Tetragonal Zirconia Polycrystals Research Articles

Electric Current Dependence of Plastic Flow Behavior with Large Tensile Elongation in Tetragonal Zirconia Polycrystal Under a DC Field

This study systematically investigated the electric direct current (DC) dependence of the plastic flow behavior in a densified tetragonal ZrO2 polycrystal (TZP). Consequently, we observed an optimal current density for tensile ductility. The maximum elongation of 135% was achieved under the current density of 250 mA∙mm−2 at a furnace temperature of 1000 °C and an initial strain rate of 1 × 10

Study of the Fracture Behavior of Tetragonal Zirconia Polycrystal with a Modified Phase Field Model.

The superior fracture toughness of zirconia is closely correlated with stress-induced martensitic phase transformation around a crack tip. In this study, a modified phase field (PF) model coupling phase transformation and fracture is proposed to study the fracture behavior and toughening effect of tetragonal zirconia polycrystal (TZP). The stress-induced tetragonal to monoclinic (t–m) phase transformation around a static or propagating crack is characterized with PF simulations. It is shown that the finite size and shape of the transformation zone under different loads and ambient temperatures can be well predicted with the proposed PF model. The phase transformation may decrease the stress level around the crack tip, which implies the toughening effect. After that, crack propagation in TZP is studied. As the stress field is perturbed by the phase transformation patterns, the crack may experience deflection and branching in the propagation process. It is found that the toughness of the grain boundaries (GBs) has important influences on the crack propagation mode. For TZP with strong GBs, the crack is more likely to propagate transgranularly while, for TZP with weak GBs, intergranular crack propagation is prevalent. Besides that, the crystal orientation and the external load can also influence the topology of crack propagation.

Effect of gadolinia addition on the mechanical and physical properties of zirconia/ceria ceramics

In this work, zirconia powders containing 5 and 10 mol % ceria were prepared by co-precipitation method followed by doping with small amounts (< 1 mol %) of gadolinia which stabilized the tetragonal phase. X-ray diffraction and scanning electron microscopy were used for phase analysis and microstructure examination, respectively. The sintered compacts showed fine grained, dense, tough and strong ceramics. Strength up to 795.8 MPa and toughness of 17 MPa√m have been obtained. These ceramics showed higher toughness than yttria-doped tetragonal zirconia polycrystals (Y-TZP) and a higher strength than the ceria tetragonal zirconia polycrystals (Ce-TZP). The high fracture toughness was attributed to the tetragonal-to-monoclinic phase transformation which was associated with ferroelastic domain switching. The domain switching toughening has been discussed in view of Chevalier's model. Four-point bending strengths for the samples tested in the as cut state are higher than those tested in the as-sintered or the ground states.

The Retentive Strength of Zirconium Oxide Crowns Cemented by Self-Adhesive Resin Cements before and after 6 Months of Aging.

The aim of this study was to evaluate the retentive strength of zirconium oxide (yttria-stabilized tetragonal zirconia polycrystals (Y-TZP)) crown-copings treated by combined mechanical and chemical treatments and cemented by four types of self-adhesive resin cements (SARCs) to human prepared teeth, before and after six months of aging in water and thermocycling. A total of 120 molar teeth were mounted, prepared using a standardized protocol and digitally scanned, and Y-TZP copings were produced. Teeth were randomly assigned to four SARC groups. Prior to cementation, the intaglio surfaces of all crowns were sandblasted and then coated with Z-Prime™ Plus (Bisco Dental, Schaumburg, IL, USA). Post cementation, each cement group was subdivided into aged and non-aged groups. After aging, the cemented assemblies were tested for retentive strength using a universal testing machine. Failure analysis was conducted by inspecting all matched debonded surfaces of the teeth and crowns at 3× magnification. Aging treatment did not affect the retentive strength of the Y-TZP crown-copings (p = 0.918). The interaction between cement and aging was statistically significant (p = 0.024). No significant differences in the retentive strengths between the different SARCs were observed pre-aging (p = 0.776), whereas post-aging, Panavia SA (PAN; Kuraray Dental Co Ltd., Osaka, Japan) showed significantly higher strength than RelyX U-200 (RU200; 3M ESPE, Seefeld, Germany). The predominant failure mode was adhesive between the cement and dentin, followed by mixed mode failure.

