Low-temperature Degradation Research Articles

A Novel Cold-Adapted Nitronate Monooxygenase from Psychrobacter sp. ANT206: Identification, Characterization and Degradation of 2-Nitropropane at Low Temperature

Aliphatic nitro compounds cause environmental pollution by being discharged into water with industrial waste. Biodegradation needs to be further explored as a green and pollution-free method of environmental remediation. In this study, we successfully cloned a novel nitronate monooxygenase gene (psnmo) from the genomic DNA library of Psychrobacter sp. ANT206 and investigated its ability to degrade 2-nitropropane (2-NP). Homology modeling demonstrated that PsNMO had a typical I nitronate monooxygenase catalytic site and cold-adapted structural features, such as few hydrogen bonds. The specific activity of purified recombinant PsNMO (rPsNMO) was 97.34 U/mg, rPsNMO exhibited thermal instability and reached maximum catalytic activity at 30 °C. Moreover, rPsNMO was most active in 1.5 M NaCl and remained at 104% of its full activity in 4.0 M NaCl, demonstrating its significant salt tolerance. Based on this finding, a novel bacterial cold-adapted enzyme was obtained in this work. Furthermore, rPsNMO protected E. coli BL21 (DE3)/pET28a(+) from the toxic effects of 2-NP at 30 °C because the 2-NP degradation rate reached 96.1% at 3 h and the final product was acetone. These results provide a reliable theoretical basis for the low-temperature degradation of 2-NP by NMO.

Realizing near-full density monophasic tetragonal 1.5-mol% yttria-stabilized zirconia ceramics via current-ramp flash sintering

This study demonstrates the successful fabrication of near-full density monophasic tetragonal 1.5-mol% yttria-stabilized zirconia (1.5YSZ) ceramics using current-ramp flash (CRF) sintering technique. The process involved regulating Joule heating in the samples by fine-tuning the input power through an alternating current field (nominal current density: 50 mA·mm−2) within a 3-minute timeframe at a furnace temperature of 1100°C. This approach effectively enhanced grain size uniformity, which is crucial for preventing sample cracking associated with spontaneous tetragonal-to-monoclinic (T→M) phase transformation, thereby promoting densification with average relative densities exceeding 99%. The highest average fracture toughness of the 1.5YSZ samples was measured at 9.2 MPa·m0.5 using the standardized single-edge pre-cracked beam method. This toughness is approximately double that of commonly used 3YSZ samples produced by CRF sintering, all of which exhibited comparable average grain sizes and relative densities. Additionally, the 1.5YSZ samples demonstrated nearly identical resistance to low-temperature degradation (LTD) compared to the 3YSZ samples after accelerated hydrothermal aging at 140°C for 15 hours, roughly equivalent to 60 years at 37°C. The reduced yttria concentration in 1.5YSZ facilitates T→M phase transformation at lower stress thresholds, enhancing toughness through increased crack shielding from a larger volume fraction of transformed grains. Furthermore, the uniform yttria distribution in 1.5YSZ, revealed by scanning transmission electron microscopy, compensates for the reduced tetragonal phase stability and contributes to improved LTD resistance. Notably, these exceptional properties were achieved at a furnace temperature 300°C lower and with a sintering duration several hours shorter than those of conventionally-sintered counterparts.

Investigation of Phase Transformation and Fracture Pattern as a Result of Long-Term Chewing Simulation and Static Loading of Reduced-Diameter Zirconia Implants.

While zirconia implants exhibit osseointegration comparable to that of titanium, concerns arise regarding low-temperature degradation and its potential impact on fracture strength. This study investigated the phase transformation and fracture characteristics of zirconia dental implants after aging through chewing simulation and subsequent static loading. The experimental setup involved 48 one-piece monobloc zirconia implants with diameters of 3.0 mm and 3.7 mm that had straight or angled abutments, with crown restorations, which were divided into six groups based on intraoral regions. The specimens underwent chewing simulation equal to five years of oral service, which was followed by static loading. Statistical analyses were performed for the data obtained from the tests. After dynamic and static loadings, the fractured samples were investigated by Raman spectroscopy to analyze the phase composition and micro-CT to evaluate fracture surfaces and volume changes. According to the results, narrow-diameter zirconia implants have low mechanical durability. The fracture levels, fracture patterns, total porosity, and implant fracture volume values varied according to the implant diameter and phase transformation grade. It was concluded that phase transformation initially guides the propagation of microcracks in zirconia implants, enhancing fracture toughness up to a specific threshold; however, beyond that point, it leads to destructive consequences.

