Accepted Manuscript

Tuning optical properties of CdTe films with nanocolumnar morphology grown

using OAD for improving light absorption in thin-film solar cells

L.G. Daza, V. Canch-Caballero, E. Chan y Daz, R. Castro-Rodrguez, A.

Iribarren

PII: S0749-6036(17)30647-X

DOI: 10.1016/j.spmi.2017.08.004

Reference: YSPMI 5179

To appear in: Superlattices and Microstructures

Received Date: 30 March 2017

Revised Date: 03 August 2017

Accepted Date: 03 August 2017

Please cite this article as: L.G. Daza, V. Canch-Caballero, E. Chan y Daz, R. Castro-Rodrguez,
A. Iribarren, Tuning optical properties of CdTe films with nanocolumnar morphology grown using
OAD for improving light absorption in thin-film solar cells, Superlattices and Microstructures (2017),
doi: 10.1016/j.spmi.2017.08.004

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 ACCEPTED MANUSCRIPT

Tuning optical properties of CdTe films with nanocolumnar

morphology grown using OAD for improving light absorption in thin-

film solar cells

L. G. Daza1, V. Canch-Caballero2, E. Chan y Daz1,3, R. Castro-Rodrguez1, and

A. Iribarren1,4,*

1 Department of Applied Physics, CINVESTAV-IPN, Unidad Mrida. 97310 Mrida Yucatn, Mxico.

2 Faculty of Engineering, University of Yucatan, CP 97130 Mrida, Yuc., Mxico.

3 Departamento de Ingeniera Mecnica, Instituto Tecnolgico de Mrida, Av. Tecnolgico km. 4.5 s/n,

97118, Mrida, Yucatn, Mxico.

4 Instituto de Ciencia y Tecnologa de Materiales, Universidad de La Habana, Zapata s/n esq. G, Vedado,

Plaza, La Habana 10400, Cuba.

ABSTRACT

CdTe films with transversal morphology in form of tilted nanocolumns were obtained

by sublimation method using a rotating vapour source combined with the oblique angle

deposition technique. The tilt angles of the nanocolumnar structures increases as the

substrate inclination also increase. CdTe films exhibited cubic zinc blend lattice under

compressive strain. Morphological and x-ray diffractometry analysis indicated that the

nanocolumns are grains stacked in the nanocolumn preferential growth direction, except

for the films with non-inclined substrate. We found an interesting dependence of band

gap energy and the refractive index as functions of the microstrain distribution due to

the nanocolumn tilt in the films from 0 to about 25. These facts evidence the

* Corresponding author. E-mails: a_iribarren@yahoo.com, augusto@imre.uh.cu

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possibility of carried out film strain engineering for optimizing optoelectronics devices

as we propose for the case of thin-film solar cells.

Keywords: CdTe thin films; oblique angle deposition; nanocolumns; optical properties;

microstrain engineering
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1. Introduction

Cadmium telluride (CdTe) is a II-VI semiconductor with 1.5 eV direct band gap energy

at room temperature and a large absorption coefficient [1]. It has constituted an

important material for thin film photovoltaic applications due to its characteristics and

low-cost production. Nowadays CdTe thin-film solar cells have reached efficiency

higher than 21% in laboratory cells and almost 19% in modules [2]. However, each

increasing of the efficiency is important and desirable.

Multiple obtaining methods for CdTe film deposition have been used and a lot of

articles have studied this material, although mainly focused to morphological, electrical,

stoichiometrical, and other characteristics in bulks as in the case of thin films [3-8].

However, the studies of the nanostructuring effects on CdTe physical properties are still

limited. Films with nanocolumnar morphological structures attract the attention [9],

since this characteristic significantly influence on optical, electrical, structural and other

properties, which can be engineered in order to improve the optoelectronic device

performance. Morphological modifications are practical ways to cause utilizable

variations of the characteristic physical properties of the materials, films, structures and

heterostructures.

