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Scientific Reports volume 14, Article number: 16813 (2024 ) Cite this article modern home decor
The demand for modern electronics and semiconductors has increased throughout the years, which has enabled the innovation and exploration of solution-processed deposition. Solution-based processes have gained a lot of interest due to the low-cost fabrication and the large fabrication areas without the need for high-vacuum equipment. In this study, we utilized the ZnO ink for inkjet printer ink to fabricate a thin film via Electrohydrodynamic printing. Three different ink solutions were prepared for experimentation. The EHD printing technique demonstrated the ink’s compatibility with and without the modifications. The outcomes of the EHD printed materials were comparable with the spin-coated thin films. The EHD-printed films demonstrated better results in comparison to spin-coated films. Ra and Rq of the EHD film measured at 3.651 nm and 4.973 nm, respectively. It improved the absorbance up to two-fold at 360 nm wavelength and electrical conductivity up to 40% compared to the spin-coated films. Furthermore, the optimization of the printing parameters can lead to the improved morphology and thickness of the EHD thin films.
The fabrication of modern electronic devices can be complex and challenging, involving intricate technologies and processes. Advancements in technology necessitate the development of high-throughput, efficient, and scalable process techniques, along with flexibility, to align with consumer demands1. Conventional manufacturing methods for silicon-based technologies are based on photolithography and chemical processes to fabricate electronic circuits with pure semiconducting materials into wafers. These established methods have a limited range of materials, lack of flexibility, and high-cost processes. In this regard, printing technologies can be an alternative process due to the ease of fabrication, wide range of printable materials, compatibility with flexible substrates, low cost and wastage, and excellent control of material properties2,3. Multiple printing processes adopted by researchers and companies, such as screen-printing4, inkjet printing5,6, and gravure printing7, etc. printing technologies demonstrate a high speed, high resolution, high throughput, and compatibility with roll-to-roll processes7. Factors that are unfavorable about these technologies are they require a controlled environment and are limited in resolution. Therefore, electrohydrodynamic printing has emerged to counter the problems faced by other printing technologies8,9.
Electrohydrodynamic (EHD) printing is a cutting-edge printing technique that uses electrohydrodynamic principles to precisely deposit materials at micro and nanoscale resolutions10,11. Unlike conventional inkjet printing, which deposits fluid in the form of large droplets onto a substrate, EHD printing employs an electric field to precisely control the fluid dynamics of the ink material under ambient conditions. This results in the creation of highly defined patterns with remarkable accuracy12. This printing technique offers three primary printing modes: direct patterning for thin electrodes or structures13, electrohydrodynamic atomization (EHDA) for fabricating thin film14,15, and electrospinning for producing fiber8,16. These diverse printing capabilities enable the technology to excel in various domains such as electronics, flexible electronics, and biotechnology, where complex structures with diverse materials and substrates are required17.
A crucial aspect of printing technologies lies in the formulation of inks containing conductive and semiconductive materials, such as nanoparticles, which is fundamental for leveraging printing techniques in electronic device fabrication. Zinc Oxide (ZnO) stands out as a versatile material utilized in semiconductors and optoelectronic devices18,19,20. It boasts environmental friendliness, non-toxicity, and abundance, making it highly promising. With a wide band gap (3.37 eV), high exciton binding energy (60 meV), excellent optical properties, and affordability21,22,23,24,25. ZnO holds significant potential for modern optoelectronic applications. Understanding the structure and quality of deposited materials is crucial for practicality and performance in device design26,27,28.
This research involved the production of ZnO thin films through the EHD printing technique, utilizing inkjet printer ink. The study highlights the application of electrohydrodynamic atomization and its optimization for thin film fabrication. Following production, the thin films underwent thorough analysis to evaluate the thin film performance and quality, focusing on parameters such as topography and morphology, electrical characteristics and optical properties.
Zinc oxide ink for inkjet printing (Helios′Ink H-SZ01034 semiconductive ink) and Indium tin oxide (ITO) coated glass slides were purchased from Sigma-Aldrich, the ITO substrate has a dimension of 25 mm by 25 mm. ZnO ink has a surface tension, viscosity, and concentration of 29 ± 5 mN/m, 10.5 ± 3.0 mPa.s (20 °C), and 1.2% respectively (as confirmed by the manufacturer). To facilitate comparison and conduct a performance evaluation, three different inks were prepared (i) Pristine ZnO inkjet ink, (ii) ZnO ink dispersed in Ethylene glycol (EG), and (iii) ZnO ink in ethanol) for analysis of their sprayability and effectiveness. EG and ethanol were added into ZnO ink at a ratio of 1:1. The modified ZnO inks were mixed with the respective solvent and put onto an orbital shaker overnight. The inks were sonicated for 10 min to eliminate aggregation of the ink particles before being loaded into the printer syringe.