Fatigue strength of bilayer yttria-stabilized zirconia after low-temperature degradation

This study examined the impact of interfacial interactions on bilayer yttria-stabilized zirconia (YSZ) used in dental restorations. In-house bilayer structures of 3YSZ and 5YSZ composition underwent hydrothermal degradation to compare the properties of control and low-temperature degradation (LTD) treated groups. Biaxial flexural strength via piston-on-three-balls, staircase fatigue strength over 106 cycles at 15 Hz, phase characterization and quantification through XRD and Rietveld refinement, and fractography were conducted. Weibull analysis was employed to determine the Weibull modulus and characteristic strength. Results demonstrated an enhancement in the mechanical performance of 3YSZ composition after LTD treatment, whereas the mechanical properties of 5YSZ remained largely unaffected post-degradation. Fractographic analysis revealed that failure originated at the surface tensile location across all specimen groups. These findings offer insights into the mechanical behavior of bilayer zirconia structures and reinforce the significance of hydrothermal treatment in enhancing their performance, particularly in the case of 3Y compositions.

Frost heaving and crack initiation characteristics of tunnel rock mass in cold regions under low-temperature degradation

Frost heaving and crack initiation characteristics of tunnel rock mass in cold regions under low-temperature degradation

Nanomechanical and microstructural properties of experimental bilayered zirconia ceramics after hydrothermal aging

Two experimental ceramic systems, 3Y-TZP/5Y-PSZ (3Y/5Y) and 4Y-PSZ/5Y-PSZ (4Y/5Y), underwent analysis before (3Y/5Yi or 4Y/5Yi) and after hydrothermal aging (3Y/5Ya or 4Y/5Ya) to simulate low-temperature degradation (LTD). The samples were sintered and characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), and Raman spectroscopy, alongside nanoindentation tests to measure elastic modulus (Em) and hardness (H). Assessments were conducted on the external surfaces and at individual layers on cross-sectioned samples at predetermined regions of interest (ROIs). Degraded superficial regions were observed in the cross-sectional SEM images of the 3Y and 4Y zirconia layers after aging. XRD indicated a tetragonal→monoclinic phase transformation in the aged groups for both 3Y (66 % m-ZrO2) and 4Y (29 % m-ZrO2). Raman spectroscopy revealed monoclinic phase amounts of 86 % for 3Y and 62 % for 4Y in the degradation regions observed in the SEM micrographs. Monoclinic phase peaks were virtually no longer detected in either material beyond a depth of 15 μm. Hydrothermal aging significantly diminished the H and Em values for the 3Y and 4Y zirconia surfaces. For the analysis of different zirconia surfaces within the same subgroup, all pairwise comparisons showed statistically significant differences, except for the values of H of 3Y/5Yi and Em for 4Y/5Yi. Regarding the nanoindentation results of cross-sectioned samples, the aging protocol did not affect the H and Em values of the equivalent ROIs (layers), regardless of the bilayered system. However, significant differences in H values were observed among the ROIs (layers) within the same bilayered system. Despite surface changes, nanomechanical properties remained preserved below the surface and at the interfaces of bilayered materials after aging. Nanoscale H values varied among some layers and interfaces, whereas the Em values exhibited differences across certain surfaces.

Effect of Hydrothermal, Chemical, and Mechanical Degradation on Flexural Strength and Phase Transformation of Ground, Glazed, and Polished Zirconia.

