Preparation of Low Volatile Organic Compounds Silver Paste Containing Ternary Conductive Fillers and Optimization of Their Performances.

Conductive silver paste is a key material in the fields of printed circuits and printed electronic devices. However, the preparation of conductive silver paste with low-cost and volatile organic compounds (VOCs) is still a challenge. In this work, conductive silver pastes with excellent comprehensive performances were developed by using water-borne polyurethane (WPU) as the bonding phase and using the ternary mixture of Ag microflakes (Ag MFs), Ag nanowires (Ag NWs), and Ag nanoparticles (Ag NPs) as the conductive phase. WPU endowed conductive silver pastes with the adhesion along with releasing a few VOCs during the curing. Results showed that a small amount of Ag NPs or Ag NWs dramatically enhanced the electrical conductivity of silver paste paint film filled only with Ag MFs. The electrical resistivity for optimal ternary mixture conductive silver paste was 0.2 × 10-3 Ω∙cm, and the conductive phase was composed of 20.0 wt% Ag MFs, 7.5 wt% Ag NWs, and 2.5 wt% Ag NPs. Meanwhile, the adhesive strength and hardness of silver paste paint film were effectively improved by increasing the curing temperature. The optimal overall performance of the conductive silver pastes was achieved at the curing temperature of 160 °C. Therefore, this work can provide a new route for preparing conductive silver pastes with high performances.

Highly Sensitive E-Textile Strain Sensors Enhanced by Geometrical Treatment for Human Monitoring.

Electronic textiles, also known as smart textiles or smart fabrics, are one of the best form factors that enable electronics to be embedded in them, presenting physical flexibility and sizes that cannot be achieved with other existing electronic manufacturing techniques. As part of smart textiles, e-sensors for human movement monitoring have attracted tremendous interest from researchers in recent years. Although there have been outstanding developments, smart e-textile sensors still present significant challenges in sensitivity, accuracy, durability, and manufacturing efficiency. This study proposes a two-step approach (from structure layers and shape) to actively enhance the performance of e-textile strain sensors and improve manufacturing ability for the industry. Indeed, the fabricated strain sensors based on the silver paste/single-walled carbon nanotube (SWCNT) layers and buffer cutting lines have fast response time, low hysteresis, and are six times more sensitive than SWCNT sensors alone. The e-textile sensors are integrated on a glove for monitoring the angle of finger motions. Interestingly, by attaching the sensor to the skin of the neck, the pharynx motions when speaking, coughing, and swallowing exhibited obvious and consistent signals. This research highlights the effect of the shapes and structures of e-textile strain sensors in the operation of a wearable e-textile system. This work also is intended as a starting point that will shape the standardization of strain fabric sensors in different applications.

Residual Stress and Warping Analysis of the Nano-Silver Pressureless Sintering Process in SiC Power Device Packaging.

Chip bonding, an essential process in power semiconductor device packaging, commonly includes welding and nano-silver sintering. Currently, most of the research on chip bonding technology focuses on the thermal stress analysis of tin-lead solder and nano-silver pressure-assisted sintering, whereas research on the thermal stress analysis of the nano-silver pressureless sintering process is more limited. In this study, the pressureless sintering process of nano-silver was studied using finite element software, with nano-silver as an interconnect material. Using the control variable method, we analyzed the influences of sintering temperature, cooling rate, solder paste thickness, and solder paste area on the residual stress and warping deformation of power devices. In addition, orthogonal experiments were designed to optimize the parameters and determine the optimal combination of the process parameters. The results showed that the maximum residual stress of the module appeared on the connection surface between the power chip and the nano-silver solder paste layer. The module warping deformation was convex warping. The residual stress of the solder layer increased with the increase in sintering temperature and cooling rate. It decreased with the increase in coating thickness. With the increase in the coating area, it showed a wave change. Each parameter influenced the stress of the solder layer in this descending order: sintering temperature, cooling rate, solder paste area, and solder paste thickness. The residual stress of the nano-silver layer was 24.83 MPa under the optimal combination of the process parameters and was reduced by 29.38% compared with the original value of 35.162 MPa.

Physical Properties of Paste Synthesized from Wet- and Dry-Processed Silver Powders.

