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Article

ZnO Deposition on Silicon and Porous Silicon Substrate via Radio Frequency Magnetron Sputtering

by
Francisco Morales-Morales
1,
Lizeth Martínez-Ayala
2,*,
María R. Jiménez-Vivanco
3 and
Heberto Gómez-Pozos
4
1
Optical Research Center, A. C., Loma del Bosque 115, Col. Lomas del Campestre, León 37150, Mexico
2
Tepeji Graduate School, Industrial Engineering, Autonomous Hidalgo State University, Av. Del Maestro No 41, Col. Noxtongo 2da Sección, Tepeji del Río de Ocampo 42855, Mexico
3
Institute of Physics, UNAM, Circuito de la Investigación Científica, Ciudad Universitaria, México City 04510, Mexico
4
Computing and Electronics Academic Area, ICBI, Autonomous Hidalgo State University, Carretera Pachuca/Tulancingo Km. 4.5, Pachuca 42184, Mexico
*
Author to whom correspondence should be addressed.
Coatings 2023, 13(11), 1839; https://doi.org/10.3390/coatings13111839
Submission received: 31 August 2023 / Revised: 17 October 2023 / Accepted: 25 October 2023 / Published: 27 October 2023
(This article belongs to the Special Issue Recent Advances in Metallic and Metal Oxide Thin Films)
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Abstract

:
Nanostructured Zinc Oxide (ZnO) was deposited on silicon (c-Si) and macroporous silicon (m-PS) using a radio frequency (RF) reactive magnetron sputtering technique. Two RF powers of 60 and 80 W were selected for ZnO deposition on the substrates. Furthermore, the c-Si and m-PS substrate temperatures were kept at 500 and 800 °C, respectively. The morphological, structural, and optical characteristics of the samples were studied using scanning electron microscopy (SEM), an X-ray diffractometer (XRD), X-ray photoelectron spectroscopy (XPS), and photoluminescence spectroscopy (PL). The SEM images revealed the formation of ZnO nanorods on the c-Si and ZnO nanostructures constituted by the assembly of nanorods. It has been found that the increasing RF sputtering power caused the rise in the residual stress. In addition, the increase in the deposition temperature caused an improvement in the arrangement of the crystals, which was attributed to the decrease in crystal defects.

1. Introduction

ZnO is a semiconductor material with a wide band gap of 3.37 eV and a high excitation binding energy of 60 meV. In comparison to other semiconductor materials, ZnO has the main characteristics of presenting piezoelectricity, thermal and chemical stability, and high stability against environmental corrosions. It is also non-toxic, and its fabrication is low-cost [1,2,3]. Such properties have made ZnO an attractive material in technological applications, especially in light-emitting diodes [4,5], solar cells [6,7], catalysis [8,9,10], gas sensors [11,12,13], and optoelectronic devices [14,15]. ZnO applications become even more interesting when it is deposited on porous nanostructure substrates such as porous silicon (PS).
Recent studies on ZnO deposited on PS via EBIC (electron-beam-induced current) have demonstrated that ZnO/PS is an isotype heterojunction with the possibility of enhancing charge carrier flow, which makes it possible to obtain light-emitting diodes and solar cells [15]. Additionally, a sensor based on ZnO/PSNW (zinc oxide on porous silicon nanowires) showed excellent gas sensing performance for various NO2 concentrations (5–50 ppm), reaching a high electrical resistance rate of 35% for 50 ppm of NO2 [16]. Furthermore, studies revealed a pyroelectric coefficient in ZnO/PS 40 times higher than in ZnO/c-Si and a pyroelectric voltage as high as 2.4 V [17].
Various techniques have been applied to deposit ZnO on PS, such as spray pyrolysis [18,19], chemical vapor deposition [20], hydrothermal [3,21], sol–gel [22], and magnetron sputtering [23]. There even exist computational methods to describe and understand the formation of ZnO, such as density functional theory (DFT) and ab initio molecular dynamics simulation (AIMD) [24,25].
In the present work, we applied the magnetron sputtering technique because is the most used and studied for its efficiency, high interfacial adhesion, and ability to deposit high-density films. Furthermore, magnetron sputtering allows thin films to be deposited on different types of substrates at high temperatures with excellent uniformity and quality crystallinity. From a practical point of view, the study of the properties of thin films at higher temperatures makes it possible to ensure the durability and repeatability of devices operated at high temperatures. Therefore, a material needs to exhibit good thermal stability at operating temperatures. In general, the thermal stability of a material depends on factors such as structural phases and the degree of crystallinity, which are correlated with the route of synthesis [26].
When the magnetron sputtering technique is adopted, the pressure, gas type, gas flow, temperature, and power deposition have a significant effect on the quality of the formed films. For example, the working pressure can change the grain size and crystal structure of deposited ZnO, allowing the films of deposited ZnO to be oriented in different crystalline planes. Likewise, deposits made with low power density show a very smooth surface and preferential orientation of the grains [27]. Furthermore, the increase in oxygen content in the argon environment results in a decrease in the deposition rate of the films [27]. Husam S. Al-Salam and M. J. Abdullah deposited ZnO on PS, maintaining an RF power deposition of 150 W with its posterior annealing at 500 °C during 2 h. The results revealed a high and deep porosity with a roughness of 178 nm [28]. K. Cicek et al. formed ZnO on PS and silicon utilizing the RF&DC magnetron sputtering technique with a flow rate of Ar and O2 at 120 W power. They found that a pyroelectric coefficient of 8.2 can be achieved for deposits on PS, which is more than ~40 times higher than the one on Si substrate [17].
Although the deposition of ZnO films on PS substrates using the magnetron sputtering technique has been carried out, there are few reports detailing the study of higher temperatures and its comparison with power deposition on the properties of ZnO on PS. Under this scenario, it is of vital importance to study the synthesis parameters for the design and development of new devices. In this work, we have deposited ZnO on macroporous silicon using the magnetron sputtering technique, varying the RF power and the deposition temperature to study the effect caused by the porous substrate on the ZnO.

