Room temperature chemical bath deposition of cadmium selenide, cadmium sulfide and cadmium sulfoselenide thin films with novel nanostructures

Accepted Manuscript Room temperature chemical bath deposition of cadmium selenide, cadmium sulfide and cadmium sulfoselenide thin films with novel nanostructures Cephas A. VanderHyde, S.D. Sartale, Jayant M. Patil, Karuna Ghoderao, Jitendra P. Sawant, Rohidas B. Kale PII:

S1293-2558(15)30027-3

DOI:

10.1016/j.solidstatesciences.2015.08.007

Reference:

SSSCIE 5177

To appear in:

Solid State Sciences

Received Date: 11 March 2015 Revised Date:

9 July 2015

Accepted Date: 8 August 2015

Please cite this article as: C.A. VanderHyde, S.D. Sartale, J.M. Patil, K. Ghoderao, J.P. Sawant, R.B. Kale, Room temperature chemical bath deposition of cadmium selenide, cadmium sulfide and cadmium sulfoselenide thin films with novel nanostructures, Solid State Sciences (2015), doi: 10.1016/ j.solidstatesciences.2015.08.007. This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to our customers we are providing this early version of the manuscript. The manuscript will undergo copyediting, typesetting, and review of the resulting proof before it is published in its final form. Please note that during the production process errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain.

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ACCEPTED MANUSCRIPT Room temperature chemical bath deposition of cadmium selenide, cadmium sulfide and cadmium sulfoselenide thin films with novel nanostructures Cephas A. VanderHydea, S. D. Sartaleb, Jayant M. Patila, Karuna Ghoderaoa, Jitendra P. Sawant and Rohidas B. Kalea,* Department of Physics, The Institute of Science, Madam Cama Road, Mumbai-400032 (M. S.), India

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a

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Department of Physics, University of Pune, Pune-410007 (M. S.), India

Abstract

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A simple, convenient and low cost chemical synthesis route has been used to deposit nanostructured cadmium sulfide, selenide and sulfoselenide thin films at room temperature. The films

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were deposited on glass substrates, using cadmium acetate as cadmium ion and sodium selenosulfate/thiourea as a selenium/sulfur ion sources. Aqueous ammonia was used as a complex reagent and also to adjust the pH of the final solution. The as-deposited films were uniform, well adherent to the glass substrate, specularly reflective and red/yellow in color depending on selenium and

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sulfur composition. The X-ray diffraction pattern of deposited cadmium selenide thin film revealed the nanocrystalline nature with cubic phase; cadmium sulfide revealed mixture of cubic along with

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hexagonal phase and cadmium sulfoselenide thin film were grown with purely hexagonal phase. The morphological observations revealed the growth and formation of interesting one, two and three-

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dimensional nanostructures. The band gap of thin films was calculated and the results are reported. Keywords: A. nanostructures; A. thin films: B. chemical synthesis; C. electron spectroscopy; C. X-ray diffraction; D. optical properties

* Corresponding author Tel.: + 91 22 5715464; fax: +91 22 5715408. E-mail address: [email protected]

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1. Introduction It is well known that the nanocrystalline semiconductors have attracted widespread attention because of their size-dependent structural, morphological, optical and electrical properties [1]. These

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nanomaterials have been widely studied for their fundamental properties and industrial applications, due to their interesting size tunable optoelectronic properties and flexible processing chemistry [2-6]. Cadmium compounds, such as cadmium sulfide (CdS), cadmium selenide (CdSe) and cadmium

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sulfoselenide (CdSSe) (group II-VI) are important semiconductor materials and have been widely used

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in many fields due to their unusual optical and electrical properties [7]. The nanocrystals of these compounds have received considerable attention because of their tunable band gap, which can vary their optical response from the infrared to the ultraviolet region [8]. The CdS and CdSe semiconductors have a direct band gap of 2.42 eV [9] and 1.71 eV [10], and are considered to be excellent materials for

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various optoelectronic applications in the visible range of the electromagnetic spectrum. Some of these applications are biological fluorescent labels, light emitting diodes, lasers, solar cells, photovoltaic cells, electroluminescence, transparent conducting oxides and bio-attachment applications [11-18].

