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CERAMICS

INTERNATIONAL

Available online at www.sciencedirect.com

Ceramics International 40 (2014) 13151– 13157

Luminescence properties of chlorine and oxygen co-doped ZnS

nanoparticles synthesized by a solid-state reaction

Zhong Chen

, Xiao Xia Li

, Guoping Du

, Quanmao Yu

,BoLi

, Xinyang Huang

School of Materials and Mechanical and Electrical Engineering, Jiangxi Science and Technology Normal University, Nanchang 330013, PR China

Institute of Functional Materials, Jiangxi University of Finance and Economics, Nanchang 330013, PR China

School of Materials Science and Engineering, Nanchang University, Nanchang 330031, PR China

School of Materials, Anshan University of Science and Technology, Anshan 114051, PR China

Received 19 March 2014; received in revised form 6 May 2014; accepted 6 May 2014

Available online 14 May 2014

Abstract



and O

2

co-doped ZnS nanoparticles were synthesized using a low temperature solid-state reaction method. X-ray diffraction (XRD),

X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), and ultraviolet–visible spectroscopy were used to characterize

their crystal structure, chemical state, diameter, surface states, and photoluminescence (PL) properties. The effects of Cl



and O

2

doping

concentration on the crystal structure, the crystallite size, and luminescence properties of ZnS nanoparticles were investigated. The results

indicated that the ZnS:Cl, O nanoparticles had a cubic blende structure, and an average crystallite size of about 4.28–5.08 nm. It was found that

the PL intensity of the Cl



and O

2

co-doped ZnS nanoparticles remarkably increased with the increase of Cl



and O

2

doping concentration.

The emission intensity of the 7 mol% Cl



and 4 mol% O

2

co-doped ZnS nanoparticles was about 4 (10) times stronger than the ZnS doped

with Cl



2

) nanoparticles. Mechanism for the enhanced luminescence of Cl



and O

2

co-doped ZnS nanoparticles was discussed.

This work suggests that the low temperature solid-state reaction method can be used to synthesize Cl



and O

2

co-doped ZnS nanoparticles with

strong PL properties.

Keywords: ZnS; Nanoparticles; Photoluminescence; Co-doped; Solid-state reaction

1. Introduction

In recent years, ZnS nanoparticles with a large surface to

volume ratio are becoming more and more attractive due to

their quantum size effect, size- and shape-dependent photo-

emission, and superior luminescent characteristics [1–5]. One

of the important properties of ZnS nanoparticles is the

luminescence property. For ZnS nanoparticles to have wider

applications in optoelectronics, they must possess a strong

luminescence property. One of the methods to improve the

luminescence property of ZnS nanoparticles is to introduce

certain dopants into ZnS nanoparticles. Elements such as Mn

[6],Cu[7,8],Al[9],Te[10],Eu[11],Mg[12],Fe[13],

Pb [14] and Cr [15] have been doped into ZnS nanoparticles,

and improved luminescence has been observed.

Although the previous studies on doped ZnS nanoparticles

were mostly focused on cation doping, anions have also been

found to be effective dopants for substituting S ions in ZnS

nanostructures. Okamoto et al. [16] found that in ZnS:TbF

thin ﬁ lm when x ¼1, this ZnS:TbF thin ﬁlm gave a high

electroluminescence efﬁciency. Manzoor et al. [17] employed

a wet-chemical precipitation method to synth esize ZnS nano-

particles co-doped with Cu

and halogen ions such as F, Cl,

Br or I, and they observed a luminescence enhancement. In

their work, the F, Cl, Br or I doping ions were supplied by

ammonium halogen salts. Yu et al. [18] observed that the

optoelectronic properties of the Cl



-doped ZnS nanoribbons

prepared via thermal evaporation was signiﬁcantly improved

as compared with the undoped ones. Akimoto et al. [19] doped

www.elsevier.com/locate/ceramint

http://dx.doi.org/10.1016/j.ceramint.2014.05.019

Corresponding author. Tel./fax: þ86 791 83874867.

E-mail address: lixiaoxia04@sina.com (X.X. Li).

2

into single-crystal line ZnS using the molecular beam

epitaxy method, and they found that O

2

dopants act as

acceptors in ZnS. In our previous work, we have synthesized

ZnS:Br, ZnS:Cl and ZnS:O nanoparticles using a low tem-

perature solid-state reaction method as one of systematical

work [20–22], and the results showed that Br



,Cl



and

2

doping enhanced remarkably the photoluminescence (PL)

properties of the ZnS nanoparticles.

In this work, we synthesized Cl



and O

2

co-doped ZnS

nanoparticles using the low temperature solid-state reaction

method for the ﬁrst time, and studied their luminescence

properties. A strong luminescence enhancement in the Cl



and O

2

co-doped ZnS nanoparticles was observed compared to

only Cl



or O

2

doped ZnS nanoparticles.

2. Experimental

A facile solid-state reaction method was used to prepare

ZnS:Cl, O nanoparticles at low temperatures. All chemicals

used in this work were analytical-grade reagents and purchased

from Sinopharm Chemical Reagent Co., Ltd. C

NS (TAA),

Zn(CH

COO)

, (ZnAc

), NaCl and NaOH were the source

materials for supplying S, Zn, Cl, and O, respectively, for the

doped ZnS nanoparticles.