This study compares the characteristics and low-temperature curing properties of pastes prepared from silver (Ag) powders synthesized by either wet powder (WP) or dry powder (DP) processing. The WP synthesis of electrode particles has the advantage of controlling the average particle size and particle size distribution but the disadvantage of producing low-purity, crystalline particles because they are synthesized through chemical reduction at less than 100 °C. Conversely, the DP synthesis of electrode particles has the advantage of producing pure, highly crystalline particles (due to synthesis at high temperatures) but the disadvantage of a high processing cost. WP and DP were used to manufacture pastes for low-temperature curing, and the physical properties of the pastes and the electrode characteristics after low-temperature curing were compared between powder types. Shear stress as a function of the shear rate shows that the WP paste is a plastic fluid, whereas the DP paste is a pseudoplastic fluid, closer to a Newtonian fluid. Screen printing the Ag pastes and curing for 30 min at 130 °C produces a nonconductive WP paste, whereas it produces a DP paste with a conductivity of 61 mΩ/sq, indicating that the highly crystalline DP paste is advantageous for low-temperature curing.

Optimizing Silver Paste Conductivity with Controlled Convection for Nanowrinkle Growth.

Conductive silver paste plays a crucial role as an interconnecting material between electrodes and circuits in electronic circuits and solar cells. The quality of the silver paste is greatly influenced by the preparation of the conductive-phase silver powder and the sintering process. This study investigated the impact of fluid dynamics on the preparation of silver powder. Combined with X-ray diffractometer characterization and molecular dynamics simulation, the formation mechanism of wrinkled silver powder was explained. The wrinkled silver powder replaced the traditional smooth spherical silver powder, and the point contact between the smooth silver powder turned into a line and surface contact. After mixing and sintering with the micrometer flake silver powder, the electrical conductivity and sintering morphology of the silver paste were improved. Compared with the silver content of conventional silver paste (≥75 wt %), the silver paste of (9.23 ± 0.68) × 10-6 Ω cm can be prepared by curing at 250 °C for 45 min when wrinkled powder/flake powder = 1:1 and silver paste content was only 66.7%. This research work provides a new idea for the morphology control of submicrometer silver powder, which has important applications in the field of low-temperature silver paste for new N-type batteries.

Study on Low-Temperature Conductive Silver Pastes Containing Bi-Based Glass for MgTiO3 Electronic Power Devices.

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/□) 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.

A Fluorinated Polyimide Based Nano Silver Paste with High Thermal Resistance and Outstanding Thixotropic Performance.

Because of high conductivity, acceptable cost and good screen-printing process performance, silver pastes have been extensively used for making flexible electronics. However, there are few reported articles focusing on high heat resistance solidified silver pastes and their rheological properties. In this paper, a fluorinated polyamic acids (FPAA) is synthesized by polymerization of the 4,4'-(hexafluoroisopropylidene) diphthalic anhydride and 3,4'-diaminodiphenylether as monomers in the diethylene glycol monobutyl. The nano silver pastes are prepared by mixing the obtained FPAA resin with nano silver powder. The agglomerated particles caused by nano silver powder are divided and the dispersion of nano silver pastes are improved by three-roll grinding process with low roll gaps. The obtained nano silver pastes possess excellent thermal resistance with 5% weight loss temperature higher than 500 °C. The volume resistivity of cured nano silver paste achieves 4.52 × 10-7 Ω·m, when the silver content is 83% and the curing temperature is 300 °C. Additionally, the nano silver pastes have high thixotropic performance, which contributes to fabricate the fine pattern with high resolution. Finally, the conductive pattern with high resolution is prepared by printing silver nano pastes onto PI (Kapton-H) film. The excellent comprehensive properties, including good electrical conductivity, outstanding heat resistance and high thixotropy, make it a potential application in flexible electronics manufacturing, especially in high-temperature fields.

A Micromechanical Analysis to the Viscoplastic Behavior of Sintered Silver Joints under Shear Loading.