Additive manufacturing of dense zirconia ceramics by fused deposition modeling via screw extrusion

A fused deposition modeling(FDM)system via screw extrusion suitable for feeding granular feedstocks with high solid loading was developed. Key parameters included aspect ratio of the screw, the compression ratio and pitch etc. In order to get constant extruded mass flow and wire diameter a processing window was determined by optimizing the barrel temperature, the nozzle diameter and the screwing speed. Microstructural characterization coupled with flexural strength measurement revealed that a higher printing temperature was beneficial to the inter layer bonding. The sintered zirconia ceramic samples with 99% of theoretical density of the 3 mol% yttria stabilized tetragonal zirconia polycrystal (3Y-TZP) and flexural strength of 890 ± 60 MPa was obtained. A set of zirconia ceramic parts with complex geometries and controllable dimensional accuracy was also successfully prepared for demonstrating the potential of the technique.

Fracture toughness enhancement of yttria-stabilized tetragonal zirconia polycrystalline ceramics through magnesia-partially stabilized zirconia addition

Abstract In this work, for the first time, we report a novel method on the fracture toughness enhancement of 3 mol % yttria-stabilized tetragonal zirconia polycrystalline (3Y-TZP) ceramics through the incorporation of 8 mol % magnesia-partially stabilized zirconia (8 Mg-PSZ) powders having high fracture toughness. Highly densified composites (x3Y-TZP/y8Mg-PSZ; where x and y vary between 0.25 and 0.75 wt. %) were obtained with a relative density over 99% by pressureless sintering. Relative density, Vickers hardness (HV) and indentation fracture toughness (KIc) were significantly improved by sintering temperature and dwell-time increment. Specifically, HV and KIc values of 0.5(3Y-TZP)/0.5(8 Mg-PSZ) composite sintered at 1500oC-2h were increased by 7% and 30%, respectively, compared to that of 3Y-TZP. Sintered bodies consisted of c-ZrO2, t-ZrO2 and m-ZrO2 phases without any new phase formation. m-ZrO2/c-ZrO2+t-ZrO2 volumetric phase ratios changed with the increase of sintering temperature and time. Stress-induced t-ZrO2→m-ZrO2 phase transformation within c-ZrO2 grains in 8 Mg-PSZ was the main mechanism for toughness enhancement. Energy absorbing mechanisms, e.g., crack-bridging, crack-deflection and crack branching were also found to contribute the blunting of cracks. It is thought that our approach presented herein can be considered not only fracture toughness enhancement but also other properties in various materials for functional and structural purposes.

Fabrication of an All-Ceramic Implant by Slip Casting of Nanoscale Zirconia Powder.

Dental implants are typically composed of 3Y-TZP (3 mol% yttria-stabilized tetragonal zirconia polycrystals). Most dental zirconia implants are currently fabricated via mechanical machining. However, during the machining of zirconia green bodies, many cracks form on the surface. To prevent surface crack formation on the implants, shape forming of the zirconia is necessary using methods such as slip casting. Herein, we fabricated green compacts using slip casting, candidate forming process to reduce surface cracking. To fabricate an optimal 3Y-TZP implant by slip casting and sintering, we prepared a suitable 3Y-TZP slurry for slip casting by adjusting the viscosity via pH, dispersant agent content, and solid loading refinement. Green compacts were prepared by the slip casting of all-ceramic zirconia implants fabricated using optimal slurry conditions, for example, 60 wt% solid content, 1 wt% dispersant, pH 12 and post-sintering at 1450 °C for 2 h. All sintered bodies contained a tetragonal phase with a high sintered density of approximately 6.07 g/cm³, good mechanical hardness of approximately 1367 Hv, grain size of 220 nm, and high surface roughness without cracks.

Effect of Powder Characteristics on Slip Casting Fabrication of Dental Zirconia Implants.

