Hot-stage Microscopy Research Articles

Depicting polymorphism in eutectic mixtures

The current investigation reveals the presence of polymorphism within linezolid eutectic mixtures containing syringic acid, fumaric acid, and isonicotinamide. Linezolid was combined with the said coformers through co-grinding in 1:1 stoichiometric ratios to produce binary mixtures. Through techniques such as differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), and Fourier transform infrared (FTIR) spectroscopy, the eutectic nature of these mixtures was confirmed. Polymorphism was identified further through the emergence of an exothermic event positioned between the two melting endotherms in DSC thermograms. This endo-exo-endo transition signifies the thermally-induced polymorphic transformation occurring within the eutectic mixtures. The observed behavior was validated through real-time visual analysis using hot-stage microscopy analysis (HSM). Utilizing PXRD data, quantitative phase analysis (QPA) was employed to determine the weight fractions of individual components in various eutectic polymorphs, yielding reliable outcomes. The morphological characteristics and surface alterations of eutectic polymorphs were scrutinized via scanning electron microscopy (SEM). Moreover, eutectic polymorphs formed by the combination of linezolid and isonicotinamide demonstrated fivefold increase in aqueous solubility and a fourfold faster intrinsic dissolution rate (IDR) compared to marketed linezolid.

Impact of Polymers on the Kinetics of the Solid-State Phase Transition of Piracetam Polymorphs.

Metastable polymorphs of active pharmaceutical ingredients can occasionally be used to enhance bioavailability or make processing more convenient. However, the thermodynamic instability of metastable polymorphs poses a severe threat to the quality and performance of the drug products. In this study, we used hot-stage microscopy and powder X-ray diffraction to quantitatively analyze the kinetics of the solid-solid phase transition of piracetam (PCM) polymorphs in the absence and presence of several polymeric excipients. The Forms I and II of PCM are enantiotropically related polymorphs, and the transition point is 75 °C. We found that 1 wt % polymer can strongly affect the transformation rate of Form II to Form I of PCM above 75 °C. PVP K30 has the highest Tg and the strongest inhibitory effect on the transition, whereas PEG has the lowest Tg and the weakest effect on the transition. Below 75 °C, the addition of 1 wt % PEG can decrease the transformation rate from Form I to Form II of PCM by a few orders of magnitude, whereas no phase transition occurs in the presence of the other investigated polymers. The inhibitory effects of the same concentration of polymers on the kinetics of the solid-solid phase transition of piracetam polymorphs are considerably greater than those on the crystallization of PCM from the amorphous phase, especially at low temperatures. We propose that the low segmental mobility of polymers enriched between the crystalline phases can considerably inhibit the nucleation and growth of the stable form at the interface during the phase transition. Our findings deepen the current understanding of the mechanisms underlying the solid-state phase transition of polymorphic drugs in the presence of polymeric excipients, providing a promising formulation approach for stabilizing the metastable pharmaceutical polymorphs.

Investigation of the effect of ferroelectric polarization on the spin state of spin crossover complexes embedded in a piezopolymer matrix

Recent experiments indicate that the spin state of molecules adjacent to ferroelectric layers depends on the magnitude and direction of the polarization. Since similar effects could arise in nanocomposites, we synthesized samples with spin crossover particles embedded in a ferroelectric polymer. The spin transition phenomenon in the poled and non-poled composites was investigated by hot-stage optical microscopy and calorimetry, but no sizeable effect of the poling on the spin-state equilibrium was detected. On the other hand, subtle matrix effects on the spin crossover properties and a rather unusual sensitivity of the spin transition on thermal annealing was detected.

ABOUT THE SINTERING OF HISTORICAL “YELLOW BRICKS” OF SOFIA

The historical “yellow cobblestones” of Sofia are a very well sintered ceramic clinker with practically zero water absorption. However, the high amount of crystal phase formed, which explains the extraordinary mechanical properties of this remarkable material, is in formal contradiction with its low final porosity. In fact, in the modern ceramics clinkers the crystallinity is similar or inferior, but the reached degree of sintering is lower; as a result, the mechanical properties are reduced. The aim of this report is to elucidate some peculiarities of the densification process of “yellow ceramics bricks” because such information is essential for the eventual successful production of replica of this emblematic pavement. The chemical and phase compositions of original “yellow paving bricks” together with those of modern clinker from “Vitosha” boulevard in Sofia were evaluated by XRF and XRD analysis, respectively. The structures of both ceramics were investigated with density measurements and SEM.Their densification behaviour was estimated by re-sintering of milled original samples by Hot Stage Microscopy (HSM) tests. The results elucidate that the sintering temperature of the historical clinker is inferior, and their sintering interval is significantly narrow. This peculiarity is explained by the rapid decreasing of apparent viscosity with temperature rise.Finally, by secondary holding at the sintering temperatures and subsequent fast quenching of a “yellow brick” sample, it is demonstrated that some phase formation occurred during the industrial cooling step. This result explains both the good degree of densification and the better properties of the “yellow cobblestones”.

