Synthesis of Novel Antimicrobial CHX-CaCl2 Coatings on Maxillofacial Fixatures for Infection Prevention.

Maxillofacial surgery placement of fixatures (Leonard Buttons, LB) at close proximity to surgical incisions provides a potential reservoir as a secondary local factor to advanced periodontal disease, with bacterial formation around failed fixatures implicating plaque. To address infection rates, we aimed to surface coat LB and Titanium (Ti) discs using a novel form of chlorhexidine (CHX), CHX-CaCl2 and 0.2% CHX digluconate mouthwash as a comparison. CHX-CaCl2 coated, double-coated and mouthwash coated LB and Ti discs were transferred to 1 mL artificial saliva (AS) at specified time points, and UV-Visible spectroscopy (254 nm) was used to measure CHX release. The zone of inhibition (ZOI) was measured using collected aliquots against bacterial strains. Specimens were characterized using Energy Dispersive X-ray Spectroscopy (EDS), X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). SEM displayed copious dendritic crystals on LB/ Ti disc surfaces. Drug release from double-coated CHX-CaCl2 was 14 days (Ti discs) and 6 days (LB) above MIC, compared to the comparison group (20 min). The ZOI for the CHX-CaCl2 coated groups was significantly different within groups (p < 0.05). CHX-CaCl2 surface crystallization is a new drug technology for controlled and sustained CHX release; its antibacterial effectiveness makes this drug an ideal adjunct following clinical and surgical procedures to maintain oral hygiene and prevent surgical site infections.

Synthesis, Drug Release, and Antibacterial Properties of Novel Dendritic CHX-SrCl2 and CHX-ZnCl2 Particles.

This work demonstrated for the first time the synthesis of novel chlorhexidine particles containing strontium and zinc, to provide an effective, affordable, and safe intervention in the treatment of recurrent infections found in Medicine and Dentistry. The CHX-SrCl2 and CHX-ZnCl2 particles were synthesized by co-precipitation of chlorhexidine diacetate (CHXD) and zinc chloride or strontium chloride, where particle size was manipulated by controlling processing time and temperature. The CHX-ZnCl2 and CHX-SrCl2 particles were characterized using SEM, FTIR, and XRD. UV-Vis using artificial saliva (pH 4 and pH 7) was used to measure the drug release and ICP-OES ion release. The antibacterial properties were examined against P. gingivalis, A. actinomycetemcomitans, and F. nucleatum subsp. Polymorphum, and cytotoxicity was evaluated using mouse fibroblast L929 cells. The novel particles were as safe as commercial CHXD, with antibacterial activity against a range of oral pathogens. UV-Vis results run in artificial saliva (pH 4 and pH 7) indicated a higher release rate in acidic rather than neutral conditions. The CHX-ZnCl2 particles provided the functionality of a smart Zinc and CHX release, with respect to environmental pH, allowing responsive antibacterial applications in the field of medicine and dentistry.

Nucleation efficacy and flexural strength of novel leucite glass-ceramics.