Dense zirconia compacts were fabricated by slip casting and sintering of nanoscale zirconia powders, and the effect of the powder characteristics (crystallite size, specific surface area, yttria content, and agglomeration) on the slurry and sintered properties was investigated. Three types of commercial 3 mol% yttria-stabilized tetragonal zirconia polycrystals powders were used as the starting powders after the powder characteristic analysis. A zirconia slurry for slip casting was prepared by mixing zirconia powder (solid loading of 60, 65, and 70 wt.%), distilled water, and a dispersant of Darvan C. The green compacts obtained from slip casting were cold isostatic pressed to enhance the close packing and densified by sintering at 1450 °C for 2 h. Highly dense zirconia compacts with a relative density of 99.5% and grain size of 350 nm were obtained based on the powder type and solid loading in the slurry. The microstructure and mechanical hardness of the sintered specimen after slip casting were dependent on the yttria content in the 3 mol% yttria-stabilized tetragonal zirconia polycrystal powder and the solid loading within the slurry.

Synthesis and Properties of Novel Calcia-Stabilized Zirconia (Ca-SZ) with Nano Calcium Oxide Derived from Cockle Shells and Commercial Source for Dental Application

Various oxides are used to stabilize zirconium oxide (ZrO2), but their superior hardness causes wear of the machining tool. Calcia-doped zirconia has been studied but reports on properties suitable for dental application are lacking. Therefore, this study aimed to fabricate and characterize zirconia stabilized by calcium oxide (CaO) derived from cockle shells and compare it with zirconia stabilized by commercial CaO, sintered at different temperatures. In this study, 176 pressed pellets of zirconia mixed with CaO either derived from cockle shells or commercial CaO were sintered between 1200 and 1500 °C to produce calcia-doped zirconia. Characterizations were made with SEM and XRD. Specimens were subjected to density, compressive and flexural strength, and Vickers hardness testing. Data were analyzed using the independent t-test and one-way ANOVA. XRD revealed the zirconia was stabilized into tetragonal and cubic phases (Ca-SZ). Ca-SZ cockle shells (CS) and Ca-SZ commercial (CC) have average particle sizes of 267 nm and 272 nm, respectively, with similar surface roughness. At 1400 °C sintering temperature, flexural strengths were 1165 and 1152 MPa, compressive strengths were 4914 and 4913 MPa, and Vickers hardness were 977 and 960 MPa for Ca-SZ(CS) and Ca-SZ(CC), respectively. Both Ca-SZ materials showed no significant difference in most properties (p &lt; 0.05) when sintered at different temperatures. The fully sintered Ca-SZ is less hard compared to the ceria-stabilized tetragonal zirconia polycrystal (Ce-TZP) available on the market. Thus, Ca-SZ may be used as an alternative to the current zirconia available on the market for dental application.

Flexural Strength of Different Monolithic Computer-Assisted Design and Computer-Assisted Manufacturing Ceramic Materials upon Different Thermal Tempering Processes.

Objective Strength of ceramics related with sintering procedure. This study investigated the influence of different tempering processes on flexural strength of three monolithic ceramic materials. Materials and Methods Specimens were prepared in bar-shape (width × length × thickness = 4 × 14 × 1.2 mm) from yttria-stabilized tetragonal zirconia polycrystalline (Y-TZP, inCoris TZI [I]), zirconia-reinforced lithium silicate (ZLS, Vita Suprinity [V]), and lithium disilicate (LS 2 , IPS e.max CAD [E]), and sintered with different tempering processes: slow (S), normal (N), and fast (F) cooling procedure ( n = 15/group). Flexural strength (σ ) was determined using three-point bending test apparatus at 1 mm/min crosshead speed. Statistical Analysis The analysis of variance and Bonferroni’s multiple comparisons were determined for significant difference (α = 0.05). Weibull analysis was applied for survival probability, Weibull modulus (m), and characteristics strength (σ o ). Microstructures were evaluated with scanning electron microscope and X-ray diffraction. Results The mean ± standard deviation (MPa) of σ, m, and σ o were: 1,183.98 ± 204.26, 6.23, 1,271.80 for IS; 1,084.43 ± 204.79, 5.76, 1,170.08 for IN; 777.19 ± 99.77, 8.78, 819.96 for IF; 267.15 ± 32.71, 9.11, 281.48 for VS; 218.43 ± 38.46, 6.40, 234.23 for VN; 252.67 ± 37.58, 7.20, 269.23 for VF; 392.09 ± 37.91, 11.37, 409.23 for ES; 378.88 ± 55.38, 7.45, 403.11 for EN, and 390.94 ± 25.34, 16.00, 403.51 for EF. Thermal tempering significantly affected flexural strength of Y-TZP ( p < 0.05), but not either ZLS or LS 2 ( p > 0.05). Y-TZP indicated significantly higher flexural strength upon slow tempering than others. Conclusion Enhancing flexural strength of Y-TZP can be achieved through slow tempering process and was suggested as a process for monolithic zirconia. Strengthening of ZLS and LS 2 cannot be accomplished through tempering; thus, either S-, N-, or F- tempering procedure can be performed. Nevertheless, to minimize sintering time, rapid thermal tempering is more preferable for both ZLS and LS 2 .

