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Journal of Crystal Growth 284 (2005) 477–485 www.elsevier.com/locate/jcrysgro
Properties of Te-rich cadmium telluride thin ﬁlms fabricated by closed space sublimation technique
N. Abbas Shah, A. Ali, Z. Ali, A. MaqsoodÃ, A.K.S. Aqili1
Thermal Physics Laboratory, Department of Physics, Quaid-i-Azam University, Islamabad 45320, Pakistan Received 4 May 2005; received in revised form 29 July 2005; accepted 1 August 2005 Communicated by P. Rudolph
Abstract Cadmium telluride (CdTe) thin ﬁlms were prepared by the closed space sublimation (CSS) technique, using CdTe powder as evaporant onto substrates of water–white glass. In the next step, the same procedure was adopted by using tellurium as evaporant and already deposited CdTe ﬁlm as substrate. Such compositions were then annealed at 300 1C for 30 min to obtain Te-enriched ﬁlms. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), spectrophotometry, DC electrical resistivity, dark conductivity and activation energy analysis as a function of temperature by two-probe method. The electron microprobe analyzer (EMPA) results showed an increase of Te content composition in the samples as the mass of the Te-deposition increased in CdTe. The Hall measurements indicated the increase in mobility and carrier concentrations of CdTe ﬁlms by addition of tellurium. A signiﬁcant change in the shape and size of the CdTe grains were observed. r 2005 Elsevier B.V. All rights reserved.
PACS: 61.10.Nz; 68.37.Àd; 78.66.Àw; 81.05.Dz Keywords: A1. Crystal structure; A1. Optical microscopy; A1. Recrystallization; A1. Substrates; B1. Cadmium compounds; B2. Semiconducting II–VI materials
ÃCorresponding author. Tel.: +92 51 2828187; fax: +92 51 9210256. E-mail addresses: email@example.com (N. Abbas Shah), firstname.lastname@example.org (A. Maqsood). 1 Physics Department, The Hashemite University, Zarqa, Jordan.
As a result of recent advances in the efﬁciency of Cadmium telluride (CdTe)-based solar cells [1–3], interest in this material for thin ﬁlm terrestrial photovoltaic applications [4–6] is increasing. CdTe has a direct band gap of 1.5 eV at room
0022-0248/$ - see front matter r 2005 Elsevier B.V. All rights reserved. doi:10.1016/j.jcrysgro.2005.08.005
the substrate was ﬁxed at a distance of about 4 mm from the source material. 4 and 5 mg.2 mm. which is optimum for single junction solar cell efﬁciency . heated by a halogen lamp (1000 W) connected to the main power through temperature controller with K-type thermocouple (Chromel & Alumel. etc. Experimental procedure Usually.99% pure) of Aldrich chemical company were prepared onto microscope slides of water–white glass substrates of size 25. electrical and optical properties such as ﬁlm thickness. Again. The successful experimental approach will open a pathway for improving devices based on CdTe. respectively. The CSS technique is one of the various techniques that have produced encouraging results. These ﬁlms were numbered 2–7 as given in Table 1. CdTe-based semi-magnets. The temperature of the source and substrate was 200 and 100 1C. The systematic research on these properties in correlation with doping/excess of materials and with the ﬁlm preparation conditions is still necessary for a more comprehensive understanding of this correlation and for the control of the properties of these ﬁlms. The chamber was evacuated down to $10À3 mbar with the help of rotary pump.23]. Abbas Shah et al. The vacuum of the system was $10À3 mbar. which makes diode technology  and ﬁeld effect transistors  possible. metal organic chemical vapour deposition (MOCVD) . g and IR detectors and ﬁeld effect transistors . we have fabricated Te-rich CdTe ﬁlms using a home made CSS system and investigated the effects of Te addition on the crystal structure. Source and substrate temperatures were 400 and 300 1C. It has been pointed out that high efﬁcient solar cells possess Te-rich CdTe surfaces with smooth interfaces of p-CdTe/ n-CdS .—270–1350 1C). morphology. 1. 