Vat Photopolymerization of Ceramic Parts: Effects of Carbon Fiber Additives on Microstructure and Mechanical Performance.

Vat photopolymerization (VPP), as an additive manufacturing (AM) technology, can conveniently produce ceramic parts with high resolution and excellent surface quality. However, due to the inherent brittleness and low toughness of ceramic materials, manufacturing defect-free ceramic parts remains a challenge. Many researchers have attempted to use carbon fibers as additives to enhance the performance of ceramic parts, but these methods are mostly applied in processes like fused deposition modeling and hot pressing. To date, no one has applied them to VPP-based AM technology. This is mainly because the black carbon fibers reduce laser penetration, making it difficult to cure the ceramic slurry and thus challenging to produce qualified ceramic parts. To address this issue, our study has strictly controlled the amount of carbon fibers by incorporating trace amounts of carbon fiber powder into the original ceramic slurry with the aim to investigate the impact of these additions on the performance of ceramic parts. In this study, ceramic slurries with three different carbon fiber contents (0 wt.%, 0.1 wt.%, 0.2 wt.%, and 0.3 wt.%) were used for additive manufacturing. A detailed comparative analysis of the microstructure, physical properties, and mechanical performance of the parts was conducted. The experimental results indicate that the 3D-printed alumina parts with added carbon fibers show varying degrees of improvement in multiple performance parameters. Notably, the samples prepared with 0.2 wt.% carbon fiber content exhibited the most significant performance enhancements.

Multi-scale structural characterization of ceramic-based photonic glasses for structural colors.

Structural colors arise from selective light interaction with (nano)structures, which give them advantages over pigmented colors such as resistance to fading and possibility to be fabricated out of traditional low-cost and non-toxic materials. Since the color arises from the photonic (nano)structures, different structural features can impact their photonic response and thus, their color. Therefore, the detailed characterization of their structural features is crucial for further improvement of structural colors. In this work, we present a detailed multi-scale structural characterization of ceramic-based photonic glasses by using a combination of high-resolution ptychographic X-ray computed tomography and small angle X-ray scattering. Our results uncover the structure-processing-properties' relationships of such nanoparticles-based photonic glasses and point out to the need of a review of the structural features used in simulation models concomitantly with the need for further investigations by experimentalists, where we point out exactly which structural features need to be improved.

Phosphor Ceramic Composite for Tunable Warm White Light.

Composite phosphor ceramics for warm white LED lighting were fabricated with K2SiF6:Mn4+ (KSF) as both a narrowband red phosphor and a translucent matrix in which yellow-emitting Y3Al5O12:Ce3+ (YAG) particles were dispersed. The emission spectra of these composites under blue LED excitation were studied as a function of YAG loading and thickness. Warm white light with a color temperature of 2716 K, a high CRI of 92.6, and an R9 of 77.6 was achieved. A modest improvement in the thermal conductivity of the KSF ceramic of up to 9% was observed with the addition of YAG particles. In addition, a simple model was developed for predicting the emission spectra based on several parameters of the composite ceramics and validated with the experimental results. The emission spectrum can be tuned by varying the dopant concentrations, thickness, YAG loading, and YAG particle size. This work demonstrates the utility of KSF/YAG composite phosphor ceramics as a means of producing warm white light, which are potentially suitable for higher-drive applications due to their increased thermal conductivity and reduced droop compared with silicone-dispersed phosphor powders.

Reactive Synthesis for Porous (Mo2/3Y1/3)2AlC Ceramics through Mo, Y, Al and Graphite Powders.

