Crystalline Ceramics Research Articles

Microstrip dielectric patch antenna fabrication and characterization using ultra low permittivity and low temperature Co-fired LiAlSiO4 ceramics

LiBxAl1-xSiO4 (x = 0.02–0.1) ceramics were prepared by conventional solid-state method with a reduction in sintering temperature by up to 250–475 °C. The relative permittivity was significantly decreased by εr = 3.3–3.7, one of the lowest ever reported values among crystalline ceramics, while maintaining exceptional quality factors (Q×f = 25,000–28,000 GHz) and low temperature coefficients of resonance frequency (τf = −23 ∼ −16 ppm/°C). Furthermore, these LiBxAl1-xSiO4 ceramics possess a low density (∼2.3 g/cm3), making them highly promising for lightweight microwave devices. The potential application of LiB0.1Al0.9SiO4 ceramics in LTCC was assessed based on their ability to achieve low densification temperature and exhibit chemical compatibility with silver electrodes. A microstrip patch antenna with an operating frequency of 6.68 GHz, featuring high efficiency (91.88 %) and wide bandwidth (400 MHz), has been designed and fabricated from LiB0.1Al0.9SiO4 ceramics substrate, which provides a good application prospect for advanced wireless systems. The development of these ultra-low permittivity dielectric ceramics opens new potential to revolutionize the field of microwave dielectric ceramics.

Structural and luminescent properties of YSZ-YSH based ceramics depending on Zr/Hf ratio

Samples of crystalline cubic phased ceramics based on (Zr1-хHfх)0.82Y0.17Eu0.01O1.91 with different contents of hafnium (х = 0; 0.21; 0.50; 0.77; 1) were synthesized. The synthesis conditions were chosen to avoid the possible formation of a minor tetragonal phase. The average grain size was 2–5 microns. The structural parameters of ceramics, their band gap, luminescent and thermoluminescent properties were studied depending on the hafnium content. It was shown that single-phase sample with calculated formula ((Zr0.77Hf0.23)0.82Y0.17Eu0.1)O1.91 demonstrated the highest cathodoluminescent intensity upon excitation by electrons. It was found that thermoluminescent properties of ceramics with hafnium content of х = 0.50–0.77 range are prospective for application in thermodosimetry. The highest luminescence yield was observed in such samples.

Concurrent Crystallization Mechanism Leading to Low Temperature Percolation of LAGP Glass-Ceramic Electrolyte.

Sintering of ceramic electrolytes (CE) is the most efficient way to obtain a dense, all ceramic solid-state battery with oxide-based materials. However, the high temperature required for this process leads to detrimental reactivity between CE and the active material. Crystalline ceramics are necessary for highly conductive oxide materials. Still, thermomechanical properties of glass-phase materials can be used to obtain a denser and more conductive CE. Glass-phase CE can be produced with Nasicon-type CE. Here, Li1.5Al0.5Ge1.5(PO4)3 (LAGP) glass is used as a model to investigate the formability, densification, and conduction properties upon crystallization. A complete study of the crystallization mechanism is first performed to fully understand how a high conductivity of 6.3 × 10-5 S·cm-1 at 30 °C with 92% relative density is obtained at a sintering temperature of only 550 °C without pressure. This is approximately 200 °C below the usual sintering temperature of LAGP. X-ray diffraction is then used to calculate the amount of crystalline phase as a function of time. A combined study of reaction kinetics and conductivity evolution reveals an autocatalytic nucleation effect, which produces an early crystallization pathway. Density is studied to quantify the ability of the glass to flow during the crystallization process.

Analysis of the Structure of Heavy Ion Irradiated LaFeO3 Using Grazing Angle X-ray Absorption Spectroscopy.

Crystalline ceramics are candidate materials for the immobilization of radionuclides, particularly transuranics (such as U, Pu, and Am), arising from the nuclear fuel cycle. Due to the α-decay of transuranics and the associated recoil of the parent nucleus, crystalline materials may eventually be rendered amorphous through changes to the crystal lattice caused by these recoil events. Previous work has shown irradiation of titanate-based ceramics to change the local cation environment significantly, particularly in the case of Ti which was shown to change from 6- to 5-fold coordination. Here, this work expands the Ti-based study to investigate the behavior in Fe-based materials, using LaFeO3 as an example material. Irradiation was simulated by heavy ion implantation of the bulk LaFeO3 ceramic, with the resulting amorphous layer characterized with grazing angle X-ray absorption spectroscopy (GA-XAS). Insights into the Fe speciation changes exhibited by the amorphized surface layer were provided through quantitative analysis, including pre-edge analysis, and modeling of the extended X-ray absorption fine structure (EXAFS), of the GA-XAS data.

