Compositions: ceramic – Ceramic compositions – Devitrified glass-ceramics
Reexamination Certificate
1999-12-10
2002-09-24
Koslow, C. Melissa (Department: 1755)
Compositions: ceramic
Ceramic compositions
Devitrified glass-ceramics
C106S035000, C264S016000, C264S019000, C433S201100, C433S202100, C433S212100
Reexamination Certificate
active
06455451
ABSTRACT:
FIELD OF INVENTION
This invention relates generally to glass-ceramics comprising lithium disilicate and more specifically to glass-ceramics for use in the manufacture of dental restorations and methods of manufacture thereof.
BACKGROUND OF THE INVENTION
The use of lithium disilicate glass ceramics for use in dental restorations has been suggested in the prior art. U.S. Pat. No. 4,189,325 to Barret et al. is directed to a glass-ceramic comprising lithium disilicate for use in dental restorations. The glass ceramic requires the presence of Nb
2
O
5
and Pt as nucleation agents. Barrett et al. introduced dental restorations made from castable lithium disilicate glass-ceramics in the Li
2
O—CaO—Al
2
O
3
—SiO
2
system nucleated by Pt and Nb
2
O
5
. According to Barret et al., dental restorations are made by casting a melt into an investment mold, and devitrifying thereafter.
U.S. Pat. No. 4,515,634 to Wu et al. is directed to a castable glass-ceramic composition wherein the glass is melted and cast into a shape and is crystallized after it has been shaped. Therefore, the crystallization process is performed by the technician making the restoration, not the manufacturer of the dental material. Wu set al. suggests one way to improve properties of castable lithium disilicate dental restorations within the same Li
2
O—CaO—Al
2
O
3
—SiO
2
system as described by Barrett et al. is by utilization of P
2
O
5
as a nucleating agent. Both Barrett et al. and Wu et al. describe castable compositions having CaO as an essential ingredient believed to improve chemical durability of the resulting glass-ceramics. Chemical durability is one of the major issues that the Wu and Barrett inventions fail to address. For example, total alkali leaching rates for materials presented in Wu's examples were four to five times higher than those for commercial dental porcelain.
Castable dental ceramics as described in Barret et al. and Wu et al. employ melting glass ingots supplied by a manufacturer and casting dental articles into a refractory investment mold. Following the casting process, the cast articles are devitrified (crystallized) by the required heat-treatment steps. This process is very similar to casting metals whereby a heat-treatment step follows the casting process to increase hardness and strength.
U.S. Pat. Nos. 5,507,981 and 5,702,514 to Petticrew teach lithium disilicate compositions for use in dental restorations, but the method described therein implies forming glass into the shape of a dental restoration at temperatures much higher than the melting temperature of lithium disilicate and heat-treating the dental restoration after forming to convert the glass into a glass-ceramic.
German Patent Application No. DE19647739 to Schweiger et al. is directed to lithium disilicate compositions for use in dental restorations. The glass-ceramic bodies or blanks used to press dental restorations are defined as “sinterable glass ceramics” which are produced from the starting amorphous glass powder by simultaneous sintering and powder crystallizing, which process is also known as surface crystallization. The glass must be in powder form to be crystallized. Additionally, the lithium disilicate compositions therein require the presence of La
2
O
3
, MgO and ZnO.
Many of the lithium disilicate compositions in the prior art require casting of the glass into the desired shape and crystallizing thereafter. The glass must be formed into the finally desired shape and thereafter heat treated to crystallize into a lithium disilicate phase. This may result in structural and other problems, since the microstructure is not formed by the dental materials manufacturer, but by the technician fabricating the dental restoration. Overprocessing by a technician may change the microstructure of the material to something not preferred or desired by the dental materials manufacturer. Moreover, some of the prior art compositions require the forming of the glass ceramics by surface crystallization, limiting the forming and compositional possibilities of the material.
It is desirable to provide a lithium disilicate glass-ceramic which is pressable after the lithium disilicate is formed. It is beneficial to provide a lithium disilicate glass ceramic for use in the fabrication of dental restorations wherein crystallization is carried out by the dental materials manufacturer in the most controlled manner. It is beneficial to provide translucent lithium disilicate glass ceramics having high strength and good presssability.
SUMMARY OF THE INVENTION
This invention is directed to lithium disilicate (Li
2
Si
2
O
5
) based glass-ceramics comprising silica, lithium oxide, alumina, potassium oxide and phosphorus pentoxide in addition to other components listed below. The glass-ceramics are useful in the fabrication of single and multi-unit dental restorations including but not limited to orthodontic appliances, bridges, space maintainers, tooth replacement appliances, splints, crowns, partial crowns, dentures, posts, teeth, jackets, inlays, onlays, facing, veneers, facets, implants, abutments, cylinders, and connectors made by heat pressing into refractory investment molds produced using lost wax techniques. The glass-ceramics have good pressability, i.e., the ability to be formed into dental articles by heat pressing, also known as hot pressing, or injection molding, using commercially available equipment.
In accordance with one embodiment directed to the process of making the glass-ceramics, the compositions herein are melted at about 1200° to about 1600° C. and preferably in the range of about 1300° to about 1400° C. for a period of time, preferably for about 4 hours and thereafter quenched (e.g., water quenched or roller quenched) or cast into steel molds, or alternately, cooled to the crystallization temperature.
The resulting glass is heat-treated to form a glass-ceramic via a one or two step heat-treatment cycle preferably in the temperature range of about 400° to about 1100° C. This crystallization heat treatment may comprise a nucleation step and a crystal growth step. Depending on the composition, the first, nucleation step, may be carried out in the range of about 450° C. to about 700° C. and preferably in the range of about 500° C. to about 650° C. for about 0.5 to about 4 hours and the second, crystal growth step, may be carried out in the range of about 800° C. to about 1000° C. and preferably in the range of about 830° C. to about 930° C. for about 0.5 to about 48 hours. The most preferable heat treatment comprises about a one hour soak at about 645° C. and a subsequent four hour soak at about 850° C.
The resulting glass ceramics are then pulverized into powder and used to form pressable pellets and/or blanks of desired shapes, sizes and structures. Additives may be mixed with the powder prior to forming into pellets or blanks. These pellets and blanks may be used for pressing cores or other frameworks or shapes for dental restorations. The blank or pellet may be subjected to viscous deformation at a temperature in the range of about 800° to about 1200° C., and more preferably in the range of about 850° to about 950° C., and most preferably at less than about 930° C., under vacuum and with the application of pressure of between about 2 to about 8 bar (0.2 to 0.8 MPa) and preferably no greater than about 6 bar (0.6 MPa) to obtain a dental restoration. Moreover, it is possible that the blanks may be machined to a dental restoration of desired geometry.
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pa
Brodkin Dmitri
Panzera Carlino
Panzera Paul
Jeneric/Pentron Inc.
Knab Ann M.
Koslow C. Melissa
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