ORIGINAL PAPER

Highly fluorescent cotton fiber based on luminescent carbonnanoparticles via a two-step hydrothermal synthesis method

Yuan Yu . Jian Wang . Jidong Wang . Jing Li . Yanan Zhu . Xiaoqiang Li .

Xiaolei Song . Mingqiao Ge

Received: 30 November 2016 / Accepted: 16 February 2017 / Published online: 6 March 2017

� Springer Science+Business Media Dordrecht 2017

Abstract A kind of highly fluorescent cotton fibers,

in which the luminescent carbon nanoparticles (CNPs)

are generated in the lumen and the mesopores directly, -

have been prepared by the method of hydrothermal

synthesis in situ using citric acid and urea as raw

materials, and hexadecyl trimethyl ammonium bromide

and tributyl phosphate as active agents. The CNPs/cotton

fibers were characterized by thermogravimetry-differen-

tial thermal analysis (TG-DTA), X-ray diffraction

(XRD), field emission scanning electron microscopy

(FESEM) and X-ray photoelectron spectroscopy (XPS),

respectively. The optical properties are investigated by

fluorescence spectrofluorometry and PR-305 long after-

glow phosphors tester. The results showed that the CNPs

were self-assembled successfully in the lumen as well as

in the mesopores of cotton fibers. The CNPs/cotton fibers

could emit bright and colorful photoluminescence under

excitation lights of different wavelengths. The afterglow

decay process could be divided into fast decay and slow

decay stages and the emission of CNPs/cotton fiber had

two peaks at 450 nm and 570 nm respectively when

the wavelength of excitation changed from 310 nm to

500 nm. The preparation of highly fluorescent cotton

fibers by self-assembly method has great significance to

the functionalization of cotton fibers.

Keywords Fluorescent � Cotton fiber � Carbonnanoparticles � Hydrothermal synthesis

Introduction

Compared to organic dyes (Qu et al. 2012; Li et al.

2011a; He et al. 2011), luminescent carbon nanoparticles

(CNPs) had distinct benefits, such as chemical inertness,

low cytotoxicity, and fantastic biocompatibility which

attracted increasing interests. So far, CNPs could be

prepared bymanymethods. Sun and his co-workers (Sun

et al. 2006) prepared the quantum-sized carbon dots by

laser ablation method for the first time, Li and his co-

workers (Li et al. 2010b) fabricated CNPs which could

emit blue, green, yellow and red lights respectively with

sizes of 1.2–2.8 nm by electrochemical method. After

Y. Yu � J. Wang � J. Wang � J. Li � Y. Zhu �X. Li � X. Song � M. Ge (&)

Key Laboratory of Eco-Textiles, Ministry of Education,

College of Textiles and Clothing, Jiangnan University,

Wuxi 214122, China

e-mail: ge_mingqiao@126.com

Y. Yu

e-mail: yuyuan8619463@163.com

J. Wang

e-mail: Jwangjn@gmail.com

J. Wang

e-mail: jidongwang23@163.com

J. Li

e-mail: lj7980062@163.com

X. Li

e-mail: 6120705016@vip.jiangnan.edu.cn

X. Song

e-mail: sxlyanc@126.com

123

Cellulose (2017) 24:1669–1677

DOI 10.1007/s10570-017-1230-0

then, Qu and his co-workers (Qu et al. 2012) prepared

CNPs with high quantum yield through simple

hydrothermal method. Zhu and his co-workers (Zhu

et al. 2009) offered a simple and economical method for

the preparation of high fluorescence quantum yield

CNPs by microwave method.

Compared to other functional materials, the lumines-

cent carbon nanoparticles could be applied on fibers

through the methods of mechanical adhesion, pad

finishing and coating (Xu et al. 2015b; Cheng et al.

2015) which needed complicated processes and various

nonfunctional auxiliaries. Unfortunately, these methods

caused some disadvantages, such as poor comfort-

able performance, bad air permeability (Yang et al. 2009;

Goncalves et al. 2009) and hindrance of mechanical

properties, which greatly limited their application.

Therefore, it was necessary to generate an efficient

fabrication method to prepare the new fluorescent fibers.

Cotton fiber is a kind of wildly used natural fiber in

our life and it gets people’s favor continually due to its

advantages of excellent water absorption, heat-resis-

tant quality, soft-feeling, comfortable to wear, low-

cost and easy to degrade (Xu et al. 2015a). More-

over, cotton fiber is known as having a large amount

of nano-scaled pores in microfibrillar, fibril, sec-

ondary cell wall, and a lumen in the center of a cotton

fiber (Mao et al. 2014). It is an excellent and unique

natural microreactor to prepare nanocomposites via

the nanomaterials generated directly in the mesopores

and lumens of cotton fibers (Li et al. 2011b). To our

knowledge, however, reports on the fabrication of

CNPs inside cotton fibers have not been reported yet.