Through an activation reaction sintering method, porous (Mo2/3Y1/3)2AlC ceramics were prepared by Mo, Y, Al, and graphite powders as raw materials. The phase composition, microstructure, element distribution, and pore structure characteristics were comprehensively studied using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), Archimedes method, and bubble point method. A detailed investigation was conducted on the influence of sintering temperature on the phase composition. Possible routes of phase transition and pore formation mechanisms during the sintering process were provided. The experimental results reveal that at 650-850 °C, transition metals react with aluminum, forming aluminum-containing intermetallics and a small amount of carbides. At 850-1250 °C, transition metals collaborate with graphite, producing transition metal carbides. Then, at 1250-1450 °C, these aluminum intermetallics interact with transition metal carbides and remaining unreacted Y, Al, and C, yielding the final product (Mo2/3Y1/3) 2AlC. Simultaneously, the pore structure alters correspondingly with the solid-phase reaction at different reaction temperatures.

Ferroelectric and Relaxor-Ferroelectric Phases Coexisting Boosts Energy Storage Performance in (Bi0.5Na0.5)TiO3-Based Ceramics.

With the intensification of the energy crisis, it is urgent to vigorously develop new environment-friendly energy storage materials. In this work, coexisting ferroelectric and relaxor-ferroelectric phases at a nanoscale were constructed in Sr(Zn1/3Nb2/3)O3 (SZN)-modified (Bi0.5Na0.5)0.94Ba0.06TiO3 (BNBT) ceramics, simultaneously contributing to large polarization and breakdown electric field and giving rise to a superior energy storage performance. Herein, a high recoverable energy density (Wrec) of 5.0 J/cm3 with a conversion efficiency of 82% at 370 kV/cm, a practical discharged energy density (Wd) of 1.74 J/cm3 at 230 kV/cm, a large power density (PD) of 157.84 MW/cm3, and an ultrafast discharge speed (t0.9) of 40 ns were achieved in the 0.85BNBT-0.15SZN ceramics characterized by the coexistence of a rhombohedral-tetragonal phase (ferroelectric state) and a pseudo-cubic phase (relaxor-ferroelectric state). Furthermore, the 0.85BNBT-0.15SZN ceramics also exhibited excellent temperature stability (25-120 °C) and cycling stability (104 cycles) of their energy storage properties. These results demonstrate the great application potential of 0.85BNBT-0.15SZN ceramics in capacitive pulse energy storage devices.

Effects of Different Concentrations of Carbamide Peroxide on Color, Surface Roughness, and Hardness of CAD/CAM Dental Ceramics.

OBJECTIVES: This study assessed the effects of 15% and 20% carbamide peroxide (CP) on color, surface roughness, and hardness of computer-aided design/computer-aided manufacturing (CAD/CAM) dental ceramics. MATERIALS AND METHODS: This in vitro study was conducted on 120 Vita Mark II, Celtra Duo, and Suprinity CAD/CAM ceramic specimens. The ceramic specimens in each group (n = 40) were randomly assigned to two subgroups (n = 20) for polishing and glazing, and their baseline color, surface roughness (Ra), and hardness were assessed. In each subgroup, half of the specimens were exposed to 15% CP, while the other half were exposed to 20% CP. Their color change (ΔE), surface roughness, and hardness were then measured again. Surface roughness, hardness, and color were analyzed sequentially by profilometer, Vickers hardness tester, and spectrophotometer, respectively. Data were analyzed by repeated measures ANOVA, one-way ANOVA, and post hoc Bonferroni test (α = 0.05). RESULTS: The surface roughness of all groups significantly increased after bleaching treatment (p < 0.05). Surface hardness of all groups decreased after bleaching treatment, but this reduction was only significant in Vita Mark II subgroups (glazed, polished, 15%, and 20% CP). The ΔE was not clinically and visually perceivable in any group. CONCLUSION: The present results revealed that concentration of CP and type of surface treatment affected the surface properties of CAD/CAM ceramics. Type of surface treatment only affected the surface hardness of Vita Mark II ceramics (p < 0.05). Concentration of CP had a significant effect only on polished Vita Mark II.

Surface treatment, liquid, and aging effects on color and surface properties of monolithic ceramics.

