The microwave properties of Li doped 0.7(Ba,Sr)TiO3-0.3MgO thick film interdigital capacitors on the alumina substrates

The crystalline and electrical properties of Li doped 0.7(Ba,Sr)TiO₃-0.3MgO thick film interdigital capacitors have been investigated. Screen printing method was employed to fabricate Li doped 0.7(Ba,Sr)TiO₃-0.3MgO thick films on the alumina substrates. (Ba,Sr)TiO₃ materials have high dielectric permittivity (>500 @ 1 MHz) and low loss tangent (0.01 @ 1 MHz) in the epitaxial thin film form. To improve dielectric properties and reduce sintering temperature, MgO and Li were added, respectively. 10 μm thick films were screen printed on the alumina substrates and then interdigital capacitors with seven fingers of 200 μm finger gap were patterned with Ag electrode. Current-voltage characteristics were analyzed with elevated temperature range. Up to 50 °C, the thick films showed positive temperature coefficient of resistivity (dρ/dT) of 6.11 × 10⁸ Ω cm/°C, then film showed negative temperature coefficient of resistivity (dρ/dT) of −1.74 × 10⁸ Ω cm/°C. From the microwave measurement, the relative dielectric permittivity of Li doped 0.7(Ba,Sr)TiO₃-0.3MgO thick films interdigital capacitors were between 313 at 1 GHz and 265 at 7 GHz.     

Li-doped (Ba,Sr)TiO3 thick film interdigital capacitors for microwave applications

Microwave properties of Li-doped (Ba,Sr)TiO₃ thick film interdigital capacitors have been investigated. According to the reported papers, BaSrTiO₃ materials, paraelectric state at the room temperature, have high dielectric permittivity (>500 @ 1 MHz) and low loss tangent (<0.01 @ 1 MHz) in epitaxial thin film form; however, the sintering temperature of BaSrTiO₃ is over 1350 °C. In order to reduce the sintering temperature, Li (3 wt%) was added to the BaSrTiO₃ materials, and 10 μm thick Li-doped (Ba,Sr)TiO₃ films were screen printed on the alumina (Al₂O₃) substrate and sintered at 900 °C. Interdigital capacitor patterns with five fingers of 200 μm gap and 250 μm length were also designed and fabricated by employing the screen printing method with Ag electrode. The structural feature was analyzed with X-ray diffraction method. Frequency and temperature-dependent dielectric properties were characterized from 1 kHz to 1 MHz and 303-403 K, respectively. Also, current-voltage characteristics were investigated with an elevated temperature. Microwave transmission and reflectance properties of thick film interdigital capacitors will be discussed, and frequency dispersion of dielectric properties will be presented. Specially, designed Au/Li-doped (Ba,Sr)TiO₃/Ag-Pd/Al₂O₃ vertical structure was prepared to measure the tunability. In this sandwich type structure, Li-doped (Ba,Sr)TiO₃ films showed tenability of 7.15% at a bias electric field of 20 kV/cm.     

Microstructure and dielectric response of SrTiO3/NdGaO3 interdigitated capacitors

Epitaxial strontium titanate (SrTiO₃ or STO) thin films were prepared by an off-axis pulsed laser deposition technique on neodymium gallate (NdGaO₃ or NGO) substrates held at temperature of 820 °C. This technique allows different film growth rates in a deposition. Coplanar capacitors were fabricated and dielectric responses were measured at 1 MHz and at 2 GHz, and from 300 K to 4 K. The electric field tunability of the dielectric constant and loss tangent were taken with a range of electric field. The structure and morphology of the films were analyzed using high-resolution X-ray diffractometry and atomic force microscopy, respectively. The results showed that the films are crystalline with (1 0 0) orientation and the grains are columnar. Increased in-plane grain size and reduced surface to volume ratio were found to play a major role in improved performance of the film coplanar capacitors. The film with the growth rate of approximate 40 Å/min showed the highest change in the dielectric constant with an electric field of 4 V/μm. The film also showed the largest in-plane grain size of about 3000 Å.     

