Journal of Experimental Nanoscience

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Preparation and properties of cotton stalk carbon/

gold nanoparticles composite

WenKun Zhu, Meng Kuang, Shoujun Wei, Tao Duan, Yanqin Wang, Dayun
Zhou, Lei Ma, Dan Fang, Jian Zhou & Weihua Yang

To cite this article: WenKun Zhu, Meng Kuang, Shoujun Wei, Tao Duan, Yanqin Wang, Dayun
Zhou, Lei Ma, Dan Fang, Jian Zhou & Weihua Yang (2016) Preparation and properties of cotton
stalk carbon/gold nanoparticles composite, Journal of Experimental Nanoscience, 11:7, 471-479,
DOI: 10.1080/17458080.2015.1079931

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Published online: 01 Oct 2015.

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JOURNAL OF EXPERIMENTAL NANOSCIENCE, 2016
VOL. 11, NO. 7, 471 479
http://dx.doi.org/10.1080/17458080.2015.1079931

Preparation and properties of cotton stalk carbon/gold

nanoparticles composite
WenKun Zhua*, Meng Kuangb*, Shoujun Weib, Tao Duana, Yanqin Wangb, Dayun Zhoub,
Lei Mab, Dan Fangb, Jian Zhouc and Weihua Yangb
a
Joint Laboratory for Extreme Conditions Matter Properties, Southwest University of Science and Technology and
Research Center of Laser Fusion, CAEP, Mianyang, PR China; bState Key Laboratory of Cotton Biology, Institute of
Cotton Research of Chinese Academy of Agriculture Sciences, Anyang, PR China; cEngineering Research Center of
Biomass Materials, Ministry of Education, Mianyang, Sichuan, PR China

ABSTRACT ARTICLE HISTORY

In this paper, cotton stalk is used as a low-cost raw material source to Received 11 May 2015
prepare activated carbon with a unique porous structure with the Accepted 2 August 2015
assistance of chemical treatment. Gold nanoparticles as a multifunction KEYWORDS
building block were in situ assembled onto the carbon material, endowing cotton stalk; CS carbon/
this hybrid more promising applications. The as-fabricated CS carbon/ AuNPs hybrid materials;
AuNPs hybrid materials have been demonstrated to behave with catalytic photothermal conversion
and photothermal conversion properties, indicating that AuNPs properties
successfully functionalise the activated carbon. The catalytic activity of the
hybrid showed a glucose concentration-dependent effect (as low as 5 £
10¡6 M). The water temperature of the sample containing the CS carbon/
Au NPs increased rapidly, and even reached 55  C, only exposed to light
for 5 min. When used as catalyst of reduction of p-nitrophenol, the hybrid
showed a good reusability up to10 cycles.

1. Introduction
Activated carbon is a widely used industrial material with an internal pore structure.[1 4] For many
applications, such as filtration and purification,[5] supercapacitors,[6] drug delivery,[7] hydrogen
storage, and catalysts, AC is of great importance as a kind of basic material. In general, these applica-
tions are related with the adsorption behaviour of AC, owing to the well-developed internal pore
structures and chemical functional groups located at the outer and inner surfaces.[8] However, its
large-scale usage is restricted by the high production cost.[9] In this connection, a number of
research groups reported the preparation of AC from cheaper and readily available precursor mate-
rials (agricultural by-products and other biomass materials) by chemical or physical activation.
Preparation of AC from renewable biomass-based agricultural byproducts, such as bamboo,[10]
coconut shell,[11] waste tea,[12] and especially bacterial cellulose,[13 15] is one of the most useful
ways chosen by researchers to reduce the cost of raw materials.
Cotton is cultivated all around the world with an increasing area. For many years, associated with
cotton production is a corresponding annual huge amount production of cotton stalk,[16] which
weighs about three million tons per year.[17] This big quantity of stalks becomes an environmental
problem, especially after they have lost their usage as fuel, or raw materials in paper-making indus-
tries. In situ burning generates great amount of microparticles which may aggravate fog and haze.

CONTACT Weihua Yang [email protected]; [email protected]

* These authors contributed equally to this work.
© 2015 Taylor & Francis
472 W. ZHU ET AL.