Synthesis and investigation of novel boron- and magnesium-doped YAG:Ce and LuAG:Ce phosphor ceramics.

YAG:Ce and LuAG:Ce ceramics are widely used as scintillator materials that convert high-energy radiation into visible light. For the practical application of such compounds, short decay times are a necessity. One way of shortening the existing decay times even more is to change the local environment of emitting ions by means of doping the matrix with additional elements, for example, boron or magnesium. Furthermore, boron ions also can help absorb gamma rays more efficiently, therefore improving overall applicability. Due to the aforementioned reasons, YAG and LuAG ceramics doped with cerium, boron, and magnesium were synthesized. Initial amorphous powders have been obtained by means of sol-gel synthesis and pressed into pellets under isostatic pressure and finally calcinated to form crystalline ceramics. The effects of boron and magnesium doping on the morphological, structural, and luminescence properties were investigated. The key results showed that doping with boron has indeed shortened the decay times of the garnet pellets. Overall, boron doping of ceramics is a relatively new research area; however, it is rather promising as it helps both to improve the luminescence properties and to increase particle growth rate.

Synthesis of ultra-high-temperature nitride amorphous bulk by reaction of halide precursors with sodium in liquid ammonia

Amorphous Si-B-N nanoparticles of uniform composition tunable over the entire range spanning pure Si3N4 to pure BN was synthesized through a simple homogeneous chemical reaction of the mixture of SiCl4 and BBr3 with Na in liquid ammonia. With these amorphous nanopowders, dense amorphous bulk material was obtained with SPS sintering at the temperature before the crystallization. The dense amorphous bulk of Si3B3N7 exhibited the highest value of hardness (8.8 GPa), flexural strength s (545 MPa), and fracture toughness KIC (10.6 MPa m1/2). These are significantly higher than those reported for other crystalline ceramics of the same composition and surpass those of the completely dense crystalline ceramics. The fully-dense amorphous bulk material exhibited excellent resistance to oxidation up to 1550 °C.

Quantitative domain evaluation in rhombohedral BS-PT piezoelectric ceramics via diffraction-plane-transformation model

The domain structure fundamentally determines the piezoelectric/ferroelectric performance of ferroelectric materials. To understand the correlation between macro-properties and microstructure, the evolution of domain structure should be clearly figured out. Here, the diffraction-plane-transformation (DPT) model is proposed for the domain evaluation in BS-PT piezoelectric ceramics of rhombohedral crystalline structure. The transformation between different crystal planes is accurately revealed by the DPT model. Then, non-180° domain reversal in rhombohedral 0.4BiScO3–0.6PbTiO3 piezoelectric ceramics (abbreviated as BS-PT) can be quantitatively estimated, whether in electric poling or thermal depoling processes. Experimentally, the correlations between piezoelectric coefficients, electromechanical coupling properties, and non-180° domain reversal percentage are investigated. It is proven that the DPT model provides an effective method for the non-180° domain estimation in rhombohedral crystalline ceramics.

High-entropy (YErYbLu)2SiO5 ceramic aerogel: A potential ceramic insulator with low thermal conductivity

Conventional oxide aerogels have limitations in terms of structural damage and phase transformation at high temperatures. A novel high-entropy (YErYbLu)2SiO5 ceramic aerogel was synthesized by a combination of the sol-gel process, supercritical drying, and high-temperature calcination. The successful synthesis of a high-entropy (YErYbLu)2SiO5 ceramic aerogel in a single phase after calcination at 1250 °C was confirmed by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The high-entropy ceramic aerogel (YErYbLu)2SiO5 still shows excellent structural and phase stability after annealing at 1400 °C. The structurally reconstructed samples (RSO) exhibit low densities ranging from 1.79 to 3.28 g/cm3, room-temperature thermal conductivities between 0.109 and 0.253 W·m-1 K-1, and fracture toughness values ranging from 0.61 to 9.70 MPa. Notably, the lowest thermal conductivity is less than 1/10 of that of the corresponding dense crystalline ceramics. Furthermore, the RSO has a low coefficient of thermal expansion within the temperature range of 360–1200 °C (ranging from 5.84 × 10−6 °C−1 to 7.36 × 10−6 °C−1). The RSO exhibits high residual strength retention after thermal shock testing. These properties position the high-entropy (YErYbLu)2SiO5 ceramic aerogel as a promising candidate for nano-thermal insulation as a porous ceramic material that undergoes structural reconstruction.