The ITO substrates were cleaned with ethanol, acetone, and Di-water in an ultrasonic bath sequentially for 10 min. Subsequently, the ITO substrates are further cleaned with ozone-UV cleaner for 10 min to enhance the wettability of the substrate.
The EHD printer used in this experiment was NanoNc ESDR300. The printer consists of 3 main parts, (i) a movable X–Y axis stage; (ii) an ink pump system, and (iii) a power supply unit. The movable stage is used to control the substrate movement speed and to position the substrate. The pump system is used to supply ink for deposition via a syringe and metallic nozzle (NanoNc, 30gauge; inner and outer diameters of 0.14 mm and 0.32 mm respectively) and a power supply unit (30 kV) is used to regulate the DC voltage applied to the nozzle.
To enable the EHD printing method, examining the jetting behavior of the respective inks for thin film development was essential. This involved evaluating the printability of the inks via EHDA. Before printing onto substrates, it was crucial to study the EHD jetting process to determine the optimal flow rate, offset distance, and applied voltage of the system. Throughout the experiment, the offset distance remained constant at 20 mm. The flow rate of the inks was systematically increased from 100 to 500 µl/h. Similarly, the applied voltage was gradually raised until the multi-jet region was reached. The combination of flow rate and applied voltage was documented to establish the operating envelope for the process.
To achieve successful fabrication of EHD-printed thin films, it's crucial to harness the cone-jet formation mechanism for depositing ZnO droplets onto the substrate29. The printing process onto the pre-cleaned ITO substrates was conducted in cone-jet mode, with a stage movement speed set at 50 mm/s for 30 passes and an ink flow rate of 100 µl/h to cover the 25 mm × 25 mm ITO substrate. Figure 1 illustrates the sequential steps of the ZnO EHD printing process. For comparison of thin film fabrication, the ZnO ink was spin-coated onto a pre-cleaned ITO substrate at 2000 rpm for 15 s. Subsequently, both the printed films and the spin-coated film were subjected to a hotplate at 150 °C for 15 min.
The sequential steps of ZnO thin film-EHD printing process.
The Scanning electron microscope (SEM) images were captured using Joel JSM-7610F Field Emission-SEM and Zeiss Supra 55 VP to assess the fabricated thin film substrate coverage and film thickness measurement. Atomic force microscopy (AFM) was used to measure the thin film roughness; roughness average (Ra), and root mean square roughness (Rq). Three different areas per sample with 500 nm scanning size were taken for AFM analysis.
The ultraviolet–visible (UV–Vis) spectroscopy outcomes were obtained utilizing the Shimadzu UV-1900 and Ossila optical spectrometer for analyzing the ZnO liquid inks and the resultant thin films, respectively. The sheet resistance, resistivity, conductivity, and current–voltage characteristics of the samples were determined by employing the Ossila four-point probe system.
EHD jet characterization was captured using a Photron high-speed camera with a high optical zoom lens. ImageJ software was used to study the captured images from SEM to analyze the particle size, cracks/fault lines, or hole formation on the deposited ZnO.
To optimize the deposition process and establish the operating parameters for ZnO inks, EHDA printing mode was utilized. This involved initiating the process at a defined flow rate and incrementally raising the applied voltage to observe jetting at the meniscus.
Figure 2a shows the different jetting of the ZnO inks. The jetting modes observed produced by the ZnO inks were dripping, micro-dripping, oscillating cone-jet, unstable-cone jet, stable cone-jet (Taylor cone), and multi-jet. Dripping mode is a state, where droplets deposited from the meniscus are larger than the nozzle size typically at a lower voltage. Whereas, micro-dripping occurs slightly at a higher voltage and the droplets produced are smaller compared to the nozzle size. An oscillating jet occurs when the cone jet starts to move and oscillate due to an unstable electrical field between the nozzle and substrate. The stable-cone jet occurs at the on-set voltage and flow rate region. Multijet occurs at higher voltage, creating a multiple stream of jet at the meniscus this is due to the higher pulling rate of the ink by the electric field and less supply of ink to accumulate at the meniscus.
