A Novel Approach for Temperature-Induced Ball Grid Array Collapse Observation.

This study presents a new approach to investigating the impact of repeated reflow on the failure of ball grid array (BGA) packages. The issue with the BGA package collapse is that the repeated reflow can lead to short circuits, particularly for BGAs with a very fine pitch between leads. A novel approach was developed to measure the collapse of BGA solder balls during the melting and solidification process, enabling in situ measurements. The study focused on two types of solders: Sn63Pb37 as a reference, and the commonly used SAC305, with measurements taken at various temperatures. The BGA samples were subjected to three different heating/cooling cycles in a thermomechanical analyzer (TMA) at temperatures of 250 °C, 280 °C, and 300 °C, with a subsequent cooling down to 100 °C. The results obtained from the TMA indicated differences in the collapse behavior of both BGA solder alloys at various temperatures. Short circuits between neighboring leads (later confirmed by an X-ray analysis) were also recognizable on the TMA. The novel approach was successfully developed and applied, yielding clear insights into the behavior of solder balls during repeated reflow.

Personal Air-Quality Monitoring with Sensor-Based Wireless Internet-of-Things Electronics Embedded in Protective Face Masks.

In this paper, the design and research of a sensor-based personal air-quality monitoring device are presented, which is retrofitted into different personal protective face masks. Due to its small size and low power consumption, the device can be integrated into and applied in practical urban usage. We present our research and the development of the sensor node based on a BME680-type environmental sensor cluster with a wireless IoT (Internet of Things)-capable central unit and overall low power consumption. The integration of the sensor node was investigated with traditional medical masks and a professional FFP2-type mask. The filtering efficiency after embedding was validated with a head model and a particle counter. We found that the professional mask withstood the embedding without losing the protective filtering aspect. We compared the inner and outer sensor data and investigated the temperature, pressure, humidity, and AQI (Air Quality Index) relations with possible sensor data-fusion options. The novelty is increased with the dual-sensor layout (inward and outward). It was found that efficient respiration monitoring is achievable with the device. With the analysis of the recorded data, characteristic signals were identified in an urban environment, enabling urban altimetry and urban zone detection. The results promote smart city concepts and help in endeavors related to SDGs (Sustainable Development Goals) 3 and 11.

Application of solid-phase microextraction arrows for characterizing volatile organic compounds from 3D printing of acrylonitrile-styrene-acrylate filament.

3D printing is an extensively used manufacturing technique that can pose specific health concerns due to the emission of volatile organic compounds (VOC). Herein, a detailed characterization of 3D printing-related VOC using solid-phase microextraction-gas chromatography/mass spectrometry (SPME-GC/MS) is described for the first time. The VOC were extracted in dynamic mode during the printing from the acrylonitrile-styrene-acrylate filament in an environmental chamber. The effect of extraction time on the extraction efficiency of 16 main VOC was studied for four different commercial SPME arrows. The volatile and semivolatile compounds were the most effectively extracted by carbon wide range-containing and polydimethyl siloxane arrows, respectively. The differences in extraction efficiency between arrows were further correlated to the molecular volume, octanol-water partition coefficient, and vapour pressure of observed VOC. The repeatability of SPME arrows towards the main VOC was assessed from static mode measurements of filament in headspace vials. In addition, we performed a group analysis of 57 VOC classified into 15 categories according to their chemical structure. Divinylbenzene-polydimethyl siloxane arrow turned out to be a good compromise between the total extracted amount and its distribution among tested VOC. Thus, this arrow was used to demonstrate the usefulness of SPME for the qualification of VOC emitted during printing in a real-life environment. A presented methodology can serve as a fast and reliable method for the qualification and semi-quantification of 3D printing-related VOC.

Filtering Efficiency of Sustainable Textile Materials Applied in Personal Protective Face Mask Production during Pandemic.

The COVID-19 outbreak increased demand for personal protective respirator masks. Textile masks based on cloth materials appeared to be a sustainable, comfortable, and cost-effective alternative available in global communities. In this study, we used laser-based particle counting for mask material qualification to determine the concentration filtering efficiency in general, everyday community use. The efficiencies of eleven different commercially available textile materials were measured in single-, double-, and triple-layer configurations according to their grammage, mesh (XY), and inter-yarn gap. It was found that in the single-layer configurations, most materials were well below the acceptable standards, with a wide variation in filtering efficiency, which ranged from 5% to ~50%. However, when testing the fabrics in two or three layers, the efficiency increased significantly, exceeding or approaching the standard for medical masks. Three layers of natural silk was able to produce a level of filtration efficiency of 84.68%. Two-layered natural silk achieved 70.98%, cotton twill achieved 75.6%, and satin-weave viscose achieved 69.77%. Further options can also be considered in cases where lower filtration is acceptable It was statistically shown that applying a second layer was more significant in terms of overall filtering than increasing the layer count to three. However, layer stacking limited the breathability. The paper presents measurement-based qualitative and quantitative recommendations for future textile applications in face mask manufacturing.