Ag paste has been recognized as a promising substitute for Sn/Pb solder in SiC or GaN power electronic devices, owing to its ability to withstand high temperatures and facilitate low-temperature packing. The reliability of these high-power circuits is greatly influenced by the mechanical properties of sintered Ag paste. However, there exist substantial voids inside the sintered silver layer after sintering, and the conventional macroscopic constitutive models have certain limitation to describe the shear stress-strain relationship of sintered silver materials. To analyze the void evolution and microstructure of sintered silver, Ag composite pastes composed of micron flake silver and nano-silver particles were prepared. The mechanical behaviors were studied at different temperatures (0-125 °C) and strain rates (1 × 10-4-1 × 10-2) for Ag composite pastes. The crystal plastic finite element method (CPFEM) was developed to describe the microstructure evolution and shear behaviors of sintered silver at varied strain rates and ambient temperatures. The model parameters were obtained by fitting experimental shear test data to a representative volume element (RVE) model built on representative volume elements, also known as Voronoi tessellations. The numerical predictions were compared with the experimental data, which showed that the introduced crystal plasticity constitutive model can describe the shear constitutive behavior of a sintered silver specimen with reasonable accuracy.

A Flexible Bi-Stable Composite Antenna with Reconfigurable Performance and Light-Responsive Behavior.

An integrated solution providing a bi-stable antenna with reconfigurable performance and light-responsive behavior is presented in this paper for the first time. The proposed antenna includes a radiation layer with conductivity, which is integrated onto the bi-stable substrate. First, the effect of the radiation layer material and substrate layer parameters on antenna performance was studied. The experiment showed that an antenna with CNTF has a wider impedance bandwidth than one with CSP, namely 10.37% versus 3.29%, respectively. The resonance frequency increases gradually with the increase in fiber laying density and fiber linear density. Second, the influence of state change of the substrate layer on the antenna radiation pattern was studied. The measured results showed that the maximum radiation angle and gain of states I and II are at 90°, 1.21 dB and 225°, 1.53 dB, respectively. The gain non-circularities of the antenna at states I and II are 4.48 dB and 8.35 dB, respectively, which shows that the antenna has good omnidirectional radiation performance in state I. The display of the array antenna, which shows that the array antenna has good omnidirectional radiation performance in state A, with gain non-circularities of 4.20 dB, proves the feasibility of this bi-stable substrate in reconfigurable antennas. Finally, the antenna deforms from state I to state II when the illumination stimulus reaches 22 s, showing good light-responsive behavior. Moreover, the bi-stable composite antenna has the characteristics of small size, light weight, high flexibility, and excellent integration.

Effects of Organic Vehicle on the Rheological and Screen-Printing Characteristics of Silver Paste for LTCC Thick Film Electrodes.

Silver paste is widely used for low-temperature co-fired ceramic (LTCC) electrodes. In this work, a kind of LTCC silver paste for fine-line screen-printing was developed by considering the effect of the organic vehicle on rheological behavior and screen-printing properties. A step-by-step volatilization mode was applied to screen the mixed organic solvent of α-terpineol, 2-(2-butoxyethoxy) ethyl acetate (BCA) and dibutyl phthalate (DBP). The α-terpineol:BCA:DBP ratio of 5:2:3 is selected by considering the volatility, viscosity, and pseudoplasticity of the organic vehicle. Both viscosity and pseudoplasticity of shear-thinning increase with the increase of ethyl cellulose (EC) organic binder content. Three interval thixotropy test (3ITT) was conducted to discuss the thixotropy of silver paste. The minimum printing line width of 13.27 µm is obtained using silver paste with 10 wt% EC, confirming that the homemade paste has good printability.

Screen-Printable Silver Paste Material for Semitransparent and Flexible Metal-Semiconductor-Metal Photodetectors with Liquid-Phase Procedure.

Photodetectors are widely applied in modern industrial fields because they convert light energy into electrical signals. We propose a printable silver (Ag) paste electrode for a highly flexible metal-semiconductor-metal (MSM) broadband visible light photodetector as a wearable and portable device. Single-crystal and surface-textured silicon substrates with thicknesses of 37.21 µm were fabricated using a wet etching process. Surface texturization on flexible Si substrates enhances the light-trapping effect and minimizes reflectance from the incident light, and the average reflectance is reduced by 16.3% with pyramid-like structures. In this study, semitransparent, conductive Ag paste electrodes were manufactured using a screen-printing with liquid-phase process to form a flexible MSM broadband visible light photodetector. The transmittance of the homemade Ag paste solution fell between 34.83% and 36.98% in the wavelength range of visible light, from 400 nm to 800 nm. The highest visible light photosensitivity was 1.75 × 104 at 19.5 W/m2. The photocurrents of the flexible MSM broadband visible light photodetector were slightly changed under concave and convex conditions, displaying stable and durable bending properties.

