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Flexible thermoelectric materials have drawn significant attention from researchers due to their potential applications in wearable electronics and the Internet of Things. Despite many reports on these materials, it remains a significant challenge to develop cost-effective methods for large-scale, patterned fabrication of materials that exhibit both excellent thermoelectric performance and remarkable flexibility. In this study, we have developed an Ag2Se-based ink with excellent printability that can be used to fabricate flexible thermoelectric films by screen printing and low-temperature sintering. The printed films exhibit a Seebeck coefficient of -161 µV/K and a power factor of 3250.9 µW/m·K2 at 400 K. Moreover, the films demonstrate remarkable flexibility, showing minimal changes in resistance after being bent 5000 times at a radius of 5 mm. Overall, this research offers a new opportunity for the large-scale patterned production of flexible thermoelectric films.
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The emergence of novel e-textile materials that combine the inherent qualities of the textile substrate (lightweight, soft, breathable, durable, etc.) with the functionality of micro/nano-electronic materials (conductive, dielectric, sensing, etc.) has resulted in a trend toward miniaturization, integration, and intelligence in new electronic devices. However, the formation of a conductive network by micro/nano-conductive materials on textiles necessitates high-temperature sintering, which inevitably causes substrate aging and component damage. Herein, a bis-hydroxy-imidazolium chloride salt as a hard segment to synthesize a waterborne polyurethane (WPU) adhesive is designed and prepared. When used in nano-silver-based printing coatings, it offers strong adherence for coatings, reaching 16 N cm-1; on the other hand, the introduction of chloride ions enables low-temperature (60 °C) chemical sintering to address the challenge of secondary treatment and high-temperature sintering (>150 °C). Printed into flexible circuits, the resistivity can be controlled by the content of imidazolium salts anchored in the molecular chain of the WPU from a maximum resistivity of 3.1 × 107 down to 5.8 × 10-5 Ω m, and it can conduct a Bluetooth-type finger pulse detector with such low resistivity. As a flexible circuit, it also offers high stability against washing and adhesion, which the resistivity only reduces less than 20% after washing 10 times and adhesion. Owing to the adjustability of the resistivity, we fabricated an all-textile flexible pressure sensor that accurately differentiates different external pressures (min. 10 g, ~29 Pa), recognizes forms, and detects joint motions (finger bending and wrist flexion).
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In this paper, Al2O3 ceramics co-doped with 0.3 wt%CuO-0.6 wt%TiO2-0.1 wt%MnCO3 (CTM, the same below) were prepared. The effect of CTM and UV irradiation on the sintering behavior, microstructure, and microwave dielectric properties have been investigated systematically. The results indicate that the sintering temperature of Al2O3 ceramics could be effectively decreased to about 1200 °C by adding 1 wt% CTM. UV irradiation can further increase the density of the Al2O3 ceramics, improve its microstructure and microwave dielectric properties. By using the Al2O3 powders UV irradiated for 15 min as raw materials, CTM co-doped Al2O3 ceramics can sintered at 1200 °C with a high density of 3.93 g/cm3 and a very high Q × f value of 175,086 GHz.