Mathematical Modelling of Temperature Distribution in Selected Parts of FFF Printer during 3D Printing Process.

This work presented an FEM (finite element method) mathematical model that describes the temperature distribution in different parts of a 3D printer based on additive manufacturing process using filament extrusion during its operation. Variation in properties also originate from inconsistent choices of process parameters employed by individual manufacturers. Therefore, a mathematical model that calculates temperature changes in the filament (and the resulting print) during an FFF (fused filament fabrication) process was deemed useful, as it can estimate otherwise immeasurable properties (such as the internal temperature of the filament during the printing). Two variants of the model (both static and dynamic) were presented in this work. They can provide the user with the material's thermal history during the print. Such knowledge may be used in further analyses of the resulting prints. Thanks to the dynamic model, the cooling of the material on the printing bed can be traced for various printing speeds. Both variants simulate the printing of a PLA (Polylactic acid) filament with the nozzle temperature of 220 °C, bed temperature of 60 °C, and printing speed of 5, 10, and 15 m/s, respectively.

Influence of Flux and Related Factors on Intermetallic Layer Growth within SAC305 Solder Joints.

Flux contained in solder paste significantly affects the process of solder joint creation during reflow soldering, including the creation of an intermetallic layer (IML). This work investigates the dependence of intermetallic layer thickness on ROL0/ROL1 flux classification, glossy or matt solder mask, and OSP/HASL/ENIG soldering pad surface finish. Two original SAC305 solder pastes differing only in the used flux were chosen for the experiment. The influence of multiple reflows was also observed. The intermetallic layer thicknesses were obtained by the image analysis of micro-section images. The flux type proved to have a significant impact on the intermetallic layer thickness. The solder paste with ROL1 caused an increase in IML thickness by up to 40% in comparison to an identical paste with ROL0 flux. Furthermore, doubling the roughness of the solder mask has increased the resulting IML thickness by 37% at HASL surface finish and by an average of 22%.

Investigation of Impacts on Printed Circuit Board Laminated Composites Caused by Surface Finish Application.

The purpose of this study was to compare the strength of the bond between resin and glass cloth for various composites (laminates) and its dependence on utilized soldering pad surface finishes. Moreover, the impact of surface finish application on the thermomechanical properties of the composites was evaluated. Three different laminates with various thermal endurances were included in the study. Soldering pads were covered with OSP and HASL surface finishes. The strength of the cohesion of the resin upper layer was examined utilizing a newly established method designed for pulling tests. Experiments studying the bond strength were performed at a selection of laminate temperatures. Changes in thermomechanical behavior were observed by thermomechanical and dynamic mechanical analyses. The results confirmed the influence of the type of laminate and used surface finish on bond strength. In particular, permanent polymer degradation caused by thermal shock during HASL application was observed in the least thermally resistant laminate. A response to thermal shock was detected in thermomechanical properties of other laminates as well, but it does not seem to be permanent.

Copolymer chain formation of 2-oxazolines by in situ 1H-NMR spectroscopy: dependence of sequential composition on substituent structure and monomer ratios.

In situ 1H NMR characterization of copolymerization reactions of various 2-oxazoline monomers at different molar ratios offers detailed insight into the build-up and composition of the polymer chains. Various 2-oxazolines were copolymerized in one single solvent, butyronitrile, with 2-dec-9'-enyl-2-oxazoline, where the double bond allows for post-polymerization modification and can function as a crosslinking unit to form polymer networks. The types of the monomers and their molar ratios in the feed have a strong effect on the microstructure of the forming copolymer chains. Copolymers comprising 2-dec-9'-enyl-2-oxazoline and either 2-ethyl-, 2-isopropyl-, 2-butyl-, 2-heptyl, 2-nonyl- or 2-phenyl-2-oxazoline, show significant differences in sequential structure of copolymers ranging from block to gradient and random ordering of the monomer units. 1H NMR was found to be a powerful tool to uncover detailed oxazoline copolymerization kinetics and evolution of chain composition.

Investigation of the Mechanical Properties of Mn-Alloyed Tin-Silver-Copper Solder Solidified with Different Cooling Rates.