One of the techniques to attain such modifications is the oblique angle deposition

(OAD) [10,11], which allows to obtain the formation of columnar films with

morphological structure. OAD, also known as glancing angle deposition (GLAD),

facilitates the nanoscale morphology control through the handle of columnar arrays.

This technique has been used for engineering optical properties, as refractive index and

absorption, in nanomaterials by controlling the columnar morphology [11]. The

technique consists on the positioning of the substrate angularly inclined to the direction

of vapour flow. This causes that the structures begin to grow and a shadowing effect of
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such structures to the vapour flow takes place. Consequently, the resulting films have

morphological structure either of nanocolumns, which grow normal to the surface if the

substrate rotate on its center [12] or of inclined nanocolumns, which can be dense or

separated by what the films present porosity.

Since polycrystalline films suffer from defects and imperfections caused by grain

boundary that are disordered, point defects and local energy barriers that favour

undesirable non-radiative recombination and transport processes and mechanisms in

solar cells [13], forming columns with relatively few defects and well organized are

highly desired. Additionally, an anomalous photovoltaic effect has been reported in

solar cells with morphology of inclined-column structures [14]. Namely, the

photovoltage is greater than the energy band gap, resulting in an improvement in the

open-circuit voltage. From the optical viewpoint, the film with morphology of inclined

columns suffer variations in their optical properties such as band gap energy and the

effective refractive index, which allows to engineer the films in order to improve the

performance of the resulting device [15]. The engineering of the physical properties of

the absorbent CdTe layer can significantly help to enhance the efficiency of a thin-film

solar cell.

In that sense we have opted for decreasing reflection in the CdS/CdTe interface,

decreasing band gap to extend the light absorption range and modulation of light

transmission within the CdTe layer by modifications of its morphological structure. In

this paper CdTe films with dense tilted-nanocolumnar structure were prepared using the

close space sublimation (CSS) combined with oblique angle deposition OAD technique,

but with a rotating sublimate vapour effusion (RSVE) source. Morphological, structural

and optical studies were made to the CdTe films, which presented tilted-nanocolumn
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structure. Besides, a preliminary approach was made of its use for enhancing the

CdS/CdTe thin-film solar cell performance.

2. Experimental

CdTe thin films were grown on Corning 2947 glass substrates. The used growth system

was close space sublimation (CSS) with a new version of rotating sublimate vapour

effusion source. The effusion source is constituted by a graphite container with a top

cover with 80 orifices of 1.5 mm diameter symmetrically distributed. Into the container

0.5 g CdTe powder (99.999 %) was placed. The container was heated up to 700 C by

mean of two halogen lamps diametrically placed at each side. That temperature induces

a CdTe vapour pressure into the container that gets out through the orifices. The

container is rotated on its axis at = 40 rpm in order to CdTe powder uniformly heats

into the container and that the CdTe vapour effusion uniformly reaches substrate. For

implementing the oblique angle deposition technique, a system, which allows to place

four arms that support the substrates symmetrically out of the central axis and at

distance L = 60 mm from the source, but inclined at 40, 50, 60, and 70. A non-

inclined substrate in its centre was added in front of the effusion source. The substrates

were static, i. e., = 0 rpm and at room temperature during the growth. Fig. 1 illustrates

the arm system. The source was described elsewhere [12].

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Fig. 1.- Scheme of the experimental setup with OAD method combined with sublimate

vapor effusion source.

Cross sectional and surface film morphologies were studied by field emission scanning

electron microscope (FESEM) with a JEOL 7600F instrument. X-ray diffractograms

(XRD) were obtained by a D5000 Siemens X-ray Diffractometer with the CuK filtered

monochromatic radiation (=0.15405 ) by 40 kV with 35 mA and aperture diaphragm

of 0.2 mm, incidence angle of 1, sampling pitch of 0.02 steps and 10 s record time.

Optical measurements were carried out using a UV-VIS Agilent 8453

spectrophotometer.