OBJECTIVES: To optimize the nucleation mechanism in leucite glass-ceramics to allow more efficacious glass-ceramic manufacture and improvements in microstructure and mechanical reliability. MATERIALS AND METHODS: An alumino-silicate glass was designed and synthesized using melt quench methods. The glass was crushed and milled using various milling times (48-93h) and spray drying. Nucleation and growth heat treatment schedules were applied to synthesize glass-ceramics. Glass/glass-ceramic powders and frit specimens were characterized using differential scanning calorimetry (DSC), transmission electron microscopy (TEM), energy-dispersive X-ray spectrometry (EDX), magic angle spinning nuclear magnetic resonance spectroscopy (MAS-NMR) and X-ray diffraction analyses (XRD). Glass-ceramic specimens were tested using the biaxial flexural strength test (BFS). RESULTS: Application of defined nucleation heat treatments resulted in the synthesis of Na/Ca titanates. NMR indicated changes to the 23Na glass spectra in the nucleated glass and TEM/EDX the presence of Na/Ca/Ti domains (<200nm) within the leucite crystals and associated with the nucleation of the leucite phase. XRD confirmed the presence of a bulk leucite phase in the glass-ceramics. SEM/TEM confirmed the crystallization of the leucite phase (65.5-69.3%) in a thermally matched glass, in conjunction with the nano Na/Ca titanate phase. The leucite glass-ceramics resulted in a high BFS (255-268MPa), with reduction in powder milling time prior to heat treatments having no significant effect on flexural strength and reliability (p>0.05). SIGNIFICANCE: Na/Ca titanates were synthesized in leucite glass-ceramics for the first time and associated with its nucleation and efficacious growth. This nucleation optimization provides opportunities for more efficient manufacturing and microstructural/mechanical reliability improvements. Improved synthesis of high strength/reliable leucite glass-ceramics is useful for construction of esthetic minimally invasive restorations.

Effect of sandblasting, etching and resin bonding on the flexural strength/bonding of novel glass-ceramics.

OBJECTIVES: To process novel leucite glass-ceramics and test the effects of surface treatment and resin bonding on the biaxial flexural strength (BFS) and shear bond strength (SBS). METHODS: Alumino-silicate glasses were ball-milled, and heat treated to form leucite glass-ceramics (LG-C, OLG-C), then sintered into ingots. Ingots were heat extruded into a refractory mould to form disc specimens (1.3×14mm diameter). IPS e.max® was used as a commercial comparison. Glass-ceramic test groups were sandblasted (Groups. 1, 4, 6), sandblasted, etched and adhesively bonded (Groups. 2, 5, 7) or lapped, etched and adhesively bonded (Groups. 3, 8). Specimens were adhesively bonded with Monobond S, followed by the application of Variolink II® cement and light curing. BFS testing was at 1mm/min and SBS testing at 0.5mm/min. Samples were characterised using XRD, SEM and profilometry. RESULTS: XRD confirmed tetragonal leucite in LG-C/OLG-C and lithium disilicate/lithium orthophosphate in IPS e.max®. Mean BFS (MPa (SD)) were: Gp1 LG-C; 193.1 (13.9), Gp2 LG-C; 217.7 (23.0), Gp3 LG-C; 273.6 (26.7), Gp4 OLG-C; 255.9 (31); Gp5 OLG-C; 288.6 (37.4), Gp6 IPS e.max®; 258.6 (20.7), Gp7 IPS e.max®; 322.3 (23.4) and Gp8 IPS e.max®; 416.4 (52.6). The Median SBS (MPa) were Gp1 LG-C; 14.2, Gp2 LG-C (10s etch); 10.6 and Gp3 IPS e.max®; 10.8. Mean surface roughness was 5-5.1µm (IPS e.max®) and 2.6µm (LG-C). SIGNIFICANCE: Novel leucite glass-ceramics with reduced flaw size and fine microstructures produced enhanced BFS and SBS by resin bonding. These properties may be useful for the fabrication of minimally invasive aesthetic and fracture resistant restorations.

Controlled release of chlorhexidine from a HEMA-UDMA resin using a magnetic field.