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In recent years, solid electrolytes (SEs) have been developed a lot due to the superior safety of solid-state batteries (SSBs) upon liquid electrolyte-based commercial batteries. Among them, garnet-type Li7La3Zr2O12 (LLZO) is one of the few SEs that is stable to lithium anode with high Li+ conductivity and the feasibility of preparation under ambient air, which makes it a promising candidate for fabricating SSBs. However, high sintering temperature (>1200 °C) prevents its large-scale production, further hindering its application. In this work, the Li5AlO4 sintering aid is proposed to decrease the sintering temperature and modify the grain boundaries of LLZO ceramics. Li5AlO4 generates in situ Li2O atmosphere and molten Li-Al-O compounds at relatively low temperatures to facilitate the gas-liquid-solid material transportation among raw LLZO grains, which decreases the densification temperature over 150 °C and strengthens the grain boundaries against lithium dendrites. As an example, Ta-doped LLZO ceramics without excessive Li sintered with 2 wt % Li5AlO4 at 1050 °C delivered high relative density > 94%, an ionic conductivity of 6.7 × 10-4 S cm-1, and an excellent critical current density (CCD) of 1.5 mA cm-2 at room temperature. In comparison, Ta-doped LLZO with 15% excessive Li sintered at 1200 °C delivered low relative density < 89%, a low ionic conductivity of â¼2 × 10-4 S cm-1, and a poor CCD of 0.5 mA cm-2. Li symmetric cells and Li-LFP full cells fabricated with Li5AlO4-assised ceramics were stably cycled at 0.2 mA cm-2 over 2000 h and at 0.8C over 100 cycles, respectively.
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Functional inks enable manufacturing of flexible electronic devices by means of printing technology. Silver nanoparticle (Ag NP) ink is widely used for printing conductive components. A sintering process is required to obtain sufficient conductivity. Thermal sintering is the most commonly used method, but the heat must be carefully applied to avoid damaging low-temperature substrates such as polymer films. In this work, two alternative sintering methods, damp heat sintering and water sintering are systematically investigated for inkjet-printed Ag tracks on polymer substrates. Both methods allow sintering polyvinyl pyrrolidone (PVP) capped Ag NPs at 85°C. In this way, the resistance is significantly reduced to only 1.7 times that of the samples on polyimide sintered in an oven at 250°C. The microstructure of sintered Ag NPs is analyzed. Taking the states of the capping layer under different conditions into account, the explanation of the sintering mechanism of Ag NPs at low temperatures is presented. Overall, both damp heat sintering and water sintering are viable options for achieving high conductivity of printed Ag tracks. They can broaden the range of substrates available for flexible electronic device fabrication while mitigating substrate damage risks. The choice between them depends on the specific application and the substrate used.
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Low-temperature lead-free silver pastes deserve thorough investigation for sustainable development and application of MgTiO3 ceramics in electronic devices. In this study, a series of Bi2O3-B2O3-ZnO-SiO2-Al2O3-CaO glasses with suitable softening temperatures were prepared via melt quenching using a type of micrometer silver powder formed by silver nanoparticle aggregates. The composite pastes containing silver powder, Bi2O3 glass powder and an organic vehicle were then screen-printed. The effects of glass powder concentration and sintering temperature on the microstructure of the surface interface were also investigated. The results showed that the silver paste for microwave dielectric ceramic filters (MgTiO3) possessed good electrical conductivity (2.28 mΩ/â¡) and high adhesion (43.46 N/mm2) after medium temperature (670 °C) sintering. Thus, this glass powder has great application potential in non-toxic lead-free silver pastes for metallization of MgTiO3 substrates.
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Lu3Al5O12:Ce3+ phosphor ceramics were fabricated by vacuum sintering. On this basis, a bi-layer composite phosphor was prepared by low-temperature sintering to cover the phosphor ceramics with a layer of SrAlSiN3:Eu2+-phosphor-in-glass (PiG). The optical, thermal, and colorimetric properties of LuAG:Ce3+ phosphor ceramics, SrAlSiN3:Eu2+ phosphors and SrAlSiN3:Eu2+-PiG were studied individually. Combining the bi-layer composite phosphors with the blue LED chip, it is found that the spectrum can be adjusted by varying the doping concentration of SrAlSiN3:Eu2+-PiG and the thickness of Lu3Al5O12:Ce3+ phosphor ceramics. The maximal color rendering index value of the white LED is 86, and the R9 is 61. Under the excitation of a laser diode, the maximum phosphor conversion efficacy of the bi-layer composite phosphors is 120 lm/W, the Ra is 83, and the correlated color temperature is 4534 K. These results show that the bi-layer composite phosphor ceramic is a candidate material to achieve high color rendering index for high brightness lighting.
