains almost constant. These results mentioned aboveindicate that the CNT/cellulose sheet can be used as a flexibleelectrothermal heating element.

The microwave absorption ability of the CNT/cellulosesheet is measured by a microwave transmitter of constant

frequency 10.5 GHz (𝜆 = 2.85 cm) and emission power 𝑃𝜇= 10mW. A schematic representation of the measurementof microwave absorption ability is shown in Figure 9(a).The CNT/cellulose sheet is made with a size of 100mm ×100mm × 0.3mm for this absorption test experiment. Thesame size of pure cellulose sheet is made for comparison.The pure cellulose sheet and the CNT/cellulose sheet areplaced on a thin plastic substrate during the experiment. Inthis absorption ability experiment, the incident microwaveis partly absorbed by the sheet, partly reflected, and partlytransmitted through the sheet. To determine the reflectionability of the sheet, the transmitter and the recorder are set insuch a way that the incident and reflected wave make equalangles to the surface normal as shown in Figure 9(b).

Figure 10 shows the experimental result of the absorptionand transmission ability versus the thickness. By increasingthicknesses, from 0.3 to 1.8mm, content ofMWNTs increasesfrom 30 to 150mg in the sheet. The absorption increases

6 Journal of NanomaterialsI

(mA

)

Vin (V)0 20 40 60 80 100 120 140 160

L = 50mm

CNT/cellulose sheet50mm

50mm

Nielectrode

A

V0

0.5

1

1.5

2

2.5

Figure 5: I-𝑉in curve for the sheet showing the linear electric con-duction (inset: schematic of the I-𝑉in characteristic measurementsetup).

with the increase of MWNTs content. Several sheets of samethickness and same content of MWNTs (30mg) are usedfor this experiment. During the experiment, thickness isincreased by adding sheets one after one on the plastic sheet.Absorption ability is found to increase with the increaseof thickness as well as MWNTs content. This increase ofabsorption could occur due to the increase of absorptionvolume of the sheet.

Figure 11 shows that the CNT/cellulose sheets exhibit verysmall reflection, and the reflection increases with the increaseof thickness of the sheet. It is conjectured that interfacialelectric polarization improves with the increase of MWNTscontent due to the interaction of microwave radiation withthe large number of charge dipoles between the MWNTsand cellulose, which would cause reflection [32]. The resultscan be comparable with the previous examinations with theother composites of MWNTs [33, 34]. This means that thereare several considerable factors, like the MWNTs content,thickness of sheet, the interfacial electric polarization, and soon, to design microwave absorbing materials [35]. It is alsofound that a zigzag setup of 4 sheets of same dimensions,each of which contains 30mg MWNTs, can absorb about50% of the incident microwave. Considering the aboveresults, this composite sheet has potential advantages as anelectromagnetic shielding material (EMS material) at themicrowave region and the ultrahigh frequency (UHF) region.

The aqueous absorption speeds are conducted to under-stand the microwettability of the composites. Generallycellulose sheets have high absorption speed which in turndegrades their mechanical properties. CNT/cellulose com-posite shows the significant improvement on the mechanicalproperty without degradation resulted from the addition ofcarbon nanotubes in the cellulose. In the bio and chemicalanalyses, liquid-absorption of cellulose sheets is commonlyused.

The pure cellulose sheet and the CNT/cellulose sheet(including 10∼30mg of MWNTs) are prepared with a size

of 100mm × 20mm × 0.3mm. In this experiment, oneend of the sheet sample is immersed in a color ink or asaline liquid. Both cellulose and CNT/cellulose sheets startto absorb aqueous solution immediately after the immersion.The sheets are kept in the solution until they get completelywet. The schematic of the absorption speed measurement isshown in Figure 12(a). The absorption speed is measuredfrom this experiment and compared with those of the purecellulose sheet. Absorbed saline amount by the sheet iscalculated bymeasuring theweight changes of the sheets afterthe experiment.

It is evident from Figure 12(b) that the absorption speedof the cellulose sheet is very high in both color ink andsaline liquid. On the other hand, the CNT/cellulose sheethas low absorption speed. A high DC voltage of about 300Vis applied through Ni electrodes to the CNT/cellulose sheetto investigate the changes in speed, and it is found thatthe absorption speed with application of the electric fieldincreases significantly in both cases of color ink and salineliquid. The various voltages are also applied by changing thepolarity, and the polarity does not have noticeable effects onabsorption speed. It is also evident from Figure 13 that theabsorption speed increases with the increase of MWNT con-tent and the applied voltage.This indicates that the absorptionspeed and absorbed aqueous amount of the CNT/cellulosesheet can be controlled by the MWNT loading. By additionof MWNTs and high voltage in the sheet, the sheet becomeselectroconductive and the electric field could control themobility of ionic liquid. The absorption speed is also relatedto other factors, for example, cellulose pulp content, anddispersion state of MWNTs in the sheet. By adding MWNTsin the pulp sheets, the absorption speed of liquid increases,but by adding DC voltage the speed can be controlled.

