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US20130216787A1 - Ceramic articles with increased surface roughness and methods for manufacturing the same - Google Patents

Ceramic articles with increased surface roughness and methods for manufacturing the same Download PDF

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Publication number
US20130216787A1
US20130216787A1 US13/562,548 US201213562548A US2013216787A1 US 20130216787 A1 US20130216787 A1 US 20130216787A1 US 201213562548 A US201213562548 A US 201213562548A US 2013216787 A1 US2013216787 A1 US 2013216787A1
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United States
Prior art keywords
ceramic
porous layer
article
particles
composite porous
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US13/562,548
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Inventor
Shu-Tuan Yeh
Yung-Chin Yang
Pei-Chi Hsu
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National Taipei University of Technology
MacKay Memorial Hospital
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Individual
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Assigned to MACKAY MEMORIAL HOSPITAL, NATIONAL TAIPEI UNIVERSITY OF TECHNOLOGY reassignment MACKAY MEMORIAL HOSPITAL ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HSU, PEI-CHI, YEH, SHU-TUAN, YANG, YUNG-CHIN
Publication of US20130216787A1 publication Critical patent/US20130216787A1/en
Priority to US14/516,225 priority Critical patent/US9387057B2/en
Abandoned legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61CDENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00Dental prostheses; Making same
    • A61C13/08Artificial teeth; Making same
    • A61C13/083Porcelain or ceramic teeth
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61CDENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00Dental prostheses; Making same
    • A61C13/0003Making bridge-work, inlays, implants or the like
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61CDENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C5/00Filling or capping teeth
    • A61C5/70Tooth crowns; Making thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61CDENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C5/00Filling or capping teeth
    • A61C5/70Tooth crowns; Making thereof
    • A61C5/77Methods or devices for making crowns
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4505Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
    • C04B41/4535Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application applied as a solution, emulsion, dispersion or suspension
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4578Coating or impregnating of green ceramics or unset concrete
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4582Porous coatings, e.g. coating containing porous fillers
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/89Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00836Uses not provided for elsewhere in C04B2111/00 for medical or dental applications
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0038Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by superficial sintering or bonding of particulate matter
    • C04B38/0041Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by superficial sintering or bonding of particulate matter the particulate matter having preselected particle sizes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/24Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24355Continuous and nonuniform or irregular surface on layer or component [e.g., roofing, etc.]
    • Y10T428/24372Particulate matter
    • Y10T428/24421Silicon containing

Definitions

  • the present disclosure relates to ceramic articles with increased surface roughness and methods for manufacturing the same. More particularly, the ceramic articles may be used as dental restorations, and the increased surface roughness thereof is advantageous in improving the bonding strength between the dental restoration and a resin adhesive for bonding the dental restoration to the abutment.
  • Oxide ceramics include aluminum oxide (alumina, Al 2 O 3 ), zirconium oxide (zirconia, ZrO 2 ), silicon dioxide (silica, SiO 2 ), aluminum silicate ((AlO) 2 SiO 3 ), magnesium oxide (magnesia, MgO), and other metal oxide based materials. These ceramics have found applications in many fields due to their engineering properties (such as high hardness, fracture toughness, high melting point, and chemical inertness) and a wide range of electrical properties. For example, silicon dioxide-based ceramics (silicate ceramics) have long been used in dentistry because of their optical and aesthetic properties. Recently, high-strength ceramics such as zirconia and alumina ceramics have gained increasing popularity in utilization by clinicians and technicians due to the material's strength, and multitude of clinical indications and applications.
  • dental restorations are often bonded to the underlying abutment (such as natural tooth/teeth and dental implant(s)) with a resin adhesive.
  • the engagement surface i.e., the surface configured to engage with an underlying abutment for retention thereto
  • Conventional surface treatments for dental restorations made of silicate ceramics include micromechanical treatments, chemical treatments, and a combined treatment including both micromechanical and chemical treatments.
  • Micromechanical treatments such as acid etching and sandblasting create micro-cracks/pores on the treated surface which allow the resin adhesive to penetrate therethrough, and thereby improve the bonding strength of the dental restoration and the resin adhesive.
  • micromechanical treatment is applicable for roughening silica-based ceramic, it has limited effect on the improvement of the surface roughness of high-strength ceramics because of the hardness and chemical inertness of these high-strength ceramics.
  • the micro-cracks/pores may result in the degradation of the flexural strength and fracture toughness of the dental restoration.
  • Chemical treatment involves the application of silane on the engagement surface.