PURPOSE: The purpose of this study was to investigate the effects of surface treatments, liquids, and aging on color, translucency, and surface properties of monolithic ceramics. MATERIALS AND METHODS: Lithium disilicate (LDS) and zirconia-reinforced lithium silicate (ZLS) ceramics (n = 135 each) were cut and divided into three groups [crystallization+glaze (single stage), crystallization-glaze (two stages), and crystallization-polish (two stages)]. One sample from each group was examined using scanning electron microscopy (SEM). Remaining samples were divided into four subgroups (distilled water, coffee, grape juice, and smoothie) (n = 11 each), stored for 12 d in the respective liquids, and thermally aged. One sample from each subgroup was analyzed using SEM. The color, gloss, and roughness values of the samples were analyzed after surface treatment (initial) and storage under different liquids+aging conditions. The initial data and both the aged data and data change values were analyzed using robust two- and three-way analyses of variance. RESULTS: The glazed groups exhibited smoother surfaces. Ceramic type and ceramic-surface treatment interactions affected the initial translucency parameter (TP) (P < .001) and the initial and aged roughness values (P ≤ .001). Surface treatment type affected the color change (P < .001), and ceramic type affected the aged TP values (P < .001). Type of ceramic, surface treatment, and their interactions affected both the initial and aged gloss (P ≤ .001) and TP change values (P ≤ .015). Surface treatment type and ceramic-surface treatment interactions affected the gloss change values (P ≤ .001). CONCLUSION: Although both ceramics and all surface treatments are clinically applicable, crystallization-glaze is recommended. When gloss and smoothness are important or when translucency is important, ZLS or LDS may be preferred, respectively.

Effect of Er,Cr: YSGG laser debonding treatment on the optical properties and surface roughness of ceramic laminate veneers: An in vitro study.

PURPOSE: The objective of this study was to evaluate the effect of (Er,Cr: YSGG) laser debonding treatment on optical properties and surface roughness of veneers made of different ceramic materials. MATERIALS AND METHODS: Thirty bovine incisors were prepared to receive laminate veneers and divided into three groups (n = 10) according to ceramic material where group (E): IPS e.max CAD, group (S): Vita Suprinity, and group (C): Celtra Duo. Blocks were sectioned into 0.5 mm thickness plates and cemented on the labial surface of incisors using resin cement. The Er,Cr: YSGG laser was applied to each specimen at 4.5 W and 25 Hz for group E and at 6 W and 25 Hz for groups S and C. Color change (△E00), translucency parameter (TP) and surface roughness in µm (Ra) values were measured and calculated before and after laser treatment. Data were analyzed using two-way mixed model ANOVA at a significance level of p < 0.05. RESULTS: The highest mean △E00 value was recorded in group E (1.35 ± 0.09) followed by group S (1.08 ± 0.16) and then group C (0.93 ± 0.10) with a significant difference between them (p < 0.001). All groups exceeded the perceptibility threshold but remained below the acceptability threshold. No statistically significant difference was found in TP except for group E (p = 0.019). Ra values after laser debonding showed significantly higher values than before laser treatment in all three groups (p < 0.001). CONCLUSION: Er,Cr: YSGG laser can be safely used for debonding ceramic veneers without altering the optical properties but it does increase the roughness of debonded ceramic restorations.

Subnanoscale Ion Beam Modification-Assisted Smoothing of Heterostructure Surfaces.

Glass ceramic (GC) is the most promising material for objective lenses for extreme ultraviolet lithography that must meet the subnanometer precision, which is characterized by low values of high spatial frequency surface roughness (HSFR). However, the HSFR of GC is typically degraded during ion beam figuring (IBF). Herein, a developed method for constructing molecular dynamics (MD) models of GC was presented, and the formation mechanisms of surface morphologies were investigated. The results indicated that the generation of the dot-like microstructure was the result of the difference in the erosion rate caused by the difference in the intrinsic properties between ceramic phases (CPs) and glass phases (GPs). Further, the difference in the microstructure of the IBF surface under different beam angles was mainly caused by the difference in the two types of sputtering. Quantum mechanical calculations showed that the presence of interstitial atoms would result in electron rearrangement and that the electron localization can lead to a reduction in CP stability. To obtain a homogeneous surface, the effects of beam parameters on the heterogeneous surface were systematically investigated based on the proposed MD model. Then, a novel ion beam modification (IBM) method was proposed and demonstrated by TEM and GIXRD. The range of ion beam smoothing parameters that could effectively converge the HSFR of the modified surface was determined through numerous experiments. Using the optimized beam parameters, an ultrathin homogeneous modified surface within 3 nm was obtained. The HSFR of GC smoothed by ion beam modification-assisted smoothing (IBMS) dropped from 0.348 to 0.090 nm, a 74% reduction. These research results offer a deeper understanding of the morphology formation mechanisms of the GC surfaces involved in ion beam processing and may point to a new approach for achieving ultrasmooth heterostructure surfaces down to the subnanometer scale.