The purpose of this work is to fabricate novel

CNPs/cotton fibers, in which CNPs are synthesized in

themesopores and lumens of cottonfibers directly through

a hydrothermalmethod. Thismethod had advantages such

as hypotoxicity, energy saving and no adhesive introduc-

ing. This new functional cotton fiber was proved to have

theproperties of non-toxic andphoto-luminescence.XRD,

FESEM, XPS and UV–Vis fluorescence were used to

evaluate the performances of this functional cotton fibers.

Experimental section

Materials

All the reagents including citric acid (C6H8O7�H2O),

urea (CH4N2O), hexadecyl trimethyl ammonium

bromide (HTAB, C19H42BrN), tributyl phosphate

(C12H27O4P), sodium hydroxyl (NaOH), absolute

ethanol (C2H5OH, 99.7%) were purchased from

Sinopharm Chemical Reagent Co., Ltd. (all AR grade,

Shanghai, China). Cotton fibers were supplied by

Jiangsu Hongdou Industrial Co., Ltd. (Wuxi, China).

Removal of non-cellulosic components

The raw cotton fibers were purified using sodium

hydroxide solution and absolute ethanol to remove the

wax, grease and other various non-cellulose compo-

nent attached to the surface of the cotton during cotton

growth and harvesting, the process was repeated three

times. Previous studies reported that the micropores

and lumens in cotton fibers vary depending on the

concentration of NaOH solution (Hauser and Gudac

2008; Hsieh et al. 1996). Therefore, 0.3 g of cotton

fibers were immersed in 30 mL of a NaOH solution,

the concentration of which were 1 wt%, 5 wt%, 10

wt%, 15 wt%, 20 wt% respectively. Then the mixture

was transferred into a 100 mL Teflon-lined stainless

steel autoclave, sealed and heating in an oven to

100 �C and kept for 1 h. After that, the distilled water

was used to rinse the fibers in neutral conditions

(pH = 7). Then the fibers were immersed in absolute

ethanol to remove wax. Pure cotton fibers were

obtained after drying in an air dry oven.

Preparation of fluorescent CNPs/cotton fibers

The preparation procedure of CNPs/cotton fibers is

showed in Fig. 1. Firstly, 3 g of urea and 3 g of citric

acid were dissolved in 30 ml deionized water, then

0.1 g hexadecyl trimethyl ammonium bromide and

40 ll tributyl phosphate were added as active agent tomake the solution infiltrate into the cotton more easily.

Secondly, 0.3 g of cotton fibers pretreated by sodium

hydroxide solution were immersed in the above

solution, subjected to ultrasonic treating for 30 min

until the fibers were transparent and well dispersed.

The mixture was transferred into a 100 mL Teflon-

lined stainless steel autoclave and the hydrothermal

synthesis reaction proceeded at 150 �C for 3 h. The

obtained cotton fibers were washed by deionized water

twice for 10 min each time in ultrasonic bath after the

hydrothermal reaction, and were then rinsed with

alcohol for three times. Finally, the fibers were dried in

1670 Cellulose (2017) 24:1669–1677

123

the air drying oven (Li et al. 2011b). The formation

mechanism of carbon nanoparticles is shown in Fig. 2.

Characterization

The thermal stability of CNPs/cotton fibers were

analyzed by TA instrument (Q500, New Castle, DE,

USA) in N2 atmosphere and the temperature range was

from 50 to 1000 �C at a scanning rate of 10 �C/min-1.

The X-ray diffraction (D8 Advance X-ray diffrac-

tormeter, Bruker AXS, Germany) was used to measure

the phase composition of pretreated cotton and

CNPs/cotton fibers by a Cu Ka radiation under

40 kV/40 mA, of which the diffraction angle 2hranges from 5� to 70� with a scanning speed 0.1 s/

step at room temperature. The test system was

equipped with a mono Al Ka X-ray source

(1486.6 eV). The data analysis was carried out under

the conditions of UHV (109 e1010 Torr). X-ray

photoelectron spectrometer (XPS) experiments were

performed by a Thermal ESCALAB 250XI X-ray

source system (USA). The cross-section morphology

of CNPs/cotton fibers was analyzed by field emission

scanning electron microscopy (QUANTA250, FEI,

USA). The excitation and emission spectra of the

CNPs/cotton fibers were tested by spectrofluorometer

(FS5, Edinburgh) at room temperature. The fluores-

cence microscope images were tested by a Nikon

ECLIPSE Ti–S fluorescence microscope. The after-

glow characteristics of the samples were evaluated

using a PR–305 long afterglow phosphors tester.