CHARACTERIZATION OF CLAYS FROM “MINES MARITSA IZTOK” AS RAW MATERIALS FOR CERAMIC INDUSTRY

The chemical and phase compositions of the clays from coal mining were evaluated by XRF and powder XRD method, respectively. Hot Stage Microscope was used to estimate the thermal behaviour. In addition, the thermal losses of the clays after 1 h thermal treatment at different temperatures were measured. This preliminary analysis elucidates potential prospects for using some of clays as raw materials for ceramic industry. It seems that samples which are montmorillonite type are more plastic, while the others, where higher sand content is observed, and the drying shrinkage is negligible could be characterized as less plastic. The initial results for the thermal behaviour and the structure of a brick sample (obtained by mixing two types of clays) and a foamed geopolymer are also reported. The first sample shows a beginning of the firing shrinkage at about 1000°C, while the second demonstrates intensive bloating after 950°C, leading to specimen with about 56 % closed porosity. Finally, X - ray Computed Tomography and SEM was used to highlight the structure of some test samples.

OBTAINING OF GARNET CERAMIC MATERIALS BY UTILIZATION OF RICE HUSK ASH AS SILICA SOURCE

The current research aims at the obtaining of new type pigments from the garnet mineral group by utilizationof rice husk ash as silica source (RHA). At the beginning, the mixtures prepared from the starting raw materials areground in a ball mill and then subjected to high temperature treatment. Green pigments were synthesized at twotemperatures: 1000°C and 1100°C. Using the tintometer RT 100 Lovibond the colour characteristics were measuredspectrophotometrically. The rice husk ash was investigated using scanning electron microscopy. The conducted hot-stage microscopic studies show that the pigments remain thermally stable when heated. The highest fire resistance - upto temperatures of 1380°C - 1400°C show the uvarovite pigments with main phase 3CaO.Cr2O3.3SiO2 or by a generalformula Ca3Cr2[SiO4 ]3. They are suitable for inserting into ceramic glazes without danger of decomposition or reaction.Keywords: ceramic pigments, SEM, colour determination, Hot-stage microscopy.

Stabilizer Effects on the Gelation of Modified Recycled PET for 3D Printing Filament Application

This research identification gel types of the modified-recycled poly (ethylene terephthalate) (modified-rPET) filament, with and without the addition of heat stabilizer Pentaerythritol tetrakis(3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate (Irganox®1010). This research also identifies the gel types and studies thermal behavior of the modified-rPET filaments above, by using a hot-stage microscopy, and a differential scanning calorimetry, respectively. rPET flakes were dried to deplete the moisture. Then, they were mixed with additives and heat stabilizer (Irganox®1010) at 0 and 0.5 pph, Then, they were extruded to be compound using twin screw extruder. The compounds were extruded into filament by using filament extruder. The two temperature profiles were used. The first and the second temperature profiles from the feed zone to the die zone were 275-275-275 oC and 290-290-290 oC, respectively. The extrudate of modified-rPET with and without heat stabilizer, were investigated the type of gel and the thermal behavior of the modified-rPET filament. From this preliminary experiment, it was found that the “unmelt-gel” defect was found from the modified-rPET filament, without the addition of Irganox®1010. On the other hand, the “crosslinked gel” defect was found from the modified-rPET filament, with the addition of Irganox®1010. Therefore, the addition of heat stabilizer (Irganox®1010) may cause the “crosslinked gel” significantly. Our future work, we will investigate the effect of another stabilizer and chain extenders on the gelation behavior, to complete this clarification systematically.

Comprehensive Advanced Physicochemical Characterization and In Vitro Human Cell Culture Assessment of BMS-202: A Novel Inhibitor of Programmed Cell Death Ligand.