Additive manufacturing of high loading concentration zirconia using high-speed drop-on-demand material jetting

Zirconia-based ceramic has generated considerable interest in specialist structural/engineering ceramics. Among current available additive manufacturing methods for fabrication of ceramic components, the conventional material jetting systems are able to create local deposition of thin layers, dense green bodies, and complex shapes. However, this method is mainly limited to low viscous ceramic inks (mostly in the range of 20–40 mPa/s) with often less than 25 vol% solid loading which has restricted the widespread adoption of this technique. In this work, we employed a novel in-house developed hybrid drop-on-demand material jetting system (DODMJ) to deposit a highly viscous paste (up to 72 wt% solid content, a viscosity of 2100 mPa/s) of yttria-stabilized-zirconia (YSZ), with approximately 20 times higher speed than the current material jetting methods, for the first time. For this study, tetragonal zirconia polycrystal containing 8 wt% Y2O3 (5Y-TPZ), which is commonly used to produce dental restorations by subtractive manufacturing, was utilized. The printability of several visible light–curable zirconia pastes was studied in terms of the rheology, paste composition, solid content, and printing parameters. The density and porosity measurements as well as a two-stage sintering process to achieve fully dense and crack-free parts were carried out. The microstructure and internal features of the printed parts were also explored by X-ray nano-computed tomography (CT) scanning and scanning electron microscopy (SEM). In this work, standard test methods were also utilized to study the Vickers hardness and fracture toughness of the sintered 5Y-TPZ parts for the first time. The results showed that specimens produced with the paste containing 62.3 wt% solid loading yielded a relative density of 99.5% and presented an average fracture toughness and micro-hardness of 5.62 MPa/m0.5 and 1516 HV, respectively. Overall, the outcomes presented in this work confirmed that the novel DODMJ technique adopted for this study has great potential in the development of a feasible, high-speed, and cost-effective manufacturing system to produce zirconia ceramic parts with adequate mechanical and structural properties that meet the demanding requirements for various applications such as dental crowns restoration.

Comparative Analysis of Biofilm Formation on Materials Used for the Fabrication of Implant-Supported Prostheses.

The purpose of this study was to compare biofilm formation on materials used for the fabrication of implant-supported dental prostheses. Twenty discs (D=15 mm, H=3 mm) were fabricated from one of the following restorative materials: yttria tetragonal zirconia polycrystal (Y-TZP); commercially pure titanium (CP-Ti); or heat-cured polymethyl methacrylate (PMMA). Specimens were polished following standard protocols. A non-contact profilometer (NPFLEX, Bruker, UK) was used to assess the surface roughness of each disk; results were reported as Ra (µm). Five strains of Gram-negative bacteria frequently associated with peri-implantitis, Aggregatibacter actinomycetemcomitans, Candida. albicans, Porphyromonas gingivalis, Prevotella intermedia, and Tannerella forsythia, were cultured on hand-polished discs fabricated from heat-cured PMMA, Y-TZP, or CP-Ti to compare biofilm formation on each type of material. The results were reported as colony-forming units per milliliter (CFU/mL). One-way ANOVA and post hoc tests were used to compare surface roughness and bacterial colonization on the respective materials. Statistical significance was set at a = 0.05. Discs fabricated from Y-TZP had a significantly higher Ra value (350 ± 30 µm) than either PMMA, or CP-Ti discs. Discs fabricated from either Y-TZP and CP-Ti may exhibit less colonization by bacteria associated with peri-mucositis and peri-implantitis. Y-TZP and CP-Ti are suggested materials for fabrication of implant-supported prostheses, considering biofilm formation.