Comparison of Microwave Dielectric Properties of Ba0.6Sr0.4TiO3 Thin Films Grown on (100) LaAlO3 and (100) MgO Single-Crystal Substrates

The microwave properties of barium strontium titanate (Ba_0.6Sr_0.4TiO₃) thin films grown on (100) LaAlO₃ (LAO) and (100) MgO single-crystal substrates through the sol–gel technique were investigated. The interdigital capacitor (IDC) technique was used to measure the nonlinear dielectric properties in the frequency range from 1 GHz to 10 GHz. The results show that the Curie temperature, capacitance, and tunability of the films are strongly dependent upon the substrate. The film fabricated on the LaAlO₃ substrate has a higher tunability of 16.77% than that grown on the MgO substrate (～8.38%), measured at 10 GHz with an applied voltage of 35 V. The loss tangent is a linear function of the frequency in the microwave range, and the film grown on the MgO substrate has a lower loss tangent than that grown on the LAO substrate. This work reveals the great potential of Ba_0.6Sr_0.4TiO₃ (BST) films for application in tunable microwave devices.     

Dielectric spectroscopy studies on (PVP + PVA) polyblend film

The thermal behavior of (PVP + PVA) polyblend film have been examined using differential scanning calorimetry and scanning electron microscopy. Capacitance and loss tangent values of polyvinyl pyrrolidone (PVP) + polyvinyl alcohol (PVA) polyblend film were measured in the frequency range 1-100 kHz and temperature range 298-423 K. Dielectric permittivity of real part (ε′) was obtained from capacitance data and dielectric permittivity of imaginary part (ε″) was obtained from real part of dielectric permittivity and loss tangent values. The decrease in dielectric permittivity was observed with increasing frequency and also observed increase in dielectric permittivity with increasing temperature. The complex dielectric constant (ε*) has been described by the electric modulus M* = (1/ε*) = M′ + iM″. The data of M* has been analysed by the stretched exponential decay of the electric field, Φ(t) = exp−(t/τ₀)^β.     

Microstrip antenna on a high dielectric constant substrate: BaTiO3 (BTO)-CaCu3Ti4O12(CCTO) composite screen-printed thick films

The performance of microstrip antennas using composite thick films of (BTO-BaTiO₃) and CCTO (CaCu₃Ti₄O₁₂) as a substrate were studied. The dielectric permittivity and loss of (BTO)_x-(CCTO)_1−x thick films with x=0, 0.2, 0.5, 0.8, 0.9, and 1 were examined. These films were prepared in two-layer geometry using the screen-printing technique on Al₂O₃ substrates. Mechanical alloying followed by the solid-state procedure was successfully employed to produce powders of CCTO (CaCu₃Ti₄O₁₂) used in the films. We also studied the films dielectric permittivity (K) and loss (D) in the medium-frequency (MF) range (100 Hz to 1 MHz). The performance of a planar microstrip antenna that uses the (BTO)_x:(CCTO)_1−x thick films as a substrate of high K was also examined in the microwave range of frequencies. From the analysis of the antenna operation of the samples, one can conclude that the higher values of K in the range of 2.5–3.3 GHz antennas is presented by the BTO substrates. For the BTO film, the K value is ∼66 (2.6 GHz) and decreases to 34 for the CCTO film (3 GHz). For the BTO and CCTO films, the antenna bandwidths (BW) are ∼50% and ∼38%, respectively. The higher bandwidth presented by the BTO compared to the CCTO is certainly associated with the higher loss presented by the BTO phase, which is a ferroelectric phase. Therefore, these measurements confirm the potential use of such materials for small microwave planar antennas, where the miniaturization of the devices is crucial.     

Analysis of high frequency properties of multilayer structures for multichip modules

The microwave surface resistance and reactance of YBa₂Cu₃O₇ multilayers for MCMs have been studied as a function of thickness and relative permittivity of dielectric layers at 500 MHz and 10 GHz propagation frequency. Additionally, frequency properties of a YBCO/CeO₂/SrTiO₃/YBCO/LaAlO₃ multilayer have been analyzed and results compared with measurement results. Performed simulations have shown that a dielectric layer of high relative permittivity, necessary for good isolation between superconducting ground planes and power planes in the multichip modules, has negligible influence on the effective surface resistance and reactance up to 0.5 μm dielectric thickness.     

