Dielectric Nanoceramics for S-Band Applications: Zinc Aluminate Enhanced with Titanium and Magnesium

doi:10.21203/rs.3.rs-4911338/v1

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Dielectric Nanoceramics for S-Band Applications: Zinc Aluminate Enhanced with Titanium and Magnesium

https://doi.org/10.21203/rs.3.rs-4911338/v1

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A straightforward sol-gel technique was used to prepare a nanoceramic composite material consisting of 89Wt%(ZnAl₂O₄TiO₂) and 11Wt%MgTiO₃ (ZTMg), designed to enhance dielectric properties for miniature patch antennas in wireless applications. X-ray diffraction (XRD) analysis revealed anatase-rutile phases in TiO₂, a wurtzite hexagonal shape in ZnAl₂O₄ (Gahnite), and MgTi₂O₅ phases. Raman spectroscopy identified distinct vibration modes corresponding to ZnO at 346 cm⁻¹ and TiO₂ at 717 cm⁻¹. The morphological structure of ZTMg was examined using field emission scanning electron microscopy (FESEM), showing the formation of agglomerated spherical nanoparticles. Energy-dispersive X-ray spectroscopy (EDS) displayed elemental peaks of Zn, Ti, Al, O, and Mg. The calculated mean grain size was 19.26 nm. The conductivity of the ZTMg nanoceramic composite material increased with frequency at various temperatures. As the operating frequency rose, the nanoceramic composite dielectric material exhibited commendable dielectric properties ranging from 13.46 to 19.39, with a reduced dielectric loss (0.25–0.64) in the temperature range of 30–150°C, making it suitable for microwave applications. The fabricated prototype antenna showed excellent performance in both measured and simulated results, with return loss (RL) values of -20.51/-12.53 dB, bandwidth (BW) of 1.36/2.02 GHz, and resonant frequency (fr) of 3.25/3.30 GHz.

Gahnite

Nanoceramics

Sol-gel method

Dielectric Loss

Return loss

Wireless communications technology has become an indispensable part of our daily lives, often being compared to wired communications in terms of information speed and service quality. As technology evolves, incorporating new features and functions, there is an increasing demand for smaller, high-quality, cost-effective, and durable antennas for microwave communications. This drives the need for developing dielectric nanoceramic composite materials with high-quality factors, low dielectric loss, and appropriate dielectric permittivity [1]. Composite materials are crucial in enhancing the dielectric properties of antenna materials. The rise of ceramic-based patch antennas is due to their simple structure and effective performance in microwave technology. These antennas, known for their miniaturization and enhanced performance, outperform conventional antennas in terms of power. Nanoceramic materials exhibit exceptional properties, including low sintering temperature, high quality factor, and high radiation efficiency.

Lei et al. analyzed the synthesis of ZnAl₂O₄-2HO-TiO₂ (H = Co, Mg, and Mn) nanoceramics, discussing their various properties. X-ray diffraction (XRD) revealed a single-phase solid solution in these ceramic materials, with a secondary phase showing the presence of MgTiO₃ and MgTi₂O₅. The microstructure, phase composition, dielectric permittivity (ranging from 9.1 to 14.1), and quality factor were found to be suitable for patch antenna fabrication via solid-state reaction [2]. Similarly, Jalal et al. synthesized a ZnTiAl₂O₄ nanoceramic composite material using sol-gel technology and explored its properties for patch antenna fabrication. XRD analysis revealed anatase and rutile phases of TiO₂, along with a three-phase system including ZnAl₂O₄. They observed increases in crystal size, grain size, ceramic density, and dielectric permittivity (13.51) with the addition of improved TiO₂. They concluded that the fabricated patch antenna exhibited a return loss of -28.71 dB and a bandwidth of 270 MHz at an operating frequency of 1.575 GHz, making it suitable for GPS applications [3]. Wang et al. investigated the dielectric characteristics of a ZnAl₂O₄-Mg2TiO₄-SrTiO₃ nanoceramic composite material designed for GPS patch antennas. They presented the mechanical and thermal properties of the nanoceramic composite, including its thermal expansion coefficient and compressive strength. The study focused on the patch antenna's operating frequency at 1.57 GHz, with an impedance bandwidth of 3% and a quality factor of 55,000 GHz [4].