OBJECTIVES: To functionalize novel chlorhexidine (CHX) particles with iron oxide (Fe3O4) nanoparticles and control their release kinetics in a dental resin using an external magnetic field. METHODS: Fe3O4 nanoparticles were synthesized and incorporated into spherical CHX particles and the powder was freeze dried. Resin disc specimens were produced using a UDMA-HEMA resin mixed with freeze dried spherical Fe3O4-CHX particles (5wt.%), which were placed into a Teflon mould (10mm diameter×1mm depth) and covered with a Mylar strip. A MACS magnet was left in contact for 0min (Group 1), 5min (Group 2) or 10min (Group 3) and the resin discs subsequently light cured (Bluedent LED pen, Bulgaria) for 60s per side. The resin discs were immersed in deionized water at various time points up to 650h. UV-Vis absorbance was used to determine the CHX content. CHX released for each time point was determined. The functionalized CHX particles and resin discs were characterized using TEM, TGA, EDX and SEM. RESULTS: Fe3O4 nanoparticles (20nm) incorporated into the spherical CHX particles led to a mean (SD) particle size reduction from 17.15 (1.99)µm to 10.39 (2.61)µm. The presence of Fe3O4 nanoparticles in the spherical CHX particles was confirmed with SEM, EDX, and TGA. SEM of Group 1 resin discs (no magnetic exposure) showed functionalized CHX spheres were homogeneously distributed within the resin discs. For resin discs which had magnetic exposure (5 or 10min) the particles started to cluster nearer the surface (Group 2: 43.7%, Group 3: 57.3%), to a depth of 94µm. UV-Vis absorbance revealed Group 1 resin discs had a cumulative CHX release of 4.4% compared to 5.9% for Group 2 and 7.4% for Group 3 resin discs, which had magnetic exposure (5, 10min). SIGNIFICANCE: Fe3O4 nanoparticle functionalized CHX spheres demonstrated a magnetic field responsive property. A magnetic field responsive release of CHX may be useful in clinical situations where the drug can be directed to give a tailored release at the site of infection.

Gold Nanorod Mediated Chlorhexidine Microparticle Formation and Near-Infrared Light Induced Release.

Gold nanorods (GNR) are good light harvesting species for elaboration of near-infrared (NIR) responsive drug delivery systems. Herein, chlorhexidine microparticles are grown directly on the surface of gold nanorods and then stabilized with polyelectrolyte multilayer encapsulation, producing novel composite drug-GNR particles with high drug loading and NIR light sensitivity. Crystallization of chlorhexidine is caused by the ionic strength of the chloride solution that has been demonstrated via formation of a homogeneous porous spherical structure at 0.33 M CaCl2. By introducing GNRs into the CaCl2 solution, the nucleation of chlorhexidine molecules and size of produced spheres are affected, since GNRs act as sites for chlorhexidine nucleation. Similarly, when GNRs are replaced by chlorhexidine seeds (5.2 ± 1.7 µm), a core-shell crystal structure is observed. The encapsulated GNR/chlorhexidine composites are responsive to NIR light (840 nm) that increases the temperature at the chlorhexidine crystals, followed by microparticle dissolution and rupture of capsules which is illustrated with confocal microscopy and SEM. Furthermore, a stepwise burst release of chlorhexidine can be induced by multiple cycles of NIR light exposure. The GNR/chlorhexidine composites show good biocompatibility and antimicrobial activity. The proposed method of antibacterial drug release may therefore indicate that this NIR responsive chlorhexidine composite may be useful for future clinical applications.

Synthesis of novel chlorhexidine spheres with controlled release from a UDMA-HEMA resin using ultrasound.

OBJECTIVE: Establish the release kinetics of new chlorhexidine particles incorporated in a dental resin, and with the application of ultrasound. METHODS: Spherical chlorhexidine particles (SCP) were synthesized (5wt%), freeze dried and incorporated into UDMA-HEMA resins. Chlorhexidine diacetate (CDP) (5wt%) was similarly incorporated in separate resins. Resin discs were immersed in deionized water, and a release profile established (650h). Ultrasound was used to trigger chlorhexidine (CHX) release from the resin discs at specific durations (10-30s) and time intervals (1-425h). Chlorhexidine content was determined by UV-vis absorption. The chlorhexidine particles/polymer composites were characterized using TGA, SEM, and confocal microscopy. RESULTS: SCP exhibited structures with high chlorhexidine content (90-95%), and a Mean (SD) diameter of 17.2 (2.5)µm which was significantly (p<0.001) smaller than the CDP crystals at 53.6 (33.7)µm. The SCP discs had a lower (7.7%) CHX release compared to the CDP group (16.2%). Ultrasonication of the resin discs with increasing durations (10-30s) resulted in higher drug release rates. CDP release rates (CHX) over 650h were: 23.5% (10s), 42.6% (20s), 51.2% (30s), and for SCP (CHX) were; 9.8% (10s), 12.3% (20s), and 14.0% (30s). SEM/confocal microscopy revealed CDP discs exhibited dissolution associated with the particle surface and SCP from the interior. SIGNIFICANCE: Chlorhexidine spheres incorporated in a dental resin demonstrated a responsive and lower CHX release. Ultrasound enhanced CHX release and is useful in clinical situations where the drug is required on demand to treat severe or persistent infections.