[18] To lower this pressure, research was to prepare AC from cotton stalk. To prepare AC, the pyrol-
ysis of agricultural waste is an important step in its thermal conversion, since it determines the split
between three different phases: char, tar and gas. The lignocellulosic waste is an excellent precursor
for the preparation of AC, not only to mitigate this serious environmental problem, but also for the
practicable application, such as catalysts carrier. For introducing catalytic functionality into the unique
pore structure of AC, nanoparticles are efficient components due to their small sizes, facile assemblies,
special properties and wide applications in traditional functional nanocomposites.[19] Previous
AuNP-based nanocomposites showed potential applications in the fields of advanced microelectron-
ics, nonlinear optics, electrochemical sensors, and bioanalysis.[20] Thus, AuNPs are highly expected
to be loaded on the surface of AC, using cotton stalks as the low-cost precursor, forming a new kind
of multifunctional hybrid.

2. Materials and methods

2.1. Preparation of activated carbon from cotton stalk
Cotton stalks were added to a concentration of 3.5% aqueous sodium hydroxide solution, stirred for
60 min, followed by an ultrasonic treatment for 90 min. The samples were washed to neutral and
immersed in deionised water for 12 h, and dried at 80  C for 12 h afterwards. The treated cotton
stalks obtained in step one was added to a concentration of 4.25% H3PO4 solution by a liquid solid
ratio of 8:1 (mL:g) and stirred for 6 h, washed to neutral with deionised water and the material was
immersed in deionised water (DIW) for 12 h, and then dried at 80  C for 12 h. The samples were
placed in a quartz reactor and swept 50 cm3 min¡1 of N2 for 30 min. Then, the reactor was intro-
duced in a horizontal tube furnace at a 5  C min¡1 heating rate, held at 850  C for 2 h in a highly
purified CO2 constant flow of 85 cm3 min¡1, and then cooled down to room temperature at a rate of
5  C min¡1. The cotton charcoal powder was collected and mixed with a mixed acid (nitric acid:sul-
phuric acid D 1:3) under ultrasonic for 4 h to uptake the oxidation process. Finally, the modified sam-
ples were sealed with DIW and set aside.

2.2. In situ assembly of gold nanoparticles onto the activated cotton stalk carbon
Oxidised cotton stalk carbon (50 mg) was added into an 18.4 mL freshly prepared 1% sodium citrate
solution. Excess deionised water was added to a total volume of 100 mL. The mixture was reflux at
120  C for 5 min, after which 1% chlorine acid solution (2, 4, 6 mL) was added respectively and
stirred rapidly. Adjust the heating source so that the solution boils slightly. After a 4 minutes’ reac-
tion, the solution colour changed to red wine. The heating source was removed and the reflux was
maintained until the solution cooled down to room temperature naturally. The sample was filtered
and dried at 80  C overnight.

2.3. Recyclable catalysis of p-nitrophenol by CS carbon/AuNPs

4-NP (0.0139 g) and NaBH4 (3.783 g) were dissolved in 100 mL DIW in a volumetric flask. 4-NP
(3.7 mL) and NaBH4 (3.65 mL) (molar ratio D 37:36,500) were diluted with DIW to 40 mL in a 100
mL conical flask. The solution was placed on a shaker. Then 30 mg catalyst was added into the coni-
cal flask, take 3 mL solution as sample every three minutes. The solution was filtered with a pinhole
filter paper to collected catalyst, taking UV visible measurement afterwards. The collected catalyst
for the following test of reusability for 10 times.

2.4. CS carbon/AuNPs hybrid for glucose detection

Glucose detection was realised as follows: first, a 40 mg mL¡1 solution of glucose oxidase (GOx;
25 mL) and a solution of glucose (500 mL) of different concentrations mixed with 0.5 mm Na2HPO4
 JOURNAL OF EXPERIMENTAL NANOSCIENCE 473

buffer (pH 7.0) were incubated at 37  C for 1 h; second, 150 mL tetramethylbenzidine (TMB) solu-
tion (1 mg mL¡1), 100 mL solution of CS carbon/Au NPs hybrid (1 mg mL¡1), and 25 mL Na2HPO4
buffer (1.5 mL; pH 4.0) were added into the above solution. Thirty minutes later, the mixture was
used to perform UV vis measurements.

2.5. Characterisation
Scanning electron microscope (SEM) images were acquired with a Zeiss Supra 40 scanning electron
microscope at an acceleration voltage of 5 kV. Transmission electron microscope (TEM) images
were acquired with a Hitachi H-7650 transmission electron microscope at an acceleration voltage of
120 kV. Photothermal conversion properties were tested with an 808 nm infrared diode laser with a
power density of 8 W cm¡2 (Changchun New Industries Optoelectronics Technology Co., Ltd.) and
a thermometer (TES-1310, TES Electrical Electronic Corp.). Powder X-ray diffraction (PXRD)
was
carried out on Japan Rigaku TTRIII X-ray diffraction with Cu Ka radiation (λ D 1.54178 A). The
UV vis transmittance and adsorption spectra of the hybrid were collected on a SHIMADZU DUV-
3700. The UV vis adsorption spectra of suspensions were recorded by a Shimadzu UV-2500 PC.