Liang Huang et al. explored the microstructure and microwave dielectric properties of a ZnAl₂O₄-TiO₂ nanoceramic composite for GPS patch antenna applications, utilizing the mixed oxide route method. Their study revealed a strong correlation between the dielectric properties of the ZnAl₂O₄-TiO₂ composite material and factors such as sintering temperature, density, and mole ratio. The dielectric constant was measured at 25.2 and was linked to the quality factor, while the resonant frequency increased with the incorporation of TiO₂ as a dopant [5]. Wang et al. investigated the dielectric properties of Mg2SiO₄-Li2TiO₃-LiF ceramics with CaTiO₃ addition, synthesized via the conventional solid-state method. The addition of CaTiO₃ significantly increased relative density, leading to a substantial improvement in Q×f. As the sintering temperature rose, both the dielectric permittivity and quality factor initially increased and then declined. The ceramic material exhibited a dielectric permittivity (εr) of 14.13, a Q×f of 54,581 GHz (at 8.06 GHz), and a return loss of -17.5 dB at 1.575 GHz. The researchers concluded that the fabricated patch antenna was particularly well-suited for GPS and co-fired ceramic applications at moderate temperatures [6].

Liu et al. demonstrated the fabrication of calcium/strontium nanoceramic composite materials based on Ga₂O₄. They found that increasing the sintering temperature improved both morphology and microstructure density. At a sintering temperature of 1275°C, SrGa₂O₄ exhibited a dielectric permittivity of 9.2 and a quality factor of 66,000 GHz. In contrast, CaGa₂O₄ at the same temperature showed a dielectric permittivity (ε_r) of 10.6 and a Q-factor of 15,400. The SrGa₂O₄ ceramic patch antenna achieved a return loss of -19.94 dB and an efficiency of -1.38 dB. The researchers highlighted the potential of SrGa₂O₄ ceramics for 5G technology applications, particularly in mid and low-frequency bands [7]. Chinnaguruswamy et al. employed the sputtering technique to fabricate a multi-band microstrip patch antenna tailored to function with minimal power requirements from transmitters and receivers. They underscored that the thickness of the fabricated patch antenna was substantially reduced, being 50 times thinner compared to conventional counterparts. Operating at 2.4 GHz, the antenna exhibited a return loss of -20 dB and a gain of 10 dB. The researchers affirmed that the fabricated antenna was excellently suited for X and C band communications [8].

The ZTMg sample underwent characterization using various techniques. X-ray diffraction analysis was conducted using an X-ray diffractometer (XRD, X-Pert Pro, UK), while Raman spectroscopy was performed using equipment from BWTEK (Japan). The morphological structure was examined via field emission scanning electron microscopy (FESEM, SUPRA 55 VP- 4132 CARL ZEISS), and elemental analysis was carried out using Energy Dispersive X-ray Spectroscopy (EDS). Additionally, the composite nanoparticles were tested for dielectric properties using an LCR meter (PSM1735 N4L, Newtons4th Ltd, UK), and the antenna performance was assessed using a VNA analyzer.

Chemicals

Titanium tetra isopropoxide (TTIP, Sigma Aldrich), Magnesium acetate (Mg(CH₃COO)₂), Zinc acetate (CH₃COO)₂Zn2H₂O (AR) (Lobychem), aluminum nitrate nonahydrate (Al(NO₃)₃.9H₂O, Molychem), ethanol (C₂H₅OH, Sigma Aldrich) were used without any purification.

Initially, 2.14 grams of magnesium acetate were dissolved in 10 ml of ethanol and heated for 1 hour at 50°C. Following this, 3 ml of TTIP solution was mixed with the above solution and stirred at room temperature for 50 minutes. Subsequently, the gel was dried in a hot oven at 180 degrees Celsius for 30 minutes. An additional 2.81 gm of Al₂(NO₃)₃.9H₂O was dissolved in 10 ml of ethanol, and then 1.64 gm of zinc acetate was added, heating the mixture to 60°C for 20 minutes. Later, 0.2 ml of TTIP solution was added to the solution. Finally, this resulting solution was dried in a hot oven at 180 degrees Celsius for 1 hour. After obtaining a transparent solution, the samples were aged for 19 hours before being dried in a hot air oven at 800 degrees Celsius for 2 hours. Lastly, following calcination at 800°C/1hr, the samples were individually ground, and 11% and 89% of the two samples were added and ground for some time to obtain fine powder. The corresponded Sol-gel process is as shown in the Fig. 1.