Effect of tungsten metal-oxide addition on physical, structural, and electrical properties of borophosphate glasses

Demand for electrical energy storage (EES) is growing, necessitating the development of improved batteries. Inorganic glassy materials are a class of essential electrodes due of their excellent conductivity and stable structures, they are appropriate for both cathode and anode applications. The most important characteristics that determine the dynamic behavior and rate performance of batteries are the ionic and electronic conductivities of active materials. In this sense, many crystalline, vitreous, and glass ceramics are investigated for their electrical properties. To create uniformly mixed glasses within the xLi2WO4–(50–x)Li2O–40P2O5–10B2O3 system, the melt-quenching technique is employed. Glasses containing up to 50 mol% Li2WO4 are synthesized with a substantial region of glass formation. They are homogeneous, transparent, and bubble-free. The structural approach and selected physical parameters of these glasses, such as density, molar volume, electrical conductivity, and glass transition temperature, are evaluated. The study emphasizes that an increase in the Li2WO4 amount leads to an elevation in both the density (ρ) and molar volume (Vm). Infrared spectroscopy identifies the presence of numerous structural units within the glass framework. Electrical conductivity measurements of the glasses are investigated using impedance spectroscopy. The measurements are taken over a wide frequency range of 10 Hz to 1 MHz and across temperatures ranging from 303K to 403K. It is highlighted that the electric conductivity rises as the Li2WO4 content is added. The glass with x = 30 mol% exhibits a dc conductivity of 8.63 × 10−7 (Ω−1 cm−1) at room temperature and 8.90 × 10−5 (Ω−1 cm−1) at 150°C. To gain insight into the conductivity relaxation mechanism, the frequency dependence of the glasses' conductivity is investigated. The results indicate that the ion transport in the glasses is governed by the correlated barrier hopping mechanism, which follows Jonscher's power behavior. The scaling conductivity spectra reveal that the conduction mechanism in the glasses is influenced by both temperature and composition.

Uranium Retention in Silica-Rich Natural Glasses: Nuclear Waste Disposal Aspect

Uranium-containing glass samples with an age of 140–145 million years were collected within the volcanic rocks of the largest volcanic-related uranium ore deposit in the world. Main features of their composition are high concentrations of silica and uranium, the largest for the rocks of this type. In contrast to this, the ages of fresh (unaltered) low-silica natural glasses of a basic composition (basalts) usually do not exceed a few million years. The volcanic low-silica glass is unstable at longer times and in older ancient rocks is transformed into a crystalline mass. The geochemistry of uranium including the behavior in solids and solutions is similar to that of long-lived transuranic actinides such as radioactive Np and Pu from high-level radioactive waste. This allows uranium to be used as a simulant of these long-lived hazardous radionuclides both at the synthesis and for the study of various nuclear wasteforms: glasses, glass crystalline materials and crystalline ceramics. The data obtained on long-term behavior of natural glasses are of importance for prognosis and validation of stability of nuclear wasteforms disposed of in geological disposal facilities (GDF).

CRYSTALLINE OXIDE CERAMICS AT VARIOUS STAGES OF THE TECHNOLOGICAL PROCESS COMPARATIVE CHARACTERISTICS OF THE TECHNOLOGICAL PROCESS

The article discusses research about microstructure of crystalline oxide ceramics at stages of the technological process. It is proved that the introduction of stabilizing substances into the composition of oxide ceramics leads to homogenization of the basic substance and to smoothing between crystal contacts. This leads to hardening of the ceramic.

Ionizing radiation source-open type fabrication using additive technology and spark plasma sintering

The paper presents an original method for open-type ionizing radiation source (IRS) fabrication by the means of spark plasma sintering-reactive synthesis (SPS-RS) of SrTiO3 ceramics as an active zone component reinforced by the titanium alloy framework produced by additive technology. Rapid heating regimes of SPS-RS are described with the focus on fabrication of perovskite-phase SrTiO3 crystalline ceramics integrated within the reinforcing Ti–Al–V framework yielding defect- and pore-free monolith. The product is characterized by the excellent crack resistance, Vickers microhardness (480–554 HV), and hydrolytic stability (leaching rate as low as 10−5 g/cm2·day). Presented results show bright prospects for high-tech radioisotope production in the form of open-type IRS meeting the requirements of international standards.