Interfacial modulus mapping of layered dental ceramics using nanoindentation.

PURPOSE: The aim of this study was to test the modulus of elasticity (E) across the interfaces of yttria stabilized zirconia (YTZP) / veneer multilayers using nanoindentation. MATERIALS AND METHODS: YTZP core material (KaVo-Everest, Germany) specimens were either coated with a liner (IPS e.max ZirLiner, Ivoclar-Vivadent) (Type-1) or left as-sintered (Type-2) and subsequently veneered with a pressable glass-ceramic (IPS e.max ZirPress, Ivoclar-Vivadent). A 5 µm (nominal tip diameter) spherical indenter was used with a UMIS CSIRO 2000 (ASI, Canberra, Australia) nanoindenter system to test E across the exposed and polished interfaces of both specimen types. The multiple point load - partial unload method was used for E determination. All materials used were characterized using Scanning Electron Microscopy (SEM) and X - ray powder diffraction (XRD). E mappings of the areas tested were produced from the nanoindentation data. RESULTS: A significantly (P<.05) lower E value between Type-1 and Type-2 specimens at a distance of 40 µm in the veneer material was associated with the liner. XRD and SEM characterization of the zirconia sample showed a fine grained bulk tetragonal phase. IPS e-max ZirPress and IPS e-max ZirLiner materials were characterized as amorphous. CONCLUSION: The liner between the YTZP core and the heat pressed veneer may act as a weak link in this dental multilayer due to its significantly (P<.05) lower E. The present study has shown nanoindentation using spherical indentation and the multiple point load - partial unload method to be reliable predictors of E and useful evaluation tools for layered dental ceramic interfaces.

Electrospun poly(lactic acid) fibers containing novel chlorhexidine particles with sustained antibacterial activity.

The treatment of persistent infections often requires a high local drug concentration and sustained release of antimicrobial agents. This paper proposes the use of novel electrospinning of poly(lactic acid) (PLA) fibers containing uncoated and encapsulated chlorhexidine particles. Chlorhexidine particles with a mean (SD) diameter of 17.15 ± 1.99 µm were fabricated by the precipitation of chlorhexidine diacetate with calcium chloride. Layer-by-layer (LbL) encapsulation of the chlorhexidine particles was carried out to produce encapsulated particles. The chlorhexidine particles had a high chlorhexidine content (90%), and when they were electrospun into PLA fibers a bead-in-string structure was obtained. The chlorhexidine content in the fibers could be tuned and a sustained release over 650 h was produced, via chlorhexidine particle encapsulation. Chlorhexidine release was governed by the polyelectrolyte multilayer encapsulation as demonstrated by SEM and confocal imaging. The incorporation of uncoated and encapsulated chlorhexidine particles (0.5% and 1% wt/wt chlorhexidine) into the fibers did not cause toxicity to healthy fibroblasts or affect cell adhesion to the fibers over a period of 5 days. The chlorhexidine-containing fibers also demonstrated sustained antibacterial activity against E. coli via an agar diffusion assay and broth transfer assay. Therefore, the chlorhexidine-containing PLA fibers may be useful in the treatment of persistent infections in medicine and dentistry.