Manganese can be an optimal alloying addition in lead-free SAC (SnAgCu) solder alloys because of its low price and harmless nature. In this research, the mechanical properties of the novel SAC0307 (Sn/Ag0.3/Cu0.7) alloyed with 0.7 wt.% Mn (designated as SAC0307-Mn07) and those of the traditionally used SAC305 (Sn96.5/Ag3/Cu0.5) solder alloys were investigated by analyzing the shear force and Vickers hardness of reflowed solder balls. During the preparation of the reflowed solder balls, different cooling rates were used in the range from 2.7 K/s to 14.7 K/s. After measuring the shear force and the Vickers hardness, the structures of the fracture surfaces and the intermetallic layer were investigated by SEM (Scanning Electron Microscopy). The mechanical property measurements showed lower shear force for the SAC0307-Mn07 alloy (20-25 N) compared with the SAC305 alloy (27-35 N), independent of the cooling rate. However, the SAC0307-Mn07 alloy was softer; its Vickers hardness was between 12 and 13 HV, whereas the Vickers hardness of the SAC305 alloy was between 19 and 20 HV. In addition, structural analyses revealed rougher intermetallic compound layers in the case of the SAC0307-Mn07 alloy, which can inhibit the propagation of cracks at the solder-substrate interface. These two properties of SAC0307-Mn07 alloy, the softer nature and the rougher intermetallic layer, might result in better thermomechanical behavior of the solder joints during the lifetime of electronic devices.

Volume Phase Transition in Gels: Its Discovery and Development.

 The history of volume phase transition of responsive gels from its theoretical prediction to experimental discovery was described and the major role of mixing Gibbs energy function in theoretical models was stressed. For detailed analysis and fine tuning of the volume phase transition, the generalized Flory-Huggins model with concentration and temperature dependent interaction function coupled with Maxwell construction as a tool is very suitable. Application of expansive stresses can uncover the potential of various swelling gels for volume phase transition. Experimentally, the abrupt, equilibrium-controlled phase transition is often hard to achieve due to passage of gel through states of mechanical instability and slow relaxation processes in macroscopic objects.

Effect of Recrystallization on ß to α-Sn Allotropic Transition in 99.3Sn-0.7Cu wt. % Solder Alloy Inoculated with InSb.

The effect of recrystallization of 99.3Sn-0.7Cu wt. % solder alloy on the allotropic transition of ß to α-Sn (so-called tin pest phenomenon) was investigated. Bulk samples were prepared, and an InSb inoculator was mechanically applied to their surfaces to enhance the transition. Half of the samples were used as the reference material and the other half were annealed at 180 °C for 72 h, which caused the recrystallization of the alloy. The samples were stored at -10 and -20 °C. The ß-Sn to α-Sn transition was monitored using electrical resistance measurements. The expansion and separation of the tin grains during the ß-Sn to α-Sn transition process were studied using scanning electron microscopy. The recrystallization of the alloy suppressed the tin pest phenomenon considerably since it decreased the number of defects in the crystal structure where heterogeneous nucleation of ß-Sn to α-Sn transition could occur. In the case of InSb inoculation, the spreading of the transition towards the bulk was as fast as the spreading parallel to the surface of the sample.

Effect of Cu Substrate Roughness and Sn Layer Thickness on Whisker Development from Sn Thin-Films.

The effect of copper substrate roughness and tin layer thickness were investigated on whisker development in the case of Sn thin-films. Sn was vacuum-evaporated onto both unpolished and mechanically polished Cu substrates with 1 µm and 2 µm average layer thicknesses. The samples were stored in room conditions for 60 days. The considerable stress-developed by the rapid intermetallic layer formation-resulted in intensive whisker formation, even in some days after the layer deposition. The developed whiskers and the layer structure underneath them were investigated with both scanning electron microscopy and ion microscopy. The Sn thin-film deposited onto unpolished Cu substrate produced less but longer whiskers than that deposited onto polished Cu substrate. This phenomenon might be explained by the dependence of IML formation on the surface roughness of substrates. The formation of IML wedges is more likely on rougher Cu substrates than on polished ones. Furthermore, it was found that with the decrease of layer thickness, the development of nodule type whiskers increases due to the easier diffusion of other atoms into the whisker bodies.

How to Force Polymer Gels to Show Volume Phase Transitions.