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In this work, Al2O3 nanoceramics were prepared by spark plasma sintering of amorphous powders and polycrystalline powders with similar particle sizes. Effective comparisons of sintering processes and ultimate products depending on starting powder conditions were explored. To ensure near-full density higher than 98% of the Al2O3 nanoceramics, the threshold temperature in SPS is 1450 °C for polycrystalline Al2O3 powders and 1300 °C for amorphous powders. The low SPS temperature for amorphous powders is attributed to the metastable state with high free energy of amorphous powders. The Al2O3 nanoceramics prepared by amorphous powders display a mean grain size of 170 nm, and superior mechanical properties, including high bending strength of 870 MPa, Vickers hardness of 20.5 GPa and fracture toughness of 4.3 MPaâm1/2. Furthermore, the Al2O3 nanoceramics prepared by amorphous powders showed a larger dynamic strength and dynamic strain. The toughening mechanism with predominant transgranular fracture is explained based on the separation of quasi-boundaries.
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Rapid developments in wide-bandgap semiconductors have led to the demand for interconnection materials that can withstand harsh conditions. In this study, novel Ag composite pastes were developed with the assistance of metal organic decomposition (MOD) to significantly reduce the sintering temperature of commercial Ag pastes. The effects of the decomposition characteristics of different MODs on the microstructure, morphology, and the shear strength of the Ag-sintered joints were systematically investigated. Additionally, the low-temperature sintering mechanisms of the MOD-assisted Ag composite pastes were studied and proposed. Among all the MODs studied, the one consisting of propylamine complexed with silver oxalate demonstrated the best performance due to its ability to form Ag nanoclusters with the smallest size (~25 nm) and highest purity (~99.07 wt.%). Notably, the bonding temperature of the MOD-modified Ag pastes decreased from 250 °C to 175 °C, while the shear strength increased from 20 MPa to 40.6 MPa when compared to the commercial Ag pastes.
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Developing piezoelectric ceramics with high piezoelectric properties and broad temperature usage ranges via low-temperature sintering is one of decisive importance for flourishing developments for emerging electromechanical applications. However, these properties are usually mutually exclusive, such as low-temperature sintering and high piezoelectricity as well as high piezoelectricity and temperature stability. Here, we report high piezoelectricity (i.e., piezoelectric constant d33 ≈ 744 pC/N, electromechanical coupling factor kp ≈ 75%, and Curie temperature TC ≈ 201 °C) and superior temperature stability (d33 varies less than 10% within 25-160 °C) in Pb0.905Ba0.095(Zr0.54Ti0.46)O3 + 1 mol % Nb2O5 + 1 wt % Bi2O3 + x wt % CdCO3 (PBZTNB-xCd) ceramics that are fabricated at a sintering temperature of as low as 960 °C, superior to those of other reported random and textured ceramics. Good piezoelectricity is attributed to the remaining rhombohedral-tetragonal (R-T) phase coexistence and the high ceramic density. Excellent temperature stability is related to the stable crystal structure and domain structure. These properties confer to the produced materials attractive characteristics for further consideration in several advanced applications, especially for piezoelectric transducer applications requiring constant structures over a broad temperature range.
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The request for extremely low-temperature and short-time sintering techniques has guided the development of alternative ceramic processing. Atmosphere-assisted FLASH sintering (AAFS) combines the direct use of electric power to packed powders with the engineering of operating atmosphere to allow low-temperature conduction. The AAFS of nanometric Potassium Sodium Niobate, K0.5Na0.5NbO3, a lead-free piezoelectric, is of great interest to electronics technology to produce efficient, low-thermal-budget sensors, actuators and piezo harvesters, among others. Not previously studied, the role of different atmospheres for the decrease in FLASH temperature (TF) of KNN is presented in this work. Additionally, the effect of the humidity presence on the operating atmosphere and the role of the compact morphology undergoing FLASH are investigated. While the low partial pressure of oxygen (reducing atmospheres) allows the decrease of TF, limited densification is observed. It is shown that AAFS is responsible for a dramatic decrease in the operating temperature (T < 320 °C), while water is essential to allow appreciable densification. In addition, the particles/pores morphology on the green compact impacts the uniformity of AAFS densification.