Figure 2 depicts the observation of crystalline phases using the X-ray diffraction (XRD) technique. XRD is utilized to discern the crystal structure phases of the ZnAl₂O₄-MgTiO₃ nanoceramic composite material prepared via the sol-gel method for microwave applications. The obtained sample confirms the presence of crystalline phases, notably the rutile phase of TiO₂ and the wurtzite hexagonal phase of ZnAl₂O₄, alongside MgTi₂O₅ phases. The sintered ZTMg nanoceramics comprise wurtzite hexagonal zinc aluminate, magnesium dititanate, and rutile and anatase phases of TiO₂, which are indexed in JCPDS file numbers 05-0669, 98-003-7232, 21-1276, and 22-1272, respectively [9, 10]. The prepared ZTMg nanoceramic compound exhibits excellent microwave dielectric properties through the sol-gel process (Fig. 1), specifically tailored for microwave applications.

Figure 3 presents the Raman spectra of the ZTMg nanoceramic composite material. The main vibration modes were identified at 346 and 717 cm⁻¹, with additional bands observed at 284, 390, and 484 cm⁻¹, corresponding to the A_1g and B_1g modes of TiO₂. Similarly, distinctive vibrations of ZnO were detected at 346 cm⁻¹ (2nd order Raman scattering, E2-E1 vibration modes) and 390 cm⁻¹ (assigned to Eg mode). Additional bands, particularly at 346 and 717 cm⁻¹, suggested the interaction between ZnO and TiO₂ in the case of hybrid ZnO/TiO₂ particles, indicating the presence of ZnTiO₃. The thermodynamically stable rutile phase exhibited a minor peak at 846 cm⁻¹ in the prepared ZTMg ceramic nanoparticle [11, 12, 13, 14].

The morphological structure was examined using field emission scanning electron microscopy (FESEM). Figure 4 displays FESEM images of the composite nanoceramic material, along with energy dispersive X-ray spectroscopy (EDS) measurements. In Fig. 4 (a, b), the spherical nanoparticles of the prepared nanoceramic composite sample (ZTMg) are visible, exhibiting agglomeration. The calculated mean diameter of the grain size is 19.26 nm. EDS measurements were employed to analyze the compositional elements, revealing distinct peaks corresponding to Zn, Al, Ti, and Mg at energy levels of 1, 1.5, 0.5, and 1.25 eV, respectively, as depicted in Fig. 4 (c). The corresponding histogram image of the ZTMg nanoparticles is presented in Fig. 4 (d). Following these characterizations, the dielectric characteristics of the produced nanoceramic composite material were evaluated using an LCR meter.

Before testing, the nanoceramic composite material underwent a transformation into pellets using the hot press method, as depicted in Fig. 5. In the pellet-making process, the initially prepared ceramic nanoparticles (ZTMg) were mixed with ethyl cellulose to improve stickiness. The resulting paste was then poured into the pellet machine, and the top handle was rotated to compress the powder into pellet form. Ultimately, pellets with precise dimensions, measuring 1.12 mm in thickness and 10 mm in diameter, were produced.

Moreover, we examined the dielectric properties of ZTMg nanoparticles using an LCR meter. The dielectric permittivity was calculated using the formula ε_r = Cd/(ε₀A), where C represents capacitance, and d and A denote the distance and area of the cross-sections of the prepared pellet. Figure 6 (a) illustrates the relationship between dielectric permittivity and frequency across various temperatures, ranging from 30 to 150 degrees Celsius. The dielectric permittivity showed variations in the range of 13.46 to 19.39. The graph depicts an initial increase in dielectric permittivity from 100 Hz to 60 KHz, followed by a consistent trend as the frequency increases from 100 KHz to 10 MHz, across the different temperatures. These fluctuations in dielectric permittivity are attributed to the dipole movements of charge carriers. At higher frequencies, the permittivity of the material stabilizes and eventually decreases to lower levels due to dipole oscillations that impede dipole orientation in response to the applied field [15].