4. Conclusions

This work provides a simple and effective method of prepar-ing CNTs/cellulose sheets. The sheets are physically strongand yet highly flexible. This CNTs/cellulose sheet exhibitsimproved electrical and thermal properties because of thegood interaction between cellulose and MWNTs. Bettermechanical properties could be expected at the optimizedprocessing condition. The sheet can be used as flexibleelectrothermal heating elements due to the thermal con-duction. The high microwave absorption and low reflectionperformance of the sheet indicate the usefulness of thecomposite for microwave technology applications.This sheetcould be also used as electromagnetic shields (EMS) forhigh-frequency devices. The water absorption speed of theCNT/cellulose sheets can be controlled by applying DCvoltage. As cellulose is biocompatible and biodegradable,applications of the sheet will be expanded to bioscience.

Competing Interests

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


Pure cellulose sheetCNT/cellulose sheet

Wei

ght (

wt%

)

T (∘C)0 100 200 300 400 500 600 700 800

Hea

t flow

(arb

. uni

t)

640

480

320

160

0

TG

DTA−80

−40

0

40

80

120

Figure 6: TG/DTA curves for a pure cellulose sheet (blue dotted line) and a CNT/cellulose sheet (red solid line).

2 s 5 s 8 s 11 s 14 s

21 s 25 s 28 s 32 s17 s

Figure 7: Photographs of flame retardancy test for the pure cellulose sheet (left white sample) and the CNT/cellulose sheet (right blacksample). At t = 0 s, a fire is added on the bottom of the samples.


50mm

50mm

Ni electrode

3 layers ofCNT/cellulose

sheet

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57∘C 123∘C

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C)

Vin = 100V

25

30

35

40

50 15 20 2510

Bending cycle

15

20

25

30

I(m

A)

(e)

Figure 8: (a) Schematic of the heating test measurement of the CNT/cellulose sheet by a thermocouple and an IR camera. Temperature versustime curves during heating and cooling of the CNT/cellulose sheet measured (b) by a thermocouple and (c) by an IR camera. (d) IR image ofthe sheet at𝑉in = 220V (𝐼in = 6mA) showing the uniform surface temperature of the area (50mm × 50mm) where the temperature scales areshown at the bottom part. (e) Variation of temperature and current after repeated bending, where the input voltage 𝑉in = 100V (𝐼in = 2mA).


10.5GHz

Transmitter

Incidentmicrowave

10 cm

Plastic sheetCNT/cellulose sheet

10cm

Transmittedmicrowave

Recorder

(a)

Incident microwave

Transmitter

10 cm

Surface normal

Plastic sheetCNT/cellulose sheet

Reflected microwave10cm

Recorder

(b)

Figure 9: Schematic representation of the (a) microwave absorption measurement and (b) reflection measurement of the CNT/cellulosesheet.

Tran

smiss

ion

(%)

40

45

50

55

60

65

70

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Figure 10: Variation of microwave transmission property of theCNT/cellulose sheet with the increase of thickness, where MWNTcontent increases with the thickness.

Acknowledgments

This study was supported by the Promotion of Nano-Biotechnology Research to Support Aging, Welfare Soci-ety from Ministry of Education, Culture, Sports, Science

Refle

ctio

n (%

)

3

4

5

6

7

8

1 20 0.5 1.5

Thickness (mm)

Figure 11: Variation of reflection property of the CNT/cellulosesheetwith the increase of thickness, whereMWNTcontent increaseswith the thickness.

and Technology, Japan. TEM and TG/DTA measurementswere done at Research Institute of Green Science &Technology, Shizuoka University. Raman measurement was


Purecellulose

sheet2 cm

2 cm

10 cm

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Solution

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0

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10

15

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Figure 12: (a) Schematic of the absorption speed of liquids measurement of the CNT/cellulose sheet and the pure cellulose sheet. (b)Absorption speeds of the cellulose sheet and the CNT/cellulose sheet in different solution conditions.

Cel

lulo

sesh

eet

CNT/

cellu

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t 10 m

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/s)

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100 150 200 250 300 35050Applied voltage (V)

(b)

Figure 13: (a) Absorption speed of the cellulose sheet and the CNT/cellulose sheet with the increase ofMWNT content. (b) Absorption speedof the CNT/cellulose sheet with the increase of applied voltage.

done at Research Institute of Electronics, Shizuoka Univer-sity.

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