Fig. 1 The process of preparation of fluorescent CNPs/cotton fibers

Fig. 2 The formation mechanism of carbon nanoparticles

Cellulose (2017) 24:1669–1677 1671

123

Results and discussion

Thermal stability of CNPs/cotton fibers

The thermal stability of the cotton fibers assembled

with CNPs was examined by TGA and was depicted in

Fig. 3. The results show that the cotton fibers

pretreated by different concentration of sodium

hydroxide had similar thermal degradation curves.

The weight loss of CNPs/cotton fibers can be divided

into three stages. The weight loss during the temper-

ature from 50 �C to 300 �C was due to the moisture in

the fibers and partial damages in the amorphous area of

the fiber. The initial temperature of the main decom-

position stage was at ca. 300 �C. In the range from

300 �C to 400 �C, the decomposition rate was signif-

icantly larger, and the weight loss was about 70% of

the total mass at the end of this stage, which is

attributed to the pyrolysis of cellulose (Yang et al.

2007; Mostashari and Mostashari 2008) hemicellu-

lose, lignin and other organic compositions. At above

400 �C, the cellulose continued to carbonize, with

decomposition much lower and the weight loss curve

levelled off at 500 �C. From the partially enlarged

region from 550 �C to 700 �C, we can see that the

weights of the final residue were different. The final

residue of pure cotton fiber was 5.5%, while the final

residue of CNPs/cotton fibers were 6.9%, 10%,

10.5%, 11.5% and 11.4%. The difference in residual

mass between the cotton fibers and the CNPs/cotton

fibers accounted for the content of CNPs assembled in

the fibers, which were calculated as 1.4%, 4.5%, 5%,

6% and 5.9%. The final residue mass almost increased

with elevated concentration of sodium hydroxide. The

reason may be that when the sample pretreated by

sodium hydroxide solution, the wax, grease and other

various non-cellulose components were removed. The

increasing of sodium hydroxide solution concentration

and the increasing of amorphous regions of cotton

made the molecules diffuse into the fibers more easily,

hence the proportion of CNPs assembling in the fiber

increased. The quality of CNPs assembled in the

cotton decline slightly when the sodium hydroxide

concentration was about 20%. The reason for this

phenomenon is that when the sodium hydroxide

concentration is higher, the cotton fibers’ swelling

performance will be more obvious, leading to the

pores and lumens within the fibers decreased or even

disappeared (Amel et al. 2013).

XRD analysis

XRD analysis was used to characterize the crystal

structure of cotton and CNPs/cotton. The XRD results

revealed that the crystal shape of CNPs/cotton fiber

changed after pretreated by sodium hydroxide. XRD

results gave 5 peaks of 2hwhen the sample was treated

with different concentrations of sodium hydroxide

solution which were 10%, 15% and 20%. These 2hwere 14.3�, 16.1�, 21.9�, 11.7�and 21.5� in which

14.3�, 16.1� and 21.9� corresponding to the charac-

teristic peaks of cellulose I (Singh et al. 2015), and

11.7�and 21.5� were close to the cellulose II charac-

teristic peaks (Li et al. 2014). This indicates that part

of cellulose I can translate to cellulose II when the

cotton fibers were pretreated by sodium hydroxide.

While there were no characteristic peaks of CNPs due

to the characteristic peaks of CNPs coincide with the

cotton fiber from about 19� to 23� (Qu et al. 2014).

It can be concluded that the crystallinity of the

CNPs/cotton decreases with increasing of sodium

hydroxide concentration, because the accessibility of

Fig. 3 TG–DTA patterns of CNPs/cotton pretreated by differ-

ent amounts of sodium hydroxide solution: a pure cotton, b 1%,

c 5%, d 10%, e 20%, f 15%

1672 Cellulose (2017) 24:1669–1677

123

the fibers increases after the pretreatment by alkali

swelling. The amount of CNPs generating through the

hydrothermal reaction increased because of more and

more solution immersed into the fiber. The CNPs

generating in the crystal region of the fiber would

damage neat crystalline form as well as the amorphous

regions. Furthermore, the cotton fibers were ultra-

sonically treated for 0.5 h, breaking part of the

macromolecular chains and the supramolecular struc-

ture thus became loose. Ultrasonic treatment could

also lead to a slight misalignment between the

crystallites, resulting in the increasing of the amor-

phous zone and the porosity (Zhang et al. 2015),

coincides with the results of TG (Fig. 4).

