Sensors and Actuators A 207 (2014) 6166

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Sensors and Actuators A: Physical

journal homepage: www.elsevier.com/locate/sna

A wide-band UV photodiode based on n-ZnO/p-Si heterojunctions

N.H. Al-Hardan a, , Azman Jalar a, , M.A. Abdul Hamid b , Lim Kar Keng b , N.M. Ahmed c , R. Shamsudin b
Institute of Microengineering and Nanoelectronics (IMEN), Universiti Kebangsaan Malaysia (UKM), 43600 Bangi, Selangor, Malaysia Faculty of Science & Technology, Universiti Kebangsaan Malaysia (UKM), 43600 Bangi, Selangor, Malaysia c School of Physics Universiti Sains Malaysia (USM), 11800 Penang, P. Pinang, Malaysia
b a

a r t i c l e

i n f o

a b s t r a c t
We report on the fabrication of zinc oxide (ZnO) nanorods on p-type silicon (p-Si) photodiodes. The nanorods are prepared by low-temperature hydrothermal processing. The fabricated photodiodes exhibit an excellent rectifying ratio of 370 at 10 V. The responsivity to ultraviolet (UV) photons is stable at 0.29 A/W up to 300 nm, with a peak value of 0.38 A/W at 360 nm. Furthermore, the prepared photodiodes demonstrate visible blind behavior, indicating that ZnO nanorods grown on p-Si substrates can be used as UV photodiodes with visible blind responses. 2013 Elsevier B.V. All rights reserved.

Article history: Received 29 July 2013 Received in revised form 11 December 2013 Accepted 13 December 2013 Available online 24 December 2013 Keywords: ZnO nanostructures Heterojunction UV photodiode Hydrothermal

1. Introduction Zinc oxide (ZnO) has become one of the most prominent potential materials for various applications due to its attractive properties. For instance, ZnO has been used in optoelectronic and electronic devices [1]. Recently, ZnO has been used in more advanced applications, such as ultraviolet (UV) light-emitting diodes (LEDs) [2], UV lasing [3], spintronics [4], and nanogenerators [5]. ZnO can be easily grown with different nanostructure morphologies [6], making it attractive for use in nanoscale devices. ZnO is a wide-band gap semiconductor (Eg = 3.37 eV) that belongs to the IIVI group. It has an exciton binding energy of approximately 60 meV, which makes it appropriate for UV optoelectronic applications. The high exciton binding energy of ZnO makes it a more attractive compound than GaN (exciton binding energy of 26 meV) and other compounds. Furthermore, high-quality ZnO can be prepared using simple methods, such as thermal evaporation [7], solgel processing [8], zinc oxidation[9], and hydrothermal processing [10], which have been used to create ZnO nanostructures with different morphologies. ZnO nanostructures prepared through hydrothermal processing have high-quality crystals with wurtzite structures [1012].

Corresponding authors. Tel.: +60 03 989217002; fax: +60 03 89216863. E-mail addresses: naif imen@ukm.my, n.h.alhardan@gmail.com (N.H. Al-Hardan), azmn@ukm.my (A. Jalar). 0924-4247/$ see front matter 2013 Elsevier B.V. All rights reserved. http://dx.doi.org/10.1016/j.sna.2013.12.024