  • Silane a molecule containing an organic group (e.g. vinyl, allyl, amino, etc.) and an inorganic group (e.g., methoxy, ethoxy, etc.), is widely used as a coupling agent.
  • the inorganic group of the silane molecule hydrolyzes to produce silanol, which forms a metal hydroxide or siloxane bond with the inorganic material such as silicate ceramics.
  • the organic group of the silane molecule reacts with the organic resin adhesive to produce a covalent bond. As a result, the organic resin adhesive and the inorganic ceramic are tightly bound.
  • the silane treatment has limited effects in improving the bonding strength between the resin adhesive and high-strength ceramics.
  • the present disclosure is directed to a ceramic article with an increased surface roughness.
  • the ceramic article has a composite porous layer disposed on an engagement surface of a ceramic body.
  • the micro- to nano-scale pores of the composite porous layer allow the penetration of resin adhesive thereby increasing the contact area of the ceramic/adhesive interface.
  • the plurality of microparticles dispersed within the composite layer, along with the pores decrease the contact angle of the engagement surface, and thus increase the wettability of the engagement surface.
  • the increased contact area and wettability of the ceramic article would improve the bonding strength between the ceramic article and the resin adhesive.
  • the present ceramic articles may be used as a component of a dental restoration; advantageously, the improved bonding strength may positively contribute to an increased service life of the dental restoration, as well as a better protection to the abutment.
  • the ceramic article comprises a ceramic body and a composite porous layer.
  • the ceramic body has an engagement surface configured to engage with an underlying structure (such as an abutment in the context of dentistry) for retention thereto.
  • the composite porous layer disposed on the engagement surface is formed from a material comprising a plurality of first ceramic particles and a plurality of second ceramic particles.
  • the sintering temperature of the first ceramic particle is lower than the melting temperature of the second ceramic particle, and at least some of the plurality of the second ceramic particles are dispersed within the composite porous layer whereby increasing the surface roughness of the engagement surface of the ceramic article.
  • the composite porous layer of the ceramic article has an average surface roughness (Ra) of at least about 0.5 ⁇ m; preferably, about 0.85-1.7 ⁇ m.
  • the ceramic body is made of a material comprising a metal oxide ceramic.
  • Metal oxide ceramics include, but are not limited to, zirconium oxide and aluminum oxide.
  • the first ceramic particle is a glass ceramic such as an opaque dental ceramic.
  • the second ceramic particle may have a Mohs hardness of at least 8.5 according to some embodiments of the present disclosure.
  • yttria-stabilized zirconia in which the yttria is present in an amount of about 0.5-35 mole percent may be used as the second ceramic particle.
  • the second ceramic particle is 8 mol % yttria-stabilized zirconia (8YSZ).
  • the composite porous layer may have a thickness of about 5-20 ⁇ m, and the second ceramic particle may have an average diameter of about 0.1-0.8 ⁇ m.
  • the present disclosure is directed to a method for manufacturing a ceramic article according to the above-mentioned aspect/embodiment(s) of the present disclosure.
  • the method involves forming a composite porous layer on an engagement surface of a ceramic body.
  • the resultant composite porous layer has pluralities of micro- to nano-scale pores and micro-particles dispersed within the composite porous layer, thereby increasing the surface roughness of the ceramic article. Accordingly, the bonding strength of the ceramic article with a resin adhesive that is used for fixing the ceramic article to an underlying structure (such as an abutment in the context of dentistry) is improved.
  • the method comprises the steps as follows.
  • step (a) a first ceramic slurry comprising a plurality of first ceramic particles is coated on the engagement surface of the ceramic body.
  • step (b) the ceramic body from step (a) is sintered at a first sintering temperature to fuse the first ceramic particles whereby forming a ceramic basal layer on the engagement surface of the ceramic body.
  • step (c) a second ceramic slurry is coated on the ceramic basal layer, in which the second ceramic slurry comprises a plurality of first ceramic particles and a plurality of second ceramic particles in a weight ratio of about 9:1 to 1:1, in which the sintering temperature of the first ceramic particles is lower than the melting temperature of the second ceramic particles.
  • step (d) the ceramic body from step (c) is sintered at a second sintering temperature to fuse the ceramic basal layer and the first ceramic particles without substantially fusing the second ceramic particles whereby forming the composite porous layer on the engagement surface of the ceramic body.