Structurally Regulated Design Strategy of Bi0.5Na0.5TiO3-Based Ceramics for High Energy-Storage Performance at a Low Electric Field.

Dielectric ceramic capacitors are prospective energy-storage devices for pulsed-power systems owing to their ultrafast charge-discharge speed. However, low energy-storage density makes them difficult to commercialize for high-pulse-power technology applications. Herein, we presented a structurally regulated design strategy to disrupt a long-range ferroelectric order, refined grains, and eventually achieve excellent comprehensive energy-storage performance in (1 - x) (0.7Bi0.5Na0.5TiO3-0.3SrTiO3)-x Sm(Zn2/3Nb1/3)O3 eco-friendly ceramics. A large Wrec of ∼7.43 ± 0.05 J/cm3 and a high η of ∼85 ± 0.5% of 0.96 (0.7Bi0.5Na0.5TiO3-0.3SrTiO3)-0.04 Sm(Zn2/3Nb1/3)O3 were obtained at a low electric field of 290 kV cm-1 with good energy-storage temperature (25-120 °C), frequency (1-100 Hz) stability, and charge-discharge properties (PD ∼ 74 ± 1 MW/cm3 and τ0.9 ∼ 159 ± 2 ns). This strategy inspires rational structurally regulated designs and aims to promote the development of eco-friendly 0.7Bi0.5Na0.5TiO3-based ceramics with excellent energy-storage characteristics.

Alternative material recommendation for facade cladding: High silica-containing stonepaste ceramics.

This study investigated the potential of using stonepaste ceramics, which were widely preferred as a coating and decoration material on the facades of architectural buildings in ancient times and continues to be produced on a workshop scale today as a cladding material on building facades. Stonepaste ceramics, made from a mixture prepared with a high amount of crystalline quartz as well as frit, plastic clay, and bentonite raw materials, were hand-shaped and sintered at 930 °C after glazing. The physico-mechanical properties of stonepaste ceramics, their behaviour under various environmental conditions (resistance to chemicals, frost, and thermal shock), and their microstructures have been characterized. The characterization results were compared with the properties of commonly used facade cladding materials. It was determined that stonepaste ceramics had a very low firing shrinkage value (2.84 %) compared to that of other ceramic cladding materials, a higher water absorption value (11.79 %) than that of porcelain tiles and floor tiles, and close to wall tiles, and a flexural strength value (33.64MPa) higher than wall tiles and close to porcelain tiles despite the high-water absorption value. Ten cycles of thermal shock resistance showed that the body and glaze layer of the stonepaste ceramic material are well bonded to each other, and there is no significant thermal expansion mismatch between them. One hundred cycles of freeze-thaw conditions indicated that the stonepaste ceramic had good adhesion and thermal expansion compatibility between the glaze and the body but only chipping damage under the action of tensile forces caused by the freezing of water entering the pores of the body. In terms of behaviour against various chemicals, stonepaste ceramics were found to be highly resistant to high and low concentrations of household chemicals, swimming pool salts, and alkalis but less resistant to low concentrations of HCl and citric acid and high concentrations of HCl and lactic acid compared to other chemicals. The results show that stonepaste ceramics, despite their high-water absorption potential, have properties close to those of traditional ceramic tiles and, like these materials, can serve for significant periods in various environmental conditions when used as facade cladding. Consequently, it has been revealed that stonepaste ceramics can be used as a facade cladding material in sustainable, long-lasting, contemporary architectural facades thanks to their technical and protective properties.

