Tuning of structural, optical, and magnetic properties of ultrathin and thin ZnO nanowire arrays for nano device applications
© Sharma et al.; licensee Springer. 2014
Received: 18 November 2013
Accepted: 19 February 2014
Published: 17 March 2014
One-dimensional (1-D) ultrathin (15 nm) and thin (100 nm) aligned 1-D (0001) and () oriented zinc oxide (ZnO) nanowire (NW) arrays were fabricated on copper substrates by one-step electrochemical deposition inside the pores of polycarbonate membranes. The aspect ratio dependence of the compressive stress because of the lattice mismatch between NW array/substrate interface and crystallite size variations is investigated. X-ray diffraction results show that the polycrystalline ZnO NWs have a wurtzite structure with a = 3.24 Å, c = 5.20 Å, and  elongation. HRTEM and SAED pattern confirmed the polycrystalline nature of ultrathin ZnO NWs and lattice spacing of 0.58 nm. The crystallite size and compressive stress in as-grown 15- and 100-nm wires are 12.8 nm and 0.2248 GPa and 22.8 nm and 0.1359 GPa, which changed to 16.1 nm and 1.0307 GPa and 47.5 nm and 1.1677 GPa after annealing at 873 K in ultrahigh vacuum (UHV), respectively. Micro-Raman spectroscopy showed that the increase in E2 (high) phonon frequency corresponds to much higher compressive stresses in ultrathin NW arrays. The minimum-maximum magnetization magnitude for the as-grown ultrathin and thin NW arrays are approximately 8.45 × 10−3 to 8.10 × 10−3 emu/g and approximately 2.22 × 10−7 to 2.190 × 10−7 emu/g, respectively. The magnetization in 15-nm NW arrays is about 4 orders of magnitude higher than that in the 100 nm arrays but can be reduced greatly by the UHV annealing. The origin of ultrathin and thin NW array ferromagnetism may be the exchange interactions between localized electron spin moments resulting from oxygen vacancies at the surfaces of ZnO NWs. The n-type conductivity of 15-nm NW array is higher by about a factor of 2 compared to that of the 100-nm ZnO NWs, and both can be greatly enhanced by UHV annealing. The ability to tune the stresses and the structural and relative occupancies of ZnO NWs in a wide range by annealing has important implications for the design of advanced photonic, electronic, and magneto-optic nano devices.
One-dimensional (1-D) inorganic nanostructures have stimulated great interest because of their unique physical and chemical properties [1–4] such as flexibility of nanostructures [5–7], metal-insulator transition [4, 8], superior mechanic toughness , higher luminescence efficiency, and lower lasing threshold [8, 9]. Moreover, 1-D nanostructure research has elucidated many biomarkers  which have the potential to greatly improve disease diagnosis. Among these materials, zinc oxide (ZnO), which is an n-type II-VI semiconductor with wide band gap energy (Eg = 3.37 eV at 300 K) and large exciton binding energy of (60 meV), has been proven as a promising candidate for multifunctional materials [11–15], variators , bulk acoustic wave devices , magneto-optic devices, UV light-emitting devices , gas sensors [10, 19], solar cells [11, 20], and field emission display devices [15, 21]. In addition to this, ZnO exhibits piezoelectricity  in surface acoustic wave (SAW) devices and bio-compatibility . Thus, ZnO-based 1-D nanostructures are very attractive materials to explore further because of their structural, electronic, optical, and magnetic properties, which can be easily tailored through doping, alloying, and nano engineering.
Many techniques have been employed to fabricate 1-D nano architectures, such as EBL , NIL , VLS , CVD , sol-gel , hydrothermal process , and thermal evaporation . Electrochemical deposition demonstrates another important approach to the synthesis of 1-D nanostructures . This approach is promising in terms of cost and ease of mass production.
Recently, the stress-related issues in the nanostructures have been considered for the integration of nano devices with high performance and functionality. Several aspects play a vital role in the control of stresses within the 1-D nanostructures [32–34]. Sheng et al.  demonstrated the conversion of mechanical energy into a 1.2-V electrical energy due to the 0.19% of strain induced in the aligned ZnO NWs. The electrical, optical, and magnetic properties of 1-D nanostructure are also affected by the residual stress . Zhang et al.  and Azaceta et al.  reported the c-axis-oriented ZnO film growth and observed that thermal annealing treatment eliminates residual stress of the film. Seipel et al.  demonstrated that the variation in electrodeposited ZnO nanostructure crystal stresses is due to interstitial defects, voids, etc. Agrawal et al.  explained the importance of uni-axial stress between bulk and thin films. All the above works are not related to the effects of the nanostructure/substrate interface stresses which can influence the structural, electronic, and magnetic properties of nanowire (NW) array. There are various proposed mechanisms for intrinsic residual stress generation . One possibility that has been often cited for the compressive intrinsic stress is the development of free surfaces or variation in crystal size of nanostructures before other competing stress is generated during process.