3. Results and discussion

3.1. Morphological characterization

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Cross sectional SEM images in Fig. 2 make evident that the film structure is constituted

by tilted nanocolumns at angles according to the substrate inclination. Cross-sectional

and surface images prove that the films are dense without cracks or porous. Cracks

observed on the cross-sectional images were caused by mechanical cleaving during the

sample preparation. For non-inclined substrate = 0, undefined column structure was

observed, although a polycrystalline structure with random grain size was observed in

the surface image. Fig. 3 displays the behaviour of the nanocolumn tilt angle as a

function of the substrate inclination angle which is consequence of the shadowing

effect during the growth process [14,16,17]. The nanocolumn tilt angle does not follow

the previously reported empirical behaviours as a function of the substrate inclination

[14], but it increases. An exponential fitting that describes the relation as a function of

is given by the expression:

= 0.769 + 0.869 ( 2.46

19.93 ). (1)

The surface SEM images display grains with spheroidal shape. Fig. 4 exhibits that the

film thickness decreases as the nanocolumn title angle increases. From processing SEM

images the grain size and nanocolumn diameter DSEM, nanocolumn tilt angle , film

thickness t, and the deposition rate , in the samples were obtained. The error in

determination of was about 1. The estimation of the grain size from surface SEM

was carried out by calculating the average grain area counting from the number of

observed grains in a specific area and considering the grain surfaces are circles. This

method and the measurement of the nanocolumn width from transversal SEM images

approximately introduce 9% error. The grain size and nanocolumn diameter obtained

from SEM images are very similar. This indicates that the nanocolumns that form the
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films are constituted by grains stacked in the column growth direction. The results were

included in Table 1.

Fig. 2. Surface and cross-sectional CdTe film SEM images according to substrate

inclination . The insets are 200 200 nm2 surface SEM images, which detail the grain

shapes.

Table 1. Data obtained from morphological analysis.

DSEM DSEM
Sample t
surface sectional
() () (m) (m/min)
(nm) (nm)
0 0 62 - 1.669 0.68

40 6.5 59 57 1.341 0.54

50 9.5 57 56 0.919 0.37

60 12 51 50 0.893 0.37

70 26 50 49 0.881 0.35
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Fig. 3. Nanocolumn tilt angle of the CdTe films as a function of the substrate inclination

angle.

Fig. 4. Film thickness as a function of the nanocolumn tilt angle. Dashed line represents

only a tendency.

Fig. 5. Behaviours of the grain and nanocolumn sizes as functions of the nanocolumn

tilt angle. The dashed line only represent tendency.

3.2. Structural analysis

X-ray diffractograms in Fig. 6a and 6b show preferential growth in the (111) direction

of the CdTe films, although very small (221) and (311) peaks and a small halo at about

42 can also be observed. The halo indicates the presence of amorphous material. The
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diffractograms correspond to the cubic zinc blend structure. The (111) peak was fitted

with a Voigt function and the central peak angular position, 2, and the full width at

half maximum, FWHM, were obtained. It is noticeable that the Gaussian components,

described by its width wG in the fitted Voigt functions, had higher contribution than the

Lorentzian components, wL. The Gaussian contribution was almost complete in the case

of the non-inclined substrate. By comparing with the reference diffraction pattern [18]

the (111) peak shifts toward higher diffraction angles, which increases as the

nanocolumn slant angle increases. This angular shift is sign of compressive strain. Figs.

7a and 7b present the plots of the (111) peak angular position and the FWHM as

functions of the nanocolumn tilt angles respectively. The (111) peak angle position is

compared with that of the diffraction pattern 20 in Fig. 7a. The 2 behaviour can be

considered linear and is described by the expression:

2 = 23.765 + 0.00268 . (2)

The shift of (111) peak toward angles higher than that of the pattern indicates that the

films are in compressive state due to a local outward lattice relaxation. This

phenomenon has been associated to lack of stoichiometry by Cd vacancies. Thus, an

excess of Te is present and as a consequence interstitial, Tei, or antisite, TeCd, tellurium

have been reported [19,20]. The formation energy of TeCd is lower than that of the Cd

vacancies under Te-rich conditions [1] and can compete with VCd, which is the cause of

p-type conductivity in CdTe. However, favoured by the high mobility of Te, TeCd would

form Te nanoclusters or precipitation centres, likely of metallic character due to its

amphoteric character after binding to nearest Te neighbours. Both defects, Tei and TeCd

favour the p-type CdTe conductivity and the compressed lattice.