The effect of photoinitiator type and filler load on physicochemical and mechanical properties of experimental light-cured resin cements through lithium disilicate ceramics of different shades and thicknesses.

OBJECTIVE: This study investigated the influence of photoinitiator types on degree of conversion (DC), rate of polymerization (RP), flexural strength (FS), flexural modulus (FM), and light transmittance (LT) of filled and unfilled light-curable resin cements through different thicknesses and shades of lithium disilicate ceramics. METHODS: Lithium disilicate ceramic discs (IPS Emax Press, background [0.0], 0.5, 1.0, 2.0, 3.0, and 4.0 mm, shades A1 and BL3) were prepared. Experimental resin-based cements [TEGDMA/BisGMA (50/50 mass%)] were prepared using either camphorquinone (CQ)/amine (0.44/1.85 mol%) or TPO (0.44 mol%)], and a micro and nanofiller loads of nil (unfilled); 40/10 mass%; and 50/10 mass%). Resin cements (0.2 mm thick) were placed on the lower surface of the ceramic specimens and light-activated for 30 s from the upper surface using a Bluephase Style curing light (exitance at tip: 1236 mW/cm2 ± 1.20). LT and distribution of irradiance through the ceramics were measured using a UV-vis spectrometer and a beam profile camera, respectively (n = 3). The DC and RP were measured in real-time using mid infrared spectroscopy in attenuated total reflectance (ATR) mode (n = 3). FS and FM were measured using a universal testing machine (n = 5). Statistical analyses were performed on LT, DC, RP, FS, and FM data using a general linear model, and supplementary ANOVA and post hoc Tukey multiple comparison test were also performed (α = .05). RESULTS: Thicknesses, shades, photoinitiator type, and fillers load significantly influenced the optical and mechanical characteristics of the resin-based materials (p < 0.05). The BL3 shade ceramic provided higher values of DC, RP, FS, FM, and LT compared with the A1 shade (p < 0.05). Increasing ceramic thickness decreased the properties of the resin-based materials (p < 0.05). Generally, TPO improved mechanical properties of the resin cement compared with CQ (p < 0.05). SIGNIFICANCE: The luting process of indirect restorations may be improved by using high molar absorptivity, more reactive, and more efficient photoinitiators such as TPO, as opposed to conventional CQ. The use of such initiator may allow the placement of thicker and more opaque indirect restorations.

Molten Salt-Assisted Synthesis of Titanium Nitride.

Titanium nitride is an exciting plasmonic material, with optical properties similar to gold. However, synthesizing TiN nanocrystals is highly challenging and typically requires solid-state reactions at very high temperatures (800-1000°C). Here, the synthesis of TiN nanocrystals is achieved at temperatures as low as 350°C, in just 1 h. The strategy comprises molten salt, Mg as reductant and Ca3N2 as nitride source. This brings TiN from the realm of solid-state chemistry into the field of solution-based synthesis in regular, borosilicate glassware.

Effect of Er:YAG laser on debonding zirconia and lithium disilicate crowns bonded with 2- and 1-bottle adhesive resin cements.