The interfacial interaction of a nanostructure with its substrate is a critical issue from the technological viewpoint, which is not clearly addressed previously. In particular, the stress-related issues in ultrathin and thin NW array grown by one-step electrochemical deposition have also not been investigated. Raman scattering has been extensively used to investigate the oxide materials, and it is a proven method for analyzing the residual stress in films . However, Raman spectroscopy has not been used for stress analysis of NW arrays.
Further, the tunable ferromagnetic properties of ZnO show great potential for the use in spintronic and magneto-optic-based devices. As the dimensions of ZnO nanostructures are comparable to that of its exciton Bohr radius (approximately 2.4 nm), interesting optical emissions have been observed due to the band gap engineering from 2.5 to 6 eV by alloying. Xu et al.  investigated magnetic properties of ZnO nanostructured film of approximately 15-nm grain size deposited by a sol-gel technique at room temperature. However, the microscopic origin of this ferromagnetic transition is poorly understood. Moreover, the variation in crystallite size poses the serious consequences on mobility of nanostructures [41, 42]. Understanding and control of these properties are the most important challenges in magnetism and photonics for the use of ZnO NWs in spintronics, lasing, and magneto-optic devices.
Recently, we reported the growth of approximately 100-nm ZnO NWs anchored on a substrate by a chronoamperometry method . Here, we consider a size-dependent (approximately 15 to 100 nm) study of one-step electrochemically grown, well-aligned ultrathin and thin ZnO NW arrays before and after ultrahigh vacuum (UHV) thermal annealing treatment. We address residual stress-generated critical issues related to structural, optical, and magnetic properties. The generation of stress influences the various crystallographic axes of 1-D ZnO NW arrays, or a range of defects and complexes, causing lattice expansion or contraction. Therefore, examining the stress in the NW arrays could provide useful information on the defect evolution, which is very important to better understand and improve the film's electrical, optical, and magnetic properties. On the other hand, it is realized that the band structure of 1-D ZnO NW arrays and localized electron spin interaction may change with the stress field and thus modify the optical, electrical, and magnetic characteristics. The morphological, structural, and compressive stress analysis of 1-D NW array is carried out by field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), and Raman spectroscopy, respectively, before and after thermal annealing treatment. Similarly, hot probe and vibrating sample magnetometer (VSM) analyses were performed to check the conductivity and magnetization properties of the 15- and 100-nm 1-D ZnO NW arrays.
Synthesis of 1-D NW array
The FESEM images of the grown ZnO nanowire arrays were captured using a Carl Zeiss Supra 40 microscope (Oberkochen, Germany) at an acceleration voltage of 10 kV. The hot probe analysis of ultrathin (15 nm) and thin (100 nm) ZnO NW arrays before and after thermal annealing treatment was carried out for majority charge carrier analysis; the detailed specifications are given elsewhere . High-resolution transmission electron microscopy, FEI (TECNAI, Hillsboro, OR, USA), having selected-area electron diffraction (SAED) facility was used for structure analysis of the grown NW such as crystallinity, d-spacing, and c-axis orientation. The XRD experiments have been conceded in order to characterize the structural evaluation of the as-grown ultrathin and thin ZnO NW arrays before and after thermal annealing treatment. Thin film XRD spectra of the ZnO NW arrays were taken on a PANalytical X'Pert PRO diffractometer (Almelo, The Netherlands) operating in the θ to 2θ Bragg configuration using CuKα (λ = 1.5405 Ǻ) radiation. Data were collected at a scan rate of 0.02° s−0 and a sampling interval of 0.0197°. The voltage was set at 45 kV with a 44-mA flux. The relative percentage intensities and crystalline quality of the NW array peaks were computed, considering the highest and full-width half maximum (FWHM) of  peak for ZnO NWs [44–48]. The stress analysis of the ZnO nanowires was carried out using a WiTec CRM 200 micro-Raman spectrometer (Ulm, Germany) coupled with a high-resolution confocal optical microscope with a laser excitation of 514.5-nm; a detailed specification is given in our previous work . Transitions between weak and strong magnetic states of ZnO NW arrays before and after UHV treatment were studied using ADC Technologies Model 32KP (GMW Magnetic system; Newport Beach, CA, USA) VSM after the necessary background diamagnetic subtraction. The magnetization of the copper substrate was first measured and corrected for the experimental data. In this work, the magnetic data are presented in emu/g.