Novel Formulation of Chlorhexidine Spheres and Sustained Release with Multilayered Encapsulation.

This work demonstrates the synthesis of new chlorhexidine polymorphs with controlled morphology and symmetry, which were used as a template for layer-by-layer (LbL) encapsulation. LbL self-assembly of oppositely charged polyelectrolytes onto the drug surface was used in the current work, as an efficient method to produce a carrier with high drug content, improved drug solubility and sustained release. Coprecipitation of the chlorhexidine polymorphs was performed using chlorhexidine diacetate and calcium chloride solutions. Porous interconnected chlorhexidine spheres were produced by tuning the concentration of calcium chloride. The size of these drug colloids could be further controlled from 5.6 µm to over 20 µm (diameter) by adjusting the coprecipitation temperature. The chlorhexidine content in the spheres was determined to be as high as 90%. These particles were further stabilized by depositing 3.5 bilayers of poly(allylamine hydrochloride) (PAH) and polystyrenesulfonate (PSS) on the surface. In vitro release kinetics of chlorhexidine capsules showed that the multilayer shells could prolong the release, which was further demonstrated by characterizing the remaining chlorhexidine capsules with SEM and confocal microscopy. The new chlorhexidine polymorph and LbL coating has created novel chlorhexidine formulations. Further modification to the chlorhexidine polymorph structure is possible to achieve both sustained and stimuli responsive release, which will enhance its clinical performance in medicine and dentistry.

The effect of spark plasma sintering on lithium disilicate glass-ceramics.

OBJECTIVES: To evaluate the effects of spark plasma sintering (SPS) on the microstructure of lithium disilicate glass-ceramics. METHODS: IPS e.max CAD glass-ceramic samples were processed using spark plasma sintering (SPS) and conventionally sintered (CS) as a comparison. Specimens were sintered at varying temperatures (T1: 840°C, T2: 820°C, T3: 800°C), heating rates (HR1: 150°C/min, HR2: 300°C/min, HR3: 500°C/min) and pressures (P1: 15MPa, P2: 50MPa, P3: 70MPa). IPS e.max Press glass powder samples were densified at 750 and 800°C (50 or 200MPa pressure). Samples were characterized using XRD, HTXRD, and SEM and quantitative image analysis. RESULTS: There was a significant increase in median crystal size (MCS) between the CS and the SPS T1 groups. A statistical difference (p>0.05) in MCS between SPS T1 and SPS T2 groups was observed. The SPS HR3 sample produced a smaller MCS than the CS, SPS HR1 and HR2 groups (p<0.05). The SPS P3 sample had a reduction in MCS compared with the CS group (p<0.05). XRD of the SPS samples revealed major lithium disilicate/lithium metasilicate phases and minor lithium orthophosphate and cristobalite/quartz phases. Densified IPS e.max Press glass samples resulted in fine fibrils or graduated lithium disilicate crystals. SIGNIFICANCE: The effects of SPS were used to refine the microstructure of IPS e.max CAD lithium disilicate glass-ceramics. Densification by SPS of IPS e.max Press glass resulted in textured and fine nano-crystalline microstructures. SPS generated glass-ceramic microstructures may have unique properties and could be useful in the production of CAD/CAM materials for dentistry.

Reduced wear of enamel with novel fine and nano-scale leucite glass-ceramics.