2. Materials and Methods

Macroporous Silicon (m-PS) substrates were fabricated on p-type crystalline Silicon (c-Si) wafers with a thickness of about 280 µm. The typical resistivity was 5–10 Ωcm and the planar orientation was (100). The native surface oxide on the reference wafers was chemically etched with a hydrofluoric acid solution (HF). Later, m-PS substrates were obtained via the electrochemical etching of c-Si, with a density current of 4 mA/cm2 for 15 min, using a mixture of hydrofluoric acid (HF, 48 wt.%) and dimetylformamide (HCON(CH3)2, 99.9 wt.%) as an electrolyte in the volumetric ratio of 1:3. Finally, m-PS substrates were oxidized for 30 min in the air to stabilize their surface [8,9,10,13]. ZnO film deposition on m-PS was achieved through magnetron sputtering (ATC Orion 8 Cluster Flange, Aja International, Hingham, MA, USA.) using two radio frequency (RF) powers of 60 W (A) and 80 W (B), respectively. It is important to note that in each deposition of ZnO, the temperature of the substrates was kept at 500 °C (A5/m-PS, B5/m-PS) and 800 °C (A8/m-PS, B8/m-PS) for 1 h. The deposition was achieved using a 2-inch ZnO target with 99.99% purity, the base pressure of the system was 2 × 10−6 Torr, and the Ar flow was 30 sccm, to obtain a working pressure of 5 × 10−3 Torr. The ZnO films were deposited on c-Si to obtain the reference samples: A5/c-Si, A8/c-Si, B5/c-Si, and B8/c-Si. Table 1 shows the summary of the prepared samples. The surface morphology of the fabricated structures was characterized using a scanning electron microscope (SEM, JEOL JSM-7800F, Tokyo, Japan). The ZnO crystal structures were studied using an X-ray diffractometer (XRD, ORION, D2 PHASER Bruker, Baden-Wurtemberg, Karlsrueh, Germany) using the CuKα radiation and λ = 0.15406 nm. An X-ray photoelectron spectroscope (XPS, Thermo K-Alpha, Waltham, MA, USA) equipped with an Al Kα monochromatic X-ray source (hv = 1486.6 eV) in an analysis chamber at a base pressure of 10−7 mbar was used to investigate the chemical state of the elements in the prepared ZnO. Photoluminescence studies were carried out using a Varian fluorescence spectrometer (Cary Eclipse, Varian Inc., Palo Alto, CA, USA) under 325 nm excitation.