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With the rapid development of the microelectronics industry, many efforts have been made to improve glass-ceramics' sinterability, thermal conductivity, and dielectric properties, which are essential components of electronic materials. In this study, low-alkali borosilicate glass-ceramics with PVA addition and glass-BN composites were prepared and successfully sintered at 770 °C. The phase composition, density, microstructure, thermal conductivity, and dielectric constant were investigated. It was shown that PVA addition contributes to the densification process of glass-ceramics (~88% relative density, with closed/open pores in the microstructure) and improves the thermal conductivity of glass material from 1.489 to 2.453 W/K.m. On the other hand, increasing BN addition improves microstructures by decreasing porosities and thus increasing relative densities. A glass-12 wt. % BN composite sample exhibited almost full densification after sintering and presented apparent and open pores of 2.6 and 0.08%, respectively. A high thermal conductivity value of 3.955 W/K.m and a low dielectric constant of 3.00 (at 5 MHz) were observed in this material. Overall, the resulting glass-ceramic samples showed dielectric constants in the range of 2.40-4.43, providing a potential candidate for various electronic applications.
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Both the pore size and surface properties of silicon carbide (SiC) membranes are demonstrated to significantly affect their separation efficiency when used for oily water treatment. However, the potential influences of open porosity together with the pore size of SiC membranes on their surface properties and oil-water separation performance have rarely been investigated. In this work, porous SiC ceramic membranes with tunable open porosity and pore size were purposely prepared and selected to systematically study the effect of pore structure-dependent wettability on the oil-water separation performance. The measured pure water flux of selected membranes as a function of open porosity (34-48%) and pore size (0.43-0.67 µm) was well-fitted by using a modified H-P equation. Interestingly, the hydrophilicity of SiC membranes was improved with the increase in open porosity and pore size, as evidenced by the gradually decreased dynamic water contact angle and underwater adhesion of oil droplets. Further, the open porosity of SiC membranes was found to contribute more to the improved surface wettability. As a result, the stable flux of SiC membranes in oil-in-water (O/W) emulsions was increased by 24% with the increased open porosity while the oil rejection rate remained above 90%. This work quantitatively reveals the contributions of the pore structure to the surface wettability of ceramic membranes, and thus provides an effective pathway to improve their performance in oil-water separation.
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A silver precursor (silver 2-ethylhexanoate) and silver nanoparticles were synthesized and used to prepare a low sintering temperature nano-silver paste (PM03). We optimized the amount of silver 2-ethylhexanoate added and the sintering temperature to obtain the best performance of the nano-silver paste. The relationship between the microstructures and properties of the paste was studied. The addition of silver 2-ethylhexanoate resulted in less porosity, leading to lower resistivity and higher shear strength. Thermal compression of the paste PM03 at 250 °C with 10 MPa pressure for 30 min was found to be the proper condition for copper-to-copper bonding. The resistivity was (3.50 ± 0.02) × 10-7 Ωâm, and the shear strength was 57.48 MPa.