2. which have not so far been completely exploited. simplifying scale-up for high-volume continuous processing [22. however. respectively. and it can exhibit a semi-conducting state as well . like CdMnTe. screen printing . thus.4 mm Â 76. Thin ﬁlms of CdTe powder (99. The CSS process offers the advantages of simple deposition apparatus and high transport efﬁciency conducted under low vacuum conditions at moderate temperatures.5%. which was evaporated onto them by CSS technique. After that the source and substrate lamps were switched off for cooling down to 100 1C before opening the chamber. 1. The deposition time for each ﬁlm was 5 min at the source temperature of 400 1C. Wu et al. respectively.ARTICLE IN PRESS 478 N. The CSS technique. Because of its low sublimation temperature. display extremely exciting properties. After that all samples were annealed at 300 1C for 30 min under the same vacuum. In the next step. CdTe can exhibit both types of conductivity. The substrate was ﬁxed at a distance of about 4 mm from the source material. It was heated by a second halogen lamp (500 W). the deposition of CdTe ﬁlms is based on the following reversible high-temperature process : 2CdTeðsÞ32CdðgÞ þ Te2 ðgÞ. Finally they were gold coated for ohmic contacting to perform Hall measurements. In the present work. absorption coefﬁcient and optical band gap. The efﬁciency of these devices is strongly determined by the electrical and optical properties of the ﬁlms. closed space sublimation (CSS) . offers the neardistance deposition without marked dissociation of the components. CdTe polycrystalline ﬁlms can be prepared by several techniques. 2.  have reported on a CdTe/CdS solar cell with an efﬁciency of 16. The time of Te evaporation was 5 min for each sample. such as solar cells. / Journal of Crystal Growth 284 (2005) 477–485 temperature. For that source material (14 mg) was put in the graphite boat of size 20 mm Â 45 mm. such as thermal evaporation . 2–7 with successively varying Te content obtained after tellurium . Table 1 compiles the samples denoted by Nos. hot-wall vacuum evaporation [19–21]. hotwall ﬂash evaporation .18]. molecular beam deposition [17. while the thermocouple was placed over the substrate to measure its surface temperature. The CSS system used in our experiment is shown in Fig. refractive index. 3. these CdTe ﬁlms were covered with varying excess Te mass of 0. n and p.5. radio frequency (RF) sputtering .
an empirical formula for the n dependence of l as n ¼ a þ b=l2 can be used with a and b constants obtained from ﬁtting the transmission spectra. The SEM accelerating voltage was 10 kV. which is true for this kind of semiconductor thin ﬁlms.5418 A) radiation with operating conditions voltage/current 40 kV/30 mA. The optical properties such as ﬁlm thickness. / Journal of Crystal Growth 284 (2005) 477–485 479 Fig. B. The most direct and perhaps the simplest method for probing the band structure of semiconductors is to measure the absorption spectrum. deposition and annealing procedure by the above technique. where k is the extinction coefﬁcient of the ﬁlm. B À Cx cosðfÞ þ Dx2 (1) where A. refractive index. Thickness should be in nanometer range for good transmission spectra and other optical measurements. The compositions of Cd and Te of all the samples were measured with the help of electron microprobe analyzer (EMPA) attached to the SEM. In case of k2 ( n2 . The microstructure of the samples was checked using scanning electron microscope (SEM). D are constants and T is the normal transmittance for the system consisting of a thin ﬁlm on transparent substrate surrounded by air (refractive index n ¼ 1) and taking all multiple reﬂections at the interface into account. calculated from the above method are used as initial least-squares ﬁtting parameters in the theoretical model  for the following equation: T¼ Ax . During the present investigation a two-point probe method was used to measure the sheet resistance Rs of all the ﬁlms by the relation Rs ¼ . The structure of the ﬁlms was studied by X-ray ˚ diffraction (XRD) using Cu-Ka (1. C.ARTICLE IN PRESS N. Schematic diagram of closed space sublimation system. 1. The values of n and d. absorption coefﬁcient and optical band gap were calculated from the transmission spectra between 300 and 2500 nm recorded by Lambda 900 spectrophotometer. A method for the calculation of the ﬁlm thickness d and refractive index n from the transmission measurements was developed by Aqili and Maqsood  where d can be determined from two maxima or minima. Abbas Shah et al.