Moreover, the hydrothermal process can be used for large-area substrates at relatively low temperatures [11]. One of the promising applications of ZnO nanostructures is in the eld of UV sensing. Previous studies have reported a variety of sensing performances for UV ZnO sensors. The UV sensing performance of ZnO sensors is correlated with the preparation conditions that produce different morphologies of ZnO [13]. ZnO-based UV sensors for metal-semiconductor-metal (MSM) devices and pn junction devices have also been demonstrated [13]. ZnO has n-type characteristics due to the low formation energy of its oxygen vacancies and zinc interstitial atoms that can be formed during the synthesis process [14,15]. However, the growth of ptype ZnO is still far from reliable due to the deep acceptor levels and low solubility of the dopant [16,17]. Hence, n-ZnO must be grown on a p-type substrate, such as silicon [14], silicon carbide [18], or gallium nitride [19]. These substrates are preferable because they serve as holders for the device. Silicon has been widely used in the electronics industry for a variety of well-developed technologies. The growth of high-quality ZnO on Si substrates is crucial for several applications, including optoelectronic devices [20,21]. n-ZnO/p-Si heterojunction-based devices are potential candidates for UV and visible light detection; however, these photodiode typically have low responsivity [20], due to the energy barrier at the junction interface. Several studies have used n-ZnO/p-Si heterojunctions for UV and visible light applications. Lie et al. [14] prepared heterojunctions with n-ZnO nanowires on a p-Si substrate for UV photodiodes using a thermal evaporation process. The photodiode exhibits a low

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response of approximately 0.07 A/W for UV light (365 nm) under a 20 V reverse bias. Cho et al. [22] reported on the effect of the thickness of RF-sputtered ZnO on its responsivity to 420 nm UV light, and the detection performance was observed to increase with increasing thickness of the ZnO thin lm. Hai et al. [23] grew ptype Si nanowires on a Si wafer and applied a ZnO coating using RF. These nanowires were used in a deep UV photodiode that displayed a higher responsivity (19.2 A/W) to 254 nm light. Despite several reports on the application of n-ZnO/p-Si in UV diode sensors, this device still has a low responsivity to UV light. Here, we report on the growth of n-ZnO on p-Si. The n-ZnO layer is grown over a thin-lm seed layer of ZnO, resulting in a high density of nanorods. The device demonstrates a wide-range of high UV responsivity, with an almost blind response to visible light. This behavior makes the device suitable for UV detection with a visible light background.

2. Experimental details Prior to the growth of the n-ZnO, the p-Si (1 0 0) substrates were cleaned ultrasonically with acetone, ethanol, and deionized (DI) water. The substrates were then dried in a stream of air. A thinlm seed layer of ZnO was coated via DC reactive sputtering with a thickness of approximately 200 nm using a PVD 75 sputtering unit (Kurt J. Lesker). The substrates with the ZnO seed layers were heat-treated at 400 C for 1 h in an air atmosphere to improve the grain structure. The ZnO nanorod arrays were prepared from 25 mM aqueous solutions of zinc nitrate hydrate (Zn(NO3 )2 6H2 O) and hexamethylenetetramine (C6 H12 N4 ), which were reagent grade and were obtained from ChemPur and Sigma-Aldrich, respectively. Both reagents were dissolved in 150 ml of DI water and stirred continuously for 1 h. The substrates were vertically immersed in the solutions in a screw-capped bottle. This bottle was moved to a convection oven and heated at a temperature of 95 C for 6 h. The bottle with the samples was then removed from the oven and cooled to room temperature. The samples were washed with DI water several times and dried in an oven at 100 C for 30 min. The samples were then post-annealed for 1 h at 400 C under ambient atmospheric conditions. The surface morphologies of the ZnO structures were investigated using eld emission scanning electron microscopy (FE-SEM), which was conducted on a LEO SUPRA 55VP (Carl Zeiss) with energy-dispersive X-ray spectroscopy (EDX, Oxford Inca) to determine the elemental compositions. X-ray diffraction (XRD, Bruker D8 ADVANCE) was used to identify the phase structures. The XRD was operated at a voltage of 60 kV and a current of 60 mA using a copper target that emitted 0.154 nm X-rays. For the optical emission measurements, the photo-luminescence (PL) spectrum was recorded using an Edinburgh Photonics FLS920 device with a xenon lamp (450 W). The measurement range was 3.871.8 eV (320800 nm). The excitation wavelength was 300 nm. The measurements were performed under atmospheric conditions (21 C, 50% relative humidity). A Keithley electrometer (model 6517A) was used to characterize the device; the electrometer was connected to a personal computer through a GPIB card to conduct the measurements and store the data for further analysis. A UV LED with a wavelength of 365 nm and an intensity of 3.2 W cm2 was used as a UV light source. The spectral responsitivity (R) measurements were obtained using a 150 W high-pressure xenon lamp (LLC-7 from Lambda Scientic Pty Ltd) and a manual type monochrometer (Photon Technology International, Inc.). The device was measured under different monochromatic lights. The measured currents at a bias voltage of 4 V were divided by the intensities of the corresponding monochromatic lights to obtain the normalized spectral responsitivity values.