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A multilayer piezoelectric material was fabricated using piezoelectric materials with low-temperature sintering capabilities and high piezoelectric coefficients to develop a functionally superior piezoelectric speaker with a large-displacement deformation. A soft relaxor was utilized to prepare the component materials, with the optimized composition of the investigated piezoelectric ceramics represented by 0.2Pb((Zn0.8Ni0.2)13Nb23)O3-0.8Pb(Zr0.5Ti0.5)O3. Li2CO3 was added to assist the low-temperature sintering conducted at 875 °C, which yielded a multilayer piezoelectric material with superior properties (d33 = 500 pC N-1, kp = 0.63, g33 = 44 mV N-1). A multilayer piezoelectric actuator with a single-layer thickness of ~40 µm and dimensions of 12 × 16 mm2 was fabricated by tape casting the prepared green sheets. Finite element analysis revealed that the use of a PEEK film and a smaller silicone-rubber film as a composite in the diaphragm realized optimal frequency-response characteristics; the vibrations generated by the piezoelectric element were amplified. The optimal structure obtained via simulations was applied to fabricate an actual piezoelectric speaker with dimensions of 20 × 24 × 1 mm3. The actual measurements exhibited a sound pressure level of ~75 dB and a total harmonic distortion ≤15% in the audible frequency range (250-20,000 Hz) at an applied voltage of 5 Vp.
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Microwave dielectric ceramics are vital for filters, dielectric resonators, and dielectric antennas in the 5G era. It was found that the (Cu1/3Nb2/3)4+ substitution can effectively adjust the TCF (temperature coefficient of resonant frequency) of Li2TiO3 and simultaneously increase its Q × f (Q and f denote the quality factor and the resonant frequency, respectively) value. Notably, excellent microwave dielectric properties (εr (permittivity) ≈ 18.3, Q × f ≈ 77,840 GHz, and TCF ≈ +9.8 ppm/°C) were achieved in the Li2Ti0.8(Cu1/3Nb2/3)0.2O3 (LTCN0.2) ceramic sintered at 1140 °C. Additionally, the sintering temperature of LTCN0.2 was reduced to 860 °C by the addition of 3 wt % H3BO3, exhibiting superior microwave dielectric properties (εr ≈ 21.0, Q × f ≈ 51,940 GHz, and TCF ≈ 1.4 ppm/°C) and being chemically compatible with silver. Moreover, LTCN0.2 + 3 wt % H3BO3 ceramics were designed as a patch antenna and a dielectric resonator antenna, both of which showed high simulated radiation efficiencies (88.4 and 93%) and gains (4.1 and 4.03 dBi) at the center frequencies (2.49 and 10.19 GHz). The LTCN0.2 + 3 wt % H3BO3 materials have promising future application for either 5G mobile communication devices and/or in low-temperature co-fired ceramic technology owing to their high Q, low sintering temperature, small density, and good temperature stability.
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Bioactive glasses are promising materials for various applications, such as bone grafts and implants. The development of sintering techniques for bioactive glasses is one of the most important ways to expand the application to biomaterials. In this paper, we demonstrate the low-temperature mineralization sintering process (LMSP) of glass nanoparticles and their crystallization behavior. LMSP is a novel process employed to densify glass nanoparticles at an extremely low temperature of 120 °C. For this new approach, the hydrothermal condition, mineralization, and the nanosize effect are integrated into LMSP. To induce mineralization in LMSP, bioactive glass nanoparticles (BGNPs, 55SiO2-40CaO-5P2O5, mol%), prepared by the sol-gel process, were mixed with a small amount of simulated body fluid (SBF) solution. As a result, 93% dense BGNPs were realized under a temperature of 120 °C and a uniaxial pressure of 300 MPa. Due to the effect of mineralization, crystalline hydroxyapatite (HAp) was clearly formed at the boundaries of BGNPs, filling particles and interstitials. As a result, the relative density was remarkably close to that of the BGNPs conventionally sintered at 1050 °C. Additionally, the Vickers hardness value of LMSP samples varied from 2.10 ± 0.12 GPa to 4.28 ± 0.11 GPa, and was higher than that of the BGNPs conventionally sintered at 850 °C (2.02 ± 0.11 GPa). These results suggest that, in addition to LMSP being an efficient densification method for obtaining bulk bioactive glasses at a significantly lower temperature level, this process has great potential for tissue engineering applications, such as scaffolds and implants.