Background/Objectives: BMS-202, is a potent small molecule with demonstrated antitumor activity. The study aimed to comprehensively characterize the physical and chemical properties of BMS-202 and evaluate its suitability for topical formulation, focusing on uniformity, stability and safety profiles. Methods: A range of analytical techniques were employed to characterize BMS-202. Scanning Electron Microscopy (SEM) was used to assess morphology, Differential Scanning Calorimetry (DSC) provided insights of thermal behavior, and Hot-Stage Microscopy (HSM) corroborated these thermal behaviors. Molecular fingerprinting was conducted using Raman spectroscopy and Fourier Transform Infrared (FTIR) spectroscopy, with chemical uniformity of the batch further validated by mapping through FTIR and Raman microscopies. The residual water content was measured using Karl Fisher Coulometric titration, and vapor sorption isotherms examined moisture uptake across varying relative humidity levels. In vitro safety assessments involved testing with skin epithelial cell lines, such as HaCaT and NHEK, and Transepithelial Electrical Resistance (TEER) to evaluate barrier integrity. Results: SEM revealed a distinctive needle-like morphology, while DSC indicated a sharp melting point at 110.90 ± 0.54 ℃ with a high enthalpy of 84.41 ± 0.38 J/g. HSM confirmed the crystalline-to-amorphous transition at the melting point. Raman and FTIR spectroscopy, alongside chemical imaging, confirmed chemical uniformity as well as validated the batch consistency. A residual water content of 2.76 ± 1.37 % (w/w) and minimal moisture uptake across relative humidity levels demonstrated its low hygroscopicity and suitability for topical formulations. Cytotoxicity testing showed dose-dependent reduction in skin epithelial cell viability at high concentrations (100 µM and 500 µM), with lower doses (0.1 µM to 10 µM) demonstrating acceptable safety. TEER studies indicated that BMS-202 does not disrupt the HaCaT cell barrier function. Conclusions: The findings from this study establish that BMS-202 has promising physicochemical and in vitro characteristics at therapeutic concentrations for topical applications, providing a foundation for future formulation development focused on skin-related cancers or localized immune modulation.

Leveraging solid solubility and miscibility of etoricoxib in Soluplus® towards manufacturing of 3D printed etoricoxib tablets by additive manufacturing

This research focuses on exploring the solid solubility and miscibility of Etoricoxib, a poorly water-soluble anti-inflammatory drug, within Soluplus®, a polymer used as a matrix for 3D-printed tablets. By utilizing hot-melt extrusion (HME), the drug was dispersed within Soluplus® to enhance its solubility. The extrudates were then employed in 3D printing to create customized solid oral dosage form. This study’s novelty lies in combining HME and 3D printing, aiming to improve drug incorporation, stability, and effectiveness in the final formulation. Comprehensive characterization techniques, including hot stage microscopy (HSM), scanning electron microscopy (SEM), micro-computed tomography (Micro-CT), florescence microscopy, optical microscopy, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), solubility studies, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and aqueous solubility study were utilized to elucidate the physicochemical properties, thermal stability, and structural integrity for the extruded filaments (the printing ink), and 3D printed tablets made thereof. Furthermore, the in vitro drug release profile of the 3D printed tablet was systematically evaluated, revealing a controlled drug release pattern from the finished dosage form. The systematic investigation reported herein, starting from theoretical miscibility to the printing ink development through HME, detailed characterization of the extruded filaments, and further solid oral formulation development by additive manufacturing can be utilized as a platform technology or a pathway for the development of personalized medicine with drugs having similar physicochemical properties.

Thermo‐rheological snapshot of melter feed conversion to glass

AbstractSlurry feed charged into an electric melter creates a layer of reacting and melting material (termed cold cap) that floats on the surface of molten glass. The rheological behavior of heated melter feed affects the spreading of slurry at the top of the cold cap and the stability of the primary foam, affecting cold‐cap coverage and melter plenum temperatures. The apparent viscosity of a high‐alumina high‐level waste melter feed was assessed by thermomechanical analysis, high‐temperature viscometer, and the hot stage microscopy method, yielding viscosity estimates from ≈107.5 Pa s at 550°C to ≈102.5 Pa s at 1050°C. As the temperature of feed materials increased, their state changed from rigid solid to dilatant fluid, to pseudoplastic bubbly liquid with dissolving solids, to fully developed foam, and finally to Newtonian glass melt.