3. Results

3.1. Scanning Electronic Microscopy (SEM)

SEM micrographs were obtained to study the effects of RF power and temperature during the deposition of ZnO on the substrates. Figure 1 shows the top-view and cross-sectional SEM images of m-PS substrates with interconnected pores. These pores had a diameter between 100 and 200 nm and a thickness around 200 nm.
Figure 2 shows SEM micrographs of ZnO deposited on c-Si and m-PS after the RF sputtering process. We can observe that ZnO film fully covers the m-PS substrate (Figure 2b,d,f,h). One may also note that the ZnO samples growth at 500 °C (Figure 2a–d) was characterized by continuous and dense ZnO agglomerates. These agglomerates were distributed uniformly on the substrates, indicating that the ZnO deposit does not have a well-defined structure. On the other hand, the SEM images of samples deposited at 800 °C (Figure 2e–h) revealed the formation of better-defined nanostructures. This could be because, with the increase in deposition temperature, coalescence is enhanced and atomic mobility increases, causing the formation of better-defined structures [29,30].
Figure 2e,g indicate the formation of ZnO nanorods on the c-Si substrates. The samples with ZnO deposited on m-PS (Figure 2f,h) revealed the formation of ZnO nanostructures constituted by the assembly of nanorods. Likewise, it can be observed that such nanostructures were grown over smaller nanoparticles with diameter sizes around 29 and 35 nm for the samples A8/m-PS and B8/m-PS, respectively (inside Figure 2f,h). Unlike ZnO grown on c-Si substrates, ZnO growth on m-PS acquires enough activation energy to occupy the correct nuclei-sites along the porous surface; thus, grains with lower surface energy tend to grow [31]. Additionally, with increasing RF power, Zn and O atoms do not have enough time to diffuse to their optimal sites in the porous substrates, causing the formation of tilted grains (Figure 2f,h) [29,30,32]. With the rise in RF power deposition from 60 to 80 W, the growth rate rises, which results in an increase in the amount of ZnO nanostructures on the substrates (Figure 2g,h). The tiny particles below the ZnO nanostructures could be on the substrate surface due to the confinement effect of the nanostructured matrix of the m-PS substrate [33].

3.2. X-ray Diffraction (XRD)

The crystal structure of our samples was investigated through X-ray diffraction spectroscopy (XRD). The diffractograms obtained from the ZnO/c-Si and ZnO/m-PS samples as a function of RF sputtering deposition power (60 and 80 W) and temperature (500 and 800 °C) are shown in Figure 3. The characteristic peak corresponds to the reflection (002) plane in ZnO/c-Si, indicating a single crystalline wurtzite phase with a preferential orientation towards the c-axis. The c-axis indicates that the ZnO growth is perpendicular to the substrate surface (Figure 3a).
On the other hand, various diffraction peaks were observed in the ZnO deposited on m-PS (Figure 3b) around 31.87°, 34.51°, and 36.35°, corresponding to the (100), (002), and (101) planes, respectively. The above indicates that the samples with ZnO deposited on m-PS are polycrystalline and have a hexagonal wurtzite structure (JCPDS No. 36-1451). The ZnO (002) orientation has been attributed to the lowest surface free energy provided by the m-PS substrates, which induces ZnO growth perpendicular to the surface [34]. At the same, all diffractograms show a peak in the plane (200), indicating the presence of silicon in the substrates [35].
The XRD measurements allowed us to evaluate the crystalline size (D), density dislocation (δ), biaxial stress ( σ ), and d-spacing (d). The D of ZnO/m-PS samples was calculated using the Debye Scherrer formula, while δ, σ, and d were calculated using the following formulas [31,36]:
δ = 1 D 2
σ = − 453.6 × 10 9 c − c 0 c 0
d = λ 2 sin θ
where c is the lattice parameter of the strained ZnO calculated from X-ray diffraction data, and c0 is the strain-free lattice parameter (c0 = 0.5206 nm) (JCPDS 36-1451). All the diffraction peaks, crystallite size, and respective d-spacing values are tabulated in Table 2. From Table 2, we can observe good agreement with the standard values. It can also show a % d error, and it has been observed that the difference between experimental and standard values is within the acceptable range. Table 3 shows the full width half maximum (FWHM), D, δ, and σ obtained for the (002) orientation in the samples.
According to Table 3 (from 500 to 800 °C), the broadening of FWHM decreased due to the temperature increase. This could be attributed to the fact that with the rise of temperature, atom diffusion (Zn and O) in the crystal’s arrangement increases, causing enhanced crystallinity. Haiyan Wang et al. demonstrated via XPS and photoluminescence analysis that the increase in annealing temperature (from 600 to 900 °C) provides a great force for O atoms to diffuse into ZnO thin films. This reduces the number of oxygen vacancies/defects and defects of Zn [37]. The enhancement in crystallinity can be corroborated with the diminution in δ values. The dislocation density represents the irregularities and the number of crystalline defects in the crystal as oxygen and zinc interstitials [38,39]. It is also observed that with the increased RF power deposition, the atoms receive more energy and have more driving force. This leads to an increase in intrinsic stress, as evidenced by the increase in residual stress on the ZnO lattice. Such intrinsic stress is due to the accumulating effect of the crystallographic flaws during deposition (increase of δ values) [38,40]. From Table 3, it can also be observed that residual stress decreases for samples A5/c-Si and B8/c-Si. This may be due to the mechanical instability of ZnO nanorods. M. Riaz et al. reported the relationship between the pore diameter of nanorods and residual stress [41]. They found that with the increase in pore diameter, the residual stress tends to increase. The above is reflected in the shift of the angle towards higher angles.