Highly red luminescent stabilized tetragonal rare earth-doped HfO2 crystalline ceramics prepared by sol-gel

We report high incorporation of rare earth ions (RE3+) into hafnia nanoparticles prepared by the sol–gel method and investigate how these dopants affect hafnia structure and phase transformation. An ethanolic suspension containing 5-nm hafnia nanoparticles was obtained from HfOCl2.8H2O in ethanol. Pure and 0.1–7 mol% Eu3+-doped materials afforded HfO2 monoclinic phase, whereas hafnia nanoparticles added with 10 and 20 mol% Eu3+ were stabilized in the tetragonal phase. Structural evolution of the nanoparticles was analyzed by Eu3+ luminescence spectroscopy and excited level lifetimes. The emission spectra in the visible region showed an increase of the Eu3+ site symmetry due to hafnia phase transformation from monoclinic to tetragonal upon increasing Eu3+ concentration. Concentration quenching, followed by lifetime measurements, occurred at high Eu3+ concentration (20 mol %). The hafnia tetragonal phase was stabilized with non-optically active La3+ (a fixed concentration of 10 mol %), co-doped with a lower concentration of Eu3+ ions (from 0.1 to 3 mol %). This strategy ensured that Eu3+ luminescence in tetragonal hafnia was intense and prevented quenching by the high Eu3+ concentration. In this sense, the hafnia structure and emission properties can be tailored by the RE3+ concentration, so that an interesting material for applications in photonics and biophotonics can be achieved.

Fabrication and characterization of high entropy pyrochlore ceramics

High-entropy rare-earth (RE) zirconates with pyrochlore structure were successfully fabricated by pressureless and spark plasma sintering. RE2Zr2O7 compound with nominal composition (La0.2Y0.2Gd0.2Nd0.2Sm0.2)Zr2O7 was prepared by simple glycine nitrate procedure (GNP). GNP process yielded powders with low crystallinity and after subsequent calcination, well crystalline ceramics were formed. During calcination defective fluorite (F-RE2Zr2O7) and crystal pyrochlore (Py-RE2Zr2O7) structures coexist. Formation of pure crystalline pyrochlore occurs after sintering at 1450°C. High-density ceramics, free of any additives, were obtained after powders compaction and pressureless (PS), as well as field assisted sintering technique (FAST) at 1450°C. Theoretical investigations of the high-entropy RE2Zr2O7 pyrochlore systems were performed. Unit cell parameter of the obtained Py-RE2Zr2O7 is 10.5892(2)Å and 10.5999(2)Å for PS and FAST sintering, respectively, which is in good agreement with the results of Density Functional Theory (DFT) calculations. The thermal diffusivity of sintered samples at room temperature was ∼0.7mm2/s for both sintering methods.

Grain size estimation in polycrystals: Solving the corpuscle problem using Maximum Likelihood Estimation

In materials science, the microstructures of materials are generally characterized by 2D observation (e.g. electron microscopy). For polycrystalline materials, such as crystalline rocks or ceramics, those observations can be used to measure the grain size distribution. However, the fact that grain sizes are measured in planar cuts introduces a statistical bias, since the real (3D) grain sizes cannot be directly measured. For almost spherical grains, this bias can be computed thanks to the so-called Wicksell's equation. This paper proposes a method, based on Maximum Likelihood Estimation (MLE) for unfolding the apparent 2D distribution. The efficiency of this method is extensively investigated in the special case of lognormal distribution. In this case, 10% uncertainty on the distribution parameters can be reached with only 580 empirical values.

Recent Advances in Corrosion Science Applicable To Disposal of High-Level Nuclear Waste.