  • FIG. 1 is a schematic diagram illustrating a ceramic article according to one embodiment of the present disclosure
  • FIG. 2 is a schematic diagram illustrating an all-ceramic Maryland bridge and a sectional, partial enlargement view thereof, according to one embodiment of the present disclosure
  • FIG. 3 is a schematic diagram illustrating an all-ceramic 3-unit bridge according to one embodiment of the present disclosure
  • FIG. 4 is a scanning electronic microscopic (SEM) photograph illustrating the surface of a VZ-A5 ceramic sample according to one example of the present disclosure
  • FIG. 5 provides scanning electronic microscopic (SEM) photographs respectively illustrating the cross-sectional views of ceramic articles after water storage for 1 day or 30 days, in which the ceramic articles are VZ-A5 samples bonded with various resin adhesive according to one example of the present disclosure;
  • FIG. 6 provides scanning electronic microscopic (SEM) photographs respectively illustrating the cross-sectional views of ceramic articles after water storage for 1 day or 30 days, in which the ceramic articles are VZ-B5 samples bonded with RELYXTM U100 resin adhesive according to one comparative example of the present disclosure;
  • FIG. 7 provides scanning electronic microscopic (SEM) photographs respectively illustrating the cross-sectional views of ceramic articles after water storage for 1 day or 30 days, in which the ceramic articles are CE-5 samples bonded with RELYXTM U100 resin adhesive and CE-10 samples bonded with PANAVIATM resin adhesive according to one example of the present disclosure; and
  • FIG. 8 provides scanning electronic microscopic (SEM) photographs respectively illustrating the cross-sectional views of ceramic articles after water storage for 1 day or 30 days, in which the ceramic articles are CP-A5 samples bonded with RELYXTM U100 resin adhesive or PANAVIATM resin adhesive according to one example of the present disclosure.
  • dental restoration means any restoration which may be used in the dental field.
  • Illustrative examples of dental restoration include inlays, onlays, veneers, crowns, bridges, and posts.
  • abutment in accordance with the present disclosure refers to both natural tooth/teeth and dental implant(s) to which a dental restoration is to be attached or fixed.
  • “Sintering” in the sense of the present disclosure means densification of a powder, by heating the material without reaching the liquid state of the main constituents of the sintered material (solid state sintering). In other words, the sintering temperature is typically below the melting point of the main constituents.
  • the exemplary ceramic article 100 as illustrated in FIG. 1 comprises a ceramic body 110 and a composite porous layer 120 disposed on an engagement surface 112 of the ceramic body 110 , and the ceramic article 100 is manufactured by a method comprising the following steps.
  • a first ceramic slurry (not shown) is coated on the engagement surface 112 of the ceramic body 110 .
  • the first ceramic slurry is prepared by mixing a first ceramic powder with a modeling liquid.
  • the modeling liquid may be distilled water.
  • the modeling liquid may be any commercially available modeling liquids that are specifically designed to create a homogeneous mixture.
  • the first ceramic slurry is then applied onto the engagement surface 112 with the aid of a suitable means such as a brush or other applicators.
  • the ceramic body 110 may be made of a material comprising a metal oxide ceramic, such as zirconium oxide and aluminum oxide.
  • the ceramic body 110 may optionally be pre-fabricated ceramics in different shapes, sizes, and even colors that suit the specific application of the final product.
  • the ceramic body 110 or the ceramic article 100 may be post-processed to give its final shape, size, and/or color to the product.
  • a pre-sintered 5 mol % yttria-stabilized zirconia substrate such as 3M-ESPE LAVATM Frame commercially available by 3M-ESPE (St Paul, Minn., USA), was used as the ceramic body 110 .
  • the first ceramic particle is a glass ceramic such as an opaque dental ceramic.
  • the VITA VM®9 EFFECT LINER 3M-ESPE, St Paul, Minn., USA was used as the first ceramic particle.
  • step (b) the ceramic body 110 from step (a) is sintered at a first sintering temperature so that the first ceramic particles of the first ceramic powder are fused (adhered) together to form a ceramic basal layer (not shown) on the engagement surface 112 of the ceramic body 110 .
  • the sintering process is generally carried out in commercially available sintering furnaces (such as the VITA VACUMAT® 40T (3M Taiwan Ltd., Taiwan) furnace used in the present disclosure) or other equivalent apparatus.
  • the choice of the first sintering temperature depends on the composition of the first ceramic particles. For most commercially available dental opaques, the sintering temperature is about 850-1000° C., and the sintering temperature for the VITA VM®9 EFFECT LINER used in the working examples is about 900-950° C.
  • the duration of the sintering process varies with factors such as the species of the first ceramic particles, and the amount of the slurry coated on the ceramic body 110 .