Low-temperature degradation of high-strength Y-TZP (yttria-stabilized tetragonal zirconia polycrystal).

The objective of this study was to investigate the low temperature degradation characteristics of 2 types of high strength yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) in order to evaluate its suitability for implant body, implant superstructure or abutment. Disk-shaped conventional Y-TZP (0.25 mass% alumina) subjected to hot isostatic press treatment (HIP-Y-TZP) and Y-TZP/4Al2O3 with additional alumina (4.0 mass%) were mirror-polished. Accelerated aging tests with 134°C for 5 h at 0.2 MPa and 180°C for 5 h at 1.0 MPa were performed using an autoclave. Biaxial flexural strength and crystal phases were evaluated. Strength decreased as the proportion of monoclinic phase increased after accelerated aging treatment for both types of high-strength Y-TZPs. Despite the low alumina content, HIP-Y-TZP showed higher static strength and strength after accelerated aging treatment compared to Y-TZP/4Al2O3. However, both types of Y-TZP had adequate strength to be used as dental restorations even after accelerated aging treatment, therefore, its clinical suitability was considered high.

Fabrication and mechanical properties of ZrO2–Al2O3–SiC(w) composites by oscillatory pressure sintering

Tetragonal zirconia polycrystalline (TZP) ceramics have been considered as the important structural materials in many key technology fields, but some of their mechanical properties do not meet the requirement under the extreme environmental conditions. In this work, SiC whiskers and Al2O3 particles were used as reinforcement additives to synergistically toughen TZP ceramics, and a newly developed oscillatory pressure sintering (OPS) technique was employed to fabricate the new zirconia-based ceramics. For comparison, the traditional hot pressing (HP) method was also used to prepare these composites. The results showed that with 15 vol% SiC whiskers addition, the toughening mechanisms such as whisker bridging, whisker pulling-out, crack deflection, and crack branching appeared apparently, thereby improving fracture toughness of such composites. In contrast to HP, OPS can eliminate defects, improve densification, obtain more uniform microstructure, and significantly enhance mechanical properties of the composites.

Role of Magnesium and the Effect of Surface Roughness on the Hydroxyapatite-Forming Ability of Zirconia Induced by Biomimetic Aqueous Solution Treatment.

Zirconia is a well-known bioceramic for dental and orthopedic applications due to its mechanical and aesthetic properties. However, it lacks sufficient bioactivity to bond with the living bone. This study was aimed to induce bioactivity to tetragonal zirconia polycrystal (3Y-TZP) by simple biomimetic aqueous solution treatment. First, hydrofluoric acid (HF) etching was performed to enhance the surface roughness of the 3Y-TZP surface. Then, the samples were treated with two types of aqueous solutions containing calcium and phosphate ions (Ca-P solutions); one solution additionally contained magnesium (Mg) ions and the other without Mg ions. Finally, hydroxyapatite (HAp)-forming ability was evaluated by the conventional simulated body fluid (SBF) test, and the effect of Mg ions on the adhesive strength of the HAp layer to the roughened 3Y-TZP surface was also investigated. The results concluded that there were no noticeable differences in the effect of Mg ions on the HAp-forming ability, and both types of solution treatments resulted in dense HAp formation in 1 day SBF immersion. However, incorporation of Mg ions in one of the Ca-P solutions significantly improved the adhesive strength of the HAp layer to the HF-etched 3Y-TZP substrate compared to the Ca-P solution with no Mg ions.