High-level radioactive waste is accumulating at temporary storage locations around the world and will eventually be placed in deep geological repositories. The waste forms and containers will be constructed from glass, crystalline ceramic, and metallic materials, which will eventually come into contact with water, considering that the period of performance required to allow sufficient decay of dangerous radionuclides is on the order of 105-106 years. Corrosion of the containers and waste forms in the aqueous repository environment is therefore a concern. This Review describes the recent advances of the field of materials corrosion that are relevant to fundamental materials science issues associated with the long-term performance assessment and the design of materials with improved performance, where performance is defined as resistance to aqueous corrosion. Glass, crystalline ceramics, and metals are discussed separately, and the near-field interactions of these different material classes are also briefly addressed. Finally, recommendations for future directions of study are provided.

(Invited) Designing Ionic Scaffold for Efficient Solid Electrolyte for All Solid State Battery

All solid state battery has gained recently much attention because of their potential to store more energy while being safer to operate compared to liquid electrolyte Li-ion batteries. The development of solid electrolytes with superior electrochemical properties is highly desirable. Representatively, sulfide and oxide-based solid electrolytes have been vigorously researched and demonstrated for high-performance all-solid-state batteries. The oxide-based solid electrolytes have superior electrochemical stability compared to the sulfide one, but relatively low ionic conductivity and low processability owing to their mechanically rigid and brittle features which must be taken into consideration to achieve high-performance all-solid-state batteries. In this presentation, different synthesis and processing approaches will be presented to design efficient Li-ion conducting ceramic. Their ionic conductivity measured at room temperature will be discussed as function of their microstructure (porosity, pparticle size, chemical composition,...).First, we study the synthesis, the fabrication of dense ion-conducting ceramic such as (Li1.3Al0.3Ti1.7(PO4)3) LATP and (Li7La3Zr2O12) LLZO and their electrochemical characterization. Starting from “sol-gel” like synthesis coupled with heating at high temperature, we have succeeded to achieve dense ceramic with ionic conductivity of ~10-4 S/cm for LLZO and for LATP, attesting good quality of the purity and crystallinity. More interestingly, we have also developed an innovative synthesis and processing approach to sinter LATP with suitable properties in one single step, with the aid of microwave heating. Pure and crystalline LATP ceramics are achieved in only one single step starting from amorphous, compacted LATP’s precursors powders. Despite a relative density of 88%, the ionic conductivity is about 3.14 x 10-4 S.cm-1 at ambient temperature.With the objective of developing hybrid organic-inorganic membrane, we extend our knowledge on the synthesis of 3-D network of crystalline LATP or LLZO fibers by coupling an electrospinning process with the sol-gel synthesis followed by an optimized thermal treatment (atmosphere, temperature and dwelling time). Depending on the processing parameters of electrospinning, different fiber mats organization and density have been achieved. The Li+ ion conductivity of these fibers mats was evaluated by impedance spectroscopy at ambient temperature. As an example, the Li ion conductivity for LATP was estimated to be 3 × 10−4 mS/cm; note that this value is not affected by the water content used in the electrospinning chamber and therefore by the microstructure of the LATP mat. Of course, this value is low compared to that observed on the dense ceramic; this is linked to the porosity of the LATP fiber mat of about 60%. Taking into account the porosity of the fiber mats, the conductivity values are corrected and finally the corrected conductivity value is 1 order of magnitude higher than the one achieved on ceramic with low relative density. This result shows that good particle−particle contact is achieved along the LATP fibers and that most of the LATP fibers are connected to each other to ensure a continuous Li ion pathway throughout the porous ceramics.

(Invited) Display and LSI Applications of Oxide Semiconductor LSIs (OS LSIs) Using Crystalline In–Ga–Zn Oxide (IGZO): Applications Related to Coronavirus COVID-19 Pandemic