High performance TaYOx-based MIM capacitors

TaYO_x-based metal-insulator-metal (MIM) capacitors with excellent electrical properties have been fabricated. Ultra-thin TaYO_x films in the thickness range of 15-30 nm (EOT ∼ 2.4-4.7 nm) were deposited on Au/SiO₂ (100 nm)/Si (100) structures by rf-magnetron co-sputtering of Ta₂O₅ and Y₂O₃ targets. TaYO_x layers were characterized by X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray (EDX) and X-ray diffraction (XRD) to examine the composition and crystallinity. An atomic percentage of Ta:Y = 58.32:41.67 was confirmed from the EDX analysis while XRD revealed an amorphous phase (up to 500 °C) during rapid thermal annealing. Besides, a high capacitance density of ∼3.7-5.4 fF/μm² at 10 kHz (ε_r ∼ 21), a low value of VCC (voltage coefficients of capacitance, α and β) have been achieved. Also, a highly stable temperature coefficient of capacitance, TCC has been obtained. Capacitance degradation phenomena in TaYO_x-based MIM capacitors under constant current stressing (CCS at 20 nA) have been studied. It is observed that degradation depends strongly on the dielectric thickness and a dielectric breakdown voltage of 3-5 MV/cm was found for TaYO_x films. The maximum energy storage density was estimated to be ∼5.69 J/cm³. Post deposition annealing (PDA) in O₂ ambient at 400 °C has been performed and further improvement in device reliability and electrical performances has been achieved.     

Epitaxial growth of Dy2O3 thin films on epitaxial Dy-germanide films on Ge(0 0 1) substrates

Ultra-thin films of Dy are grown on Ge(0 0 1) substrates by molecular beam deposition near room temperature and immediately annealed for solid phase epitaxy at higher temperatures, leading to the formation of DyGe_x films. Thin films of Dy₂O₃ are grown on the DyGe_x film on Ge(0 0 1) substrates by molecular beam epitaxy. Streaky reflection high energy electron diffraction (RHEED) patterns reveal that epitaxial DyGe_x films grow on Ge(0 0 1) substrates with flat surfaces. X-ray diffraction (XRD) spectrum suggests the growth of an orthorhombic phase of DyGe_x films with (0 0 1) orientations. After the growth of Dy₂O₃ films, there is a change in RHEED patterns to spotty features, revealing the growth of 3D crystalline islands. XRD spectrum shows the presence of a cubic phase with (1 0 0) and (1 1 1) orientations. Atomic force microscopy image shows that the surface morphology of Dy₂O₃ films is smooth with a root mean square roughness of 10 Å.     

Low-Dielectric-Loss Barium Strontium Titanate Thin Films with MgO Buffer Layer for Tunable Microwave Devices

The dielectric and microwave properties of Ba_0.6Sr_0.4TiO₃ (BST60) thin films with a MgO buffer layer deposited on Al₂O₃ substrates were investigated. Insertion of the MgO buffer layer is demonstrated to be an effective approach to fabricate low-dielectric-loss BST thin films. x-Ray pattern analysis indicates that the thin films exhibit good crystalline quality with a pure perovskite phase and that insertion of the MgO buffer layer does not change the crystal structure of BST. The nonlinear dielectric properties of the BST films were measured by using an interdigital capacitor (IDC). At room temperature, the tunability of the BST films with a MgO buffer layer was 24.1% at a frequency of 1 MHz with an applied electric field of 80 kV/cm. The dielectric loss of the BST thin films is only 0.005 to 0.007 in the frequency range from 20 Hz to 2 MHz, the same as for BST films prepared on single-crystal MgO substrates. The microwave dielectric properties of the BST thin films were also measured by a vector network analyzer from 50 MHz to 10 GHz.     