INTRODUCTION: Erbium-doped yttrium-aluminum-garnet (Er:YAG) laser debonding of zirconia and lithium disilicate restorations is increasingly used for a range of clinical applications. Using rotary instruments to remove such restorations for any purpose has proven to be challenging. Erbium laser has been reported to be a conservative method for removing ceramic restorations. There is little data in the literature about the effect of adhesive resin cement type on the debonding time of the ceramic restoration using the Er:YAG laser. OBJECTIVES: To evaluate and compare the time required for the Er:YAG laser to debond zirconia and lithium disilicate crowns bonded with a 2- and 1-bottle adhesive resin cement systems. MATERIALS AND METHODS: Forty extracted premolar teeth were prepared and scanned for milled 40 CAD/CAM crowns. Teeth were randomly assigned into groups (n = 10 per group): 3 mol% yttria-partially stabilized zirconia crowns 3Y-PSZ (G1a) bonded with Panavia™ V5 (2-bottle adhesive resin cement), Zirconia 3Y-PSZ crowns (G1b) bonded with RelyX™ Ultimate (1-bottle adhesive resin cement), and for the lithium disilicate crowns bonded with the two types of cements (G2a, G2b). Each specimen was irradiated with an Er:YAG laser at 335 mJ, 15 Hz, 5.0 W, and 50-ms pulse duration (super short pulse mode). The irradiation time required for crowns to be successfully debonded was recorded for each specimen. Data were statistically analyzed using ANOVA and Tukey HSD post-hoc test (p < 0.05), at the 95 percent level of confidence. The intaglio surface of the debonded crown was analyzed using scanning electron microscopy (SEM). RESULTS: The mean ± standard deviation times needed for crown debonding were 5.75 ± 2.00 min for the G1a group, 4.79 ± 1.20 min for group G1b, 1.69 ± 0.49 min for group G2a, and 1.12 ± 0.17 for group G2b. There was no statistically significant difference in debonding time between the 2- and 1- bottle adhesive resin cement within the groups G1a and b (p = 0.2914), or between groups G2a b (p = 0.7116). A statistically significant difference (p < 0.05) was found between groups G1a and G2a and b and between groups G1b and G2a and b were SEM analysis showed no changes in the microstructure of the ceramic surface after Er:YAG laser irradiation. CONCLUSION: Zirconia and lithium disilicate restorations can be debonded using Er:YAG lasers in a safe and efficient manner. There is no significant difference in the debonding time between the 2- and 1- bottle adhesive resin cement systems used in this study. CLINICAL SIGNIFICANCE: Retrieving zirconia and lithium disilicate ceramics can be a challenging process when using diamond rotary instruments. ER:YAG lasers may efficiently debond these ceramics from the tooth structure, independent of the bonding process used for bonding them.

Preparation of Fibrous Three-Dimensional Porous Materials and Their Research Progress in the Field of Stealth Protection.

Intelligent and diversified development of modern detection technology greatly affects the battlefield survivability of military targets, especially infrared, acoustic wave, and radar detection expose targets by capturing their unavoidable infrared radiation, acoustic wave, and electromagnetic wave information, greatly affecting their battlefield survival and penetration capabilities. Therefore, there is an urgent need to develop stealth-protective materials that can suppress infrared radiation, reduce acoustic characteristics, and weaken electromagnetic signals. Fibrous three-dimensional porous materials, with their high porosity, excellent structural adjustability, and superior mechanical properties, possess strong potential for development in the field of stealth protection. This article introduced and reviewed the characteristics and development process of fibrous three-dimensional porous materials at both the micrometer and nanometer scales. Then, the process and characteristics of preparing fibrous three-dimensional porous materials through vacuum forming, gel solidification, freeze-casting, and impregnation stacking methods were analyzed and discussed. Meanwhile, their current application status in infrared, acoustic wave, and radar stealth fields was summarized and their existing problems and development trends in these areas from the perspectives of preparation processes and applicability were analyzed. Finally, several prospects for the current challenges faced by fibrous three-dimensional porous materials were proposed as follows: functionally modifying fibers to enhance their applicability through self-cross-linking; establishing theoretical models for the transmission of thermal energy, acoustic waves, and electromagnetic waves within fibrous porous materials; constructing fibrous porous materials resistant to impact, shear, and fracture to meet the needs of practical applications; developing multifunctional stealth fibrous porous materials to confer full-spectrum broadband stealth capability; and exploring the relationship between material size and mechanical properties as a basis for preparing large-scale samples that meet the application's requirement. This review is very timely and aims to focus researchers' attention on the importance and research progress of fibrous porous materials in the field of stealth protection, so as to solve the problems and challenges of fibrous porous materials in the field of stealth protection and to promote the further innovation of fibrous porous materials in terms of structure and function.