3.3. X-ray Photoelectron Spectroscopy (XPS)

The oxidation state of ZnO on c-Si and m-PS via RF sputtered at different temperatures and deposition powers was investigated using XPS (Figure 4). Figure 4a,b show the characteristics peaks assigned to zinc (Zn), oxygen (O), and carbon (C). Figure 4c,d show high-resolution spectra of the Zn 2p region for the samples. It can be observed that the Zn2p3/2 core levels are located at around 1022.00 and 1022.05 eV for ZnO deposited on c-Si and m-PS, respectively, while the Zn2p1/2 core levels are located at around 1045.13 and 1045.05 eV for ZnO deposited on c-Si and m-PS, respectively. The core level from Zn2p3/2 has been assigned to the Zn2+ ions in the ZnO thin films [42]. It can be seen that the position of the peaks differs slightly; this is probably because of the different surface morphologies of the deposited ZnO [43].
The high-resolution spectra and deconvolution of the O1s peak were obtained to further study the binding state of Zn and O. The deconvolution of the XPS peaks was performed using Fityk software (1.3.1 version). Figure 5 shows the O1s scan spectra of ZnO deposited on c-Si and m-PS at different temperatures and power depositions. Three peaks were observed around 527.62 eV (1), 530.54 eV (2), and 533.34 eV (3). The peak (1) is characteristic of the metal oxides [44]. The peak (2), at a low binding energy, is associated with O2- ions in the deficient regions within the ZnO array [45]. It can also be associated with hydrated oxides that could have been incorporated from the deposition chamber or the presence of weakly bound oxygen on the surface of the films [45]. Weijia Yang et al. attributed binding energy of around 530.75 eV to oxygen defects/vacancies. The central level of peak (2) shows asymmetry, indicating the presence of various forms of oxygen bonds in the near-surface region of ZnO [46]. The intensity is associated with the number of oxygen vacancies [42,47]. The peak (3) is associated with hydroxyl groups (–OH), O2, or C–O bonds of chemisorbed or adsorbed species on the sample surface [43,47,48]. Previously, it has been reported that intrinsic defects, such as zinc interstitial atoms (Zni) and oxygen vacancies (VO), are electrically active and can induce localized states near the conduction band. These species can act as donors [48].