Microstructure and electrical characteristics of Ba0.65Sr0.35TiO3 thin films etched in CF4/Ar/O2 plasma

Radio frequency magnetron sputtered Ba_0.65Sr_0.35TiO₃ (BST) thin films were etched in CF₄/Ar/O₂ plasma by magnetically enhanced reactive ion etching technique. The etching characteristics of BST films were characterized in terms of microstructure and electrical properties. Atomic force microscopy and X-ray diffraction results indicate that the microstructure of the etched BST film is degraded because of the rugged surface and lowered intensities of BST (1 0 0), (1 1 0), (1 1 1) and (2 0 0) peaks compared to the unetched counterparts. Dielectric constant and dielectric dissipation of the unetched, etched and postannealed-after-etched BST film capacitors are 419, 346, 371, 0.018, 0.039 and 0.031 at 100 kHz, respectively. The corresponding dielectric tunability, figure of merit and remnant polarization are 19.57%, 11.56%, 17.25%, 10.87, 2.96, 5.56, 3.62 μC/cm², 2.32 and 2.81 μC/cm² at 25 V, respectively. The leakage current density of 1.75 × 10⁻⁴ A/cm² at 15 V for the etched BST capacitor is over two orders of magnitude higher than 1.28 × 10⁻⁶ A/cm² for the unetched capacitor, while leakage current density of the postannealed-after-etched capacitor decreases slightly. It means that the electrical properties of the etched BST film are deteriorated due to the CF₄/Ar/O₂ plasma-induced damage. Furthermore, the damage is alleviated, and the degraded microstructure and electrical properties are partially recovered after the etched BST film is postannealed at 923 K for 20 min under a flowing O₂ ambience.     

Improvement on low-temperature deposited HfO2 film and interfacial layer by high-pressure oxygen treatment

In this study, high-pressure oxygen (O₂ and O₂ + UV light) technologies were employed to effectively improve the properties of low-temperature-deposited metal oxide dielectric films and interfacial layer. In this work, 13 nm HfO₂ thin films were deposited by sputtering method at room temperature. Then, the oxygen treatments with a high-pressure of 1500 psi at 150 °C were performed to replace the conventional high temperature annealing. According to the XPS analyses, integration area of the absorption peaks of O-Hf and O-Hf-Si bonding energies apparently raise and the quantity of oxygen in deposited thin films also increases from XPS measurement. In addition, the leakage current density of standard HfO₂ film after O₂ and O₂ + UV light treatments can be improved from 3.12 × 10⁻⁶ A/cm² to 6.27 × 10⁻⁷ and 1.3 × 10⁻⁸ A/cm² at |Vg| = 3 V. The proposed low-temperature and high pressure O₂ or O₂ + UV light treatment for improving high-k dielectric films is applicable for the future flexible electronics.     

Influence of the metal electrode on the characteristics of thermal Ta2O5 capacitors

The effect of various electrodes (Al, W, TiN) deposited by evaporation (Al) and sputtering (W, TiN) on the electrical characteristics of thermal thin film (15-35 nm) Ta₂O₅ capacitors has been investigated. The absolute level of leakage currents, breakdown fields, mechanism of conductivity, dielectric constant values are discussed in the terms of possible reactions between Ta₂O₅ and electrode material as well as electrode deposition process-induced defects acting as electrically active centers. The dielectric constant values are in the range 12-26 in dependence on both Ta₂O₅ thickness and gate material. The results show that during deposition of TiN and Al a reaction that worsens the properties of Ta₂O₅ occurs while there is not an indication for detectable reduction of Ta₂O₅ when top electrode is W, and the leakage current is 5-7 orders of magnitude lower as compared to Al and TiN-electroded capacitors. The high level of leakage current for TiN and Al gate capacitors are related to the radiation defects generated in Ta₂O₅ during sputtering of TiN, and damaged interface at the electrode due to a reaction between Al and Ta₂O₅, respectively. It is demonstrated that the quality of the top electrode affects the electrical characteristics of the capacitors and the sputtered W is found to be the best. The sputtered W gate provides Ta₂O₅ capacitors with a good quality: the current density <7 × 10⁻¹⁰ A/cm² at 1 V (0.7 MV/cm, 15 nm thick Ta₂O₅). W deposition is not accompanied by an introduction of a detectable damage leading to a change of the properties of the initial as-grown Ta₂O₅ as in the case of TiN electrode. Damage introduced during TiN sputtering is responsible for current deterioration (high leakage current) and poor breakdown characteristics. It is concluded that the sputtered W top electrode is a good candidate as a top electrode of storage capacitors in dynamic random access memories giving a stable contact with Ta₂O₅, but sputtering technique is less suitable (favorable) for deposition of TiN as a metal electrode due to the introduction of radiation defects causing both deterioration of leakage current and poor breakdown characteristics.     