Fig. 1. XRD of the prepared ZnO nanorods on p-Si substrates.

We also investigated the dark capacitance as a function of the applied voltage using an Agilent 4294A impedance analyzer at room temperature with a frequency of 1 MHz. The ZnO/Si photodiode heterojunctions were coated with silver as a contact material (with thickness of approximately 130 nm) for both sides of the device. The samples were then heat-treated at 300 C for 10 min to ensure good Ohmic contact. Thin copper wires were pasted on the silver contacts using an electrical conductive paste to connect the device to the measurement unit. 3. Results and discussion 3.1. Structure and morphology of the ZnO The XRD pattern of the ZnO layer is depicted in Fig. 1. The scanning Bragg angle was 2060 . The samples exhibited preferential orientation along the (0 0 2) plane, as indicated by the dominant peak at approximately 34.5 , which was attributed to the (0 0 2) phase of the hexagonal ZnO structure (with reference to JCPDS No. 36-1451). This phase is typically dominant for ZnO, as it has the lowest surface energy among the possible orientations of the hexagonal ZnO structure. The seed layer of the sputtered ZnO likely enhanced the growth of ZnO (0 0 2) phase. The sharp diffraction peak from the (0 0 2) plane indicated the excellent crystallinity of the prepared sample. FE-SEM images of the ZnO layer are presented in Fig. 2, which illustrates that highly packed ZnO nanorods with well-dened hexagonal structures were formed perpendicular to the surface of the substrate (inset of the gure). These data agree with the XRD pattern of the prepared ZnO. The EDX peaks (not shown) at 0.52 and 1.2 keV belonged to oxygen and zinc, respectively. The quantitative EDX analysis of the surface indicated that the oxygen content was higher than the zinc content. Fig. 3 presents the room-temperature PL spectrum using excitation energy of 300 nm for the ZnO nanorods on the p-Si substrate. The photon range was 1.83.87 eV. The spectrum exhibits a UV emission peak at approximately 3.20 eV. The origin of this emission can be attributed to the excitonic recombination of the near-band edge emission. The width of the UV emission indicates that the peak consists of several emissions. The emissions can be attributed to the two-phonon replicas due to two transverse optical phonons with a separation of approximately 100 meV [24]. The PL spectrum also revealed a strong emission band at 2.83 eV (blue), which was attributed to singlet ionized VZn [25]. Weak emissions were

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Fig. 4. IV characteristics of the n-ZnO/p-Si heterojunction measured at room temperature. Fig. 2. SEM image of the ZnO nanorods on a p-type Si substrate. The inset shows the cross section n-ZnO/p-Si.