6. The resistivity.35 Â 106 3. 2. Resistivity r (O cm) at 200 1C Sheet resistance (O/ sq) at 200 1C 1.50 1.26 59. 6 and 7) 6.84 60.0 Â 106 2.88 42.23 2. 2. The increase in the lattice constant of the Te enriched samples can be explained as follows.54(3) A. 5. DC resistivity.43 2.12 Â 106 122. dark conductivity and activation energy as functions of temperature (50–200 1C) were measured by the two-probe method at a pressure of 10À6 mbar in a 306 A Edward vacuum coating unit.55 52. It matches with CdO mineral powder diffraction ﬁle (5-640) according to data book published by Joint Committee on Powder Diffraction Standards ICDD USA 1980.54(3) a 732 323 348 416 400 264 663 I CDD 15–770.467 1.ARTICLE IN PRESS 480 N.55 2.57(2) 6.37 3. These values are calculated and averaged after comparison of respective experimental d values in agreement with the d standard values of the lattice constant according to 1999 JCPDS–International Centre for Diffraction Data 10-0207. Silver paste was used above the gold coatings for electrical contacts.09 Â 106 4. sheet resistance and electrical resistivity of the CSS grown CdTe samples 1–7 Energy gap Eg (ev) ðV =IÞ À Ri where Ri is the internal resistance of the multimeter DM 350. It was observed in sample 3 that all the peaks were shifted by (0. / Journal of Crystal Growth 284 (2005) 477–485 Table 1 Te composition. 2.43 1 2 3 4 5 6 7 6.48 2.44.49 6. 15-0770. During the annealing the diffusing Te atoms may replace the Cd atoms by a kick off mechanism besides its diffusion at interstitial position in the lattice.24 73.44 6.44 1. 3. which results in an increase of the lattice constant.02).23 47.19 Â 106 3. In sample 5 a new peak corresponding to 200 reﬂex appeared as shown in Fig.43 5.461 1.48 1.86(3) 6. The electrical properties such as sheet resistance. The values of the lattice constant a0 are for the sample (1) and for Teenriched samples (3.44 6.86(3).80 57. 5.57(2) and 6. 75-2086 and 75-2083 (PCPDFWIN v. Results and discussion The XRD patterns (arranged by XRD software) of the samples 1.21 a 43384 167493 138367 128460 138562 196591 366486 b . 3.49 6. where-as the (1 1 1) plane disappeared completely.37 4.47 1. lattice constant.58 Â 106 5.05 50. thickness. optical constants.1 Â 106 3. 6 and 7 are compared in Fig.41) towards the higher range (right side). This shows that the lattice is in uniform strain due to expansion of the cell. The presence of oxide is due to the heat treatment under low vacuum. The main reﬂections of four samples (1.481a 6. respectively.52 2. The expansion of the cell can be explained on the basis Refractive index n ¼ a þ b=l2 Thickness d (nm) Experimental ˚ (A) ˚ Standard (A) Lattice constant ao Te (at%) 52. mobility and carrier concentrations were determined by room temperature Hall measurements. ˚ 6. Abbas Shah et al.49 and 6.38 44.66 54. no. 2c. 6 and 7) are the same and can be indexed according to fcc CdTe lattice. Sl.70 55.61 2.
From Hall measurements samples 1–7 show p-type conductivity. c) are about 990 nm and 2 mm. as in samples 1–7. the average grain size of as-deposited ﬁlm is under 540 nm while that of Te-enriched ﬁlms in Figs. The Te content was increased up to 60. 3(b. Thus.ARTICLE IN PRESS N. less than 1 which is considered the reason for CdTe ﬁlms with slight p-type conduction due to the formation of Cd vacancies in CdTe lattice acting as acceptor centers.55 to 60. This is consistent with the above results of XRD. The ratio of at% of Cd and Te in asdeposited CdTe sample is 47. 10À3 mbar. SEM images in Fig. i. c.e.43 at%. e) Te. The strongest (1 1 1) reﬂection in the pattern indicates a preferential orientation of [1 1 1] in the ﬁlms as already reported . which can be almost 5 at%. / Journal of Crystal Growth 284 (2005) 477–485 481 Fig. of radius of the Te atom. 3 show the main feature of the CSS technique. which is larger than that of the Cd atom. After optimization of annealing time. A similar observation has been reported by Li et al. As can be seen from Table 1 the resistivity of the samples decreases with increasing Te content by two orders of magnitude. the additional Te in the source leads to an increase of the Te content from 52. respectively. The Te content after its deposition and annealing determined by EMPA is shown in Table 1. The amount of excess Te in the ﬁlms mainly affects their electrical properties. i. The crystallographic arrangements are related to the stress in the layer and to the application of annealing at high temperature. . It appears that the annealing in the presence of Te facilitates the grain growth in the CdTe ﬁlms in such a way that some of the small grains coalesce together and . the Te-enriched ﬁlms have larger grains. It is clear from these values that already the samples grown from the pure CdTe source have a deﬁciency in Cd.43% in sample 7. the incorporation of extra Te leads to the expansion of the CdTe lattice. which is maximum Te-enriched. The lower Cd content gives rise to the formation of vacancies of Cd in the CdTe lattice.enriched according Table 1 after heat treatment at 300 1C for 30 min. Also the grains of the ﬁlm became larger with the increase of Te content in the samples. d. 3(c). 2. Abbas Shah et al. On the other hand. The results show that the Te content in samples 1–7 is increasing.e. X-ray diffraction patterns of CdTe samples: (a) as deposited and (b. The creation of larger grains is as a result of coalescence of small grains into bigger ones which can be seen from Fig. Also a signiﬁcant change of the grain shape was observed. The change in intensities was also observed.45:52. which indicates that the crystallinity of the ﬁlms can be improved by appropriate Te enrichment.55.
