Jitrin Chaiprapa

This paper elucidates the mechanical performance, microstructure, and porosity evolution of fly ash geopolymer after 10 years of curing age. Given their wide range of applications, understanding the microstructure of geopolymers is critical for their long-term use. The outcome of fly ash geopolymer on mechanical performance and microstructural characteristics was compared between 28 days of curing (FA28D) and after 10 years of curing age (FA10Y) at similar mixing designs. The results of this work reveal that the FA10Y has a beneficial effect on strength development and denser microstructure compared to FA28D. The total porosity of FA10Y was also lower than FA28D due to the anorthite formation resulting in the compacted matrix. After 10 years of curing age, the 3D pore distribution showed a considerable decrease in the range of 5–30 µm with the formation of isolated and intergranular holes.

Geopolymer materials are used as construction materials due to their lower carbon dioxide (CO₂) emissions compared with conventional cementitious materials. An example of a geopolymer material is alkali-activated kaolin, which is a viable alternative for producing high-strength ceramics. Producing high-performing kaolin ceramics using the conventional method requires a high processing temperature (over 1200 °C). However, properties such as pore size and distribution are affected at high sintering temperatures. Therefore, knowledge regarding the sintering process and related pore structures on alkali-activated kaolin geopolymer ceramic is crucial for optimizing the properties of the aforementioned materials. Pore size was analyzed using neutron tomography, while pore distribution was observed using synchrotron micro-XRF. This study elucidated the pore structure of alkali-activated kaolin at various sintering temperatures. The experiments showed the presence of open pores and closed pores in alkali-activated kaolin geopolymer ceramic samples. The distributions of the main elements within the geopolymer ceramic edifice were found with Si and Al maps, allowing for the identification of the kaolin geopolymer. The results also confirmed that increasing the sintering temperature to 1100 °C resulted in the alkali-activated kaolin geopolymer ceramic samples having large pores, with an average size of ~80 µm³ and a layered porosity distribution.

This manuscript reports the isothermal annealing effect on the mechanical and microstructure characteristics of Sn-0.7Cu-1.5Bi solder joints. A detailed microstructure observation was carried out, including measuring the activation energy of the intermetallic compound (IMC) layer of the solder joints. Additionally, the synchrotron µX-ray fluorescence (XRF) method was adopted to precisely explore the elemental distribution in the joints. Results indicated that the Cu₆Sn₅ and Cu3Sn intermetallic layers thickness at the solder/Cu interface rises with annealing time at a rate of 0.042 µm/h for Sn-0.7Cu and 0.037 µm/h for Sn-0.7Cu-1.5Bi. The IMC growth’s activation energy during annealing is 48.96 kJ mol-1 for Sn-0.7Cu, while adding Bi into Sn-0.7Cu solder increased the activation energy to 55.76 kJ mol⁻¹. The µ-XRF shows a lower Cu concentration level in Sn-0.7Cu-1.5Bi, where the Bi element was well dispersed in the β-Sn area as a result of the solid solution mechanism. The shape of the IMC layer also reconstructs from a scallop shape to a planar shape after the annealing process. The Sn-0.7Cu hardness and shear strength increased significantly with 1.5 wt.% Bi addition in reflowed and after isothermal annealing conditions.

The investigation on tin (Sn) whiskers formation has been widely applied in the field of lead-free electronic packaging. This is due to the fact that use of the Sn–Pb finishes has converted to Pb-free finishes in the electronic industry. Sn whiskers can grow long enough to cause a short circuit, which affects electronic devices’ reliability. This study investigates Sn whiskers’ formation in the thin Sn–0.7Cu–0.05Ga Pb-free solder under the influence of electromigration and thermal ageing for surface finish applications. The samples were stored in ambient conditions for 1000 h before being exposed to electromigration and thermal ageing to study the corresponding whiskers’ growth. A scanning electron microscope (SEM) was used to study the Sn whiskers’ microstructure, while an optical microscope (OM) was utilized to investigate the IMC layers in the samples. The results show that the addition of 0.05 wt.% gallium (Ga) decreased the Sn whisker’s length and growth density while simultaneously refining the IMC layers. Synchrotron micro-XRF (µ-XRF) shows the existence and distribution of Ga addition in both electromigration and thermal ageing samples. The shear test was used to determine the solder alloys’ mechanical properties. As a result, the addition of Ga to the Sn–0.7Cu solder improved the fracture morphology of solder joints. In conclusion, Ga’s addition resulted in decreasing Sn whisker formation and refining of the IMCs while also increasing the shear strength of the Sn–0.7Cu solder by ~14%.