  • the duration may be determined by persons having ordinary skills in the art based on their experiences or protocols provided by the manufacturers of the ceramic materials or sintering furnaces.
  • the first sintering process is carried out in multiple stages having various temperatures and durations so as to achieve a more desirable sintering effect.
  • step (c) a second ceramic slurry is coated on the ceramic basal layer of the ceramic body 110 .
  • the second slurry is coated onto the ceramic basal layer with the aid of a brush or other suitable applicators.
  • the second ceramic slurry is formed from a mixture comprising the first ceramic powder and a second ceramic powder in a weight ratio of about 9:1 to 1:1; preferably, about 5:1 to 1:1.
  • the second ceramic powder shall have a melting temperature which is greater than the sintering temperature of the first ceramic powder such that the ceramic particles of the second ceramic powder would not be fused under a sintering condition that is sufficient to fuse the first ceramic particles.
  • the melting temperature of the first ceramic particle is lower than the melting temperature of the second ceramic particle.
  • the second ceramic particles have an average diameter of about 0.1-0.8 ⁇ m; preferably, about 0.1-0.2 ⁇ m.
  • the average diameter may be about 0.1, 0.15, 0.2, 0.25, 0.3, 0.35, 0.4, 0.45, 0.5, 0.55, 0.6, 0.65, 0.7, 0.75, or 0.8 ⁇ m.
  • the second ceramic particle may have a Mohs hardness of at least 8.5 according to some embodiments of the present disclosure.
  • the second ceramic particles are preferably biocompatible.
  • yttria-stabilized zirconia (YSZ) in which the yttria is present in an amount of about 0.5-35 mole percent may be used as the second ceramic particle.
  • the second ceramic particle is 8 mol % yttria-stabilized zirconia (8YSZ), which has a melting temperature of about 2680° C. and a Mohs hardness of about 8.5.
  • the two ceramic powders may come in a pre-mixed or mixed-on-site form.
  • the first and second ceramic powders are ball-milled to provide a mixture with a more satisfactory homogeneity.
  • the mixture comprising the first and second ceramic powders are mixed with a suitable modeling liquid to give the second ceramic slurry.
  • the modeling liquid used in step (c) may be same as or different from the modeling liquid used in step (a); however, in preferable embodiments, they are the same.
  • step (d) the ceramic body 110 from step (c) is sintered at a second sintering temperature so as to fuse the ceramic basal layer with the first ceramic particles without substantially fusing the second ceramic particles and whereby forming the composite porous layer 120 on the engagement surface 112 of the ceramic body 110 .
  • a second sintering temperature that is lower than the sintering temperature (and thus the melting temperature) of the second ceramic particles, so as to prevent fusion of the second ceramic particles with the ceramic basal layer.
  • the sintered, first ceramic material 122 including the ceramic basal layer as well as the first ceramic particles in the second ceramic slurry
  • the presence of the un-sintered, second ceramic particles 124 would impede the continuous flow of the first ceramic material. Therefore, multiple pores (voids) are formed on the surface of the composite porous layer 120 , and some of the second ceramic particles 124 are dispersed within the composite porous layer 120 .
  • the pores allow the penetration of the resin adhesive (not shown) that is used to fix the ceramic article 100 to an underlying structure (not shown), thereby increasing the bonding strength between the ceramic article 100 and the resin adhesive.
  • the pores and second ceramic particles 124 on the surface contribute to the increased surface roughness of the ceramic article 100 , and the increased contact area resulting from the increased surface roughness would also improve the bonding strength between the ceramic article 100 and the resin adhesive.
  • the composite porous layer 120 has a thickness of about 5-20 ⁇ m; preferably, 10-20 ⁇ m. In some embodiments, the average surface roughness (Ra) of the composite porous layer 120 is at least 0.5 ⁇ m; preferably, about 0.85-1.7 ⁇ m.
  • a conventional Maryland bridge consists of at least one artificial ceramic tooth and two metal wings (retainers) attached to the sides of the artificial tooth.
  • the metal wings are prepared in a way that each possesses a porous surface so that it can receive a bonding agent, and then the wings are bonded to the back sides of the teeth (abutments) on either side of the missing tooth.
  • the ceramic article may be manufactured as an all-ceramic Maryland bridge 200 as illustrated in FIG. 2 .
  • the all-ceramic Maryland bridge 200 comprises an artificial tooth 202 and two wings (retainers) 204 .
  • the artificial tooth 202 and the two wings (retainers) 204 may be integrally formed from a high-strength ceramic material 210 such as LAVATM FRAME, and then the engagement surfaces 212 of the wings 204 are treated in accordance with the present method thereby forming a composite porous layer 220 on the engagement surfaces 212 .
