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- 1 -

Preparation and Gas Sensing Properties of Novel

CdS-Supramolecular Organogel Hybrid Films

Xia Huiyun，Peng Junxia，Liu Kaiqiang，Fang Yu

∗

Key Laboratory of Applied Surface and Colloid Chemistry of Ministry of Education，School of

Chemistry and Materials Science，Shaanxi Normal University，Xi’an （710062），PRC

E-mail：yfang@snnu.edu.cn

Abstract

A novel CdS-supramolecular organogel hybrid film with an unusual surface morphology has been

fabricated by exposing a supramolecular organogel film containing Cd(Ac)

in an H

S atmosphere at

room temperature. The organogel film was prepared by spin-coating a LMOG (low-molecular mass

organic gelator) gel of dmethyl sulfoxide (DMSO) onto a glass plate substrate. XRD, SEM, EDS,

TG-DTA, UV-vis, PL (photoluminescence) spectroscopy and PL lifetime measurements were

employed to characterize the film. It was shown that the organogel film had functioned as a template to

control the morphology of the final hybrid film. The quantities and sizes of the CdS particles embedded

in the organogel film can be easily altered by varying the initial concentration of Cd(Ac)

. Importantly,

the PL of the hybrid film is very sensitive to the presence of some organic monoamines and diamines.

The selectivity and reversibility of the sensing process were investigated.

Keywords：CdS，organic monoamines and diamine，LMOG，hybrid films，sensing

1．Introduction

Amines are a family of compounds, and have become intense pollutants due to their extensive uses in

the preparation of fertilizers, pharmaceuticals, surfactants, biological buffers, and colorants, etc.

[1a]

Furthermore, volatile amines can be found in agricultural areas, and presence of them may be taken as

an indicator of decayed food, as is the case of fish products

[1b]

, and thereby accurate and fast detection

of amines is of great interests. It is well known that CdS films and particles have been widely used in

gas-sensing

[2]

. Ellis and co-workers have embarked on the area for years, and found that n-CdS or

n-CdSe in single crystal state can be used as a “luminescent litmus test” to sense the presence of a

variety of Lewis acids and bases. The photoluminescence (PL) was found to increase when n-CdS or

n-CdSe was exposed to Lewis bases and decrease when exposed to Lewis acids

[3]

. The direction of the

PL response appears to reflect adsorbate-induced changes in the semiconductor’s depletion width and

can be modeled by treating a near-surface region of this approximate thickness as non-emissive layer

(dead-layer model). The photoconductivity and electrical conductivity of CdS have been used for the

detection of CO and SO

, respectively

[4, 5]

. In addition, NH

can be also determined by monitoring the

PL emission of a powered CdS:Te phosphor

[6]

Different from fluorescence sensors based upon organic fluorophores, the gas-sensing properties

of CdS are highly dependent upon its morphological and microstructural features, such as particle size,

size distribution, shape and density, etc.

[7]

. Recently, considerable efforts have been devoted to develop

film sensors. This is because film sensors are, generally speaking, re-usable, and easy to be made into

devices

[8]

. Film sensors can be fabricated by employing vacuum evaporation, chemical vapor

deposition (CVD), molecular beam epitaxy (MBE), sputtering, electrochemical co-deposition, and

electrochemical atomic layer epitaxy (ECALE), etc.

[9]

. However, many of these known methods suffer

from one or more drawbacks such as prolonged post-process (e.g., annealing) time, expensive

apparatus, and production of a large amount of wastewater, etc.

[9e]

∗

This work is supported by Natural Science Foundation of China (Nos. 20674048), Doctoral Program Foundation

of the Ministry of Education of China (Nos. 20040718001, 306015).

http://www.paper.edu.cn

- 2 -

Chemical gels are interesting materials, in which gelator molecules are crosslinked into network

structures and the solvent are fixed by the networks. It is these gels that have been used as templates for

the “bottom-up” fabrication of various nano-structured inorganic and inorganic-organic composite

materials

[10]

. It is believed that the gel networks can control and direct the crystallization and

precipitation of the inorganic compounds formed within the gels, and result in composite materials with

specific structures

[11]

. Unlike chemical gels, physical gels formed by low-molecular-weight organic

gelators (LMOGs) are thermo-reversible, and of particular importance and interest because of the

essential differences in properties and forming mechanisms

[12]

. Very recently, these physical gels have

been adopted as templates to produce various nano-structured materials, including rods, belts, tubes,

balls etc.

[13]

. In addition, integration of inorganic nano-particles into the interior of a gel network have

aroused great interest since this would result in inorganic/organic nano-composite materials, which

would combine the advantages of inorganic, organic and nano-materials and offer opportunities to

explore their novel collective mechanical, thermal, optical, magnetic, and electronic properties

[10,12]

On the basis of above discussion and the work already conducted in our group

[14]

, an organogel

film based upon a LMOG was employed as a template for the preparation of organogel-CdS hybrid

film. It was found that the hybrid film occupies an unusual morphology, and the PL is selectively

sensitive to the presence of some organic monoamines and diamines. The details are reported in this

paper.

2．Experimental Details

2.1 Materials

All reagents are analytically pure. Cd(Ac)

, thioacetamide, Boc-L-alanine, cholesterol,

dicyclohexylcarbodiimide (DCC), N,N-dimethylamino-pyridine (DMAP), and sodium hydroxide were

used as received. Dichloromethane, tetrahydrofuran (THF), benzene, dimethyl sulfoxide (DMSO),

n-hexane and triethylamine (TEA) were used after further purification by standard literature methods.

Other chemicals, such as methylamine aqueous solution, butylamine, octylamine, dodecylamine,

aniline, N-methylaniline, N,N-dimethylaniline, acetylaniline, ethylenediamine (EDA),

1,3-propanediamine (PDA), 1,4-butanediamine (BDA), 1,5-pentanediamine, 1,6-hexanediamine

(HDA), pyridine, ammonia, water, hydrochloric acid, acetic acid, methanol, ethanol, formaldehyde,

acetone and cyclohexane were used without further purification. Water used throughout was deionized

and then double distilled.

2.2 Preparation of a gel film

The gelator, di-acid amides of di-cholesteryl L-alaninates, was prepared and characterized in the way as

reported in a former report

[14c]

. In a typical preparation of the gel film, 0.0125 g of the gelator and 1 mL

of DMSO containing Cd(Ac)

were placed into a sealed glass tube, and the system was heated in an oil

bath until the gelator was dissolved. Then, suck out 200 μL of the hot solution, and drop it onto the

surface of a pre-cleaned and heated glass plate (~ 0.90 cm×3.50 cm). Finally, the glass plate was

gradually cooled to room temperature, and a stable organogel film was produced.

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