Effect of different fabrication techniques on the marginal precision of polyetheretherketone single-crown copings

Statement of problemDemand is increasing for polyetheretherketone (PEEK) as a fixed dental prosthesis core material. However, information is lacking about how the precision of these restorations is affected by the fabrication procedures. PurposeThe purpose of this in vitro study was to evaluate the influence of different fabrication techniques on the marginal precision of PEEK single-crown copings. Material and methodsA stainless-steel master die was designed to simulate a prepared mandibular second molar to receive ceramic crowns. Thirty PEEK copings were fabricated and divided into 3 groups (n=10) according to the fabrication technique: milled from a prefabricated PEEK blank by using a computer-aided design and computer-aided manufacturing (CAD-CAM) system (PC); pressed from prefabricated PEEK pellets (PP); and pressed from PEEK granules (PG); in addition, 3-mol yttria-stabilized tetragonal zirconia polycrystal (3Y-TZP) copings (n=10) were produced by using the same CAD-CAM system and served as a control. Marginal precision measurements (in μm) were recorded at 4 reference points on each coping by using a digital microscope. The data obtained were statistically analyzed by using 1-way ANOVA and the pair-wise Tukey (HSD) test to study the difference between group mean values (α=.05). ResultsThe overall mean ±standard deviation marginal gap at the marginal opening for the copings was 78 ±10 μm for PEEK granules copings, 72 ±9 μm for PEEK pellet copings, 45 ±6 μm for PEEK CAD-CAM copings, and 43 ±1 μm for the 3Y-TZP CAD-CAM control. A statistically significant difference was found between the milled and pressed copings as indicated by the ANOVA test (P<.001). The pair-wise Tukey honestly significant difference (HSD) test showed a nonsignificant difference (P>.05) between milled 3Y-TZP and milled PEEK copings; moreover, no significant difference was observed between the PEEK copings pressed from pellets or granules (P>.05). ConclusionsThe marginal precision of PEEK CAD-CAM–fabricated copings showed significantly lower mean marginal gap values than PEEK pressed copings. The marginal gap mean values recorded were all within a clinically acceptable range (120 μm).

Measuring the Static and Dynamic Elastic Modulus in Y-TZP Ceramic Applied to Dentistry

Abstract Yttria tetragonal zirconia polycrystal in the form of presintered commercial blocks is used to manufacture dental prostheses through computer-aided design/computer-aided manufacturing technology. Although it presents appropriate mechanical properties, it may fail because of defects resulting from the forming, presintering, machining, or sintering processes. The aim of the current study is to evaluate the influence of the presintering process on the microhardness of presintered blocks and on the elastic modulus of sintered materials. Blocks were formed by means of uniaxial and isostatic pressing. Next, they were presintered at different temperatures and soaking times, besides being subjected to the Vickers microhardness and mechanical tests to evaluate their elastic modulus. Statistical analyses showed that the presintering time at 900°C had no effect on microhardness, although it was significant at 950°C. The postsintering elastic modulus ranged from 205.7 to 231.9 GPa, which is similar to the range recorded in the literature. The presintering process had no influence on the postsintering mechanical resistance results.

The Effects of Syndecan on Osteoblastic Cell Adhesion Onto Nano-Zirconia Surface.

PurposeZirconia is one of the most promising implant materials due to its favorable physical, mechanical and biological properties. However, until now, we know little about the mechanism of osseointegration on zirconia. The purpose of this study is to evaluate the effect of Syndecan (Sdc) on osteoblastic cell (MC3T3-E1) adhesion and proliferation onto zirconia materials.Materials and MethodsThe mirror-polished disks 15 mm in diameter and 1.5 mm in thick of commercial pure titanium (CpTi), 3mol% yttria-stabilized tetragonal zirconia polycrystalline (3Y-TZP) and nano-zirconia (NanoZr) are used in this study. MC3T3-E1 cells were seeded onto specimen surfaces and subjected to RNA interference (RNAi) for Syndecan-1, Syndecan-2, Syndecan-3, and Syndecan-4. At 48h post-transfection, the cell morphology, actin cytoskeleton, and focal adhesion were observed using scanning electron microscopy or laser scanning confocal fluorescence microscopy. At 24h and 48h post-transfection, cell counting kit-8 (CCK-8) assay was used to investigate cell proliferation.ResultsThe cell morphology of MC3T3-E1 cells on CpTi, 3Y-TZP, and NanoZr changed into abnormal shape after gene silencing of Syndecan. Among the Syndecan family, Sdc-2 is responsible for NanoZr-specific morphology regulation, via maintenance of cytoskeletal conformation without affecting cellular attachment. According to CCK-8 assay, Sdc-2 affects the osteoblastic cell proliferation onto NanoZr.ConclusionWithin the limitation of this study, we suggest that Syndecan affects osteoblastic cell adhesion on CpTi, 3Y-TZP, and NanoZr. Sdc-2 might be an important heparin-sensitive cell membrane regulator in osteoblastic cell adhesion, specifically on NanoZr, through the organization of actin cytoskeleton and affects osteoblastic cell proliferation.