A zero-carbon emission approach for the reduction of refractory iron ores: Mineral phase, magnetic property and surface transformation in hydrogen system

In this study, a feasible strategy, named hydrogen mineral phase transformation (HMPT) technology, is proposed and employed to achieve efficient and clean recovery of Hainan Shilu refractory iron ore (HSRIO). The influences of HMPT roasting temperature, roasting time, and H2 concentration on the separation index of HSRIO are investigated. Under the optimal experimental conditions, the iron concentrate grade increases from 62.5% to 67.9%, and the iron recovery increases from 65.0% to 94.7% compared with the original beneficiation process. In addition, the evolution of mineral phases, magnetic properties, and mineral microstructures is analyzed using XRD, VSM, SEM, and high-temperature hot-stage microscopy. It is revealed that the transformation of hematite to magnetite occurs during the HMPT process, with the newly formed magnetite exhibiting a loose and porous reticulation structure. This study is of guiding significance for the development of Hainan Shilu refractory iron ore with high efficiency and zero-carbon emission.

Impact of polymer molecular weight and dispersity on the coalescence of polypropylene powders suitable for laser powder bed fusion

Understanding and controlling the fundamental processes governing the coalescence of polymers is vital to enable the design of polymeric materials for improved mechanical performance and quality of manufactured structures, including those fabricated via additive manufacturing techniques. Our group has utilized thermally induced phase separation (TIPS) to produce spherical and size controlled polypropylene (PP) powders from 12,000 (12k), 250,000 (250k), and 340,000 (340k) molecular weight (Mw) PP, including 50-50 wt% blends of 12k/250k,12k/340k, and 250k/340k, and a 33-33-33 wt% blend of 12k/250k/340k to investigate the impact of polymer Mw, and thus zero-shear viscosity, on particle coalescence and its implication in laser powder bed fusion. The particles exhibit similar size distributions with an average particle size, Dx(50), in the range of 58 μm–86 μm. The coalescence behavior of the powders, evaluated via hot-stage microscopy, show that adding 12k PP in the blend significantly alters the coalescence dynamics of the 250k and 340k PP, dramatically increasing their coalescence rate. The substantial drop in zero-shear viscosity with addition of 12k PP provides the driving force for the pronounced enhancement in coalescence. Strong agreement between experimental results and the Hopper model of coalescence is observed only if corrected for extensional flow, exemplifying the importance of extensional flow on the coalescence process. The results also indicate that the 12k PP in the blend does not surface segregate in the TIPS process, but is homogeneously distributed in the blend. More broadly, these results provide molecular-level insight into how control of powder molecular weight characteristics and viscosity can offer pathways to optimize the consolidation of particles in manufacturing processes, including laser powder bed fusion.

Effect of sintering behavior and phase evolution on glass-ceramics entirely derived from ferrochrome slag and fluorite tailings

The recycling of solid waste is widely regarded as the one of the most crucial issues of sustainability. This is particularly evident in the industrial sector, where the production of slags is huge and their handling presents a significant challenge. In this study, solid wastes from the industrial sector, namely ferrochrome slag (Fs) and fluorite tailings (Ft), were employed for the preparation of glass-ceramics by the sintering method. Three glasses were prepared by using the melt-quenching method, with a weight ratio of 60∼70 % Fs and 40∼30 % Ft (designated S30, S35, and S40, where the higher number indicates a greater Fs content). The sintering and crystallization behaviors of these glasses were characterized by hot-stage microscopy (HSM) and differential thermal analysis (DTA). It was observed that S40 glass exhibited a weak sintering capacity in comparison to that of S30 and S35 glass, which can be attributed to the robust crystallization propensity of S40 glass. The coarser glass frits were subjected to sintering experiments at varying temperatures, which demonstrates that the predominant crystalline phase is augite and that Cr2O3 remains present in all sintered samples. Besides, a transition of the Cr2O3 crystal into uvarovite was observed in S40 glass sintered at 1050 °C. The sintering time controlling experiment demonstrated that both wollastonite and the Ca-rich flow formed during sintering are vital for the formation of uvarovite. The formation of uvarovite can enhance the hardness of GCs. All GCs samples sintered at 1050 °C and 1120 °C exhibit comparable mechanical performance.