Characteristics of ZnO jets via EHD and the operating envelope (a) jetting profiles; (b) Pristine ZnO ink; (c) ZnO:EG; (d) ZnO: ETH.
Figure 2b–d illustrates the performance characteristics of three ZnO inks (pristine ZnO ink, ZnO:EG, ZnO: ETH) used for the experiments. Dripping modes were found at 0 to ~ 3.7 kV, 0 to ~ 4.0 kV, and 0 to ~ 3.5 kV for ZnO inks, ZnO:EG, and ZnO:ETH, respectively. Micro-dripping occurred at ~ 2.5 to 4 kV, 4.0 to ~ 6.0 kV, and ~ 3.5 to 5.9 kV for the respective inks. The oscillating cone jet was exclusive to the ZnO ink at 3.8 to ~ 5.1 kV with a low flow rate of 100 µl/h. Unstable cone jet were observed at ~ 3.4 to 5.2 kV, ~ 6.1 to ~ 8.0 kV, and ~ 4.6 to 8.0 kV, respectively. The ideal EHD printing mode, characterized by a stable cone-jet, was observed at ~ 5.0 to 6.5 kV, ~ 7.0 to ~ 9.8 kV, and ~ 6.0 to 8.0 kV for the respective ZnO inks. MultiJet-jet was identified at higher voltages, starting from > 6.0 kV onwards. These findings offer valuable insights for optimizing ink behavior in EHD printing processes.
The three inks were sprayed onto a steel plate to test the wetting and coverage during the printing process. The testing was conducted with a flow rate of 100 µl/h, an offset distance of 20 mm, and a printing speed of 50 mm/s. Figure 3 illustrates the path and traces of EHDA ZnO inks at 10 repetitive vertical movements. The images show the pristine ZnO covered approximately 1.4 mm in width in a single pass and 0.8 mm in width was measured to have concentrated area after 10 repetitive movements. The modified ink was measured to have 1.2 mm overall coverage with 0.5 mm concentrated area for ZnO:ETH, and 2.4 overall coverage and 1.2 mm concentrated area for ZnO:EG. These results were used to determine the homogeneity of the EHDA thin film, as well as the path and number of zigzag patterns to optimize the usage of ink for the target ITO substrate.
The printing path and spraying traces of the ZnO inks.
After fine-tuning the printing settings, we successfully used an EHD stable-cone jet in EHDA mode to print materials onto the target substrate. Figure 4 a–c shows topography SEM images of three EHD-developed films, with a spin-coated ZnO (Fig. 4d) film for comparison. The SEM pictures of the developed ZnO films show a densely packed particle without any presence of major cracks. The EHD-developed films show larger grain-like structures compared to the spin-coated films. Further examining the images shows that the ZnO:EG (Fig. 4b) blend exhibits a clump of elongated particle material and the ZnO:ETH (Fig. 4c) shows multiple groups of larger islands. The difference in the formation of the particles can be due to the reaction during the post-annealing process. Figure 5 shows the grouping 100 k zoom to be used to estimate the particle group size. The estimated average particle size for EHD ZnO, ZnO:EG, and ZnO:ETH were found to be approximately 5544.65 nm2, 5685.84 nm2, and 11,874 nm2, respectively. In comparison, the SC ZnO group exhibited an average particle area of 5050.72 nm2.
SEM morphology of ZnO the film, (a) EHD prisoner ZnO; (b) EHD IN ZnO:EG; (c) EHD IS: and (d) spin-coated ZnO.
Grouping of the ZnO particles as deposited via EHDA (a) pristine ZnO; (b) ZnO:EG; (c) ZnO:ETH and (d) spin-coated ZnO.
Figure 6 illustrates the side view of the developed film EHDA ZnO, ZnO:EG. ZnO:ETH and ZnO SC. Notably, the pristine ZnO film exhibits a thicker layer with an average thickness of 1289.81 nm, in contrast to the spin-coated counterpart, which has an average thickness of 232.92 nm—a sixfold reduction in thickness. The EHD ZnO film's thickness can be optimized for a finer result comparable to spin coating by simply reducing the number of passes. Moreover, the use of modified ZnO ink in ethanol and EG results in significantly thinner films, averaging 131.64 nm and 124.26 nm, respectively. This improvement is attributed to the 1:1 ink and solution blend, these blends also enhanced the annealing process of the film. However, it is important to note that a potential drawback of this blend is a reduction in the number of ZnO particles in the solution. Using the EHD stable-cone jet in EHDA mode led to successful printing and revealed interesting differences in film structures. These findings help improve thin film development techniques.