Atomic-Scale Insights into the Effects of the Foaming Degree on the Glass-Ceramic Matrix Derived from Waste Glass and Incineration Bottom Ash.

Precise management of the inverse correlation between the total porosity and compressive strength is crucial for the progress of foaming glass-ceramics (FGCs). To deeply understand this relationship, we investigated the atomic-level transformations of five CO2-foaming FGC samples using molecular dynamics simulation. The short-range and intermediate-range structures of the FGCs with varying total porosities (36.68%, 66.28%, 66.96%, 72.21%, and 79.88%) in the system were elucidated. Na cations were observed to exhibit a strong interaction with CO2, accumulating at the surface of the pore wall and influencing the oxygen species. Therefore, the change in the atomic structure of the matrix was accompanied by an increase in the total porosity with an increasing CO2 content. Specifically, as the total porosity increased, the bridging oxygen content within the FGCs rose accordingly. However, once the total porosity exceeded 66.96%, the bridging oxygen content began to decline. This observation was significant considering the role of the bridging oxygen content in forming a continuous cross-linked network of chemical bonds, which contributed to the enhanced mechanical strength. Consequently, the influence of the total porosity on the oxygen species resulted in a two-stage reduction in the compressive strength. This study offers valuable insights for the development of high-strength lightweight FGCs.

Effect of Water-Soluble Polymers on the Rheology and Microstructure of Polymer-Modified Geopolymer Glass-Ceramics.

This work explores the effects of rigid (0.1, 0.25, and 0.5 wt. %) and semi-flexible (0.5, 1.0, and 2.5 wt. %) all-aromatic polyelectrolyte reinforcements as rheological and morphological modifiers for preparing phosphate geopolymer glass-ceramic composites. Polymer-modified aluminosilicate-phosphate geopolymer resins were prepared by high-shear mixing of a metakaolin powder with 9M phosphoric acid and two all-aromatic, sulfonated polyamides. Polymer loadings between 0.5-2.5 wt. % exhibited gel-like behavior and an increase in the modulus of the geopolymer resin as a function of polymer concentration. The incorporation of a 0.5 wt. % rigid polymer resulted in a three-fold increase in viscosity relative to the control phosphate geopolymer resin. Hardening, dehydration, and crystallization of the geopolymer resins to glass-ceramics was achieved through mold casting, curing at 80 °C for 24 h, and a final heat treatment up to 260 °C. Scanning electron microscopy revealed a decrease in microstructure porosity in the range of 0.78 µm to 0.31 µm for geopolymer plaques containing loadings of 0.5 wt. % rigid polymer. Nano-porosity values of the composites were measured between 10-40 nm using nitrogen adsorption (Brunauer-Emmett-Teller method) and transmission electron microscopy. Nanoindentation studies revealed geopolymer composites with Young's modulus values of 15-24 GPa and hardness values of 1-2 GPa, suggesting an increase in modulus and hardness with polymer incorporation. Additional structural and chemical analyses were performed via thermal gravimetric analysis, Fourier transform infrared radiation, X-ray diffraction, and energy dispersive spectroscopy. This work provides a fundamental understanding of the processing, microstructure, and mechanical behavior of water-soluble, high-performance polyelectrolyte-reinforced geopolymer composites.

Effect of the CAD/CAM Milling Protocol on the Fracture Behavior of Zirconia Monolithic Crowns.