OBJECTIVES: Leucite glass-ceramics used to produce all-ceramic restorations can suffer from brittle fracture and wear the opposing teeth. High strength and fine crystal sized leucite glass-ceramics have recently been reported. The objective of this study is to investigate whether fine and nano-scale leucite glass-ceramics with minimal matrix microcracking are associated with a reduction in in vitro tooth wear. METHODS: Human molar cusps (n=12) were wear tested using a Bionix-858 testing machine (300,000 simulated masticatory cycles) against experimental fine crystal sized (FS), nano-scale crystal sized (NS) leucite glass-ceramics and a commercial leucite glass-ceramic (Ceramco-3, Dentsply, USA). Wear was imaged using Secondary Electron Imaging (SEI) and quantified using white-light profilometry. RESULTS: Both experimental groups were found to produce significantly (p<0.05) less volume and mean-height tooth loss compared to Ceramco-3. The NS group had significantly (p<0.05) less tooth mean-height loss and less combined (tooth and ceramic) loss than the FS group. Increased waviness and damage was observed on the wear surfaces of the Ceramco-3 glass-ceramic disc/tooth group in comparison to the experimental groups. This was also indicated by higher surface roughness values for the Ceramco-3 glass-ceramic disc/tooth group. CONCLUSIONS: Fine and nano-sized leucite glass-ceramics produced a reduction in in vitro tooth wear. The high strength low wear materials of this study may help address the many problems associated with tooth enamel wear and restoration failure.

Crystallization and flexural strength optimization of fine-grained leucite glass-ceramics for dentistry.

OBJECTIVES: Leucite glass-ceramics with fine-grained leucite crystals promote improved mechanical strength and increased translucency. The objectives of the study were to optimize the microstructure of a fine-grained leucite glass-ceramic in order to increase its flexural strength and reliability as measured by its Weibull modulus. METHODS: Glass was prepared by a melt-derived method and ground into a powder (M1A). The glass crystallization kinetics were investigated using high temperature XRD and DSC. A series of two-step heat treatments with different nucleation/crystal growth temperatures and holds were carried out to establish the optimized crystallization heat treatment. Glass-ceramics were characterized using XRD, SEM and dilatometry. The glass-ceramic heat treated at the optimized crystallization parameters (M1A(opt)) was both sintered (SM1A(opt)) and heat extruded (EM1A(opt)) into discs and tested using the biaxial flexural strength (BFS) test. RESULTS: High temperature XRD suggested leucite and sanidine crystallization at different temperatures. Optimized crystallization resulted in an even distribution of fine leucite crystals (0.15 (0.09) µm(2)) in the glassy matrix, with no signs of microcracking. Glass-ceramic M1A(opt) showed BFS values of [mean (SD), MPa]: SM1A(opt)=252.4 (38.7); and EM1A(opt)=245.0 (24.3). Weibull results were: SM1A(opt); m=8.7 (C.I.=7.5-10.1) and EM1A(opt); m=11.9 (C.I.=9.3-15.1). Both experimental groups had a significantly higher BFS and characteristic strength than the IPS Empress Esthetic glass-ceramic, with a higher m value for the EM1A(opt) material (p<0.05). SIGNIFICANCE: A processable fine-grained leucite glass-ceramic with high flexural strength and improved reliability was the outcome of this study.

The development and testing of glaze materials for application to the fit surface of dental ceramic restorations.