Objectives: Evaluation of the effect of grinding on flexural strength of zirconia after low temperature degradation (LTD) and pH-cycling. Materials and Methods: Sixty-four bar-shaped specimens of yttria-stabilized tetragonal polycrystalline zirconia were milled, sintered, wet-polished, and divided into 8 groups (N=8). The four control groups were not aged while artificial aging was performed in the 4 experimental groups in three steps including LTD in steam for 40h, pH-cycling, and tooth brushing for artificial aging. All groups underwent surface preparations as follows: standard polishing without surface treatment (Sp), grinding with a blue-yellow band diamond instrument (Gr); grinding with a diamond rotary instrument (DRI) and then over-glazing (Gl); grinding with a DRI followed by two-step intraoral polishing (Po); standard polishing and aging (Sp-Ag); grinding and aging (Gr-Ag), grinding, over-glazing and aging (Gl-Ag); and grinding, polishing and aging (Po-Ag). Monoclinic content was assessed in one specimen of each group by X-ray diffraction (XRD). The 3-point flexural strength test was performed in a universal testing machine. The results were analyzed with two-way ANOVA and Tukey's test (α=0.05). Results: Mean flexural strength (Mpa) was significantly higher in groups Gr and Po compared to group Sp (both, P<0.0001) and group Gl (both, P<0.0001). In XRD analyses, the highest monoclinic phase before aging was observed in group Gr (12.6%), and after aging in group Gr-Ag (51.2%). Conclusion: Grinding and polishing increased the flexural strength, while glazing did not exhibit any significant effect on this parameter. Furthermore, aging did not adversely affect flexural strength.

Cyclic fatigue behavior of Y‐TZP nanostructures with non‐homogeneous yttria distribution

AbstractNanostructured Y‐TZP samples with Non‐Homogeneous Yttria Distribution (NNHYD) were prepared by mixing co‐precipitated 3Y‐TZP powder (Tosoh TZ‐3Y) with yttria‐free monoclinic powder (Tosoh TZ‐0), yielding an overall yttria content of 2 mol%. The cyclic fatigue behavior of NNHYD was evaluated by Step‐Stress Accelerated Life Testing (SSALT) and mechanical cycling in a biaxial flexural strength test (BFST) setup and compared to Conventional Submicrometric 3Y‐TZP (CS). Physical, structural, microstructural, and mechanical characterizations of all groups were also evaluated and compared before and after artificial aging in autoclave. NNHYD presented a higher capacity for damage accumulation and maintenance of phase transformation potential than CS, associated with elevated resistance to the propagation of Low‐Temperature Degradation (LTD). A nanostructured 3Y‐TZP surface layer introduced in NNHYD by dip coating (DC‐NNHYD) improved resistance to LTD at the cost of reduced reliability under cyclic fatigue by increasing the stability of the tetragonal phase. This surface alteration highlights the impact of surface properties on mechanical performance. The results of this study present practical possibilities to help achieve the ideal balance between strength, toughness, and LTD resistance to improve the lifetime of zirconia‐based biomaterials.

Dielectric probing of low-temperature degradation resistance of commercial zirconia bio-ceramics

ObjectivesTo investigate the effect of the stability of oxygen vacancies on the low-temperature degradation (LTD) resistance of two kinds of commercial zirconia-based materials (3Y-TZP ceramics and Ce-TZP/Al2O3 composites) via the dielectric probing methods. MethodsThe commercial 3Y-TZP ceramics and Ce-TZP/Al2O3 composites were prepared via conventional solid-state methods. Density, phase content, microstructure, strain, and biaxial flexural strength (BFS) of two materials were investigated using Archimedes method, XRD, SEM, strain-electric field (S-E) loops and ball-on-ring methods, respectively. The concentration of oxygen vacancies before and after LTD of two materials were evaluated using dielectric probing and XPS methods. ResultsThe XRD analysis revealed that compared to the 3Y-TZP ceramics, the Ce-TZP/Al2O3 composites showed better LTD resistance, without clear LTD. The greater LTD resistance for Ce-TZP/Al2O3 composites was associated with their stability of oxygen vacancies, by higher activation energy based on the dielectric measurements and XPS results. For the 3Y-TZP ceramics that underwent the tetragonal to the monoclinic phase transition during the LTD treatment, the concentration of their oxygen vacancies decreased after LTD. In addition, the Ce-TZP/Al2O3 composites exhibited higher flexural strength and potential fracture toughness based on the BFS testing and strain vs electric field measurement results, indicating a great potential for use in fixed restorative dental applications. SignificanceThis work suggested the stability of oxygen vacancies played a key role in the resistance to LTD. Optimizing the stability of the oxygen vacancies is key to the development of more reliable zirconia- based dental biomaterials with greater resistance to LTD.