Although advancements in CAD/CAM technology allow for more personalized treatments, it is not clear how modifications in the CAD/CAM milling process could affect the restoration surface conditions and their mechanical behavior. The objective of this study was to evaluate the effect of different CAD/CAM milling protocols on the topography and fracture behavior of zirconia monolithic crowns (3Y-PSZ) subjected to a chewing simulation. Monolithic 3Y-PSZ premolar crowns were milled using three protocols (n = 13) (slow (S), normal (N), and fast (F)). Crowns were cemented on a dentin analog abutment and subjected to mechanical aging (200 N, 2 Hz, 1,500,000 cycles, 37 °C water). Surviving crowns were subjected to compressive load test and analyzed using fractography. Fracture load data were analyzed with two-parameter Weibull analysis. The surface topography of the crowns was examined with a stereomicroscope and a 3D non-contact profiler. All crowns survived the chewing simulation. Crowns milled using the F protocol had the greatest characteristic fracture load, while crowns produced with the S protocol showed high Weibull modulus. Groups N and S had a more uniform surface and detailed occlusal anatomy than group F. The CAD/CAM milling protocol affected the topography and mechanical behavior of 3Y-PSZ monolithic crowns.

Sophisticated Structural Ceramics Shaped from 3D Printed Hydrogel Preceramic Skeleton.

Shaping ceramic materials into sophisticated architecture with 3D hierarchical structure is desirable in multiapplication yet remains challenge due to their brittle and stiff nature. Herein, a new method to achieve ceramic architectures with unsupported and large-spanning structure by shaping vat photopolymerization 3D printed hydrogel preceramic skeleton with unique flexible and deformable character is proposed. Specifically, the present photopolymerizable hydrogel preceramic achieves one stone, two birds: the photosensitive polymer matrix coupled with ceramic nanoparticles for the first shaping by vat photopolymerization 3D printing and the secondary plasticity of the 3D printed ceramic body through flexible shape deformation of hydrogel networks. Inorganic binder aluminum dihydrogen phosphate serves as hydrogel dispersion medium to achieve ultralow shrinkage photopolymerization ceramic. Compared with conventional polymer-derived photocuring ceramics, the linear shrinkage of lamina structure is solely 2%, and which of cubic ceramic structure is just 13.3%. More importantly, one 3D printed preceramic is conducted to reshape repeatedly myriad constructions, realizing reusability of intrinsic brittle ceramic, improving manufacturing fault tolerance rate. Finally, a variety of paradigms for ceramic structure applications are proposed toward stereo circuit, biomedicine, and catalytic applications, breaking the limitation of intrinsic brittleness of ceramic in high-precision manufacturing of complex ceramic devices.

Brittle-Ductile Threshold in Lithium Disilicate under Sharp Sliding Contact.

Computer-aided design (CAD)/computer-aided manufacturing (CAM) milling and handpiece grinding are critical procedures in the fabrication and adjustment of ceramic dental restorations. However, due to the formation of microfractures, these procedures are detrimental to the strength of ceramics. This study analyzes the damage associated with current brittle-regime grinding and presents a potential remedy in the application of a safer yet still efficient grinding regime known as "ductile-regime grinding." Disc-shaped specimens of a lithium disilicate glass-ceramic material (IPS e.max CAD) were obtained by cutting and crystallizing the lithium metasilicate CAD/CAM blanks (the so-called blue blocks) following the manufacturer's instructions. The discs were then polished to a 1 µm diamond suspension finish. Single-particle micro-scratch tests (n = 10) with a conical diamond indenter were conducted to reproduce basic modes of deformation and fracture. Key parameters such as coefficient of friction and penetration depth were recorded as a function of scratch load. Further, biaxial flexure strength tests (n = 6) were performed after applying various scratch loads to analyze their effects on ceramic strength. Scanning electron microscopy (SEM) and focused ion beam (FIB) were used to characterize surface and subsurface damage. Statistical analysis was performed using one-way analysis of variance and Tukey tests. While the SEM surface analysis of scratch tracks revealed the occurrence of both ductile and brittle removal modes, it failed to accurately determine the threshold load for the brittle-ductile transition. The threshold load for brittle-ductile transition was determined to be 70 mN based on FIB subsurface damage analyses in conjunction with strength degradation studies. Below 70 mN, the specimens exhibited neither strength degradation nor the formation of subsurface cracks. Determination of the brittle-ductile thresholds is significant because it sets a foundation for future research on the feasibility of implementing ductile-regime milling/grinding protocols for fabricating damage-free ceramic dental restorations.