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These nanomaterials are also used in polymer-light emitting diode applications [19] and in polymer electronics [20]. Semiconducting CdSxSe1-x is among most studied alloys due to their wide-range

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tunable band gap from visible 2.42 eV (CdS) to near IR 1.71 eV (CdSe) that have prospective applications in optoelectronics [21]. These metal chalcogenide thin films were deposited using different methods such as chemical vapor deposition [21-24], spray pyrolysis [25-27], physical vapor deposition [28, 29], electrodeposition [30-32] and chemical bath deposition method (CBD) [8, 33, 34]. Among these methods, CBD is the cheapest method to deposit thin films in the form of nanomaterials or nanostructures. It does not require expensive equipment and can be easily upgraded for large area 2

ACCEPTED MANUSCRIPT deposition on the substrates of any desired shape and size. The major advantage of CBD is that it requires only solution containers. The CBD method yields stable, well adherent and uniform thin films with good reproducibility by a relatively simple process even at room temperature. It is suitable method for preparing highly efficient thin films in a simple manner. The nature and features of deposited

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nanocrystalline thin films can be easily varied with growth conditions: such as concentrations of metal and chalcogenide ions, deposition period, temperature of solution, complex reagent, topographical and chemical nature of the substrate as well as mechanical stirring.

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In the present communication, we report on structural, morphological and optical properties of

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chemically deposited CdS, CdSe and CdSSe thin films at room temperature. The results were reported for optimized preparative parameters that are used to deposit good quality thin films with interesting nanostructures. 2. Experimental Procedure

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2.1 Deposition of thin films

Cadmium selenide thin films were deposited using analytical grade cadmium acetate [Cd(CH3COO)2], aqueous ammonia [NH3.H2O], and freshly prepared sodium selenosulfate (Na2SeSO3)

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solution. All AR grade chemicals were purchased from s. d. fine Chem Ltd. and used without further purification. For the deposition of CdSe thin films, 50 ml of 0.25 M Cd(CH3COO)2 solution was added

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in a 100 ml capacity glass beaker. In this solution aqueous ammonia solution was slowly added with constant stirring, so as to make the solution clear and transparent. Further to this, 50 ml of freshly prepared Na2SeSO3 (0.25 M) solution was added slowly with constant stirring. The cleaned glass substrates were subsequently immersed in the aqueous solution containing precursors, with suitable angle to the wall of the beaker. The deposition was carried out at room temperature without mechanical

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ACCEPTED MANUSCRIPT stirring. The substrates that were coated with CdSe thin films were removed after 24 h, rinsed in deionized water, and dried in air. In similar way deposition of CdS films were carried out by replacing Na2SeSO3 with thiourea SC(NH2)2 solution.

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For the deposition of CdSSe thin films Cd(CH3COO)2 (0.25 M, 50 ml), SC(NH2)2 (0.25 M, 25 ml) and Na2SeSO3 (0.25 M, 25 ml) solutions were used. 2.2 Characterizations

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The film thickness was measured with weight difference method by using a sensitive digital

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microbalance. X-ray diffraction (XRD) patterns of the deposited thin films were recorded using a Rigaku miniflex tabletop X-ray Diffractometer with CuKα radiation. The XRD data was collected with a scan rate of 3o per minute. The shape, size and distribution of nanostructures were observed with scanning electron microscope (SEM) model JEOL JSM-6010, attached to an energy dispersive X-ray

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analyzer (EDXA), to measure the elemental composition. To study the optical properties, the optical absorption spectra were recorded with UV-Visible spectrophotometer (Shimadzu UV 1800). 3. Results and discussion

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3. 1 Growth and reaction mechanism

There are two possible growth mechanisms leading to solid material that forms thin films in

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CBD method: (1) Cluster by cluster (homogeneous precipitation) within the solution; (2) Ion by ion (heterogeneous precipitation) on the surface of substrate. Under specific conditions both the mechanisms are simultaneously involved during the deposition. The predominance of one mechanism over the other is governed by the experimental condition that includes the type of anion and cation precursors, their relative concentrations, complex reagent, time and temperature of the deposition, thermal and mechanical agitation, catalytic activity of substrate surface etc [35]. 4

ACCEPTED MANUSCRIPT The reaction mechanism involved during the deposition of CdS thin films are as follows: Cd(NH3)42+ + [CH3COO]22-

Cd[CH3COO]2 + 4NH3

(1)

NH4 + OH-

(2)

(NH2)2 CS + OH-

CH2N2 +H2O + HS-

(3)

S2- + H2O

(4)

-

HS + OHCd(NH3)42+ + S2-

CdS

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NH3 + H2O

+ 4NH3

(5)

Na2SeSO3 + OH-

Na2SO4 + HSe-

HSe- + OH-

H2O + Se2Cd(NH3)42+

Cd(NH3)42+ + Se2-

CdSe

(6)

(7)

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Cd2+ + 4NH3

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The reaction mechanism for the growth of CdSe thin films proceeds via following steps:

+ 4NH3

(8) (9)

The overall chemical reactions for the preparation of CdSSe microstructures proceed in the following

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way: Cd(NH3)42+ + Se2- + S2-

CdSSe

+ 4NH3

(10)

The thickness of CdSe, CdSSe and CdS thin films were found to be 0.582, 1.261 and 1.560 µm,

3.2 XRD and EDAX study

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respectively.