Microwave absorption and permittivity of polyaniline thin films using overlay technique

This paper reports the use of nonresonating microstripline for investigation of polyaniline thin film using overlay technique. Microwave absorption, DC conductivity, microwave conductivity, shielding effectiveness and microwave permittivity and dielectric loss of the conducting PANI films are reported. DC conductivity was between 0.15×10⁻³ and 3.13×10⁻³ S/cm. Microwave conductivity was between 0.1 and 10 S/cm. The PANI films coated on alumina gave shielding effectiveness values of −1 to −8 db. The ε′ was between 40 and 350. Measurements have been carried out over the frequency range 8.2-18 GHz. The effect of thickness of the overlay is also reported.     

Formation of aluminum oxide films from aluminum hexafluoroacetylacetonate at 350–450° c

A study of the thermally activated decomposition of Al(hfa)₃ (aluminum hexafluoroacetylacetonate) from the gas phase to form Al₂O₃ on silicon substrates is reported. The decomposition process was carried out in an open tube atmospheric pressure reactor in either argon or oxygen/argon mixtures in the temperature range, 350–450° C. The chemical vapor deposition process resulted in the formation of aluminum oxide films in all instances. The dielectric strength of Al/Al₂O₃/Si capacitors which received a post-metal anneal, but did not receive a high temperature annealing treatment, with aluminum oxide films prepared from Al(hfa)₃ in argon, was found to be in the range 2–6 MV/cm. The difference between the flatband voltage of the MOS structures and the metal-silicon work function difference was positive, indicative of a net negative oxide charge with a density of approximately 3 × 10¹¹ – 3 × 10¹² cm^-2, assuming the charge is located at the oxide-silicon interface. Decomposition of Al(hfa)₃ was also carried out in oxygen/argon mixtures with the oxygen concentration in the range 10–60 vol %. This process led to the deposition of aluminum oxide films with breakdown fields in the range 8–9 MV/cm. However, the flatband voltages of the Al/Al₂O₃/Si capacitors were even more positive than those obtained with Al₂O₃ formed in pure argon. High temperature (800–1000° C) oxygen or nitrogen annealing treatments of alumina films deposited in either argon or oxygen/argon mixtures were evaluated from the point of view of their influence on the oxide film properties. In particular, an annealing process in oxygen at 1000° C for 15 min was found to result in a reduction of the net negative oxide charge, and an improvement of the dielectric strength of films deposited in argon. Films formed in oxygen/argon mixtures did not change appreciably following oxygen annealing, as far as breakdown fields are concerned, but the oxide net negative charge was reduced. As in an earlier study by the authors, of copper film deposition from Cu(hfa)₂, it was found that essentially carbon free films could be obtained under appropriate conditions.     

Frequency and temperature dependent dielectric properties of Al/Si3N4/p-Si(1 0 0) MIS structure

The dielectric properties of Al/Si₃N₄/p-Si(1 0 0) MIS structure were studied from the C-V and G-V measurements in the frequency range of 1 kHz to 1 MHz and temperature range of 80-300 K. Experimental results shows that the ε′ and ε″ are found to decrease with increasing frequency while the value of ε′ and ε″ increase with increasing temperature, especially, above 160 K. As typical values, the dielectric constant ε′ and dielectric loss ε″ have the values of 7.49, 1.03 at 1 kHz, and only 0.9, 0.02 at 1 MHz, respectively. The ac electrical conductivity (σ_ac) increases with both increasing frequency and temperature. The activation energy of 24 meV was calculated from Arrhenius plot at 1 MHz. The results indicate that the interfacial polarization can be more easily occurred at low frequencies and high temperatures.     