Relatively few polymer gels are known to show volume phase transition where the gels undergo an abrupt change in the degree of swelling by passing through a three-phase equilibrium. Characteristic for such transition is the existence of van der Waals (vdW) loop on the dependence of solvent chemical potential versus polymer concentration. For the χ-induced transition, the existence of vdW loop is determined by the concentration dependence of the interaction function. It is shown that expansive mechanical strains can assist in development of the vdW loop. Systems characterized by continuous change of the degree of swelling transform upon such strain into ones where the degree of swelling changes much and abruptly. Also, expansive modes of strain can make the transition wider and more robust in gels where transition is already observed under free swelling condition. The possibility to induce the volume phase transition by external stresses can be utilized for finding other stimuli sensitive gels, strengthening of gel response, and in modeling of properties of gel constructs by Finite Element Method.

Influence of Manufacturing Mechanical and Thermal Histories on Dimensional Stabilities of FR4 Laminate and FR4/Cu-Plated Holes.

Irreversible dimension changes of an FR4 laminate board in the z-direction and FR4 laminate/Cu plated holes that depend on their manufacturing histories have been studied by thermal mechanical analysis in the temperature range from room temperature to 240 °C. It is found that the compression residual stresses generated in both materials due to manufacturing pressing are released during heating, leading to an elongation in the specified direction. This increase depends on the composition of the studied composite and number of pressing cycles. The second reason for the observed dimensional changes is insufficient curing during manufacture that causes post-curing after the first heating cycle and related board shrinkage in the z-direction. The temperature regions of these two processes are not the same. The post-curing process occurs in the transition temperature range (near the glass transition temperature), whereas the release of the compression residual stress is observed at higher temperatures. Both these processes are temperature-dependent and do not proceed to completion during one heating cycle. Moreover, the compression residual stress strongly influences the post-curing process.

Surface Area Evaluation of Electrically Conductive Polymer-Based Textiles.

In this paper, the surface area of coated polymer-based textiles, i.e., copper and nickel plated woven polyester fabric, copper and acrylic coated woven polyester fabric, and copper and acrylic coated non-woven polyamide fabric, is investigated. In order to evaluate the surface area of the woven fabrics, Peirce's geometrical model of the interlacing point and measurement using an electron microscope are used. Non-woven fabrics are evaluated using an optical method, handmade method, and MATLAB functions. An electrochemical method, based on the measurement of the resistance between two electrodes, is used for relative comparison of the effective surface area of the coated woven and non-woven fabrics. The experimental results show that the measured and calculated warp lengths do not differ within the standard deviation. The model for the surface area evaluation of the Pierce's geometrical model for monofilament (non-fibrous) yarns is extended to multifilament yarns and to a uniform sample size. The experimental results show the increasing trend of surface area evaluation using both modeling and electrochemical methods, i.e., the surface area of the copper and acrylic coated woven Polyester fabric (PES) is the smallest surface area of investigated samples, followed by the surface area of the copper and acrylic coated non-woven fabric, and by copper and nickel plated woven PES fabric. These methods can be used for surface area evaluation of coated polymer-based textiles in the development of supercapacitors, electrochemical cells, or electrochemical catalysts.

Arbuscular mycorrhiza differentially affects synthesis of essential oils in coriander and dill.

Research on the role of arbuscular mycorrhizal fungi (AMF) in the synthesis of essential oils (EOs) by aromatic plants has seldom been conducted in field-relevant conditions, and then, only limited spectra of EO constituents have been analyzed. The effect was investigated of inoculation with AMF on the synthesis of a wide range of EO in two aromatic species, coriander (Coriandrum sativum) and dill (Anethum graveolens), in a garden experiment under outdoor conditions. Plants were grown in 4-l pots filled with soil, which was either γ-irradiated (eliminating native AMF) or left non-sterile (containing native AMF), and inoculated or not with an isolate of Rhizophagus irregularis. AMF inoculation significantly stimulated EO synthesis in both plant species. EO synthesis (total EO and several individual constituents) was increased in dill in all mycorrhizal treatments (containing native and/or inoculated AMF) compared to non-mycorrhizal plants. In contrast, EO concentrations in coriander (total EO and most constituents) were increased only in the treatment combining both inoculated and native AMF. A clear positive effect of AMF on EO synthesis was found for both aromatic plants, which was, however, specific for each plant species and modified by the pool of AMF present in the soil.

Coiled-Coil Hydrogels. Effect of Grafted Copolymer Composition and Cyclization on Gelation.