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Cadmium sulfide/selenide commonly grows with metastable cubic (β-CdSe/CdS) or stable hexagonal (α-CdSe/CdS) crystal structure. The XRD pattern of CdSe thin film is shown in Fig. 1(a). The CdSe film is of poor crystallinity and no well-defined peaks were observed. The low intensity peak (111), (220), (311) can be indexed to cubic phase. Hence, CdSe thin film grows with cubic (β-CdSe) polymorphic phase [JCPDS File Nos. 19-0191]. The low intensity diffraction peaks reveals the nanocrystalline nature of CdSe thin film and broad hump in between 20o to 30o reveals the presence of 5

ACCEPTED MANUSCRIPT amorphous phase in chemically deposited CdSe thin film. Thus XRD data analysis confirmed that the CdSe film reveals the coexistence of cubic phase along with amorphous phase. Fig. 1(b) shows the XRD pattern of CdSSe thin film. It clearly shows the well resolved diffraction peaks that could be assigned to hexagonal crystal structure and matches with the standard pattern of Cd10S5.71Se4.29 (JCPDS

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40-0838). The XRD pattern of CdS thin film is shown in Fig. 1(c). Sharp diffraction peaks with high intensity reveals well crystalline nature of CdS thin film. The XRD data analysis confirms coexistence of cubic (dominating) and hexagonal phases (JCPDS 42-1411 & 41-1049). The crystallite size of the

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deposited thin films was calculated using Williamson-Hall method and found to be 5, 8 and 11 nm for

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CdSe, CdSSe and CdS respectively. It is observed that the crystalline nature of thin films was improved with sulfur content. It is inevitable to note that the CdSe thin film was poorly crystallized as compared to CdS and CdSSe thin films, deposited under same experimental conditions. It may be due to fast release of S2- ions from thiourea and slow release of Se2- ions from relatively stable Na2SeSO3

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precursor. This results into formation of tiny CdSe nanocrystallites that are engaged into microspheres. The elemental analysis of the deposited thin films was carried out with EDXA technique. Fig. 2 shows a representative EDXA pattern for chemically deposited CdSSe film. The strong peaks for Cd, S

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and Se were detected in the spectrum, and no impurity peaks were detected. The Si peak observed in the EDXA pattern is due to the glass substrate.

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3.3 Morphological study

The SEM images of CdSe thin film with different magnifications are shown in Fig. 3(a-c). It shows interesting morphological features with the combinations of microspheres and interconnected nanofibers. The overgrowth of some nanostructure was also observed at lower magnification. The microspheres were uniformly distributed over the substrate surface having diameter of the order of 1 µm and the nanofibers on the surfaces of microspheres. The diameter of the nanofibers is in the range 6

ACCEPTED MANUSCRIPT of 15 nm. Fig. 4(a-c) shows the SEM images of CdSSe thin film that clearly reveals interesting two types of morphological features. It consists of microspheres (Inset of Fig. 4(a)) that are deposited onto the substrate surface over which the hierarchically grown microstructures were settled down. The microstructure consisted of numerous thin nanosheets that are interconnected with each other to form

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hierarchical flowerlike structure. The thickness of the nanosheets is ~ 40 nm. Fig. 5(a-c) depicts the SEM images of CdS thin film deposited at room temperature. It shows homogeneous and uniform deposition of CdS thin film on the glass surface and the flowerlike morphology uniformly grown on the

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surface of substrate. It consists of numerous nanosheets with thickness is in the range of 25 nm. The

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nanosheets are interconnected with each other to form the marigold flowerlike morphology. It is worth to mention that these hierarchal nanostructures were grown by using simple, inexpensive CBD method at room temperature. Most of the techniques have limitations to synthesize interesting hierarchal nanostructures relatively at lower temperature.