Solid–Liquid Phase Equilibrium of the n-Nonane + n-Undecane System for Low-Temperature Thermal Energy Storage

The current article presents an exploration of the solid–liquid phase diagram for a binary system comprising n-alkanes with an odd number of carbon atoms, specifically n-nonane (n-C9) and n-undecane (n-C11). This binary system exhibits promising characteristics for application as a phase change material (PCM) in low-temperature thermal energy storage (TES), due to the fusion temperatures of the individual components, thereby motivating an in-depth investigation of the solid–liquid phase diagram of their mixtures. The n-nonane (n-C9) + n-undecane (n-C11) solid–liquid phase equilibrium study herein reported includes the construction of the phase diagram using Differential Scanning Calorimetry (DSC) data, complemented with Hot–Stage Microscopy (HSM) and low-temperature Raman Spectroscopy results. From the DSC analysis, both the temperature and the enthalpy of solid–solid and solid–liquid transitions were obtained. The binary system n-C9 + n-C11 has evidenced a congruent melting solid solution at low temperatures. In particular, the blend with a molar composition xundecane = 0.10 shows to be a congruent melting solid solution with a melting point at 215.84 K and an enthalpy of fusion of 13.6 kJ·mol–1. For this reason, this system has confirmed the initial signs to be a candidate with good potential to be applied as a PCM in low-temperature TES applications. This work aims not only to contribute to gather information on the solid–liquid phase equilibrium on the system n-C9 + n-C11, which presently are not available in the literature, but especially to obtain essential and practical information on the possibility to use this system as PCM at low temperatures. The solid–liquid phase diagram of the system n-C9 + n-C11 is being published for the first time, as far as the authors are aware.

Thermogravimetric analysis and kinetic modeling for empty fruit bunch date palm pyrolysis

This study presents a comparative analysis of different kinetic models applied to the thermochemical pyrolysis of palm empty fruit bunch (PEFB). The kinetic parameters, particularly the activation energy, are determined through thermogravimetric analysis (TGA) of samples that underwent heating rates ranging from 10 to 50 °C/min. Image analysis of PEFB in a hot-stage microscope reveals an intriguing correlation between the observed shrinkage and the conversion rate (α) and indicates that significant physical and chemical transformations occurred within α between 0.2 and 0.8. The experimental data from TGA demonstrates good alignment with four distinct kinetic models. The Coast-Redfern model gives activation energies ranging from 60 to 134 kJ/mol for α between 0.2 and 0.8. In contrast, the Kissinger model and the isoconversion models, Kissinger-Akahira-Sunose and Ozawa-Flyn-Wall, show higher activation energy of 151, 156, and 157 kJ/mol, respectively. The findings underscore the significant impact of the selected kinetic model on determining kinetic parameters.

Possibilities of producing lightweight aggregates from silica-clay raw material and cellulosic waste

The subject of the work is the characterization of lightweight aggregates intended for construction using the example of silica-clay raw material from south-eastern Poland (Dylągówka-Zapady deposit). The primary objective of the research is to assess the possibility of managing the accumulated organic waste, including cellulose pulp. This storage is problematic for processing plants and local government bodies and incurs high costs annually. Therefore, based on the patent (Kukułka et al. Method of producing raw meal, dried clay granules, and fired clay granules and the production line of raw meal, dried clay granules, and baked clay granules. Patent RP no P.429284.), an attempt was made to confirm the assumptions of the technology of fired clay granules, which can be used for zootechnical, agricultural, and construction purposes. The presented work assessed the physicochemical transformations in the clay-silica raw material after adding a significant amount of cellulose waste (10%, 20%, and 30%) in the temperature range of 25–1300 °C were assessed. Thermal methods such as thermodilatometry, Hot-Stage Microscopy with image analysis (IA-HSM) and thermal DSC/TG analysis with gas analysis were used for this purpose. Based on the first method, a temperature range was established in which sintering occurs without an apparent effect of densification. Therefore, the range of 850–950 °C was used to obtain fired granules, which were tested as a material for lightweight aggregates.