Side profile SEM images (a–c) EHD printed and (d) spin-coated.
Figure 7 shows the AFM surface topography results of the printed ZnO films and spin-coated ZnO. Ra and Rq were used as quantitative measurements to characterize the roughness of the fabricated films. The EHD printed film i.e. pristine EHD ZnO, ZnO:EG and ZnO:ETH have the Ra measured on average of 4.649 nm, 3.651 nm, and 4.845 nm respectively, while the spin-coated Ra was measured on average of 3.653 nm. The Rq of the EHD printed films were measured on average at 5.741 nm, 4.973 nm, and 6.061 nm respectively, and the spin-coated counterpart Rq was measured at 4.576 nm. The increase in surface roughness measurement of Ra and Rq of the EHD film was due to the grouping of the particles that created a localized island, especially in the modified ink (ZnO:EH and ZnO:ETH) and the results also show that the thickness of the ZnO films contributes directly to the surface roughness.
AFM images of the EHD and spin-coated ZnO films (a) pristine ZnO; (b) ZnO:EG; (c) ZnO:ETH and (d) ZnO SC.
The comparison of the developed ZnO thin-film I–V characteristics measured in ambient conditions are as shown in Fig. 8. Subsequently,
I–V characteristic of the ZnO thin films.
Table 1 listed the measurement of ZnO developed film taken with the 4-point probe. By incorporating the known thickness measurement of the film, the resistivity, and conductivity of the film can be calculated by using Eqs. (1) and (2) respectively;
where ρ is resistivity, σ is the conductivity, tf is the film thickness, V is the voltage and I is the current applied with the 4-point probe.
From the results in Table 1, the sheet resistance measured for EHD printed samples is significantly lower compared to the reference sample (ZnO SC). The EHD deposition is capable of reducing the sheet resistance up to > 1.3%. The EHD-deposited samples demonstrate a higher conductivity and lower resistivity of the film compared to the spin-coated film except for the pristine ZnO ink. The ZnO:EG and ZnO:ETH have an increase in conductivity of approximately 47.2% and 50.8% respectively. The increase in conductivity can be due to the increase in free carrier concentration and the thinner film of ZnO:EG and ZnO:ETH. The lower conductivity found in the EHD-printed ZnO film was because of the charge carrier scattering. This effect is commonly found in thicker films where an increase in charge scattering delays the flow of charge carriers which leads to higher resistivity and lower conductivity30.
Figure 9 shows the absorption spectra across wavelengths from 300 to 850 nm for ZnO inks and the ZnO inks used in the experiments. Existing research confirms that ZnO nanoparticles absorb light in the UV–Vis range, specifically between 350 and 380 nm31. In the liquid ink form, the pristine ZnO ink has a slightly yellow. The pristine ZnO inks exhibit high absorption at the known spectra, the results indicate the ink is highly concentrated. The addition of the solvents reduced the concentration of the original solvents in the ZnO inks and altered the natural color of the ink. Adding ethylene glycol (ZnO:EG) changes the yellowish nature to a slightly yellow-to-clear color. The addition of the EG caused a significant drop in absorbance at 370 nm. Adding ethanol (ZnO:ETH) changes the natural yellow ZnO ink color to white and cloudy ink. This led to a significant decrease at 400 nm. The results also show that the additional solvents work as blue (~ 430 to 490 nm) and green (~ 490 to 560 nm) reducing agents. These observations provide insight into the influence of solvents on the optical properties of the ZnO nanoparticles, which is essential for thin-film fabrication.
The ZnO inks (a) UV–Vis optical absorption spectrum and (b) the ZnO-inks, pristine ZnO, ZnO:EG, and ZnO:ETH respectively.