Recent progress of (Ba,Sr)TiO<Subscript>3</Subscript> thin films for tunable microwave devices

The (Ba_1−xSr_x)TiO₃ (BST) ferroelectric thin films exhibit outstanding dielectric properties, even at high frequencies (>1 GHz), and large, electric-field dielectric tunability. This feature makes them suitable for developing a new class of tunable microwave devices. The dielectric properties and dielectric tuning property of BST thin films are closely related to the film compositions, substrate types, and post-deposition process. The successful implementation of BST films as high-frequency dielectrics in electrically tunable microwave devices requires a detailed understanding of both their processing and material properties. This paper will review the recent progress of BST thin films as active dielectrics for tunable microwave devices. The technical aspects of BST thin films, such as processing methods, post-annealing process, film compositions, film stress, oxygen defects, and interfacial structures between film and substrate, are briefly reviewed and discussed with specific samples from the recent literature. The major issues requiring additional investigations to improve the dielectric properties of BST thin films for tunable microwave applications are also discussed.     

Epitaxial ferroelectric PbZrxTi1–xO3 thin films for non-volatile memory applications

Epitaxial ferroelectric PbZr_xTi_1–xO₃ (PZT) thin film capacitors with SrRuO₃ (SRO) bottom electrodes have been fabricated by pulsed laser deposition on LaAlO₃ (0 0 1) substrates. X-ray diffraction measurements revealed that epitaxial heterostructures with a high crystalline quality were obtained. Ferroelectric capacitors were defined by thermal evaporation of aluminium contact pads onto the PZT films. Remnant polarizations of about 13 μC/cm² and coercive fields of about 150 kV/cm are obtained at a frequency of 10 Hz. The capacitors show very little fatigue of the remnant polarization with cumulative switching. A tendency to imprint, arising from the use of asymmetric electrodes, is observed.     

Impact of the CMP process on the electrical properties of ultra low k porous SiOCH

The impact of chemical mechanical polishing (CMP) on SiOCH films (thickness = 300 nm) for the 32-45 nm node Cu-interconnect process is investigated by low-frequency dielectric spectroscopy and thermally stimulated depolarization current (TSDC). After CMP process, the dielectric permittivity is degraded of about 25% in the whole range of the investigated frequency (10⁻¹ Hz-100 kHz). In a same way, the dielectric losses tan δ increase at the lowest frequencies. An annealing (300 °C during 20 min) carried out after CMP induces a reduction of the dielectric permittivity without however reaching the value of initial as-deposited material. In agreement with other published papers focusing on the damage caused by the CMP, OH bonding and water adsorption due to surfactants explain the degradation of these dielectric properties. The identification of OH bonds and an increase in the intensity of CH_x in the 2800-3050 cm⁻¹ range after CMP seems to confirm this point. The moderate temperature of annealing, used to restore layers and to avoid the degradation of copper lines, suppresses the physisorbed water but not the chemisorbed water. TSDC measurements confirm that dipolar relaxation, due to water in the material, result in a peak of relaxation at a temperature around 175 °C.     

ALD of LaHfOx nano-laminates for high-κ gate dielectric applications

Electrical properties and thermal stability of LaHfO_x nano-laminate films deposited on Si substrates by atomic layer deposition (ALD) have been investigated for future high-κ gate dielectric applications. A novel La precursor, tris(N,N′-diisopropylformamidinato) lanthanum [La(ⁱPrfAMD)₃], was employed in conjunction with conventional tetrakis-(ethylmethyl)amido Hf (TEMA Hf) and water (H₂O). The capacitance-voltage curves of the metal oxide semiconductor capacitors (MOSCAPs) showed negligible hysteresis and frequency dispersion, indicating minimal deterioration of the interface and bulk properties. A systematic shift in the flat-band voltage (V_fb) was observed with respect to the change in structure of nano-laminate stacks as well as La₂O₃ to HfO₂ content in the films. The EOTs obtained were in the range of ∼1.23-1.5 nm with leakage current densities of ∼1.3 × 10⁻⁸ A/cm² to 1.3 × 10⁻⁵ A/cm² at V_fb − 1 V. In addition, the films with a higher content of La₂O₃ remained amorphous up to 950 °C indicating very good thermal stability, whereas the HfO₂ rich films crystallized at lower temperatures.