At elevated frequencies, ferroelectrics typically exhibit a reduction in dielectric permittivity. At high temperatures (150°C), the measured dielectric permittivity was 18.9. However, for each composition at lower temperatures, the dielectric permittivity value remained steady as the frequency increased, suggesting the absence of charge accumulation at the interface.

As depicted in the graph, the dielectric loss decreases with increasing frequency from 30°C to 150°C. This loss is attributed to a delay in polarization response to an alternating field, as well as impurities, imperfections, and electron hopping from Ti^+ 2 to Zn^+ 2. Maintaining a low loss tangent is critical for effective antennas as it enhances overall radiation efficiency [16]. The observed dielectric loss ranged between 0.25–0.64. According to the graph, the dielectric loss decreased from 1 KHz onwards, with a more significant reduction observed at each subsequent frequency step. This pattern repeated at higher frequencies and temperatures, as depicted in Fig. 6 (b).

Similarly, in Fig. 7, the conductivity graph depicts the relationship between dielectric conductivity (σ_AC) and frequency across various temperatures (30–150°C). The conductivity demonstrates a gradual rise from 100 Hz to 10 MHz, and beyond 10 KHz, all curves exhibit a slow but steady increase, reaching their peak levels. The conductivity can be explained using the expression σ = ωε_oεtanδ. This pattern is attributed to thermally induced charge carrier hopping between different localized states. Furthermore, the maximum value of AC conductivity increases with frequency due to enhanced electron migration [16].

Figure 8 (a) presents the real section of the impedance for the developed nanoceramic composite material. The Z value decreases as frequency and temperature increase, indicating a direct correlation with the material's electrical conductivity. At different temperatures, the multiple curves display varying impedance values that eventually converge to sustain a constant value, possibly diminishing towards zero.

Concurrently, the imaginary component of the impedance (Fig. 8 (b)) holds significance in the fabrication of microstrip patch antennas employing microwave dielectric materials. It also fluctuates with frequency across various temperatures. The impedance values steadily diminish in a positive trajectory and stabilize as the curves converge, ultimately approaching zero [17].

Upon transforming the dielectric properties of the prepared composite material from powder to paste form for antenna fabrication, commence by blending 0.9 grams of ZTMg powder with 1 milliliter of CH₃COOH for 20 minutes. Subsequently, introduce 0.20 milliliters of PEG and grind the mixture for 30 minutes. Transfer the resulting solution and excess acetic acid into a glass bottle and subject it to heating in a hot air oven at temperatures exceeding 120°C until it reaches a viscous paste consistency. Utilize a doctor blade to apply this thick paste onto the fluorine-doped tin oxide (FTO) plate. Once the FTO substrate is coated with ZTMg, employ magnetron sputtering to deposit a silver layer onto the patch antenna for electrical connectivity. Additionally, apply silver to the bottom of the FTO substrate. Finally, to assemble the 3.16 mm × 2.03 mm microstrip patch antenna, affix it to an SMA coaxial connector and conduct testing using a vector network analyzer. The entire process is depicted in Fig. 9.

Following the fabrication of the antenna, its performance underwent assessment utilizing a Vector Network Analyzer (VNA). The VNA furnished comprehensive measurements of the antenna's parameters, encompassing return loss, bandwidth, and impedance matching. These outcomes were meticulously documented and scrutinized. To ensure the precision of the physical measurements, the antenna's performance underwent verification through simulations employing the High-Frequency Structure Simulator (HFSS). The HFSS simulations established a comparative reference point to evaluate real-world performance, facilitating a comprehensive validation of the fabricated antenna's attributes against the designated specifications. The corresponding flow diagram is depicted in Fig. 10.