Results and discussion
Variation in peak intensities measured from XRD diffractograms of ultrathin (15 nm) ZnO NW arrays
300 K (room temperature)
Variation in peak intensities measured from XRD diffractograms of thin (100 nm) ZnO NW arrays
300 K (room temperature)
The percentage of relative intensity of the  peak varies from 0.23 to 0.68 cts for as-grown to the thermally treated ultrathin NW arrays at 873 K. Similarly, this value varies from 0.03 to 0.11 cts for thin NWs. Thus, thermal treatment of NW arrays at 873 K causes a significant shifts of approximately 0.45 and approximately 0.08 cts for ultrathin and thin NWs. Thus, annealing effect enhanced the fraction of crystallites in well-aligned ZnO NW arrays . These XRD studies confirm that the as-grown 15-nm ZnO NWs are found to have higher crystallinity than 100-nm NWs.
FWHM, d-spacing, crystallite size, and compressive stress variation computed from the XRD diffractograms
15-nm ZnO NWs
100-nm ZnO NWs
Crystallite size (nm)
Crystallite size (nm)
Likewise, the residual compressive stress drives the Zn ions of the outermost layer inward and results in the reduction of Zn-O bond length of dimmers due to thermal annealing. The surface energies of the polar surfaces  and  are greater than those of the non-polar  and  surfaces for all nanostructures [53–55]. The variations in the bond length of Zn-O dimmers cause tilting from its alignment perpendicular to the direction as shown in Figure 12b. The variation in compressive stress related to the change in bond length alignment in the dimmers can cause the increase in Zn concentration as a result of adsorption/desorption of oxygen atoms within NW array due to the effect of thermal annealing treatment. The formation of newly crystal faces as a consequence in the variation of crystallites and grain boundaries related to the compressive stress could be another, possible reason. It is thus concluded that lattice mismatch, defects, grain boundaries, NW/substrate interaction, and annealing treatment are major causes for the stress variations.
The estimation of majority charge carriers in the ZnO NW array is done through hot probe technique. The ultrathin and thin as-grown and thermally treated NWs at 473, 673, and 873 K in the presence of UHV show positive voltages of 320, 360, 392, and 482 mV, respectively, for 15-nm NW arrays and 109, 157, 205, and 286 mV, respectively, for 100-nm NW arrays. The positive magnitude of voltage indicates that the grown ZnO nanowires are n-type semiconductors. The higher values of readout voltage for ultrathin as compared to the thin indicate that the ZnO segregation as a separate phase in the grain boundary regions results in the higher number of majority charge carries for ultrathin NW arrays . Indeed, the most important parameters that influence their electrical properties are the crystallite size and the adsorption/desorption processes of oxygen. Moreover, the changes in conductivity of ZnO NW arrays with UHV annealing most likely result from variations in the number of oxygen species adsorbed/desorbed on the ZnO surfaces or in the number of oxygen vacancies in the ZnO bulk. Therefore, the UHV annealing in vacuum should decrease the number of adsorbed oxygen species onto the surface and increase the number of bulk oxygen vacancies; these act as electron donors for ZnO NW arrays. This effect is more prominent for the ultrathin as compared to the thin NW arrays because of the small dimensional quantum confinement and higher oxygen vacancies in the former. It might have the order of 1020 surface oxygen sites per cubic centimeter of nanostructures. Thus, even for partial changes in the concentration of adsorbed oxygen species, large changes in NW arrays conductivity can be observed. Hence, the strong dependence of the conductance on the oxygen vacancies occupancy in ZnO 1-D NW arrays is an important characteristic of functional oxide, using one that can tune and control the electrical properties of the nano device, especially the threshold voltage of ZnO-based field effect transistors (FinFETs and MOSFETs). Nevertheless, the charge carrier behavior may be a composite effect of oxygen vacancy, oxygen interstitial site, zinc vacancy, and zinc interstitial site within the ZnO NW arrays. Therefore, the evolution of the majority of charge carrier mobility does not follow an expression rigorously proportional to crystallite size and oxygen vacancy [41, 42, 56, 59]. As shown in Table 3, the gradual increase in the crystallite size for all samples with the annealing effect of UHV treatment reveals the redistribution of oxygen vacancies and deoxidization of trap density. Similar evolution was also observed by Kishimoto et al.  in undoped ZnO thin films for the critical film thickness of approximately 130 nm.