Adhesion of streptococci to titanium and zirconia.

The purpose of this study was to evaluate the adherence of streptococci to disks of titanium (commercially pure titanium: CpTi) and zirconia (tetragonal zirconia polycrystals: TZP). CpTi and yttria-stabilized TZP disks with a mirror-polished surface were used as specimens. The arithmetic mean surface roughness (Ra and Sa) and the surface wettability of the experimental specimens were measured. For analyzing the outermost layer of the experimental specimens, X-ray photoelectron spectroscopy (XPS) analysis was performed. Streptococcus sanguinis, S. gordonii, S. oralis, and S. mutans were used as streptococcal bacterial strains. These bacterial cultures were grown for 24 h on CpTi and TZP. The number of bacterial adhesions was estimated using an ATP-bioluminescent assay, and scanning electron microscope (SEM) observation of the adhered bacterial specimens was performed. No significant differences in surface roughness or wettability were found between CpTi and TZP. In XPS analyses, outermost layer of CpTi included Ti0 and Ti4+, and outermost layer of TZP included Zr4+. In the cell adhesion assay, the adherences of S. sanguinis, S. gordonii, and S. oralis to TZP were significantly lower than those to CpTi (p < 0.05); however, significant difference was not observed for S. mutans among the specimens. The adherence to CpTi and TZP of S. mutans was significantly lower than that of S. sanguinis, S. gordonii, and S. oralis. These results were confirmed by SEM. S. sanguinis, S. gordonii, and S. oralis adhered less to TZP than to CpTi, but the adherence of S. mutans was similar to both surfaces. S. mutans was less adherent compare with the other streptococci tested in those specimens.

Fracture toughness of zirconia with a nanometer size notch fabricated using focused ion beam milling.

ObjectivesZirconia with 3 mol% yttria (3Y‐TZP) has been used for dental crowns and bridges due to its excellent mechanical behavior. Performing fracture toughness testing on this nanograin material, however, can be a challenge. For reliable results, fracture toughness testing requires an extremely sharp notch in the test specimen that closely approximates a very sharp crack. This study was to investigate an alternative method to produce nanometer‐sized notches, which are less than the average grain size of 3Y‐TZP, during the preparation of single‐edge V‐notched beam specimens and report the resulting fracture toughness value.MethodsWe present a method using focused ion beam (FIB) milling to fabricate nanometer‐sized notches in 3Y‐TZP. The notch tip is <100 nm wide, which is smaller than the grain size, and is consistent throughout the thickness of the specimen.ResultsThe FIB‐notched specimens show a much reduced average fracture toughness of 5.64 ± 1.14 MPa√m compared to 8.90 ± 0.23 MPa√m for the specimens without FIB‐notches. The FIB‐milling did not appear to create any monoclinic phase prior to fracture toughness testing. Fractures originated at the FIB‐notches, and the notch size can be readily identified post‐mortem using a microscope. A considerable amount of tetragonal‐to‐monoclinic phase transformation was observed throughout the fracture surfaces.SignificanceFIB milling provides an alternative method to fabricate nanometer‐sized notches that are smaller than the grain size of tetragonal zirconia polycrystal. The fracture toughness determined using FIB‐notches was ~5.64 MPa√m, smaller than the specimens with V‐notches fabricated using saw blades.