3.2. UV sensing performance of the Si/ZnO heterojunctions Fig. 4 presents the IV characteristics of the ZnO/Si heterojunctions in dark conditions. The prepared device has excellent rectifying behavior with a leakage current of approximately 4 A at 10 V. The result of the reverse current was comparable to other published values [32]. Moreover, the forward current of 1.47 mA at 10 V indicated the formation of a reasonably good rectifying diode. The rectifying behavior also conrmed the formation of a heterojunction barrier at the interface of the n-ZnO and p-Si substrate, as well as a built-in potential in the sample (the contacts on each side of the device display an Ohmic behavior). The rectication ratio (If /Ir , where If and Ir denote the forward and reverse current at 10 V, respectively) of the prepared pn heterojunction was 370. The turn-on voltages were determined by extrapolating the IV curve to the intersection of the abscissa. The value was approximately 7.0 V, indicating the exponential behavior of the IV curve. The higher value for the turn-on voltage can be attributed to the interfacial layer between the ZnO and Si substrate, which is believed to be the seed layer of the ZnO lm or the native oxide layer of the Si substrate. Because the standard cleaning procedure was not used in this work, this layer inuences the electronic conduction through the device [19,33]. Furthermore, the breakdown voltage of the sample was larger than 30 V (not shown), which is one of the highest values published to date [3436]. The rectifying behaviors of the ZnO/Si heterojunctions can be explained using the Anderson model [37]. The electron afnity of the Si and ZnO were 4.05 and 4.35 eV, respectively, for the respective band gaps of 1.12 and 3.37 eV [36,38]. The discontinuity in the conduction band ( EC ) was smaller than the discontinuity of the valance band ( EV ). This lower value resulted from the difference between the electron afnities of the two semiconductors. EC was 0.30 eV under the forward bias, indicating that electrons moved easily to the p-Si, constituting the forward current. The barrier from the valance offset to the ow of holes from the p-Si to the n-ZnO was high ( EV = 2.55 eV). Therefore, the current was small under the reverse bias, which resulted in a high rectifying ratio. The potential barrier at the junction can be measured by the capacitancevoltage (CV) technique. The capacitance of the junction results from the charges that escape from the depletion region. Fig. 5 depicts the CV measurements of the device measured at a high frequency of 1 MHz in the dark at room temperature. The C2 vs. voltage relationship was linear, which conrmed the formation of a heterojunction diode at the ZnO/Si interface. Under reverse bias conditions, the capacitance decreased as the reverse bias

Fig. 3. PL emission of the ZnO nanorods grown on p-Si.

observed at 2.75 and 2.64 eV. These peaks represent the transition from shallow donor oxygen vacancies (VO ) to valance bands [26,27]. The last emission band was a strong emission at approximately 2.0 eV (yellow-orange band). This band was attributed to the transition from the bottom of the conduction band to the oxygen interstitial (deep-level emission, DLE) [28]. PL measurements cannot be correlated with optical transitions from the defects to their origins. Thus, the PL emissions from the ZnO defect energy levels are extremely complex and still not fully understood. The ratio of the UV peak to the visible peak heights is typically used to indicate the quality of the ZnO. However, an increase in excitation energy always results in an increase in the ratio of the UV to the visible emission. Thus, high-intensity UV emission is not sufcient proof of high-quality crystallinity [24,29,30]. Furthermore, the emission intensity decreases with increases in the grain size of the ZnO nanoparticles [31]. In light of our XRD results, the ZnO is believed to be highly crystalline. However, the grain size of the ZnO was large, as shown in Fig. 2, because most of the grains were attached to neighboring grains to form large grains. The grain size of the sample plays a key role in the emission of light using PL spectroscopy techniques.

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Fig. 5. C2 vs. voltage relationship for the n-ZnO/p-Si pn heterojunction at 1 MHz.

Fig. 6. IV characteristics of the n-ZnO/p-Si heterojunction measured at room temperature under dark, ambient light and 365 nm UV light of 3.2 W cm2 .