The optical absorbance of EHD ZnO thin films and spin-coated film with wavelengths of 300 to 850 nm were studied to compare the two thin film deposition methods with the thickness of films of approximately ± 200 nm after printing optimization. Figure 10 shows the UV–Vis absorbance spectra of ZnO thin films on ITO substrate with the respective inks and deposition methods. The sharp peak at approximately 360 nm indicates the presence of ZnO nanoparticle spectra in the fabricated thin films using both methods and inks. The absorption edges of the EHD ZnO and ZnO:ETH, ZnO:EG, and ZnO SC show the transition from absorbance to transmittance from lower to higher wavelengths initiated around ~ 370 nm, this was due to the high transparency film developed using after post-annealing. The results of EHD printed ZnO with EG as precursor solvent show that the respective films have a stronger absorption and broader absorbance spectrum range in the visible region. The EG solvent in the ZnO ink helps to improve the dispersion of the deposited materials by preventing nanoparticle aggregation and enhancing the crystallinity of the ZnO post-annealing32. Additionally, ZnO films created via EHDA demonstrated higher absorbance levels compared to those produced through spin coating up to two-fold of the absorbance unit. This maybe contributed to better solvent removal during the atomization process in EHD, however more investigations in to this phenomenon remain a good future research topic.
UV–Vis optical absorption spectrum of ZnO thin film deposited with EHD and spin-coated.
The optical reflectance spectrum for ZnO thin film as shown in Fig. 11 confirmed the low optical reflection of EHD and spin-coated thin films. It was observed that the peak reflectivity of the developed films was approximately 6% at 400 nm wavelength. The reflectivity decreases with increasing wavelength from 450 to 800 nm. The slight increase in the reflectivity of the films was due to the deposition of materials using the EHD-printing method, which was in the form of tiny droplets that scattered light and affected the final appearance of the films.
Reflectance spectra for ZnO thin film.
ZnO thin films were successfully deposited on an ITO-coated glass substrate using the EHDA method. The structural, morphology, optical, and electrical properties of the EHD-developed films were characterized. Three modified ZnO inks were employed to assess compatibility with the EHD system. The EHD fabricated film demonstrated performance on par with spin-coated film. Morphology studies of the films showed the effect of particle formation and thickness for both pristine ZnO and modified inks. The electrical properties of the films were thickness-dependent, with the thicker EHD pristine ZnO films showing the lowest conductivity. However, ZnO:EG and ZnO:ETH improved the conductivity by more than 40% compared to the reference sample at half of the thickness of the reference sample. The optical properties shown in EHD-ZnO films exhibited a high absorbance rate, up to two-fold than the reference sample in the visible range. The EHD-printed films exhibit slightly higher reflectivity compared to the reference sample because the printed materials were deposited in tiny droplets. This result is very important for the application of optoelectronic devices. The outcome of this study suggests that controlling the deposition rate of materials can further enhance the properties of EHD-developed films. The favourable optical and electrical characteristics of the EHD fabricated films indicated the potential suitability of this process as an alternative fabrication method.
The datasets used and/or analysed during the current study available from the corresponding author on reasonable request.
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The work presented in the article is financially supported by Universiti Brunei Darussalam, Brunei Darussalam, through its University Research Grant scheme (grant number: UBD/RSCH/1.3/FICBF(b)/2022/019)
Faculty of Integrated Technologies, Universiti Brunei Darussalam, Bandar Seri Begawan, 1410, Brunei Darussalam
Zulfikre Esa, Malik Muhammad Nauman, Muhammad Abid, Asif IQBAL, Juliana HJ Zayi & Kamran Ali
Department of Mechanical Engineering, Baluchistan University of Information Technology, Engineering and Management Sciences, Quetta, 87300, Pakistan
Department of Mechanical Engineering, NED University of Engineering and Technology, Karachi, Pakistan
College of Computer and Information Sciences, Imam Mohammad Ibn Saud Islamic University, Riyadh, 11564, Saudi Arabia
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Conception: Z.E., M.M.N., K.A. Experimental design: M.U., M.U.K., A.I. E Experimentation and Characterizations: Z.E., M.M.N., K.A. Funding, Supervision and Project Management: K. A., M.A. Manuscript Preparation and Review: Z.E., S.M.M., M.U.,
Correspondence to Malik Muhammad Nauman or Kamran Ali.
The authors declare no competing interests.
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Esa, Z., Nauman, M.M., ullah, M. et al. Compatibility and performance study of electrohydrodynamic printing using zinc oxide inkjet ink. Sci Rep 14, 16813 (2024). https://doi.org/10.1038/s41598-024-67858-1
DOI: https://doi.org/10.1038/s41598-024-67858-1
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