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Fig. 6. Normalized diffractograms of the CdTe films (a) and comparison of the (111)

peaks (b) for different substrate inclination.

Fig. 7. Angle (2) (a) and FWHM (b) shifts of the (111) peak as functions of the

nanocolumn tilt angle.

The a lattice parameter was calculated from the expression [21]:

2(2 + 2 + 2)
= (3)
4 2

where h, k and l are the Miller indexes, = 0.15405 nm and the (111) peak Bragg

angle. Fig. 8 exhibits the behaviour of the lattice parameter as a linear function of the
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nanocolumn tilt given by the expression () = 0.6477 6.82 10 4 with a

standard error a 210-4 nm. The comparison of the lattice parameters with that of

the pattern proves the lattice shrinkage.

Fig. 8. Lattice constant variation as function of the nanocolumn tilt angle.

The lattice strain or distortion was calculated from the expression:

= (4)

where a0=0.6481 nm is the pattern lattice parameter [18]. The integral width of the non-

uniform microstrain distribution , is given by the expression [21,22]:

= 4 . (5)

FWHM is ruled by non-uniform strain, by fine particle size or both. In this case,

although a change of the crystallite size is observed it does not follow the FWHM

behaviour. Then it is possible to consider that the FWHM variation is highly influenced

by non-uniform strain. In rigor, the FWHM is influenced by the contribution of the

instrumental broadening FWHM0 [22]. However, since FWHM0 is a constant for the

studied diffraction peak, it does not significantly affect the behaviour and it was
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ignored. The strain distribution behaviour as a function of the nanocolumn tilt angle is

plotted in Fig. 9. The resulting values of the diffraction analysis are tabulated in Table

2.

Table 2. Structural parameters found for the CdTe films.

2 FWHM wG wL a DXRD

() () () () () (nm) (nm) (10-3) (10-3)

Pattern 23.7581 - - - 0.6481 - - -

0 23.78 0.166 0.155 0.02 0.648 7 -0.78 3.21

40 23.79 0.136 0.099 0.06 0.647 4 -1.61 2.05

50 23.78 0.147 0.119 0.046 0.647 3 -1.19 2.47

60 23.79 0.156 0.126 0.052 0.647 3 -1.49 2.61

70 23.84 0.163 0.142 0.082 0.646 2 -3.56 2.94

The crystallite grain size DXRD determinated from the Scherrer equation [21], with an

error DXRD 1 nm, indicates that the grains are formed by several crystallites. For

films grown with non-inclined substrates the crystallite are larger than those grown with

inclined substrate, which can induce variations of the microstrain distribution into the

grain.
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Fig. 9. Behaviour of strain distribution as a function of the nanocolumn tilt angle. The

dashed line only represents tendency

3.3. Optical characterization

Fig. 10 displays the transmission spectra of the CdTe films. In the region bellow 750 nm

the transmission is low, which corresponds to absorption edge region. The transmission

beyond 850 nm is strongly modulated by interference and it is in the range of 50% to

80%. Fig. 11 exhibits the CdTe films absorption profiles. The band gap energy, Eg (

0.001 eV) was calculated from a Tauc plot, i. e., from the intercept of the absorption-

edge straight region with the energy axis in a (h)2 vs. h plot as shown in the inset of

Fig. 11. In Table 3 the optical parameters are tabulated. The results plotted in Fig. 12a

show that Eg sharply decreases between non-inclined and 40 inclined substrate in Eg

8 meV. The band tail parameter E0 ( 1 meV), which characterizes the disorder, was

estimated from the exponential regions [23] of the absorption profiles that is around and

bellow 1.5 eV and is plotted in Fig. 12b. The band tail behaviour was linearly fitted as a

function of the nanocolumn tilt, since the evident tendency to increase as increases

and is described by:

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0 = 32.64 + 0.726 (6)

represented in Fig. 12b as a dashed line. This increasing tendency of E0 agrees with the

increasing of microstrain presumably due to decreasing of the crystallite size for more

tilted nanocolumns in the films. However, taking into account the behaviour of Eg as a

function of , we plotted a second dash-dot-dot line with the only aim of suggesting

other tendency that includes the tail parameter for =40. In Fig. 12b E0 for =40

seems to be a point out of the linear behaviour, but Fig. 12c proves that this point is

really in the linear behaviour of the films with tilted nanocolumn structure and it is not a

deviation. The tail parameter E0 increasing from =0 to 70 agrees with the increasing

of the integral strain obtained from x-ray diffraction. This is associated to lattice

deformation due to Tei, TeCd and VCd defects.

Fig. 10. Transmission spectra of the CdTe films.

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Fig. 11. CdTe-film absorption coefficients as function of the energy. The inset shows

details of the Tauc plot of the sample absorption edges and some of their prolongations.

Table 3. Values of band gap energies and band tail parameters obtained for the CdTe

films.

Eg E0

() () (eV) (meV)

0 0 1.520 34

40 6.5 1.512 33

50 9.5 1.513 42

60 12 1.514 43

70 26 1.516 51
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Fig. 12. Behaviours of the band gap energy (a), band tail parameter (b) as functions of

the nanocolumn tilt and the behaviour of the band tail parameter versus the band gap

energy (c). The dashed lines only represent tendency.

It is noteworthy that the behaviours of Eg and FWHM as functions of the film

nanocolumn tilt angle are similar, although both variables were obtained by techniques

and processing very different. The refractive indexes as a function of the nanocolumn

tilt were estimated from the mean value at = 1000 nm of the upper and lower

envelopes of transmission spectra in the low absorption region, and using the expression

[15]:

4
= ( )+
1+
1 (1 )2
(7)

where R is the normal-incident light reflection and k = /4 is the extinction

coefficient. In this region below the band gap energy the absorption is negligible. Thus

the expression of energy conservation T+R+A=1 reduces to R = 1 T. Fig. 13 presents

the resulting refractive index at = 1000 nm as function of the nanocolumn tilt angle.

Note that n sharply diminishes from non-inclined nanocolumn films to that with 40
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nanocolumn tilt angle. For higher nanocolumn tilt the refractive index increases, but

softly.

Fig. 13. Behaviour of the refractive index at =1000 nm as a function of the

nanocolumn tilt angle.

The compressive strain has been found to cause decrease in the band gap energy and

vice versa [24]. The relationship between Eg and has been described by a linear

function Eg() = Eg0 + d [25-27] where Eg0 is the non-strained band gap energy and

d1.235 eV [27,28] is the deformation potential for CdTe. However, we found no

linear behaviour of the band gap energy as a function of the maximum strain. Firstly, we

had into account the component weight into the Voigt fitting of the (111) peak. If the

peak broadening responds to a Lorentzian fit component it is due to size crystallite, but

in case of Gaussian fit component is present and predominates the peak broadening

responds to microstrain distribution [22]. In our films the peak fit was practically

Gaussian for the samples with non-inclined substrate, and both functions complement

the (111) peak fitting in the films grown with inclined substrate. However, the Gaussian

component had higher weight than the Lorentzian one and the former more contributed

to the FWHM. Those facts indicate that the StokesWilson approximation [29] can be
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applied, but the FWHM is ruled by the overlapping of the size and microstrain

distributions [30]. The broadening distribution stablishes a spread around the central

lattice parameter and changes with the nanocolumn tilt. Thus, the behaviour of the band

gap energy is related to the lattice strain given by the unit cell dimensions, but it is also

linked to the causes of the peak broadening, which is mainly ruled by the microstrain

distribution. Both contributions constitute the integral distribution breadth , given by

the overlapping of both distributions. These factors split the behaviour of the band gap

energy from the simple linear average strain dependence. Similar behaviour was found

in the refraction index. It is noticeable that the plots break with the order of and the

behaviours respond to the relation band gap energy and refractive index to integral

breadth as displayed in Figs. 14a and 14b. We use exponential fitting to describe the

dependence on Eg and n, which gave:

( )
0.00202
= 1.511 + 7.253 10 4 (8)
4.807 10 4

and

( )
+ 0.00144
= 2.928 + 4.4 10 3 (9)
9.082 10 4

The equations show that the refraction index dependence on the integral distribution

breadth is stronger than that of the band gap energy. Both expressions indicate the

asymptotic values for minimal microstrain dispersion, i. e., Eg0 = 1.511 eV, which well

agrees with the bulk CdTe band gap energy, and n0 = 2.928. These results open the

possibility of modifying optical properties by mean of strain engineering.

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Fig. 14. Behaviour of the band gap energy (a) and the refractive index (b) as functions

of the microstrain distribution.

Fig. 13 shows that the refractive index sharply diminishes up to a difference n 0.5,

when the substrate is inclined to 40. For higher substrate inclination the refractive

index again increases in n 0.36, although softer. The refractive indexes agree with

previous reports where the OAD technique was used [14,31]. It is possible to observe

that the tendency of the refractive index is similar to that of the band gap energy, which

induces to suppose that its variation could be related to the same cause as the band gap

energy variation, as manifests in Fig. 12a. This behaviour is also similar to the

diffraction peak broads plotted in Fig. 7b. Such the variations can be exploited in

optoelectronic devices as thin film solar cells with CdS/CdTe interface. On the one

hand, a reduction of light reflection in the CdTe/CdS interface can be attained by

reducing the difference between the refractive indices of both materials. Simple

calculations using the expression [32]:

|
1 2
= 1 + 2 | 2
(10)
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where n1 and n2 are the refractive index of the interface materials, show that in a CdS-

CdTe interface where the index of refraction of CdTe is the lowest one we found in this

work the reflection reduces from R 5% to R 2% . Moreover, in a homogeneous

CdTe layer the light travels through it until it is absorbed into it. However, the refractive

index can be changed within the same absorbent CdTe from the change of the CdTe

structure. Changing the refractive index from nmax 3.66 to nmin 3.15 within the

proper CdTe layer an internal reflection of R 0.5% can be achieved in such a way that

the reflected light could be absorbed closer the CdS-CdTe interface, which reduces the

electron trapping or recombination probability during its transport to the interface.

Additionally the band gap energy decreasing favours the harvesting of light.

4. Conclusions

We obtained CdTe thin films with nanocolumnar morphological structure by close

space sublimation method using a rotating sublimate vapour effusion source and the

oblique angle deposition technique. Films exhibit CdTe cubic zinc blend lattice. The

nanocolumn tilt follows an angular increase as the substrate inclines. In films where the

substrate was inclined the nanocolumns are formed by stacked grains in their growing

direction. A supralinear behaviour of the band gap energy as a function of the integral

microstrain and fine size distribution was found. Similar behaviour had the refractive

index. By strain engineering it is possible to modify the band gap energy and the

refractive index in order to enhance the performance of optoelectronic devices,

including the solar cells.

Acknowledgment
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Authors thank Oswaldo Gmez, Mario Herrera, Daniel Aguilar, Elsa Hernndez, and

Marcela Mireles Ramrez for technical assistance and to Lourdes Pinelo for secretary

assistance. This work has been supported by the Project No. CB/2012/178748

CONACYT/Mxico. One of the authors (A. Iribarren) thanks to CONACYT/Mxico

under the program No. 260967 for sabbatical stances for Mexican and foreign

researchers living abroad for supporting this research and to the Project PNCB-51-UH-

15, Cuba. Authors also thank to Department of Materials Science and Engineering from

the University of Texas at Dallas by the help and use of its facilities.

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Highlights:

CdTe thin films grown by CSS with oblique angle deposition

CdTe thin films with nanocolumnar morphological structure
Physical properties change with the column tilt angle
Microstrain distribution depends on column tilt angle
Band gap energy and refractive index depend of microstrain distribution