Materials with important combinations of properties such as room-temperature ferromagnetism and semi-conductive properties are required for spintronic and magneto-optic device application. Novel functionalities can be achieved, for example, in spin-FETs or spin-LEDs, if the injection, transfer, and detection of carrier spin can be controlled electrically or optically. ZnO-based ultrathin and thin NWs are thought to be ideal systems for spintronics and magneto-optic device application because of two most promising material criteria: (i) ferromagnetism should be retained up to room temperature and above the room temperature and (ii) the electrical and optical properties of ferromagnetic semiconductors should allow for spin manipulation.
However, Figure 18 shows the hysteretic behavior and non-saturation of the magnetization for thin NW arrays even after the UHV treatment. Further, there is a steady decrease of magnetization in 15-nm as well as in 100-nm ZnO NW arrays with the UHV annealing treatment at different temperatures as shown in the Figure 17 curves b, c, and d and Figure 18 curves b, c, and d. In contrast, the saturation of magnetization for ultrathin NWs occurs at relatively lower fields, approximately 5,000 Oe. These results indicate a relatively small factor of 2 shifts in the magnetization of ultrathin (15 nm) ZnO NW arrays even after UHV annealing. In contrast, a much larger change of 2 orders is observed for thin (100 nm) NW arrays. In fact, the as-grown ultrathin NWs have higher magnetization, approximately of the order of 4 as compared to the thin ZnO NW array, though the observed magnetism in well-aligned ZnO NW arrays is unexpected, because neither Zn2+ nor O2− is magnetic. Thus, there is no apparent source for magnetism in undoped ZnO . As no magnetic impurities were present, it appears that the origin of ultrathin and thin NW array ferromagnetism may be the exchange interactions between localized electron spin moments resulting from oxygen vacancies at the surfaces of the ZnO NWs. Furthermore, the observed magnetization in the ZnO NW array may be probably due to the defects. We presumed that those defects are located close to each other and mostly are at the NW surfaces (skin effect), and after UHV treatment, reduction in magnetism indicates the decrease in the number of density defects as those in ultrathin films . It supports our previous observation of XRD and Raman analyses. These studies will pave the way for the use of high-aspect-ratio 15-nm ZnO NWs as nanoscale spin-based devices, such as spin valves and spin FETs. The 100-nm ZnO NWs for deep UV magneto-optic device application with the ultimate goal of manipulating a single electron spin and polarization reflected intensity rather than the charge and source as in more conventional devices. The summary of most important scientific results of ultra-thin and thin NW array and respective device applications is in Additional file 1.
We synthesized 1-D well-aligned ultrathin (15 nm) and thin (100 nm) ZnO NW arrays by the one-step chronoamperometry at reduction potential of −1.2 V. The structural, optical, electrical, and magnetic analyses of ultrathin and thin NWs are conceded by FESEM, HRTEM, X-ray diffraction, micro-Raman, hot probe, and VSM. FESEM images illustrate the aspect ratio of 133 and 20, respectively, for well-aligned 15- and 100-nm ZnO NW arrays. HRTEM and SAED patterns confirmed the polycrystalline nature of the ultrathin ZnO NWs and lattice spacing of 0.58 nm. X-ray diffraction results show the wurtzite structure of the as-grown polycrystalline ZnO NW and  elongation. There is higher noteworthy shift in the  peak intensity for ultrathin than that for thin as-grown and thermally treated NW arrays at 873 K, revealing that the 15-nm ZnO NWs are much better suited for optical emission-based applications than 100-nm NWs. Furthermore, structural stress-related critical issues on the understanding of 1-D ZnO NW arrays will provide useful information on the defect evolution, which is very important to better understand and improve the electrical, optical, and magnetic properties of nanostructures.
Therefore, the higher shift in magnitude of compressive stress for the as-grown ultrathin than thin ZnO NW arrays and UHV annealed at 873 K indicates that the 15-nm ZnO NW arrays are at higher compressive stress than the 100 nm. Micro-Raman results show the increase in E2 (high) peak intensity, and the decrease in FWHM represents the increase in crystallite size and an improvement in the crystalline quality of NW arrays after the annealing treatment. These results demonstrate that 15-nm ZnO NW have lower lasing power threshold than 100-nm NW due to the higher crystallinity of the ultrathin ZnO NW arrays. The positive voltage for hot probe measurements points out that the grown ZnO NWs are n-type, and the higher values of voltage and vacancies for 15 nm as compared to those of the 100-nm NWs indicate the higher number of majority charge carries for ultrathin NW arrays than that for thin. Therefore, by tuning the oxygen vacancies occupancy, one can control the electrical properties of the nano device, especially the threshold voltage of ZnO-based field effect transistors (FinFETs and MOSFETs). The VSM results reveal that the as-grown 15-nm NWs have the higher magnetization approximately of the order of 4 as compared to the 100-nm ZnO NW array. In fact, there is a shift in magnetization and a propensity of saturation of magnetization for 15-nm ZnO NW arrays by factor 2 and at approximately 5,000 Oe even after UHV annealing at 873 K. In contrast, a much larger change of 2 orders and a tendency of saturation of magnetization occur at approximately 10,000 Oe for 100-nm NW arrays. These studies will pave way for the use of high-aspect-ratio 15-nm ZnO NWs as nanoscale spin-based devices, such as spin valves and spin FETs and 100-nm ZnO NWs for deep UV magneto-optic device application.