This paper clarified the microstructural element distribution and electrical conductivity changes of kaolin, fly ash, and slag geopolymer at 900 °C. The surface microstructure analysis showed the development in surface densification within the geopolymer when in contact with sintering temperature. It was found that the electrical conductivity was majorly influenced by the existence of the crystalline phase within the geopolymer sample. The highest electrical conductivity (8.3 × 10⁻⁴ Ωm⁻¹) was delivered by slag geopolymer due to the crystalline mineral of gehlenite (3Ca₂Al₂SiO₇). Using synchrotron radiation X-ray fluorescence, the high concentration Ca boundaries revealed the appearance of gehlenite crystallisation, which was believed to contribute to development of denser microstructure and electrical conductivity.

The primary motivation of developing ceramic materials using geopolymer method is to minimize the reliance on high sintering temperatures. The ultra-high molecular weight polyethylene (UHMWPE) was added as binder and reinforces the nepheline ceramics based geopolymer. The samples were sintered at 900 °C, 1000 °C, 1100 °C, and 1200 °C to elucidate the influence of sintering on the physical and microstructural properties. The results indicated that a maximum flexural strength of 92 MPa is attainable once the samples are used to be sintered at 1200 °C. It was also determined that the density, porosity, volumetric shrinkage, and water absorption of the samples also affected by the sintering due to the change of microstructure and crystallinity. The IR spectra reveal that the band at around 1400 cm⁻¹ becomes weak, indicating that sodium carbonate decomposed and began to react with the silica and alumina released from gels to form nepheline phases. The sintering process influence in the development of the final microstructure thus improving the properties of the ceramic materials.

The evolution of internal compressive stress from the intermetallic compound (IMC) Cu₆Sn₅ growth is commonly acknowledged as the key inducement initiating the nucleation and growth of tin (Sn) whisker. This study investigates the effect of Sn-0.7Cu-0.05Ni on the nucleation and growth of Sn whisker under continuous mechanical stress induced. The Sn-0.7Cu-0.05Ni solder joint has a noticeable effect of suppression by diminishing the susceptibility of nucleation and growth of Sn whisker. By using a synchrotron micro X-ray fluorescence (µ-XRF) spectroscopy, it was found that a small amount of Ni alters the microstructure of Cu₆Sn₅ to form a (Cu,Ni)₆Sn₅ intermetallic layer. The morphology structure of the (Cu,Ni)₆Sn₅ interfacial intermetallic layer and Sn whisker growth were investigated by scanning electron microscope (SEM) in secondary and backscattered electron imaging mode, which showed that there is a strong correlation between the formation of Sn whisker and the composition of solder alloy. The thickness of the (Cu,Ni)₆Sn₅ IMC interfacial layer was relatively thinner and more refined, with a continuous fine scallop-shaped IMC interfacial layer, and consequently enhanced a greater incubation period for the nucleation and growth of the Sn whisker. These verification outcomes proposes a scientifically foundation to mitigate Sn whisker growth in lead-free solder joint.

A geopolymer has been reckoned as a rising technology with huge potential for application across the globe. Dolomite refers to a material that can be used raw in producing geopolymers. Nevertheless, dolomite has slow strength development due to its low reactivity as a geopolymer. In this study, dolomite/fly ash (DFA) geopolymer composites were produced with dolomite, fly ash, sodium hydroxide, and liquid sodium silicate. A compression test was carried out on DFA geopolymers to determine the strength of the composite, while a synchrotron Micro-Xray Fluorescence (Micro-XRF) test was performed to assess the elemental distribution in the geopolymer composite. The temperature applied in this study generated promising properties of DFA geopolymers, especially in strength, which displayed increments up to 74.48 MPa as the optimum value. Heat seemed to enhance the strength development of DFA geopolymer composites. The elemental distribution analysis revealed exceptional outcomes for the composites, particularly exposure up to 400 °C, which signified the homogeneity of the DFA composites. Temperatures exceeding 400 °C accelerated the strength development, thus increasing the strength of the DFA composites. This appears to be unique because the strength of ordinary Portland Cement (OPC) and other geopolymers composed of other raw materials is typically either maintained or decreases due to increased heat.