Development and characterization of Al2O3/SrAl12O19 reinforced zirconia with high fracture toughness and low-temperature degradation-resistant for dental applications

The low fracture toughness and sensitivity to low-temperature degradation (LTD) are the primary reasons for the suboptimal long-term performance of dental zirconia. Composite ceramics of zirconia have gained popularity due to their ability to combine the benefits of various reinforcements. In this study, Al2O3–SrAl12O19–3Y/4Y/5Y–ZrO2 composite ceramics were fabricated using the Pechini method, and the optimal sintering temperature and time were investigated. The relative density, microstructure, grain size, mechanical properties, and LTD resistance of the samples were characterized. The results indicated that the composite achieved optimal performance when sintered at 1500 °C for 3 h. Al2O3 and SrAl12O19 primarily influence the properties of the zirconia composite ceramics by modulating their density and grain size. With an increase in the content of Al2O3 and SrAl12O19, the relative density first increases and then decreases, while the grain size exhibits an inverse trend, resulting in an initial increase followed by a decrease in fracture toughness. Additionally, the rate of increase in the m-phase fraction of the zirconia composite slowed down, but it reached a similar level after 64 h of LTD. The incorporation of 8 vol% Al2O3 and 8 vol% SrAl12O19 into 3Y–ZrO2 resulted in a ceramic composite with the highest fracture toughness values and acceptable LTD sensitivity, measured at 5.23 ± 0.25 MPa m1/2 and 48.35 ± 5.70% m-phase (LTD 64 h), respectively. This composite also exhibited high bending strength (990.09 MPa) and hardness (16.52 GPa), making it a promising alternative to conventional 3Y-TZP ceramics commonly used in dentistry.

Sintering, mechanical properties and hydrothermal resistance of ZrO2/ZrSiO4 slip cast composites

Yttria-doped tetragonal zirconia polycrystalline (Y-TZP) is one of the most widely used materials in thermal applications and as a structural component due to its mechanical properties. Its drawbacks are the high cost of the starting raw materials and its polymorphic transformation to monoclinic phase associated with the occurrence of mechanical failures. In the present work, tetragonal zirconia materials were obtained by slip casting and also ZrO2/ZrSiO4 composites by partially replacing the zirconia with low cost and high corrosion resistance zircon. The different parts showed a high microstructural homogeneity, as well as high hardness and Young's modulus (up to 16.7 and 354 GPa, respectively), even with the incorporation of 20 vol% zircon. The zircon-containing composites subjected to hydrothermal low-temperature degradation (LTD) at 205 °C for 240 h exhibited similar mechanical properties, unaffected microstructural integrity, and a crystallographic phase composition equal to the as-sintered samples, without phase transformation from t-ZrO2 to m-ZrO2.

Phase transformations in yttria-partly stabilized zirconia induced by dental polishing regimes

The study examined how three polishing methods, using equipment from NTI CeraGlaze (NTI), Komet Dental (Komet), and EVE Diacera (EVE) and employing either wet or dry grinding, affect the texture (roughness) and phase composition of Y-PSZ dental crowns. Dental crowns made from VITA’s 3Y-/4Y-/5Y-partly stabilized zirconia (Y-PSZ; YZ-HT/ST/XT), utilizing a standard CAD/CAM process, underwent both wet or dry grinding and polishing. The effects of distinct polishing treatments on Y-PSZ surface phase content were investigated using X-ray diffraction (XRD) and Rietveld refinement, the grain size was measured by field emission scanning electron microscopy (FE-SEM), and confocal scanning laser microscopy (CLSM) was used to determine the surface roughness as the arithmetical mean height (Sa). To analyse the different mode of action, the components of the polishers were analysed using XRD, along with micro X-ray computer tomography (µXCT), FE-SEM, and CLSM for microstructural examination. The Komet and NTI polishing regimes reduced roughness significantly better than the EVE regime for the 3Y and all wet specimens, but caused a rhombohedral phase fraction. A possible explanation for this result is the overall finer structure of the EVE coarse polisher (abrasive particle size and content, texture density), which probably results in a lower force on the Y-PSZ surface. Therefore, the rhombohedral phase boundary would not be reached. Due to rhombohedral phase having larger volume expansion and shear than the monoclinic phase, it may result in enhanced transformation toughening or detrimental low-temperature degradation effects.Graphical abstract