3. Result and discussion

3.1. Textural properties of activated carbon
Herein, our designed fabrication procedure involves the synthesis of highly porous cotton stalk car-
bon and self-assembly of as-synthesised Au NPs onto CS carbon to form hybrid nanomaterials. The
whole fabrication procedure of the functional Au NPs CS carbon hybrid powder or suspension is
depicted in Figure 1. First, cotton stalk was crushed into powder and treated with sodium hydroxide
and phosphoric acid. Second, the pyrolysis of the obtained raw material resulted in CS carbon,
which would act as carrier and building blocks in our hybrid. Finally, Au NPs CS carbon functional
hybrid was synthesised by taking advantage of in situ growth of Au NPs on CS carbon via a one-
step reaction. The synthesised Au NPs CS carbon hybrid was collected by centrifugation and then
dispersed to take further characterisation.
The microstructure of the activated carbons produced from cotton stalk is shown in Figure 1. The
SEM and TEM images show that the shape was maintained after the activation. The final carbon
sample is a crushed small rod or cylinder at macroscopic scale. External surface gives us an interest-
ing perspective of the microscopic aspect of the cross section of the carbon particle, which resembles
a wispy-type structure consisting of nanotubes, most of which were in irregular shape though.

Figure 1. Fabrication procedure of cotton stalk (CS) carbon/gold nanoparticles (Au NPs) hybrid. (a) SEM image of cotton stalk car-
bon (CS carbon). (b) TEM image of CS carbon. (c) Nitrogen adsorption desorption isotherms and (d) pore size distribution of CS
carbon.
474 W. ZHU ET AL.

Figure 1(b) indicates the high-resolution TEM of the activated carbon. High porosity is the most sig-
nificant character, corresponding to the ultra-low density. In conclusion, not only the macroscopic
aspect is maintained but also the interior part of the precursor is directly transformed from the cot-
ton stalk to the activated carbon.
Porosity is an important factor in the selection of activated carbons for a particular application.[9]
Physical activation of lignocellulosic materials tends to generate microporous activated carbons.
Phosphoric acid leads to the development of both micropores and mesopores in the resulting carbon
structure.[21,22] The production conditions and the biopolymer composition of the biomass
material, including cellulose, hemicellulose and lignin, are the main influential factors of mesopore
fraction.[23]
Figure 1(c) and 1(d) shows the N2 adsorption desorption isotherms and pore size distribution of
the CS carbon. From the adsorption isotherm, the characteristic adsorption is below a relative pres-
sure of 0.2 due

to the filling of the micropores. The micropore size distribution becomes intense
around 140 A, as shown in Figure 1(d) and calculated using the Horvath Kawazoe method. As is
known, nanoporous carbon materials with high surface area can be prepared by physical or chemical
activation or templating method.[24,25] Herein, we present a universal method to prepare the car-
bon material with high surface area and abundant micropores. Activated carbon powder with a very
high surface area is a promising candidate for the preparation of catalysts carriers.[26] To enhance
catalytic performance, nanoscale porosity is highly desired, facilitating high mass transfer fluxes and
high active loading.[27]

3.2. Characterisation of CS carbon/AuNPs

In addition, by adjusting the concentration ratio of the cotton stalk carbon and chloroauric acid in
suspension, the distribution density of AuNPs on cotton stalk carbon can be easily tuned. As con-
firmed by SEM images (Figure 2(b) and 2(d)), when the concentration ratio of the chloroauric acid
solution and cotton stalk carbon in suspension gradually increased, the distribution density of
AuNPs on the cotton stalk carbon also increased. In particular, when the adding volume of