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3.4 Optical properties

The Tauc plot was used to obtain the band gap of all films using equation: α = A (hν – Eg)1/2 / hν

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Where A is a constant, α is the absorption coefficient of semiconductor, Eg is the band gap energy of semiconductor, hν is the photon energy and n is the constant. For allowed direct transitions n = 1/2 and

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for indirect transition n = 2. The extrapolation of straight line portions of curve (αhν)2 versus hν to zero absorption coefficient (α = 0), gives the value of Eg. Fig. 6(a) shows the plot of (αhν)2 versus ‘hν’ for CdSe thin film. The ‘Eg’ of CdSe thin film is ~ 2.0 eV, which is greater than the standard bulk ‘Eg’ value of CdSe ( Eg,bulk= 1.72 eV). Such a higher value of ‘Eg’ energy is due to a size quantization effect commonly observed in CdSe nanocrystallites. When the crystallite size of nanocrystalline semiconductor is less than the exciton Bohr radius (rb), size quantization takes place and this results to 7

ACCEPTED MANUSCRIPT increase in effective ‘Eg’ value of semiconductors. The XRD pattern also reveals the nanocrystalline nature of CdSe along with presence of amorphous phase. It is well known that, often amorphous semiconductors exhibit wider optical band gap energy than their bulk counterparts due to lack of long range order. There is noticeable variation in the reported ‘Eg’ value of CdSe thin films that varies from

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1.71 to 2.3 eV [8, 36-38]. Figure 6(b) shows the Tauc plot of CdSSe thin film and ‘Eg’ value was equal to 2.15 eV. It is intermediate between the ‘Eg’ values of observed CdSe and CdS. From Fig. 6(c) the optical ‘Eg’ of CdS thin films is found to 2.45 eV greater than the bulk band gap value. The CdS

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standard (bulk) band gap energy is 2.42 eV. However, previously reported ‘Eg’ values for CdS thin

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films were in between 1.85 eV and 2.6 eV [39-44]. Appreciable size quantization effect was not observed in CdS and CdSSe thin films due to their improved crystallinity as depicted in XRD patterns, and also small value of the exciton Bohr radius of CdS ( rb ~ 2.5 nm) compared to that of CdSe ( rb ~ 5.6 nm). The ‘Eg’ value of chalcogenide semiconducting thin films mainly governed by the method of

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preparation and their preparative conditions that includes precursors and relative concentrations of metal and chalcogenide ions, substrate temperature, solution pH, nature of complex reagent, reaction time etc. It also critically depends on relative elemental composition of metal and chalcogenide,

4. Conclusion

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thin films.

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crystallinity of deposited film, structural phase and various types of defects originated during growth of

A simple, low-cost and inexpensive chemical bath deposition method was used to deposit CdSe, CdSSe and CdS thin films. The deposited CdSe thin films were poorly crystallized, whereas CdSSe and CdS films were grown with improved crystallinity. The deposited CdSe thin film grew with cubic phase while CdS thin film grew with mixed cubic along with hexagonal phase and CdSSe thin film revealed purely hexagonal crystal structure. The morphological observations revealed the formation of 8

ACCEPTED MANUSCRIPT interesting nano and microstructures. It includes one dimensional fibrous like network, two dimensional nanosheets that were united together to form flowerlike nanostructure and three dimensional microspheres. The optical absorption study showed significant blue shift in the optical spectrum of CdSe thin film, compared with CdS and CdSSe due to their improved crystalline nature.

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The present method is simple, mild, low-cost for large-production, which is suitable for the deposition

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of homogeneous nanostructured thin films of other metal sulfides and selenides.

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Figure captions

XRD patterns of (a) CdSe, (b) CdSSe and (c) CdS thin films.

Fig. 2

Typical EDAX pattern of CdS thin film.

Fig. 3

SEM micrographs of CdSe thin film with different magnifications (a) 3

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Fig. 1

KX, (b) 10 KX and (c) 60 KX.

SEM micrographs of CdSSe thin film with different magnifications (a) 3

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Fig. 5

SEM micrographs of CdS thin film with different magnifications (a) 3 KX, (b) 10 KX and (c) 30 KX.

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Plots of (αhν)2 versus hν of (a) CdSe, (b) CdSSe and (c) CdS thin films.

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Fig. 6

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KX, (b) 10 KX and (c) 30 KX.

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Highlights • The CdS, CdSe and CdSSe nanostructure thin films were deposited using CBD method • Crystal structure of thin films depends on sulphur and selenium

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composition

• The thin films were grown with different interesting 1D and 3D morphologies

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The CdSe thin films showed prominent size quantization effect

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•