Sintering Nano-Silver Paste by Resistive Joule Heating Process for 2G HTS Tape Joints.

Developing a joining technology for 2G HTS tapes without significantly reducing their superconducting property is crucial for numerous applications (MRI, motor/generator, power transmission, etc.). In this study, low sintering temperature (~230 °C) nano-silver paste was used as solder to join two 2G HTS tapes. In addition, two heating methods, i.e., furnace heating (heat flux outside-in) and resistive Joule heating (heat flux inside-out), were studied. This study indicates that the heat flux from internal by resistive Joule heating method shows less deteriorating impact to the 2G RE-Ba-Cu-O tape (RE: rare earth element) during the sintering process with the best specific resistance of 0.074 µΩ∙cm2 and Ic retention percentage of 99% (i.e., Ic reduced from 100 A before joining to 99 A after joining). This study indicates that nano-silver paste together with resistive Joule heating can possibly be used as soldering materials to join 2G HTS tapes.

Experimental Investigation of Effect of Flake Silver Powder Content on Sintering Structure and Properties of Front Silver Paste of Silicon Solar Cell.

Optimizing the performance of front silver paste is of great significance in improving the efficiency of the photoelectric conversion of crystalline silicon solar cells. As a conductive functional phase of silver paste, the structure and performance of silver powder have an important influence on the sintering process of silver paste and the conductivity of silver electrodes. Because of their two-dimensional structure, flake silver powders can effectively increase the contact area with other silver powders and silicon cells before sintering. Additionally, flake silver particles have higher surface energy and sintering activity than spherical silver particles of the same particle size. However, recent research has mainly focused on the influence of the particle size of silver powder. This paper fills the research gap regarding the morphology of silver powders and clarifies the influence of flake silver powders on the performance of silver paste. The influence of the ratio of spherical silver powder to flake silver powder in silver paste on the sheet resistance, adhesion, and specific contact resistivity of silver film after sintering at 800 °C was studied, and the optimal ratio was determined according to a cross-sectional contact picture of the silver film. The results showed that with the increase in the mass fraction of the flake silver powder, the sheet resistance of the sintered silver film gradually increased, the adhesion first increased and then decreased, and the specific contact resistance first decreased and then increased. When the flake silver powder content was 0%, the minimum sheet resistance of the silver film was 2.41 m Ω/☐. When the flake silver powder content was 30%, the maximum adhesion of the silver film was 6.07 N. When the flake silver powder content was 50%, the minimum specific contact resistivity of the silver film was 0.25 Ω·cm2. In conclusion, when the flake silver powder content was 30%, the comprehensive performance of the silver film was the best.

Enhanced Field Emission of Single-Wall Carbon Nanotube Cathode Prepared by Screen Printing with a Silver Paste Buffer Layer.

A high emission current with relatively low operating voltage is critical for field emission cathodes in vacuum electronic devices (VEDs). This paper studied the field emission performance of single-wall carbon nanotube (SWCNT) cold cathodes prepared by screen printing with a silver paste buffer layer. The buffer layer can both enforce the adhesion between the SWCNTs and substrate, and decrease their contact resistance, so as to increase emission current. Compared with paste mixing CNTs and screen printed cathodes, the buffer layer can avoid excessive wrapping of CNTs in the silver slurry and increase effective emission area to reduce the operating voltage. The experimental results show that the turn-on field of the screen-printed SWCNT cathodes is 0.9 V/µm, which is lower than that of electrophoretic SWCNT cathodes at 2.0 V/µm. Meanwhile, the maximum emission current of the screen-printed SWCNT cathodes reaches 5.55 mA at DC mode and reaches 10.4 mA at pulse mode, which is an order magnitude higher than that of electrophoretic SWCNTs emitters. This study also shows the application insight of small or medium-power VEDs.

Comparison of Metallization Schemes on Glass Dielectrics for X-Band Glass Antennas and Energy Harvesting.