Figure 2. (a c) SEM images of CS carbon/Au NPs prepared by adding different amount of chloroauric (2, 4, 6 mL, 1 wt%), respec-
tively. (d) Size distribution of the prepared gold nanoparticles. (e) XRD spectra of CS carbon and CS carbon/AuNPs hybrid.
 JOURNAL OF EXPERIMENTAL NANOSCIENCE 475

chloroauric acid reached 6 mL, the formed AuNPs next with each other began to appear overlapping
part. Thus, the 6-mL group was considered as a favourable ratio.
Figure 2(d) and 2(e) demonstrates the size and distribution of gold nanoparticles loaded on
the cotton stalk carbon. The gold nanoparticles size range from several nanometer to 50 nm.
The procedure also yielded dispersions of narrow size distribution at around 20 nm as exem-
plified by Figure 2(d). The X-ray diffraction (XRD) patterns of CS carbon/Au NPs hybrid
index well with Au nanoparticles. Besides, the peaks at around 24 were also observed, result-
ing from the cotton stalk carbon. The diffraction peaks at Figure 2(e) reveal that the hybrid
was composed of two kinds of materials with distinct crystal structures. Except for those dif-
fraction peaks assigned to cotton stalk carbon, the residual diffraction peaks matched well
with the XRD pattern of Au nanoparticle at around 40 which is assigned to diffraction peaks
from various published crystal structure data.[28]

3.3. Photothermal effect of CS carbon/AuNPs hybrid

The relationship between the photothermal effect of the CS carbon hybrid and amounts of chlorine
acid gold was studied. CS carbon/Au NPs hybrid was dispersed in water forming a uniform suspen-
sion. As shown in Figure 3, when the amounts of chlorine acid gold increased, which indicated the
higher density of gold nanoparticles, the photothermal effect became more and more obvious. The
solution temperature for the CS carbon/Au NPs containing group increased rapidly, and even can
reach 55  C, only exposed to light for 5 min, compared with only a slight increase in bare CS carbon
acting as control groups. In addition, as the amount of the AuNPs in CS carbon decreased, the heat-
ing rate was lower. As the concentration of chlorine acid gold increased from 0 to 2 mL, there was
an apparent increase of the photothermal effect. However, when the concentration of chlorine acid
gold increased from 4 to 6 mL, increment in the slope of the curve decreased. So, it is reasonable to
believe that there is a saturation value of chlorine acid gold to reach the strongest photothermal
effect. The uniform distribution of AuNPs on the surface of the porous carbon should contribute to
the excellent photothermal efficiency owing to the collective electromagnetic coupling effect.[29]
These results demonstrate that the combination of CS carbon and Au NPs is a feasible and effective
method to prepare functional materials. CS carbon serves as carrier, while AuNPs as functional
elementary.

60
CS carbon
CS carbon/Au NPs 2mL
CS carbon/Au NPs 4mL
50
Temperature ( C)

CS carbon/Au NPs 6mL

o

40

30

20
0 1 2 3 4 5 6
Time (min)
Figure 3. Temperature rise traces of the solution added with different CS carbon/AuNPs hybrid under irradiation of an 808 nm
infrared diode laser with a power density of 8 W cm¡2.
476 W. ZHU ET AL.

3.4. Property CS carbon/AuNPs for glucose detection

AuNPs are also observed to enhance the activities of glucose oxidase (GOx) and horseradish peroxi-
dase.[30] Because of strong surface plasmas resonance absorption and high extinction coefficient in
the visible region, AuNPs extend its application according to the brilliant red colour. AuNPs can cat-
alyse the conversion of glucose into H2O2 by GOx, colorimetric glucose detection could be readily
realised.[31]
Using the intrinsic peroxidase-like activity of AuNPs, we designed a colorimetric method to
detect glucose. A typical concentration versus absorption response curve for glucose detection by
using the colorimetric method is shown in Figure 4(a). The method we designed shows high selectiv-
ity for glucose because GOx has a high affinity to oxidise glucose. Thus, the colorimetric method
developed herein is highly selective toward glucose detection. Figure 4(b) shows a typical glucose
concentration response curve under optimal conditions. From Figure 4(b), the catalytic activity of
AuNPs shows a glucose concentration-dependent effect, as low as 5 £ 10¡6 M, which is much lower
than values reported in the literature for Fe3O4.[32] Glucose could be detected with a linear range
from 5 £ 10¡6 to 5 £ 10¡4 M by this method. Because GOx could be denatured in pH 4.0 buffer
solution, glucose detection was realised in two separate steps, as described in detail in Materials and
methods section. The oxidation of glucose with GOx was performed in pH 7.0 buffer solution to
produce H2O2, which was detected by using the as-prepared CS carbon/Au NPs. Therefore, the
colorimetric detection of glucose could be easily realised.