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A novel process is proposed in this paper for a green and efficient utilization of copper slag. The basic premise involved the addition of different amounts of Na2O into molten copper slag and evaluation of the effects on the magnetic fraction and the properties of ceramics generated from the non-magnetic residue, and mechanisms of the effects were further studied by XRD, SEM, EDS, viscosity test, hysteresis loop and FTIR. The results showed that Na2O additions dropped the viscosity of the slag markedly, which promoted the growth of magnetite, but decrease quantity of magnetite due to oxidization of Fe2+ and precipitation of crystals containing Fe3+. With the addition of 4 % Na2O, solidification temperature of slag decreased from 1790 K to 1530 K, optimum iron recovery rate of 81.08 % was achieved. Na2O as flux in ceramics obviously reduced its sintering temperature and meantime decreased its bending strength because of insufficient crystallization of its main minerals. The non-magnetic residue from magnetic separation of slag with addition of 4% Na2O was converted into ceramics with a much low sintering temperature of 1268 K (995 °C) and qualified bending strength of 64.5 MPa.
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Whilst the highest power conversion efficiency (PCE) perovskite solar cell (PSC) devices that have reported to date have been fabricated by high temperature sintering (>500 °C) of mesoporous metal oxide scaffolds, lower temperature processing is desirable for increasing the range of substrates available and also decrease the energy requirements during device manufacture. In this work, titanium dioxide (TiO2) mesoporous scaffolds have been compared with metal oxide oxidation catalysts: cerium dioxide (CeO2) and manganese dioxide (MnO2). For MnO2, to the best of our knowledge, this is the first time a low energy band gap metal oxide has been used as a scaffold in the PSC devices. Thermal gravimetric analysis (TGA) shows that organic binder removal is completed at temperatures of 350 °C and 275 °C for CeO2 and MnO2, respectively. By comparison, the binder removal from TiO2 pastes requires temperatures >500 °C. CH3NH3PbBr3 PSC devices that were fabricated while using MnO2 pastes sintered at 550 °C show slightly improved PCE (η = 3.9%) versus mesoporous TiO2 devices (η = 3.8%) as a result of increased open circuit voltage (Voc). However, the resultant PSC devices showed no efficiency despite apparently complete binder removal during lower temperature (325 °C) sintering using CeO2 or MnO2 pastes.
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Printed electronics (PE) technology shows huge promise for the realisation of low-cost and flexible electronics, with the ability to pattern heat- or pressure-sensitive materials. In future developments of the PE market, the ability to produce highly conductive, high-resolution patterns using low-cost and roll-to-roll processes, such as inkjet printing, is a critical technology component for the fabrication of printed electronics and displays. Here, we demonstrate inkjet printing of polyacrylic acid (PAA) capped silver nanoparticle dispersions onto paper for high-conductivity electronic interconnects. We characterise the resulting print quality, feature geometry and electrical performance of inkjet patterned features and demonstrate the high-resolution printing, sub-100 micron feature size, of silver nanoparticle materials onto flexible paper substrate. Printed onto photo-paper, these materials then undergo chemically triggered sintering on exposure to chloride contained in the paper. We investigated the effect of substrate temperature on the properties of printed silver material from room temperature to 50 °C. At room temperature, the resistivity of single layer printed features, of average thickness of 500 nm and width 85 µm, was found to be 2.17 × 10-7 Ω·m or 13 times resistivity of bulk silver (RBS). The resistivity initially decreased with an increase in material thickness, when achieved by overprinting successive layers or by decreasing print pitch, and a resistivity of around 10 times RBS was observed after overprinting two times at pitch 75 µm and with single pass print pitch of between 60 and 80 µm, resulting in line thickness up to 920 nm. On further increases in thickness the resistivity increased and reached 27 times RBS at print pitch of 15 µm. On moderate heating of the substrate to 50 °C, more compact silver nanoparticle films were formed, reducing thickness to 200 nm from a single pass print, and lower material resistivity approaching five times RBS was achieved.