2.1. Synthesis of ZnS

0.93 x

0.07

nanoparticles

2

doping concentration in the ZnS:Cl, O nanoparticles was

set according to the molecular formula ZnS

0.93x

0.07

,where

x=0, 0.02, 0.04, 0.06, 0.08 and 0.1 (the molar ratio of NaOH to

NaCl to TAA to ZnAc

,namely,O:Cl:S:Zn=0:0.07:0. 93:1,

0.02:0.07:0.91:1, 0.04:0.07:0.89:1, 0.06:0.07:0.87:1 , 0.08:0.07:

0.85:1 and 0.1:0.07:0.83:1). Source materials according to a desired

stoichiometric ratio were weighed, and they were intimately mixed.

After mixing the starting materials with ethanol, the mixture

reacted at 120 1C for 3 h, and then was dispersed into the water

solution. The precipitates were retrieved by centrifugation and

washed several times with acetone to remove the residues. The

washed precipitates were then dried at 30 1C for 10 h.

2.2. Synthesis of ZnS

0.96 y

0.04

nanoparticles



doping concentration in the ZnS:Cl, O nanoparticles

was set according to the molecular formula ZnS

0.96y

0.04

where y=0, 0.01, 0.03, 0.05, 0.07 and 0.09 (the molar ratio Cl:

O:S:Zn=0:0.04:0.96:1, 0.01:0.04:0.95:1, 0.03:0.04:0.93:1,

0.05:0.04:0.91:1, 0.07:0.04:0.89:1 and 0.09:0.04:0.87:1).

The synthesis process was the same as that stated in the

Section 2.1.

2.3. Characterization

The crystal structure of the samples was investigated by the

X-ray diffraction (XRD) technique (GMBH Bruker D8

ADVANCE, CuKα) at room temperature. Silicon powder

was used as the internal standard. The scanning speed and

step for measurements were 21/min, and 0.021 in the range of

(2θ ¼20–701). The microstructures of ZnS:Cl, O nanoparticles

were observed with transmission electron microscopy (TEM,

JEM-2010). X-ray photoelectron spectroscopy (XPS) measure-

ments were performed on a PerkinElmer PHI 5000C electron

spectroscopy for chemical analysis system (made by Perki-

nElmer Corporation in America). All the binding energies

were calibrated by using the contaminant carbon (C 1s¼284.6

eV) as a reference. Diffuse reﬂection spectroscope measure-

ments were carried out on a UV–vis–NIR Cary-5G spectro-

photometer. Absorption spectra of the samples were obtained

from the diffuse reﬂectance values by using the Kubelka–

Munk function [23]:

FðRÞ¼

ð1RÞ

ð1Þ

where R, K and S are the re ﬂection, the absorption and the

scattering coefﬁcient, respectively. The excitation and emis-

sion spectra were measured by an F-2500 spectrophotometer

with Xe900 (450 W xenon arc lamp) as the excitation source

with spectral slits width of 1 nm. The scanning speed and step

for measurements were 60 nm/min and 0.5 nm, respectively.

All the spectra were recorded at room temperature.

3. Results and discussion

Fig. 1 shows the XRD patterns of ZnS

0.93x

0.07

(0r xr 0.1) (a) and ZnS

0.96y

0.04

(0r yr 0.09) (b)

samples. The three diffraction peaks in the XRD patterns for

all products were indexed as the (111), (220) and (311) crystal

planes of cubic zinc blende ZnS crystal structure and no

observable impurity phases were seen, which matches very

well with the standard card (JCPDS no. 77-2100) showed by

the short lines in Fig. 1. Diffraction peaks from high angles

have submerged in the background in the XRD patt erns due to

large line broadening, which may be due to the nanosized of

particles [24].

Also, the typical broadening of the diffraction peaks was

observed in Fig. 1, whi ch indicated that the particle sizes of

the samples were very small. The average crystallite size of

the samples can be calculated from the XRD patterns using

Scherrer's formula [25] , and was within a range from 4.24 to

4.65 nm and from 4.24 to 5.08 nm for ZnS

0.93 x

0.07

and

ZnS

0.96 y

0.04

samples, respectively (Tables 1 and 2).

Thus, all th\e samples were in fact nanoparticles.

The lattice constant a was estimated using the Bragg

formula [25]:

a ¼

2 sin θ

ﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ

þk

þl

ð2Þ

where λ is the X-ray wavelength (1.54056 Å), θ is the Bragg

angle, and the Miller index of the crystal plane is (hkl). The

lattice constant of ZnS

0.93x

0.07

and ZnS

0.96y

0.04

was obtained by Eq. (2) and was from 5.3397 to 5.3864 Å

(Table 1) and from 5.3746 to 5.3798 Å ( Table 2), respectively.

It was found in Tables 1 and 2 that the lattice constant a

decreased with the increase of O

2

and Cl



content. This can

be explained by the fact that O

2

(1.38 Å) and Cl



(1.67 Å)

Z. Chen et al. / Ceramics International 40 (2014) 13151–1315713152

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