3.5. Catalytic performance of p-nitrophenol

Besides, the AuNPs loading on the porous activated cotton stalk carbon could also endow these
hybrids with catalytic properties such as catalytic reduction of p-nitrophenol. After the addition of
CS carbon/Au NPs hybrids into a yellow mixed solution of p-nitrophenol and NaBH4 and a shake
at room temperature for 3 min, the solution became colourless. In contrast, the solution without
adding hybrid catalyst was still yellow. The colour fade of the solution mixed with the CS carbon/
Au NPs hybrid indicated the highly catalytic role of the hybrid on the reduction of p-nitrophenol by
NaBH4. The process of the reduction action of p-nitrophenol was further revealed by UV vis
absorption spectra.
As shown in Figure 5(a), with the time prolonging, the absorption of p-nitrophenol at 400 nm
decreases; meanwhile, a new peak at 295 nm appears and gradually increases, indicating the reduc-
tion of p-nitrophenol to generate p-aminophenol. More attractively, the CS carbon/Au NPs hybrid
has a good stabilisation and cyclic capability. The reusability of the CS carbon/Au NPs hybrid was
investigated by repeated collection and redispersion in a fresh mixture of p-nitrophenol and NaBH4.
This may result from the AuNPs stably anchored on CS carbon, taking the inevitable loss of AuNPs

Figure 4. (a) UV absorption spectra of TMB upon the addition of different concentrations of glucose. (b) The line arrangement of
different concentrations of glucose (R2 D 0.998).
 JOURNAL OF EXPERIMENTAL NANOSCIENCE 477

102 0
2 0min First catalysis
3min -1 Tenth catalysis

Conversion efficiency (%)

6min
9min 100
12min -2
Abs. (a. u.)

ln(C/Co)
15min
1 -3
98

-4

0 96 -5
250 300 350 400 450 500 2 4 6 8 10 0 5 10 15 20 25 30
Cycle times Time (minutes)
Wavelength (nm)

Figure 5. (a) The reduction of p-nitrophenol in aqueous solution recorded at several intervals using CS carbon/AuNPs hybrid as a
catalyst. (b) The reusability of the CS carbon/AuNPs hybrid as a catalyst for the reduction of 4-nitrophenol by NaBH4. (c) The rela-
tionship between ln(Ct/C0) and reaction time (t), wherein Ct/C0 values of 4-nitrophenol were directly given by the relative intensity
of the respective absorbance At/A0.

into consideration. Figure 5(b) shows that even after 10 cycles, the hybrid separated from the previ-
ous reaction solution by filtration exhibited similar catalytic performance without an obvious
decrease in the conversion efficiency for the same reaction time (15 min). The linear relationship
between ln(Ct/C0) and reaction time (t) shown in Figure 5(c) reveals the reaction rate of this reduc-
tion process, which matches with the first-order reaction kinetics because reductant concentration is
much higher than that of p-nitrophenol (CNaBH4/Cnitrophenol D 158). The rate constant k was calcu-
lated to be 9.9 £ 10¡3 s¡1 and 3.1£10¡3 s¡1 for the first catalysis and tenth catalysis reactions,
respectively, which indicates that the reaction rate decreased threefold after reusing the hybrid cata-
lyst for 10 times.

4. Conclusions
In the present work, we propose the use of cotton stalk to prepare activated carbon with porous
structure, by treating the sample with sodium hydroxide, phosphate, followed by pyrolysis at
850  C. High porosity is the most significant

character, considering the micropore size distribution
of AC which is intensely around 140 A. Gold nanoparticles distribute uniformly on the surface
resulting from the functional chemical group in and out of the nanopores. Thus, the assembly pro-
cess is thought to be facile and successful.
As to the characterisation of the performance, the hybrid shows its multifunctionality due to the
introduction of the AuNPs. The catalytic activity of the hybrid shows a glucose concentration-
dependent effect, of which the lowest concentration is 5 £ 10¡6 M. The photothermal effect was
demonstrated, heating the water containing the hybrid up to 55  C, only exposed under light for
5 min. When used as catalyst for the reduction of p-nitrophenol, the hybrid shows a good reusability
up to 10 cycles. This facile and universal preparing method for multifunctional hybrid materials not
only satisfies requirements for practical applications but also provides an alternative idea to func-
tionalise carbon materials.

Disclosure statement
No potential conflict of interest was reported by the authors.

Funding
This work was supported by the Open Foundation of Joint Laboratory for Extreme Conditions Matter Properties,
Southwest University of Science and Technology and Research Center of Laser Fusion, CAEP [12zxjk09]; Science and
Technology Project of Mianyang City [12G031-2]; Scientific Research Fund of Sichuan Provincial Education Depart-
ment [11ZB191]; the Open Project of State Key Laboratory Cultivation Base for Nonmetal Composites and Functional
Materials [12zxnp08]; Fundamental Science on Nuclear Waste and Environmental Security Laboratory [12zxnp08].
478 W. ZHU ET AL.

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