The fabricated prototype microstrip patch antenna showcases outstanding performance concerning return loss and voltage standing wave ratio (VSWR < 2) in both simulated and measured evaluations. Illustrated in Fig. 11 are the return loss (RL) characteristics of the synthesized 89Wt%(ZnAl₂O₄TiO₂)11Wt%MgTiO₃ (ZTMg) ceramic nanoparticles within the fabricated antenna, spanning operating frequencies from 1 to 10 GHz. Specifically, at the designated operating frequency of 3.25 GHz, accompanied by a bandwidth spanning 1.36 GHz, the return loss measured at -20.51 dB [18–20]. In comparison, Mazumdar et al. reported a fabricated antenna resonating at 3.68 GHz with a return loss of -16.15 dB and a bandwidth of 15.58 MHz [21]. Our investigation underscores that the microstrip patch antenna, leveraging ZTMg composite nanoparticles, demonstrates the lowest return loss, rendering it highly compatible with S-band communication applications. Furthermore, the inset of Fig. 10 showcases a digital image of the microstrip patch antenna, featuring dimensions of 3.16×2.03 mm², thereby providing additional insights into the physical dimensions and structure of the fabricated antenna.

Ultimately, the crafted ceramic dielectric nanoparticles emerged as exceptionally adept for microwave applications. Leveraging these nanoparticles, the fabricated antenna exhibited outstanding performance attributes, positioning it as an optimal choice for S-band applications. The harmonious integration of the nanoparticles' dielectric properties and the antenna's design culminated in an efficient and dependable device, proficient in meeting the rigorous demands of S-band communication systems. This symbiotic relationship not only ensures enhanced performance but also offers several advantages. For instance, the utilization of ceramic dielectric nanoparticles contributes to the antenna's compactness, lightweight nature, and durability, making it ideal for deployment in various S-band communication scenarios. Additionally, the inherent stability and reliability of ceramic materials enhance the antenna's longevity and operational consistency, ensuring uninterrupted communication even in challenging environments. Thus, the adoption of these advanced materials and design strategies underscores the antenna's prowess in delivering optimal performance and fulfilling the diverse requirements of modern S-band communication networks.

In conclusion, we have successfully synthesized and characterized an 89wt%(0.7ZnAl₂O₄-0.3TiO₂)-11wt%MgTiO₃ (ZTMg) nanoceramic composite material suitable for fabricating patch antennas in microwave applications using the sol-gel method. Through X-ray diffraction (XRD) analysis, we confirmed the presence of ZnAl₂O₄, rutile-TiO₂, and MgTiO₃ phases, while Raman spectroscopy validated various vibration modes associated with ZnO, ZnTiO₃, and MgTi₂O₅ phases. Field emission scanning electron microscopy (FESEM) revealed the fabrication of spherical-shaped nanoceramic particles with an average size of 19.26 nm. Our investigations demonstrated the suitability of the prepared nanoceramic composite material for microwave applications, characterized by a high dielectric permittivity of 13.46, low tangent loss of 0.25, robust conductivity across varied temperatures (30–150°C), and appropriate impedance properties. Moreover, the fabricated antenna exhibited commendable performance metrics, including a return loss of -20.51 dB, bandwidth of 1.26 GHz, and VSWR (< 2) at an operating frequency of 3.25 GHz. Notably, the antenna's performance was validated through both simulated (RL=-20.51 dB, B. W = 1.36 GHz, and VSWR = 1.97 at f_r=3.30 GHz) and measured (RL=-12.53 dB, B. W = 2.02 GHz, and VSWR = 1.02 at fr = 3.25 GHz) assessments, highlighting its successful implementation.

Acknowledgements

Dr. Srilali Siragam highly acknowledges the provided access of the research facilities by Department of Nanotechnology, Swarnandhra College of Engineering & Technology.

Author Contribution

Conceptualization, Srilali; methodology, Srilali.; validation, Srilali.; formal analysis, Srilali; investigation, Srilali; resources, Srilali; data curation, Srilali; writing─original draft preparation, Srilali; writing─review and editing, Srilali; visualization, Srilali,; supervision, Srilali.

Conflicts of interest or competing interests

The author declares no competing interest.

Data availability

Due to technical or time constraints, the raw/processed data required to recreate these findings cannot be given at this time. However, it may be shared in the future if requested.

Supplementary information

Not Applicable

Ethical approval

Not Applicable

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Competing interest reported. The author declares no competing interest.

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Dielectric Nanoceramics for S-Band Applications: Zinc Aluminate Enhanced with Titanium and Magnesium

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