SKS earned his M.Sc. degree in Physics (Electronic Science) from H.P.U., Shimla, H.P., India in 2002 and his Ph.D. from the Department of Electronics Science, Kurukshetra University, Kurukshetra (Haryana), India, in 2007. He worked as a Post-Doctoral Fellow in the DST Unit on Nanoscience and Nanotechnology, Department of Chemical Engineering at Indian Institute of Technology (IIT)-Kanpur, India, from 2007 to 2010. He was employed as a faculty in the Electronics and Microelectronics Division, Indian Institute of Information Technology, (IIIT)-Allahabad, India, from 2010 to 2012. He is currently an Assistant Professor in the School of Computing and Electrical Engineering, Indian Institute of Technology (IIT)-Mandi, India. His current research interests include microelectronic circuits and system, CMOS device fabrication and characterization, nanoelectronics, nano/micro fabrication and design, polymer nanocomposite, and sensors, photovoltaic and self assembly. NS is currently working as a Project Scientist at Rajiv Gandhi Institute of Petroleum Technology (RGIPT), Raebareli, Uttar Pradesh, India. Prior to joining the RGIPT, she worked as a Project Scientist in the DST Unit on Nanoscience, Department of Chemical Engineering, Indian Institute of Technology (IIT), Kanpur, India. She holds two M.S. degrees in Physics, one from Shri Shahu Ji Maharaj University Kanpur, India, with a specialization electronics, and the other from the National University of Singapore (NUS), Singapore. Her research work was mainly focused on the synthesis/fabrication and applications of nano-structures. SB is currently a Ph.D. scholar at the Department of Bio and Nano Chemistry, Kookmin University, Seoul, South Korea. He received his M.Sc. degree in Chemistry from Shri Shahu Ji Maharaj University Kanpur, India. He worked as a Project Associate in the DST Unit on Nanosciences, Department of Chemical Engineering at Indian Institute of Technology (IIT), Kanpur, India. His research work is focused on superamphiphobic surfaces, nonporous materials, surface topography analysis, nano structures, flexible sensors, etc. RK completed his B.Sc. degree in Chemical Engineering from BIT Sindri (Jharkhand), India, in 2009 and M.Tech. degree from the Indian Institute of Technology Kharagpur in Chemical Engineering (West Bengal), India, in 2011. Currently, he is doing his Ph.D. in the Indian Institute of Technology Kanpur (India) in Chemical Engineering under the guidance of Prof. Ashutosh Sharma. His research interest includes fabrication of porous carbon materials, graphene, amorphous carbon, and carbon aerogel for supercapacitor and biological applications. AS is currently an Institute Chair Professor in Chemical Engineering and Coordinator of Nanosciences Center at the Indian Institute of Technology at Kanpur. AS received his Ph.D. from the State University of New York at Buffalo (1987), his MS from the Pennsylvania State University (1984), and B. Tech. from IIT Kanpur (1982). AS research interests are in soft functional interfaces, micro/nano-mechanics of soft matter, self-organized patterning, colloid and interfacial engineering, carbon MEMS/NEMS in energy, health and environmental applications, wetting, adhesion and thin films - areas in which he has published over 270 peer-reviewed papers. He is currently an associate editor of ACS Applied Materials and Interfaces and has been a member of the editorial boards of ACS Applied Materials and Interfaces, Industrial and Engineering Chemistry Research, ASME Journal of Micro- and Nano-Manufacturing, Nanomaterials and Energy, Chemical Engineering Science, Journal of Colloid and Interface Science, Canadian Journal of Chemical Engineering, and Indian Chemical Engineer.
Authors acknowledge the support of the Department of Science and Technology (DST), New Delhi, through its financial support from DST-IRPHA grant and the Thematic Unit of Excellence (Nanoscience and Nanotechnology in Nanofabrication: Top-down, Bottom-up and Beyond) at IIT Kanpur, for providing the state-of-the-art experimental facility available at Indian Institute of Technology Kanpur.
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