XPS analysis

The surface elemental composition of CNPs/cotton

and cotton fiber were investigated by X-ray photo-

electron spectroscopy (XPS) as shown in Table 1. The

XPS spectrum of the cotton (Fig. 5a) shows two peaks

at 284.0 and 530.6 eV, attributed to C1s and O1s,

respectively. While the XPS spectrum of the

CNPs/cotton had three peaks at 284.0, 400.0, and

530.6 eV, which were attributed to C1s, N1s and O1s.

The main component of pure cotton fiber was cellu-

lose, which was nitrogen-free (Tatjana et al. 2007).

The C1s spectrum of the cotton fiber showed three

peaks at 283.3, 285.1 and 286.2 eV (Fig. 5b), which

were attributed to C–C, C–OH/C–O and O–C–O/C=O

respectively. The C1s XPS spectrum of the CNPs/cot-

ton fiber showed three peaks at 283.2, 284.7, 286 eV

assigned to C–C, C–OH/C–O and C=N/C=O respec-

tively. Besides, a peak at 285.3 eV is attributed to C–

N. The N1s spectrum of CNPs/cotton included three

peaks at 397.8, 398.6 and 400.9 eV typical of C–N–C,

N–(C)3 and N–H, confirming the presence of CNPs in

the cotton fibers.

Surface morphology of fluorescent cotton fiber

Cotton fiber with nanoscale porous structure could be

used as a unique template for preparing the nanocom-

posite (Marques et al. 2006). The mixed solutions

could be absorbed into the lumen and pores of the

fibers and the CNPs could be generated in the lumens,

pores and the surface of the fibers through hydrother-

mal treatment. The CNPs attached on the surface of

the fiber could be rinsed away by the deionized water

while the particles in fibers were swaddled by fiber

membrane which could not be washed away easily.

The cross section of CNPs/cotton fiber was

observed by field emission scanning electron micro-

scopy (FESEM) as presented in Fig. 6. From the

photographs at a high magnification, we could clearly

see that there were a large number of carbon

nanoparticles in the porosities, lumen as well as at

the surface of cotton cross-section. The size of the

carbon nanoparticles was extremely small (ca. 3–10

nm) (Fig. 6a, c). A lot of pores exist in the primary and

secondary layers of cotton fibers (Fig. 6b) and the

cross-section of the cotton fiber was spiral-like

network structure. The diameter of pores lied in the

Fig. 4 XRD patterns of pure cotton and CNPs/cotton pre-

treated by different amounts of sodium hydroxide solution: 1%,

5%, 10%, 15%, 20%

Table 1 Binding energies of C1s and N1s by XPS spectras

Sample Peak Binding energy (eV) Assignment

Cotton C1s 283.3 C–C

285.1 C–OH/C–O

286.2 O–C–O/C=O

CNPs/cotton C1s 283.2 C–C

284.7 C–OH/C–O

285.3 C–N

286 C=N/C=O

CNPs/cotton N1s 397.8 C–N–C

398.6 N–(C)3

400.9 N–H

Cellulose (2017) 24:1669–1677 1673

123

range of 50–400 nm, which was larger than those of

ordinary cotton fibers (Mao et al. 2014) due to the

pretreatment by sodium hydroxide solution. It further

proved that proper pretreatment could increase the

porosities size of cotton fibers, thereby enhancing the

ability of absorbing solutions.

Excitation and emission spectral analysis

The CNPs/cotton fibers had a broad absorption band

(Fig. 7a) with two excitation peaks at 312 and 367 nm.

Cotton fibers almost neither competed with CNPs in

absorbing light from the UV to visible wavelengths,

Fig. 5 XPS survey spectra of: a cotton and CNPs/cotton; b C1s element of cotton; c C1s element of CNPs/cotton; d N1s element of

CNPs/cotton

Fig. 6 FESEM images of a the lumen of the CNPs assembled cotton fiber; b the porosities of the cotton fiber; c TEM image of CNPs

1674 Cellulose (2017) 24:1669–1677

123

nor absorbed the emission light of CNPs, which

realized highly efficient emission of CNPs. The fluores-

cent cotton fibers have the property of excitation-

wavelength-dependent photoluminescence (PL) like

CNPs (Qu et al. 2012), with two emission peaks at

450 nm and 570 nm respectively when the wavelength

of excitation varied from 340 to 500 nm as shown in

Fig. 7b. The citric acid and urea did not emit under the

exciting of visible or near-UV light. Therefore, the PL is

attributable to the CNPs generated in the cotton fibers.