increased. The carrier concentration in the n-ZnO was calculated to be 2 1017 cm3 from the slope. Low carrier concentrations have been reported to enhance the rectifying behavior of the diode [39]; this relationship was also observed in our diode. The carrier concentration was lower than the previously published concentrations for ZnO prepared via atomic layer deposition, pulsed laser deposition, and spray pyrolysis [3941]. However, it was similar to the published results for ZnO samples prepared using sputtering processes [42,43]. The lower carrier concentrations were due to better crystallinity, as indicated by the XRD results. The CV characteristics can be described using conventional heterojunction theory using [41]. C2 = qNA ND 1 2 1 2(ND 1 + NA 2 ) Vb V (1)

where ND and NA are the donor densities in the ZnO and the acceptor density in the Si, respectively, and 1 and 2 are the dielectric constants of the ZnO and Si, respectively. The applied bias voltage is denoted by V, where Vb is the built-in potential or potential barrier height. According to Eq. (1) and assuming that the doping level is uniform in the ZnO, for the extrapolated intercept of C2 with the voltage axis, the Vb value is estimated to be 1.5 V, which is similar to the value reported by Zhang et al. [44]. This value is high compared to most published results [41,45]. The high value for Vb is due to the different interface state densities at the heterojunction interfaces [44,46]. Furthermore, a thin layer of silicon dioxide can grow at the interface, thereby modifying the junction properties [32]. However, the value of Vb is still lower than the value obtained by Mansour and Yakuphanoglu [47]. Fig. 6 presents the IV characteristics of the pn heterojunction under a reverse bias. The device was exposed to UV LED light at 365 nm. The gure reveals that the fabricated diode is a visible blind, as the change in the current is insignicant after exposure of the device to ambient light. The measured current from the device with an applied voltage of 5 V noticeably increased from 2 to 45 A after the device was exposed to UV LED light. Fig. 7 presents the spectral responsivity (R) of the prepared photodiode at a reverse bias voltage of 4 V. The responsivity (R) can be calculated as follows [15]: R= IPh Iinc (2)

Fig. 7. Spectral response of the ZnO/p-Si heterojunction at a reverse bias of 4 V.

where IPh is the photocurrent (Iilluminated Idark ) and Iinc is the incident UV light power. The photo responsivity is nearly constant from 200 to 300 nm, with a decreased response from 320 to 340 nm. A drastic increase in the photo responsivity was noted at 360 nm (near the energy band gap of ZnO) with a responsivity

of 0.38 A/W. A sharp decrease in the responsivity was observed at 380 nm. The R decreased monotonically up to the maximum wavelength of 500 nm, indicating a nearly visible blind UV photodiode [29]. Previous published results for n-ZnO/p-Si structures report low responsivities [20,48]. The UV responsivity obtained here was higher than the published results for the p-NiO/n-ZnO [29], MgZnO/ZnO [49], and n-ZnO/p-SiC UV heterojunctions [18] and thin-lm ZnO/p-Si [20]. Fig. 8 presents the repeatability of the photodiode at a reverse voltage of 4 V. The prepared photodiode is highly repeatable, with a stable output. There is an exponential increase in the response as the LED is turned on. The response is almost stable, with photocurrent saturation. The rise time of the prepared photodiode is 11 s, with a full time of 14 s. The lower timing constant of the prepared heterojunction may be due to the effect of the surface state [50]. The photogenerated carriers were captured by the surface states of the ZnO nanostructures, which reduced the mobility of the photoexcited carriers. Furthermore, the oxygen molecules were adsorbed on the surface of the ZnO. The electrons from the ZnO surface were captured by the oxygen ions, resulting in the formation of a depletion layer near the surface. The surface depletion layer acted as a diffusion barrier, resulting in increased recombination and suppression of the photo-responsivity. In general, our time constants were similar to previously published constants [15,51]. However,

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pairs in the depleted ZnO nanorods. This result may be due to the large depletion layer of the ZnO nanorods. 4. Conclusions In summary, UV photodiodes with visible blind characteristics were fabricated using n-ZnO nanorods grown on p-Si. The photodiode was well-rectifying. The photodiodes displayed a wide range of UV responses from 200 to 300 nm with an almost xed responsivity; however, a peak was observed at 360 nm. Moreover, the photodiode exhibited a low response to visible light. Thus, it can be considered a visible blind photodiode. Acknowledgements This work was supported by the Universiti Kebangsaan Malaysia (UKM) through the short-term grant number DPP-2013-035. The authors are also thankful to the Centre for Research and Instrumentation Management (CRIM) at UKM for providing the PL measurements and FESEM. References
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Fig. 8. Dynamic behavior of the ZnO/p-Si UV photodiode for a reverse bias voltage of 4 V and a UV wavelength of 365 nm.