The transmission spectrum of the ﬁlms did not change signiﬁcantly after the optimization of heat treatment for 30 min.30]. The increase in the refractive index is due to the change in the lattice constant. illustrates the change of refractive index n with Te content. reorient themselves. (2) Here A is a constant. these ﬁlms are optically well-suited for use as an absorber in solar cells. Usually CdTe ﬁlms have a high absorption in the region of visible and near infrared. hn the photon energy. / Journal of Crystal Growth 284 (2005) 477–485 Fig. Fig. the same was observed in the ﬁlms deposited during this study. Fig. c) Te-enriched CdTe ﬁlms. (1) to experimental data. For the calculation of absorption coefﬁcient a in the high absorption region the values of n and d from the ﬁtted curve are used. Large absorption coefﬁcient permits the absorber layer to be thin and hence less material is necessary for photovoltaic device fabrication. which ensured the diffusion of Te in the samples. 4(b) shows the resulting ﬁt of Eq. Indeed. the incident photon energy (hn) plot the band gap can be obtained. As a result an improved different microstructure and morphology is created. The obtained thickness values are in the range of 264–730 nm. By extrapolating (ahn)2 vs.ARTICLE IN PRESS 482 N. The transmittance slightly decreases with increase of Te content as shown in Fig. Since the region of high absorption in our ﬁlms matches well with the solar spectrum. which decrease the number of grain boundaries. 4(a). Abbas Shah et al. 5. A high absorption coefﬁcient is important from both technological and economic considerations. For the band gap determination the following relation can be used : ahn ¼ Aðhn À E g ÞN=2 . A good ﬁtting in the transparent region is obvious. Eg the optical band energy gap and N depends on the nature of the transition (N ¼ 1 for direct band gap and N ¼ 4 for indirect band gap transition). The values . 3. SEM images of the grown samples: (a) as-deposited and (b. Grain growth in CdTe is well known and reported for a solid-state recrystallization (SSR) method [29.
09 Â 1014 cmÀ3. as-prepared CdTe ﬁlms.0 0.ARTICLE IN PRESS N. Abbas Shah et al. 0. wavelength (a) for samples 1 and 7 and (b) transmittance data along the curve ﬁtted for sample 2. The resistivity of sample 7 with a van der Pauw geometry was $156 O cm at room temperature. d the thickness. ‘ (3) where Rs is the sheet resistance. The change in sheet resistance and resistivity of the samples as function of Te content at temperature 200 1C is shown in Table 1. fabricated by various techniques. The grains of Te-rich samples become larger and the crystallinity improves which results in the decrease of the number of grain boundary and.2 0.deposited (sample 1) Te enriched (sample 7) 10 (1) (7) n 9 8 7 6 5 4 Sample(2) Sample(3) Sample(4) Sample(5) Sample(6) Sample(7) 1000 λ (nm) 1500 2000 3 2 1. The change of the electrical property of Teenriched samples can be easily understood according to the above analysis of the sample microstructure. 4. The representative activation energy of one of the Te. It is shown in Figs. The slope gives the activation energy.4 0.8 Transmittence 0. The sheet resistance in the present case for the as-deposited sample 1 was 5.6 0. / Journal of Crystal Growth 284 (2005) 477–485 483 1. The dark conductivity activation energy (E a ¼ E f 2E v ) was deduced by linear ﬁtting ln (s) vs. while the mobility and carrier concentration at room temperature were about 129.2 0. The decrease in the energy gap is also due to tellurium diffusion into the CdTe ﬁlms. In general. As can be seen these values decrease with the increase of Te content.58 Â 106 O/sq at 200 1C.0 500 (b) 1000 1500 λ (nm) 2000 2500 