Influence Of Low-Temperature Degradation On Phase Transformation And Biaxial Flexural Strength On Different High-Translucent 4Y-PSZ, 5Y-PSZ, 6Y-PSZ Monolithic Zirconia

Objective: This study aimed to investigate the effect of low-temperature degradation (LTD) in phase transformation and biaxial flexural strength of high-translucent yttria partially stabilized zirconia (Y-PSZ) and yttria tetragonal zirconia polycrystalline (3-YTZP).&#x0D; Methods: A total of 120 new high-translucent 3-YTZP (NMS) and Y – PSZ (KST, KUT, NQ3MS) zirconia disc specimens were manufactured according to ISO 6872 for biaxial flexural strength (14 mm., 1.2 ± 0.02 mm). The specimens from each type of material were divided into 3 subgroups (n:30) according to the LTD in an autoclave at 134 C0 at 2 bar (n:10) (at 5, 20 hour (h)). Specimens without LTD served as the control. Data of the monoclinic phase changes (Xm) and flexural strength were analyzed using two-way ANOVA followed by post hoc MannWhitney U test. Weibull statistics were used to analyze strength reliability.&#x0D; Results: LTD increased the monoclinic content significantly for NMS and slightly for the KST group. A monoclinic phase was not detected for KUT and NQ3MS groups. The biaxial flexural strength of the NMS group was affected significantly and decreased with an increase in the 20 h aging. For flexural strength values, there was no significant difference in aging times for each of the KST, KUT, and NQ3MS groups. Weibull analysis showed the highest characteristic strength for NMS (1412.9), KST (750.1), NQ3MS(790.5) and KUT (615.2) groups. The Weibull modulus (m) increased in the NMS, KUT, and NQ3MS groups compared with the control group and decreased in the KST group.&#x0D; Conclusion: LTD caused a significant decrease in the biaxial flexural strength results of the NMS group but did not significantly affect the KST, KUT, and NQ3MS groups’ values.

Preparation and properties optimization of CeO2–Y2O3 Co-stabilized zirconia via vat photopolymerization

Employed ubiquitously in oral restorations, zirconia-based bioceramics face challenges with low-temperature degradation (LTD) in the tetragonal phase (t-ZrO2) within oral environments. In order to improve the resistance of ZrO2 ceramics to LTD, this study utilized vat photopolymerization technology to prepare 7Ce3Y–ZrO2 (7 mol% CeO2 and 3 mol% Y2O3). By adjusting the dispersant content and photosensitive resin ratio enabled the attainment of a 63.5 μm curing depth with a 400 mJ/cm2 exposure, meeting the requirements for vat photopolymerization printing. After sintering at 1550 °C, these ceramics shown a relative density of 97.84 % and an impressive flexural strength of 503.1 MPa. Accelerated LTD tests were conducted to assess LTD-resistance, revealing no degradation in mechanical properties or evidence of tetragonal to monoclinic phase transitions. This stability is credited to the cerium ions' efficacy in hindering oxygen vacancy formation and subsequent aging within the ZrO2. This study affirms that CeO2–Y2O3 co-stabilized ZrO2 ceramics prepared using vat photopolymerization technology exhibit outstanding properties and resistance to LTD, showcasing significant potential in the field of oral restoration.

Effect of low-temperature degradation and sintering protocols on the color of monolithic zirconia crowns with different yttria contents.

This study investigated the effects of low-temperature degradation (LTD) on the L*, a*, and b* values of highly translucent zirconia crowns. Four types of zirconia disks with different yttria contents (IPS e.max ZirCAD LT, IPS e.max ZirCAD MT, IPS e.max ZirCAD MT Multi, IPS e.max ZirCAD Prime, Ivoclar) and two shades (A2 and BL) were used. A crown was manufactured using four types of zirconia and LTD treated. Color measurements were performed, and the color difference (ΔE00) before and after LTD was calculated. The microstructure was determined through X-ray fluorescence and X-ray diffractometry. Highly translucent zirconia crowns showed greater changes in the a* and b* values than in the L* value after LTD, regardless of the shade. The Multi2 crowns exhibited a discernible color change due to the LTD treatment. The X-ray fluorescence results did not reveal any apparent change in the microstructure between sintering programs for all zirconia specimens.