We prepare and test four types of glass antennas for X-band applications and energy harvesting. These antennas are made of three different glass metallization schemes, including conductive copper foil (CCF), conductive silver paste (CSP) and indium tin oxide (ITO) thin film. Compared with conventional microstrip patch antennas, the dielectric substrate materials of these designs are replaced with silicon-boron glass (εr = 6, tangent δ = 0.002). The antenna with CCF as a radiator and ground plane (case one) is compared with the antenna with ITO replacing the radiator (case two) and ground plane (case three), respectively, and the glass antenna made of CSP (case four) is also presented. In this paper, these four types of glass antennas are measured and analyzed, and a comparison of the fabrication process and performance of these antennas is demonstrated. This study could contribute to the development of human-machine interactivity (HMI) systems with glass dielectric substrates.

Ecofriendly Catechol Lipid Bioresin for Low-Temperature Processed Electrode Patterns with Strong Durability.

We demonstrated catechol lipid-based bioresin, which is collected from lacquer trees, to produce conductive pastes that can be processed at low temperatures, which are highly adhesive and multidurable. Our conductive paste, which consists of catechol lipid-based urushiol resin and a multimodal mixture of silver fillers, exhibited stable dispersion with shear thinning properties. The urushiol lacquer induced spontaneous reduction of silver salt at the surface of the silver fillers, thereby contributing to lower the contact resistance between conductive fillers in the electrical conduction. Furthermore, the directional volume shrinkage of the urushiol lacquer matrix in a cross-linking reaction resulted in a highly ordered microstructure of the silver fillers with layer-by-layer stacking of the silver flakes. This structure contributed to the improvement of the electrical contact between fillers as well as excellent mechanical hardness, anti-scratch capability, and the long-term environmental stability of the conductive films. Conductive films based on the silver paste with urushiol lacquer exhibited low electrical resistivity below 4.4 × 10-5 Ω cm, 5B-class strong adhesion strength, and high hardness exceeding 200 MPa. Finally, we demonstrated the facile room-temperature processability and screen printability of the UL-Ag paste by fabricating a printed antenna and three-dimensional (3D) electrode assembly based on a plastic 3D block.

Preparation of Nano Silver Paste and Applications in Transparent Electrodes via Electric-Field Driven Micro-Scale 3D Printing.

Nano-silver paste, as an important basic material for manufacturing thick film components, ultra-fine circuits, and transparent conductive films, has been widely used in various fields of electronics. Here, aiming at the shortcomings of the existing nano-silver paste in printing technology and the problem that the existing printing technology cannot achieve the printing of high viscosity, high solid content nano-silver paste, a nano-silver paste suitable for electric-field-driven (EFD) micro-scale 3D printing is developed. The result shows that there is no oxidation and settlement agglomeration of nano-silver paste with a storage time of over six months, which indicates that it has good dispersibility. We focus on the printing process parameters, sintering process, and electrical conductivity of nano-silver paste. The properties of the nano-silver paste were analyzed and the feasibility and practicability of the prepared nano-silver paste in EFD micro-scale 3D printing technology were verified. The experiment results indicate that the printed silver mesh which can act as transparent electrodes shows high conductivity (1.48 Ω/sq) and excellent transmittance (82.88%). The practical viability of the prepared nano-silver paste is successfully demonstrated with a deicing test. Additionally, the experimental results show that the prepared silver mesh has excellent heating properties, which can be used as transparent heaters.

Atmospheric scanning electron microscope system with an open sample chamber: configuration and applications.

An atmospheric scanning electron microscope (ASEM) with an open sample chamber and optical microscope (OM) is described and recent developments are reported. In this ClairScope system, the base of the open sample dish is sealed to the top of the inverted SEM column, allowing the liquid-immersed sample to be observed by OM from above and by SEM from below. The optical axes of the two microscopes are aligned, ensuring that the same sample areas are imaged to realize quasi-simultaneous correlative microscopy in solution. For example, the cathodoluminescence of ZnO particles was directly demonstrated. The improved system has (i) a fully motorized sample stage, (ii) a column protection system in the case of accidental window breakage, and (iii) an OM/SEM operation system controlled by a graphical user interface. The open sample chamber allows the external administration of reagents during sample observation. We monitored the influence of added NaCl on the random motion of silica particles in liquid. Further, using fluorescence as a transfection marker, the effect of small interfering RNA-mediated knockdown of endogenous Varp on Tyrp1 trafficking in melanocytes was examined. A temperature-regulated titanium ASEM dish allowed the dynamic observation of colloidal silver nanoparticles as they were heated to 240°C and sintered.