3.4. Photoluminescence (PL)

Photoluminescence (PL) is a very sensitive characterization technique that helps to identify the crystallinity and defects present in ZnO. The spectra and bandgap transition schematic of the ZnO/m-PS samples are shown in Figure 6. ZnO PL emission spectra are composed of the near-band-edge (NBE) in the UV region, which is considered a characteristic emission of ZnO [49], and the deep-level-emission region (DL) in the visible region, which is universally associated with native defects in ZnO. The emission peak at ~360 nm is primarily related to the free exciton transition in the NBE. In contrast, the multiple jumps from DL emission are attributed to the photogenerated hole recombination on the ZnO structural defects [50,51]. On the other hand, violet emission in the 388–440 nm range is mainly referred to by the Zn interstitials found in the space charge region near the surface [52,53,54]. Furthermore, blue-green emission placed at 520 nm is commonly associated with the oxygen vacancies (VZn) [53,55,56], and 545 nm emission is attributed to the oxygen vacancies (Vo) [50,54]. Yellow emission in 595 nm and orange in 643–648 nm are related to oxygen anti-sites [54,57]. Finally, red emission at 720–724 nm is due to (Vo) [58,59].
As is shown in the previous figure, there is no shift in the peak position during RF power and temperature variation. However, a significant change in peak emission intensity is observed. The peak intensity is reduced as the deposition temperature increases. This phenomenon may indicate that there is a Zn and O defect decrease on the m-PS substrate, as can be noted in Table 3. In a similar way, the peak emission is affected inversely by the RF power. An increment in the RF power causes a reduction in the peak emission intensity, which is attributed to the crystallinity reduction in the samples, as indicated in the XRD results [51,59].

4. Conclusions

ZnO was successfully deposited over c-Si and m-PS using the reactive RF magnetron sputtering method. The formation of ZnO nanorods on the c-Si and ZnO nanostructures constituted by nanorod assembly on m-PS was revealed. Increased RF energy deposition results in an increase in ZnO nanostructures on the substrates and a rise in residual stress. All the ZnO nanostructures show evident (002)-preferred orientation, corresponding to the wurtzite structure. On the other hand, the increase in deposition temperature caused an improvement in the arrangement of the crystals, which was attributed to the decrease in crystal defects. XPS and PL results confirm the presence of ZnO structural defects, which can conduce the fabrication of sensors and gas devices.

Author Contributions

Conceptualization, data curation, formal analysis, and investigation, L.M.-A. and F.M.-M.; methodology and project administration, L.M.-A.; resources, F.M.-M.; visualization and supervision, M.R.J.-V.; validation, writing—review and editing, M.R.J.-V. and H.G.-P. All authors have read and agreed to the published version of the manuscript.

Funding

This research received no external funding.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

Not applicable.

Acknowledgments

The authors are grateful to Vivechana Agarwal and Y. Kumar (CIICAp-UAEM) and CINVESTAV-IPN for help with PL and XPS measurements, respectively.

Conflicts of Interest

The authors declare no conflict of interest.