OBJECTIVES: The aims of the study were to develop and test overglaze materials for application to the fit surface of dental ceramic restorations, which could be etched and adhesively bonded and increase the flexural strength of the ceramic substrate. METHODS: Three glaze materials were developed using commercial glass powders (P25 and P54, Pemco, Canada). P25 (90 wt%) was mixed with P54 (10 wt%) to produce (P25/P54). P54 (90 wt%) was mixed with P25 (10 wt%) to produce (P54/P25). P25 (90 wt%) was mixed with 10 wt% of an experimental glass powder (P25/frit). Eighty-two disc specimens (14 mm x 2 mm) were produced by heat pressing a leucite glass-ceramic and were sandblasted with 50 microm glass beads. Group 1 control specimens (10) were sandblasted. Groups 2-4 (10 per group) were coated using P25/frit (Group 2), P25/P54 (Group 3) and P54/P25 (Group 4) overglazes before sintering. Groups 1-4 were etched for 2 min using 9.5% HF (Gresco, USA). Composite cylinders (Marathon v, Den-Mat) were light cured and bonded to the glazed and prepared disc surfaces and groups water stored for 8 days. Groups were tested using shear bond strength (SBS) testing at 0.5mm/min. Disc specimens (42) were tested using the biaxial flexural strength (BFS) test at a crosshead speed of 0.15 mm/min. Group 1 was tested as sandblasted (21) and Group 2 (21) after coating the tensile surface with P25/frit. Xrd, Eds and Sem analyzes were carried out. RESULTS: Mean SBS (MPa+/-S.D.) were: Group 1: 10.7+/-2.1; Group 2: 9.8+/-1.9; Group 3: 1.8+/-1.0 and Group 4: 2.6+/-1.7. Groups 1 and 2 were statistically different to Groups 3 and 4 (p<0.001), but there was no difference between Groups 1 and 2 and 3 and 4 (p>0.05). The mean BFS (MPa+/-S.D.) of the overglazed Group 2 (200.2+/-22.9) was statistically different (p<0.001) to Group 1 (150.4+/-14.3). SIGNIFICANCE: The P25/frit overglaze significantly (p<0.001) increased the biaxial flexural strength of the leucite glass-ceramic substrate and produced comparable shear bond strengths to an etched and bonded control. The application of etched overglaze materials to dental glass-ceramic and ceramic substrates may be useful in adhesive dentistry.

The nucleation and crystallization of fine grained leucite glass-ceramics for dental applications.

OBJECTIVES: The aims of the study were to control the nucleation and crystal growth of selected aluminosilicate glass powders, to produce uniform leucite glass-ceramic microstructures consisting of fine (<1000 nm) grained leucite crystals. METHODS: A starting glass composition of wt%; 64.2% SiO(2), 16.1% Al(2)O(3), 10.9% K(2)O, 4.3% Na(2)O, 1.7% CaO, 0.5% LiO(2) and 0.4% TiO(2) was heated in an electric furnace and later quenched to produce glasses. The glass powders were ball milled to two different particle sizes and heat-treated using one and two-step crystallization heat treatments. Dta, Xrd, and Sem analyses was used to characterise and explore the crystallization kinetics of the glasses. RESULTS: Selected heat treatments of the glass powders produced a uniform distribution of fine tetragonal leucite crystals (mean+/-S.D.) 0.1+/-0.2 microm(2) in the glassy matrix, with minimal matrix microcraking in the glass-ceramics produced. The addition of a two-step heat treatment increased the leucite volume fraction in all instances. SIGNIFICANCE: Selected crystallization heat treatments and powder particle sizes were used to control the leucite crystal size, distribution and volume fraction, in order to produce uniformly distributed ultra fine grained tetragonal leucite glass-ceramics for dental applications.

The crystallization of an aluminosilicate glass in the K2O-Al2O3-SiO2 system.

OBJECTIVES: The aims of the study were to explore the nucleation and crystallization kinetics of an aluminosilicate glass in K2O-Al2O3-SiO2 system and to characterize it. OBJECTIVES: A starting glass composition of wt%; 64.2% SiO2, 16.1% Al2O3, 10.9% K2O, 4.3% Na2O, 1.7% CaO, 0.5% LiO and 0.4% TiO2 was heated in an electric furnace and later quenched to produce glasses. The glass powders were heat treated using differing heat treatment schedules and quenched. Dta, Xrd, Eds and Sem analyses were used to characterize and explore the crystallization kinetics of the glasses. RESULTS: Phase separation of the glasses was identified and characterized in the glasses. Tetragonal leucite, cubic leucite and sanadine glass-ceramics were produced. Fine leucite crystals (1 microm2) were crystallized with minimal matrix microcracking. SIGNIFICANCE: Amorphous phase separation appeared to be an important precursor to nucleation and crystal growth in the alkali aluminosilicate glasses explored. It was possible to control the crystallization of tetragonal leucite and sanidine phases by selected heat treatment of glass powders and monoliths, resulting in the production of fine grained tetragonal leucite glass-ceramics.