Fig. 9. The switching behavior of the n-ZnO/p-Si junction for different on-off state timing: (a) 30 mHz, (b) 100 mHz, and (c) 200 mHz.

our values were lower than those reported by Mridha and Basak [32]. One of the promising applications of photodiodes is in optical switching. Fig. 9 presents the effect of different frequencies of the LED on and off states. The on and off states of the LED were controlled using an Agilent 33220A function generator. The gure illustrates LED on-off timings, for (a) 30 mHz, (b) 100 mHz, and (c) 200 mHz. The ZnO/p-Si heterojunction is reasonably responsive for different frequencies. The mechanism for ZnO/p-Si detection of UV light can be introduced based on the above results. High-energy photons (hv > Eg) are absorbed in the ZnO layer. The electronhole pairs are then photo generated (hv e + h+ ). The photogenerated electronhole pairs diffuse into the built-in electric eld. The electrons and holes drift to the positive and negative electrodes of the ZnO and Si, respectively. Thus, the current increases due to the increasing reverse bias. On the other hand, the visible light photogenerated the electronhole pairs in the underlying p-Si. The electric eld drives the photogenerated holes toward the n-ZnO. The interface layer between the p-Si and n-ZnO (the SiO2 and ZnO seed layer) represents a high potential barrier that prevents the holes from crossing the interface layer. This barrier results in a low response for the visible light detection [48]. The results demonstrate that the higherenergy UV photons result in nearly xed numbers of electronhole

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Biographies
N.H. Al-Hardan (Naif H. Al-Hardan) obtained his B.Sc. and M.Sc. degrees in 1987 and 1998 from University of Mosul and University of Baghdad IRAQ, and his PhD degree from Universiti Sains Malaysia (USM) in 2011. Currently he is a Postdoctoral fellow at the Institute of Microengineering and Nanoelectronics (IMEN) Universiti Kebangsaan Malaysia (UKM). His interest research area is in the nanometer functional materials and their applications in optoelectric and chemical sensor devices. Azman Jalar received his B.Sc. (Hons) in Materials Science (1995) from Universiti Kebangsaan Malaysia (UKM), and his PhD in 2001 from University of Birmingham, UK. Currently he is Associate Prof. and Deputy Director of the Institute of Microengineering and Nanoelectronics (IMEN) (UKM). M.A. Abdul Hamid received his PhD (1999) from University of Liverpool, currently he is Associate Prof. in the School of Physics Universiti Kebangsaan Malaysia (UKM). His interest work is in the semiconductor materials and their applications in optoelectronic and chemical sensor devices. Lim Kar Keng graduated with a Bachelor of Science with Honors in Materials Science at the National University of Malaysia (UKM) in 2011. Currently, he is active as a PhD student at the National University of Malaysia (UKM). His present area of interest is the metal oxides thin lms and its applications. N.M. Ahmed (Dr. Naser M. Ahmed) received the B.Sc. degree in Physics from AlMustansiriya University, Iraq (1984), M.Sc. degree in Laser Physics from University of Technology, Iraq (1988), and PhD in Nanotechnology from University Sains Malaysia (USM), Malaysia (2006). Currently he is Assistant Prof. of School of Physics USM. His interest work is in the laser and optoelectronic elds. R. Shamsudin received her PhD (1999) from University of Shefeld, currently she is a Senior Lecturer in the School of Physics Universiti Kebangsaan Malaysia (UKM). Her interest work is in the ceramic materials.