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Coatings 13 01839 g001
Figure 1. SEM image of top view (a) and cross-section (b) of bare m-PS substrates.
Figure 1. SEM image of top view (a) and cross-section (b) of bare m-PS substrates.
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Figure 2. SEM images of ZnO deposited on c-Si (left images) and m-PS (right images) at RF power of 60 W (a,b,e,f) and 80 W (c,d,g,h) for different temperature deposition: 500 °C (a–d) and 800 °C (e–h).
Figure 2. SEM images of ZnO deposited on c-Si (left images) and m-PS (right images) at RF power of 60 W (a,b,e,f) and 80 W (c,d,g,h) for different temperature deposition: 500 °C (a–d) and 800 °C (e–h).
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Figure 3. X-ray diffraction spectra for the ZnO deposited on c-Si (a) and m-PS (b) at different temperatures and power deposition via RF magnetron sputtering.
Figure 3. X-ray diffraction spectra for the ZnO deposited on c-Si (a) and m-PS (b) at different temperatures and power deposition via RF magnetron sputtering.
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Figure 4. XPS spectra (a,b) and high-resolution spectra of Zn 2p (c,d) for the ZnO deposited on c-Si (left spectra) and m-PS (right spectra) via RF magnetron sputtering technique at different temperatures and power deposition.
Figure 4. XPS spectra (a,b) and high-resolution spectra of Zn 2p (c,d) for the ZnO deposited on c-Si (left spectra) and m-PS (right spectra) via RF magnetron sputtering technique at different temperatures and power deposition.
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Figure 5. High-resolution and deconvolution of the O1s scan spectra of ZnO deposited on c-Si (a) and m-PS (b) at different temperatures and power deposition via RF magnetron sputtering.
Figure 5. High-resolution and deconvolution of the O1s scan spectra of ZnO deposited on c-Si (a) and m-PS (b) at different temperatures and power deposition via RF magnetron sputtering.
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Figure 6. Photoluminescence spectra of ZnO/c-Si (a) and ZnO/m-PS (b) samples. The lower subfigure shows the schematic bandgap diagram (c).
Figure 6. Photoluminescence spectra of ZnO/c-Si (a) and ZnO/m-PS (b) samples. The lower subfigure shows the schematic bandgap diagram (c).
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Table 1. Summary of samples fabricated.
Table 1. Summary of samples fabricated.
SampleSubstrateTemperature (°C)RF Power (W)
A5/c-Sisilicon50060
B5/c-Si80
A8/c-Si80060
B8/c-Si80
A5/m-PSmacroporous silicon50060
B5/m-PS80
A8/m-PS80060
B8/m-PS80
Table 2. The X-ray diffraction peaks, 2Ɵ, d-spacing, % d error, crystal size, and average crystal size of ZnO deposited on c-Si and m-PS.
Table 2. The X-ray diffraction peaks, 2Ɵ, d-spacing, % d error, crystal size, and average crystal size of ZnO deposited on c-Si and m-PS.
Sample(hkl)2Ɵ JCPDS2Ɵ Experimentald-Spacing JCPDSd-Spacing Experimental% d ErrorD (nm)Average D (nm)
A5/c-Si(002)34.493734.40442.603322.6050.0515.0115
B5/c-Si(002)34.493734.22692.603322.6180.5511.7212
A8/c-Si(002)34.493733.83572.603322.6471.6818.4218
B8/c-Si(002)34.493733.70262.603322.6572.0722.2422
A5/m-PS(002)34.493734.47002.603322.6000.1413.7617
(101)36.408436.39042.475922.4670.3619.32
B5/m-PS(002)34.493734.47832.603322.5990.1611.1915
(101)36.408436.25742.475922.4760.0117.89
A8/m-PS(100)31.838431.84592.814302.8080.2333.6533
(002)34.493734.35302.603322.6080.1936.15
(101)36.408436.27552.475922.4740.0629.21
B8/m-PS(100)31.838431.89322.814302.8040.3825.0424
(002)34.493734.53272.603322.5950.3123.63
(101)36.408436.37422.475922.4680.3222.55
Table 3. FWHM, crystallite size, dislocation density, and biaxial stress of ZnO deposited on c-Si and m-PS via RF magnetron sputtering.
Table 3. FWHM, crystallite size, dislocation density, and biaxial stress of ZnO deposited on c-Si and m-PS via RF magnetron sputtering.
Sample2Ɵ (°)FWHMD (nm)δ (1/nm2)σ (Gpa)
A5/c-Si34.40440.5544150.0044−1.2631
B5/c-Si34.22690.7094120.0073−0.9764
A8/c-Si33.83570.4508180.0029−1.5607
B8/c-Si33.70260.3732220.002−1.8944
A5/m-PS34.41510.5572150.0045−1.2561
B5/m-PS34.32640.96390.0134−0.7075
A8/m-PS34.49460.2054410.0006−3.486
B8/m-PS34.53170.3015280.0013−2.3607
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MDPI and ACS Style

Morales-Morales, F.; Martínez-Ayala, L.; Jiménez-Vivanco, M.R.; Gómez-Pozos, H. ZnO Deposition on Silicon and Porous Silicon Substrate via Radio Frequency Magnetron Sputtering. Coatings 2023, 13, 1839. https://doi.org/10.3390/coatings13111839

AMA Style

Morales-Morales F, Martínez-Ayala L, Jiménez-Vivanco MR, Gómez-Pozos H. ZnO Deposition on Silicon and Porous Silicon Substrate via Radio Frequency Magnetron Sputtering. Coatings. 2023; 13(11):1839. https://doi.org/10.3390/coatings13111839

Chicago/Turabian Style

Morales-Morales, Francisco, Lizeth Martínez-Ayala, María R. Jiménez-Vivanco, and Heberto Gómez-Pozos. 2023. "ZnO Deposition on Silicon and Porous Silicon Substrate via Radio Frequency Magnetron Sputtering" Coatings 13, no. 11: 1839. https://doi.org/10.3390/coatings13111839

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