Fig. of the decrease in the grain barriers.1/kBT (kBBoltzmann constant). show a high electrical resistivity (107–109 O cm) at room temperature . Transmittance vs. Refractive index as a function of wavelength.6 0.4 0. w the width and ‘ the length of the ﬁlm. respectively.0 500 (a) As. 6 and 7 that the dark conductivity of the samples as a function of temperature (50–200 1C) is increasing.rich sample 7 is shown in Fig. All these changes are favorable for the transport of carriers.12 Â 105 O/sq in Teenriched sample 7 at the same temperature. thickness and refractive index of all the sample series are listed in Table 1.0 0 500 1000 1500 λ (nm) 2000 2500 3000 0. of energy gap.3 cm2 VÀ1 sÀ1 and 3. hence.8 Transmittence Fig. For the resistivity determination by two-probe method the following relation could be used: r ¼ Rs d w . 5. while it dropped to 2. After Te addition the conductivity of the samples was markedly . 7.
This improvement of the ﬁlm conductivity could be attributed to the increased grain growth taking place in the CdTe ﬁlms in presence of Te. Dr. Phys. The samples show large grains with size $2 mm which can grow larger with increasing Te content. Abbas Shah et al. Liu.0 Log (σ) (Ω cm)-1 -2.cm )-1 -3 -4 -5 -6 24 26 28 30 32 34 36 1 / kBT (ev)-1 Acknowledgements This work was supported by Pakistan Science Foundation project No. Fitting of ln (s) against 1/kB T of sample 7.5 -5. Similar results are reported by Turkevych et al.0 -3. J. Further work on this material is under progress and will be addressed in future. Te-enriched CdTe ﬁlms have been fabricated by the CSS technique with subsequent annealing. / Journal of Crystal Growth 284 (2005) 477–485 lattice that might create Cd vacancies.5 -2.5 -3. Dr. It has been observed by Hall measurements that p-type doping is achieved in Te-enriched CdTe ﬁlms prepared by CSS technique.2 2.(121). The increase of the ﬁlm mobility could be due to the enlargement of the grains size. Fulop. On the basis of the XRD. C. Appl. 6. Doty. Fig. 40 (1982) 327. Nakayama. H. Riaz Khan of Central Resource Laboratory. for providing the SEM facilities. PSF/Res /C-QU/ PHY.0 -4. improved. J. probably due to the Te doping effect in CdTe.0 sample1 sample2 sample3 sample4 sample5 sample6 sample7 2. Meyers.0 3. DC electrical resistivity and activation energy of Te-rich samples were decreased but the dark conductivity. Jpn. Dark conductivity of the heated samples (1–7) plotted against 1/T. The values of refractive index increases with the increase of Te concentration.6 1000 / T (K)-1 2. Ikegami. Fig. M. The authors would like to thank Prof.5 -4. The sheet resistance.5 2. SEM and Hall measurements one can conclude that the post annealing strongly affects the morphology as well as electrical properties. 15 (1976) 1575. 4. M. Betz.2 N. Appl. This is caused by the excess of Te atoms replacing a part of the . -1 Conductivity of sample (7) Linear fit to the data -2 ln (σ) (Ω . mobility and carrier concentration were increased signiﬁcantly compared to pure CdTe samples.  for similar temperatures. Pakistan. References  G. Phys. Naghma Haider are thanked for their help in the X-ray diffraction analysis. The band gap values are also inﬂuenced by Te incorporation. Peshawar University.8 3. 7.5 -1.0 -5.0 -1. Matsumoto. Lett. P. S. N.  K. Conclusion In this work.ARTICLE IN PRESS 484 -0.4 2. Yamaguchi. which increase the p-type carriers. while the diffusion of Te in the CdTe ﬁlms cause an increase in the number of the charge carriers. The transmission spectra showed a decrease of transmittance with increase of Te. M Anees-ur Rehman and Mrs. As the concentration of Te increased the resistivity was reduced.H.
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