The fluorescent images as shown in Fig. 8 further

confirmed the excitation-wavelength-dependent

Fig. 7 Excitation (a) and emission (b) spectrum of CNPs/cotton fiber

Fig. 8 Fiber (a: cotton; b1–b5: CNPs/cotton of 1, 5, 10, 15,

20%) optical images illuminated under white (1, daylight lamp)

and UV light (2, 365 nm); the CIE chromaticity coordinates of

CNP/cotton (3); fluorescence microscope images (4–6) of

CNPs/cotton fiber (the excitation are green light, UV-light and

blue light respectively). (Color figure online)

Cellulose (2017) 24:1669–1677 1675

123

photoluminescence (PL) of the CNPs/cotton fibers.

The images proved that the fibers had a strong

fluorescence emission under the excitation light.

Under the excitation of green, UV and blue light, the

color of the emission was red, blue and green,

respectively. The images also demonstrate the uni-

form dispersion of CNPs in the fibers. Furthermore,

assembling the CNPs into the fibers by hydrothermal

synthesis can inhibit fluorescence quenching (Kwon

et al. 2013, 2014) caused by excessive CNPs accu-

mulation. Afterglow property of fluorescent cotton

fiber.

The afterglow decay curves of the CNPs/cotton

fibers prepared by different concentration of sodium

hydroxide were shown in Fig. 9. The afterglow decay

processes which could be divided into two parts

showed the similar characteristics, quick decay and

slow decay processes. The initial afterglow intensity

of the samples was decreased with reduced

concentration of sodium hydroxide, which further

confirmed that the accessibility of cotton fibers

increased with the increase of sodium hydroxide

solution concentration within a certain range.

The decay trace was fitted with the double expo-

nential decay based on non-linear least squares

analysis.

I ¼ I1 expð�t=s1Þ þ I2 expð�t=s2Þ ð1Þ

In the formula, I is the fluorescence intensity, I1 and

I2 are constants relative to initial brightness, t is time,

and s1 and s2 are lifetimes for fast and slow decays

(Zhu et al. 2014) respectively. The data were obtained

by fitting as shown in Table 2.

Conclusions

The novel CNPs/cotton fibers, in which CNPs

were synthesized inside the mesopores and lumens

of cotton fibers directly via a two-step hydrother-

mal synthesis method were prepared successfully.

The nanoscale pores in the cotton are able to

control the orientation and morphology of the

CNPs, and therefore the nanoparticles can dis-

perse in the porous and lumen of the fibers at nano

scale. The effects of different conditions of sodium

hydroxide solution pretreatment for cotton were

investigated, which showed that the fluorescence

intensity and the proportion of CNPs assembled in

the fibers were highest when the condition of

sodium hydroxide solution was 15%. The

CNPs/cotton fibers have excellent fluorescence

property and excitation-wavelength-dependent pho-

toluminescence. The novel fibers can be applied in

the fields of sensors, anti-counterfeiting materials,

etc. It provides new insights into flexible and

wearable fabric sensors, fiber/ion sensors and anti-

counterfeiting fabrics.

Acknowledgments The authors are grateful for the financial

support of the Priority Academic Program Development of

Jiangsu Higher Education Institutions. The National Natural

Science Funds (NO. 51503083), Jiangsu Province Ordinary

University Academic Degree Graduate Student Scientific

Research Innovation Projects (NO. KYLX16_0798).

Production, Education & Research Cooperative Innovation

Fund Project of Jiangsu Province (No. BY2015057-23). The

Fundamental Research Funds for the Central Universities (NO.

JUSRP51505, JUSRP116020, JUSRP51723B).

Fig. 9 The afterglow decay curves of CNPs/cotton pretreated

by different amounts of sodium hydroxide solution: 1, 5, 10, 15,

20%

Table 2 The parameters of exponential decay of CNPs/cotton

pretreated by different amounts of sodium hydroxide solution:

1, 5, 10, 15, 20%

Samples (%) I1 (a.u.) s1 (s) I2 (a.u.) s2 (s)

1 0.03294 3.92481 0.01528 34.47248

5 0.03800 3.62406 0.01636 34.53264

10 0.04006 3.19934 0.01573 32.82616

15 0.04753 3.66595 0.02108 34.28399

20 0.05318 3.12926 0.01997 32.61001

1676 Cellulose (2017) 24:1669–1677

123

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