A mean-field theoretical approach was developed to model gelation of solutions of hydrophilic polymers with grafted peptide motifs capable of forming associates of coiled-coil type. The model addresses the competition between associates engaged in branching and cyclization. It results in relative concentrations of intra- and intermolecular associates in dependence on associate strength and motif concentration. The cyclization probability is derived from the model of equivalent Gaussian chain and takes into account all possible paths connecting the interacting motifs. Examination of the association-dissociation equilibria, controlled by the equilibrium constant for association taken as input information, determines the fractions of inter- and intramolecularly associated motifs. The gelation model is based on the statistical theory of branching processes and in combination with the cyclization model predicts the critical concentration delimiting the regions of gelled and liquid states of the system. A comparison between predictions of the model and experimental data available for aqueous solutions of poly[N-(2-hydroxypropyl)methacrylamide] grafted with oppositely charged pentaheptad peptides, CCE and CCK, indicates that the association constant of grafted motifs by four orders of magnitude lower than that of free motifs. It is predicted that at the critical concentration of each motif of about 6×10(-7) mol/cm(3), about half of motifs in associated state is engaged in intramolecular bonds.

Synthesis and characterization of novel aromatic azo bond-containing pH-sensitive and hydrolytically cleavable IPN hydrogels.

Novel interpenetrating network (IPN) hydrogels, composed of pH-sensitive, aromatic azo group containing network as one component (Network A), and a hydrolyzable network as the other (Network B), were prepared by a sequential process. The first network was formed by crosslinking of a reactive polymer precursor (copolymer of N,N-dimethylacrylamide, acrylic acid, N-tert.butylacrylamide, and N-methacryloylglycylglycine p-nitrophenyl ester) with an aromatic azo group containing diamine ((N,N'-epsilon-aminocaproyl)-4,4'-diaminoazobenzene). The second network was formed by radical crosslinking copolymerization of N-(2-hydroxypropyl)methacrylamide with N,O-dimethacryloylhydroxylamine. The composition of the hydrogels was manipulated to determine the influence of hydrogel composition on the equilibrium degree of swelling, modulus of elasticity in compression, and on the rate of degradation of Network B. Modeling of network structure was accomplished using the statistical branching theory. The major advantage of IPN hydrogels, when compared to traditional pH-sensitive networks, is the linear swelling profile following abrupt change of pH from 2 to 7.4. This indicates the suitability of IPN as carriers for oral drug delivery.

Swelling pressure induced phase-volume transition in hybrid biopolymer gels caused by unfolding of folded crosslinks: a model.

A thermodynamic model is proposed describing swelling changes and swelling transitions of hybrid gels in which domains of folded chains are chemically built in as cross-links. These folded domains can be unfolded to random coils by osmotic forces produced by the synthetic gel matrix. Uncoiling takes place if the osmotic force acting on the cross-links exceeds the critical value. By unfolding, a new interacting surface is exposed to interactions and affects the swelling pressure. The chains of the folded domains may have ionized groups. The model is based on mean-field statistical-thermodynamic treatment of swelling of polyelectrolyte gels with finite extensibility of network chains. This study is related to hybrid hydrogels with built in protein motifs. A continuous change in external variables increasing the degree of swelling of the hydrogel brings about an abrupt increase in volume (transition) of the gel. The position and magnitude of the transition depend on structural parameters of the hybrid gel, such as fraction of the folded domains in the gel, degree of ionization of chains in the domain, presence of additional chemical cross-links, or degree of dilution at gel formation. Two options for reversibility of the changes are considered: (a) unfolding is irreversible and deswelling proceeds along other curve than swelling and (b) swelling is reversible when the osmotic force decrease below the critical value. In the latter case, swelling changes are described by a closed loop with two transitions. Under certain conditions (high dilution at network formation and sufficiently high degree of ionization of chains of the folded domains), a transition appears known as the collapse transition induced by balance of hydrophobic and hydrophillic interactions. This collapse transition induces the folding transition by which the folded domains are reformed.

Structure and properties of triolein-based polyurethane networks.

Polyurethane networks based on vegetable oils have very heterogeneous composition, and it is difficult to find a close correlation between their structure and properties. To establish benchmark structure-properties relationships, we have prepared model polyurethane networks based on triolein and 4,4'-diphenylmethane diisocyanate (MDI). Cross-linking in the middle of fatty acid chains leaves significant parts of the triglyceride as dangling chains. To examine their effect on properties, we have synthesized another polyurethane network using triolein without dangling chains (removed by metathesis). The structure of polyols was studied in detail since it affects the structure of polyurethane networks. The network structure was analyzed from swelling and mechanical measurements and by applying network and rubber elasticity theories. The cross-linking density in both networks was found to be close to theoretical. The triolein-based model network displayed modulus (around 6 MPa), tensile strength (8.7 MPa), and elongation at break (136%), characteristic of hard rubbers. Glass transition temperatures of the networks from triolein and its metathesis analogue were 25 and 31.5 degrees C, respectively.