Unveiling the confinement and interface effect on low temperature degradation of toluene over mesoporous zeolite encapsulated Pt-CeO2 catalyst

The efficient degradation of volatile organic compounds (VOCs) at low temperatures is urgently needed due to the serious environmental and health hazards they pose. While precious metal-based catalysts offer excellent performance, their application is limited by high-temperature sintering and aggregation. Therefore, inhibiting the migration and aggregation of precious metals during the reaction process can effectively improve their utilization and alleviate catalyst deactivation. In this study, a novel encapsulated catalyst (Pt-CeO@meso-S1) containing Pt-CeO2 interfaces was constructed using mesoporous-rich zeolite as a shell layer and applied to the catalytic oxidation of toluene. The introduction of CeO2 constructed a Pt-CeO2 active interface that promoted the low-temperature degradation of toluene, achieving complete oxidation of toluene at 160 ℃. The crystalline phase transition strategy enhanced the specific surface area, improving the dispersion of platinum and facilitating the construction of the Pt-CeO2 interface. The zeolite shell and mesoporous pores effectively confined/stabilized the Pt-CeO2 active components and inhibited platinum sintering, resulting in outstanding water resistance and high-temperature stability. DFT calculations demonstrated that the presence of the Pt-CeO2 active interfaces reduced oxygen vacancy formation energy and facilitated gas-phase oxygen activation. DFT calculations demonstrated that the presence of the Pt-CeO2 active interfaces reduces the oxygen vacancy formation energy and boosts the activation of gas-phase oxygen. The Mars-van-Krevelen (MvK) mechanism governing toluene degradation over Pt-CeO2@meso-S1 was revealed by in situ DRIFTS. This work provides a promising candidate for industrial high-performance catalytic removal of VOCs at low temperatures.

Effect of grain boundary segregation and oxygen vacancy annihilation on aging resistance of cobalt oxide-doped 3Y-TZP ceramics for biomedical applications

Abstract This study aims to investigate the diffusion stabilization process of nano-Co2O3 during the non-precursor transformation of 3Y-TZP. 3Y-TZP was set as the control group, and the experimental groups were 0.1–0.3 mol% nano-Co2O3-doped 3Y-TZP. The samples were prepared by the ball milling process, isostatic cool pressing, and sintering. All samples were hydrothermally treated at 134°C and 2 bar for different time periods. The resistance to low-temperature degradation of nano-Co2O3-doped 3Y-TZP was analyzed by X-ray diffraction. The microstructure of zirconia ceramic samples was determined by scanning electron microscopy, transmission electron microscopy, atomic force microscopy, and electron paramagnetic resonance studies. The addition of nano-Co2O3 into 3Y-TZP resulted in higher hydrothermal aging resistance than 3Y-TZP. The addition of 0.2 mol% nano-Co2O3 dopants resulted in the highest hydrothermal aging resistance among nano-Co2O3-doped 3Y-TZP ceramics. The grain sizes of 3Y-0.2Co are smaller than those in the control group. With the increase of cobaltous oxide doping contents, the segregation of Co3+ ions at the crystal boundary increased. The content of oxygen vacancies on the surface of the sample increased with the increase of the Co2O3 doping content. The oxygen vacancy concentrations of 3Y-0.2Co increased obviously after aging. 3Y-0.1Co, 3Y-0.3Co, and the control showed decreased oxygen vacancy concentrations after aging. Trivalent element doping of 3Y-TZP effectively improved the aging resistance of 3Y-TZP. The addition of 0.2 mol% nano-Co2O3 resulted in the highest hydrothermal aging resistance. Improved aging resistance is attributed to the nano-Co2O3 doping resulting in the 3Y-TZP grain size inhibition, grain boundary segregation of cobalt ions, and oxygen vacancy maintenance. This work is expected to provide an effective reference for the development and application of budget dental materials by regulating grain boundary engineering.

Effect of speed sintering and aging on the translucency of high-translucent zirconia.