The coronavirus COVID-19 pandemic is becoming a global crisis in 2020. Global climate change is an indirect cause of the spread of infectious diseases [1]. The increase in greenhouse gas as a result of increased power consumption has an adverse effect on this climate change. The amount of power consumption continues to increase as human society advances, and Japan Science and Technology Agency’s report says that global and Japan’s annual power consumption concerning IT equipment in 2050 will be nearly 200 times as large as the present global and Japan’s total annual power consumption.” [2]. This means that one of the main causes of the global climate change would be the increase in the amount of power consumption through the spread of fast-growing Internet of Things (IoT) and artificial intelligence (AI) technologies.An anwer to the question of how to reduce power consumption and defend against infectious diseases that may threaten human beings while developing the IoT and AI technologies is to reduce the power consumption of semiconductor devices intensely and reduce the power consumption concerning IT equipment to 1/1000 of the present power consumption.A field-effect transistor (FET) fabricated using a c-axis aligned crystalline In–Ga–Zn oxide (CAAC-IGZO), which is a typical example of crystalline oxide semiconductor (OS) ceramics, exhibits an off-state current I off in the order of yA/mm (10- 24 A/mm) at 85°C [3,4]. The FET we developed is a FinFET with a trench-gate self-aligned (TGSA) structure [5].As shown in the figure, the upper limit of operation efficiency of AI accelerators fabricated using Si LSIs is 10 TOPS/W, whereas normally-off CPUs [6,7] and AI accelerators fabricated using CAAC-IGZO could achieve an operation efficiency of 100 TOPS/W (8 bits) or 1 POPS/W (1 bit). If this technology is adopted in all VLSI devices and supercomputers, reducing the power consumption of those devices by 1000 times will come closer to reality even in the AI/IoT era. Therefore, we believe that the use of the CAAC-IGZO technology is the only solution to the global climate change.OS LSIs are applicable to all kinds of displays including displays for augmented reality and virtual reality, dynamic random access memories, and 3D OS NANDs (3D NANDs fabricated using IGZO). This work introduces crystalline IGZO ceramics, which would be a future key technology, and LSI and display applications of LSI of the crystalline IGZO ceramics.

(Invited) Surface Analysis of Corrosion Products Built up at Interfaces of Different Nuclear Waste Forms in Near-Field Environment

In this study, we applied a series of surface analysis techniques to explore the structure and chemistry of the corrosion products built up at the interface of different materials, which is relevant to the permanent disposal of world-wide high-level nuclear waste. Metallic alloys, amorphous glass, and crystalline ceramics are typical candidate nuclear waste forms planned for immobilizing and isolating the dangerous radionuclides enriched in the waste. The near-field corrosion interactions between these dissimilar materials are the focus of this study. The experiments were performed by corroding metallic alloys in intimate proximity to glass or ceramics in Cl--containing solutions at 90 oC. The exposed materials were subsequently subjected to comprehensive surface characterization using X-ray photoelectron spectroscopy, scanning transmission electron microscopy, energy dispersive spectroscopy, time-of-flight secondary ion mass spectrometry, and Raman/infrared spectroscopy analysis. The systematic study revealed localized damage on the alloy surface due to crevice corrosion. Interestingly, localized corrosion was also identified on the surface of some glasses and ceramics that were present nearby, while an inhibition effect was observed in other systems. These interactions were found to strongly depend on the type of materials and environment, which led to different corrosion phenomena.

In-Operando Study of Shape Retention and Microstructure Development in a Hydrolyzing Sol-Gel Ink during 3D-Printing.

3D printing of amorphous and crystalline ceramics is of paramount importance for the fabrication of a wide range of devices with applications across different technology fields. Printed ceramics are remarkably enabled by the sol-gel synthesis method in conjunction with continuous filament direct ink writing. During printing, multiple processes contribute to the evolution of inks including shape retention, chemical conversion, solidification, and microstructure formation. Traditionally, depending on the ink composition and printing environment, several mechanisms have been associated with the shape retention and solidification of 3D printed structures: gelation, rapid solvent evaporation, energy-driven phase transformation, and chemical-driven phase transformation. Understanding the fundamental differences between these mechanisms becomes key since they strongly influence the spatiotemporal evolution of the materials, as the out-of-equilibrium processes inherent to the extrusion, relaxation, and solidification of printed materials have significant effects on the materials properties. In this work, we investigate the shape retention mechanism and the hydrolysis-induced material conversion and microstructure formation during the 3D printing of a water reactive sol-gel ink that transforms into titanium dioxide-based ceramic. This study aims at identifying characteristic mechanisms associated with the material transformation, establishing connections between the microstructure development and the timescales associated with solidification under operando 3D-printing conditions. The investigation of this material's out-of-equilibrium pathways under processing conditions is enabled by time-resolved coherent X-ray scattering, providing simultaneous access to temporospatially resolved microstructural and dynamics information. Furthermore, we explore X-ray speckle tracking as a tool to resolve deformations of the microstructure in a printed filament associated with the deposition of consecutive filaments. Through this work, we aim at providing a fundamental understanding of the relationships behind these transformative processes in 3D printing and their timescales as the basis for achieving unprecedented control over printed materials microstructure.