Combining fast scanning chip calorimetry and nanoindentation: Young's modulus and hardness of poly (l-lactic acid) containing α′- and α-crystals

Fast scanning chip calorimetry (FSC) allows subjecting polymer melts to well-defined vitrification, crystal nucleation, and crystal growth pathways and, therefore, precise control of morphologies, from fully amorphous glassy states to semicrystalline structures containing perfect crystals. Due to the required use of nanogram-sized samples, needed to achieve high cooling rates, their mechanical properties, in order to establish structure-property relations, are difficult to assess. In this work, indentation modulus and indentation hardness of FSC samples are successfully determined on example of semicrystalline poly (ʟ-lactic acid) (PLLA) containing spherulitically grown disorder α′- or rather perfect α-crystals, with the correctness of the applied preparation and analyses routes confirmed by nanoindentation measurements on milligram-sized samples prepared through hotstage microscopy, and by applying both static single-step and quasi-continuous stiffness measurements. Modulus and hardness data are consistent with prior analyses of bulk samples, confirming that semicrystalline PLLA containing α-crystals exhibits around 10–20 % higher values of these properties compared to PLLA containing α′-crystals, related to the different molecular-chain packing in the crystal lattice. This work demonstrates that combination of FSC and nanoindentation techniques is an effective tool for determining mechanical properties of samples solidified at specific thermal pathways which otherwise cannot be realized.

Non-monotonic dependence of high-temperature stability of stone wool fibres on pre-oxidation time and temperature

Stone wool is a sustainable, fire-safe insulation material, and its fire-safety depends on its high-temperature stability (HTS). It is known that the HTS of stone wool fibres can be enhanced by pre-oxidation (i.e., heat treatment in air) at temperatures below or at its glass transition temperature (Tg). However, so far, a quantitative trend of HTS with varying pre-oxidation temperature (Tpre-ox) and time (tpre-ox) remains unknown. In this study, we quantified the change of HTS of stone wool fibres with a Tg of 677 °C as functions of both Tpre-ox and tpre-ox through a hot-stage microscope. The derived results revealed striking non-monotonic trends in the HTS of stone wool fibres. The HTS first increased with Tpre-ox from 500 to 630 °C for tpre-ox of 15 minutes, but declined beyond 630 °C. The HTS was significantly improved upon pre-oxidation for merely 2 minutes, at 677 °C, then dropped with extending tpre-ox to 16 hours, and finally increased again with tpre-ox up to 16 days. The origin of the non-monotonic trend was explored by characterizing the crystallization behaviour, thermal expansion, surface composition, and surface morphology in stone wool fibres after pre-oxidation.

Low-temperature synthesis of dense Si-based nitride ceramics for solar thermal storage: Role of cordierite as sintering additive

Direct nitridation method was used to prepare dense Si-based ceramics for solar thermal storage, and the effect of cordierite as sintering additive on the sintering behaviors of the ceramics was studied. The influence priority between densification and nitride content on the properties of thermal storage ceramics was discussed. Cordierite exhibited a good capability of promoting densification, and the densification temperature could reach 1500 °C. The liquid formed by cordierite helped to construct an interlocking structure of well-grown Si2N2O flakes. Results of hot stage microscopy and DTA indicated that the endothermic silicothermic reaction between Si and cordierite proceeded at 1440–1460 °C, and released SiO gas. The SiO gas inhibited the densification, but resulted in the low-temperature synthesis of nano-sized Si3N4 whiskers. Samples added with more cordierite showed the cost-effective merits as the smaller costs of raw materials, lower densification temperature, higher thermal conductivity (1.72 W m−1 K−1 deviation), and higher bending strength (34.3–68.1 MPa deviations), compared with the samples having the larger nitride content. Densification by adding cordierite as sintering additive showed the priority on the properties of thermal storage ceramics than increasing the nitride content.

Effect of particle size distribution on the properties of celsian based glazes

The microstructure and surface properties of ceramic glaze are influenced by chemical composition, particle size distribution, glaze application conditions, and firing parameters. This study specifically focused on the influence of glaze particle size distribution on the thermal behavior, microstructure, and surface appearance of barium frit based ceramic glaze in the floor tile firing process. The investigation involved examining the impact of four distinct particle size dimensions (d50: 5.7 μm, 6.8 μm, 7.5 μm, 10.9 μm) on the glaze properties by using hot stage microscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), color and gloss measurements. The studies indicated that celsian is the dominant phase in the glaze structure. The sintering and softening temperatures of glazes decreased with the increase of milling time. A decrease in the particle size of the glaze slurry increased the whiteness index. As the average particle size (d50) of the glaze decreased, the number of crystals was also increased. The investigation results also suggested a relation between specular reflection and milling time. As the milling time extended, there was a corresponding increase in the magnitude of glossiness.