This work aimed to evaluate the effect of speed sintering and low-temperature degradation on the translucency of high-translucent zirconia. The ST and TT specimens were randomly divided into two groups depending on the sintering process: conventional sintering and speed sintering. The sintered specimens were divided into three subgroups according to the aging time: aged for 0, 5, and 20 h. Chromatic parameters (L*, a*, and b* values) were measured by Shade Eye NCC computer colorimeter in a dark environment under black and white background, and the translucency parameter (TP) was used to evaluate the translucency of zirconia. Speed sintering may decrease the TP of ST and increase the TP of TT. As for the effect of low-temperature degradation on the translucency of zirconia, the TP of ST decreased with the extension of aging time, and no significant difference was found in rapid sintering ST. Although the TP of TT decreased, no statistical difference was observed. Speed sintering may decrease the translucency of high-strength zirconia and increase the translucency of high-translucent zirconia. Low-temperature degradation had no effect on the translucency of high-translucent zirconia. Speed sintering can be recommended for high-translucent zirconia in terms of translucency.

Effect of low-temperature degradation on the fatigue performance of dental strength-gradient multilayered zirconia restorations

ObjectivesFatigue and low-temperature degradation (LTD) are the main factors contributing to zirconia restoration failure. This study evaluated the effect of LTD on the fatigue performance of the novel “strength & shade-gradient” multilayered zirconia restorations. MethodsDiscs (15 mm × 1.2 mm) of each yttria content layer from a newly developed strength-gradient multilayered zirconia were fabricated and under accelerated aging in an autoclave at 134℃ for 0 h, 32 h, and 64 h. Then, the phase transformation, microstructure, and mechanical properties after LTD were assessed. In addition, the crown samples, including the multi-Zir, 3Y-Zir, and 5Y-Zir were fabricated, and their monotonic and fatigue load before and after LTD, percentage of fatigue degradation (Sd) and the fracture morphology were investigated. Statistical analyses were performed using paired samples t-test (α′ = α/3 = 0.017), one-way ANOVA and Weibull analysis. ResultsAfter LTD, the phase transformation, surface roughness, depth of transformed zone, and residual stress were increased and inversely associated with the yttria content. The indentation elastic modulus and hardness after LTD decreased; however, there was no significant difference between the different yttria content layers. The monotonic and fatigue load of multi-Zir restorations decreased, but their Weibull modulus increased, and Sd decreased, similar to 3Y-Zir. The crack origin was associated with the cervical region. ConclusionThese results show that although LTD reduces the absolute fatigue strength of strength-gradient multilayered zirconia restorations, it also reduces the effect of cyclic fatigue itself on the strength of zirconia (relative to monotonic strength), which might be due to the increase of residual stress. Clinical significanceThe novel “strength & shade-gradient” multilayered zirconia restorations show a promising performance during in vitro LTD and fatigue test and their reliability to some extent is comparable to 3Y-Zir. Yet, further in vivo longitudinal studies are warranted to confirm their precise performance.

Low-temperature degradation of waste epoxy resin polymer improved by swelling-assisted pyrolysis

The disposal of waste epoxy resin matrix composite becomes an urgent issue, and pyrolysis is an effective method to decompose the epoxy resin polymer, but the high operating temperature hinders its application. In this study, a swelling-assisted pyrolysis method was proposed for the low-temperature decomposition of epoxy resin. It was found that the degradation ratio of epoxy resin increased from 59.13 % to 79.10 % at 300 °C after the swelling treatment with acetic acid. Compared with traditional pyrolysis, the cracking of epoxy resin was promoted in the swelling-assisted pyrolysis, increasing the yields of pyrolysis gas and oil, as well as enriching the light components in pyrolysis oil and raising the graphite degree of pyrolysis char. Following the characterizations and reactive force field molecular dynamics (ReaxFF-MD) simulation, the key mechanisms of swelling-assisted pyrolysis were determined as the interaction of the enhanced heat transfer and the accelerated ring-open reactions. After the swelling treatment, epoxy resin became porous, improving the heat transfer in the pyrolysis process. Meanwhile, abundant O radicals were generated with the decomposition of acetic acid, accelerating the ring-open reactions of benzene rings. The results could provide promising guidance for the pyrolysis recovery of epoxy resin matrix composites towards the circular economy.