  • the composite porous layer 220 is formed from a material comprising a first ceramic material 222 (e.g., VITA VM®9 EFFECT LINER), and a plurality of second ceramic particles 224 (e.g., 8-YSZ). Together, the pores formed on the surface of the composite porous layer 220 and the second ceramic particles 224 dispersed within the composite porous layer 220 may increase the contact area of the composite porous layer 220 . In this way, the bonding strength between the wings 204 of the all-ceramic Maryland bridge 200 and the adhesive resin is enhanced.
  • a first ceramic material 222 e.g., VITA VM®9 EFFECT LINER
  • second ceramic particles 224 e.g., 8-YSZ
  • the thickness of the composite porous layer 220 is about 10-20 ⁇ m, and therefore, the formation of the composite porous layer 220 on the wings 204 would not substantially increase the occlusal height of the Maryland bridge 200 .
  • the second ceramic particles 224 may have an average diameter of about 0.1-0.8 ⁇ m; more favorably, 0.1-0.2 ⁇ m.
  • the ceramic article may be manufactured as an all-ceramic three-unit bridge 300 as illustrated in FIG. 3 .
  • the all-ceramic 3-unit bridge 300 comprises three artificial teeth 304 a - c joined alongside each other in a row, the two artificial teeth 304 a and 304 c on each side are intended to be attached over two abutments 306 (such as the natural tooth, dental post, or other dental implant).
  • the artificial teeth 304 a and 304 c are shaped to have an insertion recess 330 therein for fittingly engaging with the abutments 306 .
  • the three-unit bridge 300 may be integrally made from a high-strength ceramic material such as LAVATM FRAME.
  • the engagement surface 312 defining the insertion recess 330 is treated in accordance with the method described herein to form a composite, porous layer 320 thereon.
  • the composite porous layer 320 like the composite porous layer 220 , is formed from a material comprising a first ceramic material (e.g., VITA VM®9 EFFECT LINER), and pluralities of second ceramic particles (e.g., 8-YSZ). Therefore, the bonding strength between the all-ceramic three-unit bridge 300 and the resin adhesive is improved.
  • the green blank of pre-sintered zirconia (3M-ESPE LAVATM Frame, 3M-ESPE, St Paul, Minn., USA) was dry-cut by a low-speed cutting machine into a size of 20 ⁇ 15 ⁇ 4 mm 3 so as to give a sample having a size of 18 ⁇ 13 ⁇ 3 mm 3 after firing.
  • the sample was sanded with waterproof sand paper (grit #100, 200, 400, 800, 1000, 1200, 1500, and 2000) and polished with polishing fluid containing Al 2 O 3 powders (1.0 ⁇ m and 0.3 ⁇ m) thereby giving the sample an average surface roughness of about 0.02 ⁇ m. Afterwards, the sample was cleaned with 95% alcohol under ultrasonic vibration and then oven-dried.
  • the ceramic samples were treated in accordance with methods according to embodiments of the present disclosure.
  • VITA VM®9 EFFECT LINER 3M-ESPE, St Paul, Minn., USA
  • VITA VM® modeling liquid VITA VM® modeling liquid
  • a thin, even layer of the first slurry was applied to a surface of the sample using a brush, and the sample was left standing in the air for about 10 minutes.
  • the sample was sintered in VITA VACUMAT® 40T furnace with the sintering process as follows. The starting temperature of about 575° C. is maintained for about 6 minutes. Thereafter, the furnace was heated to the sintering temperature of about 930° C.
  • the furnace was vacuumed for about 7.5 minutes.
  • the furnace was cooled down to about 540° C. and lasted for about 1 minute.
  • the second slurry comprising two different ceramic particles was prepared as follows.
  • the VITA VM®9 EFFECT LINER and the 8YSZ powder (diameter of 0.15 ⁇ m or 1 ⁇ m) were mixed in the amount summarized in Table 1.
  • the mixture (about 0.4 g) was then mixed with a suitable amount of deionized water and zirconia balls (as milling medium), and then subjected to wet-milling for about 24 hours (rpm: 360).
  • the mixture was then dried and grounded to give a composite powder.
  • the composite powder was mixed with mixed with VITA VM® modeling liquid to give the second slurry.
  • a thin, even layer of the second slurry was applied over the ceramic basal layer with a brush, and the sample was stood in the air for about 10 minutes. Then, the sample was sintered in VITA VACUMAT® 40T furnace with a second sintering process same as the sintering process for forming the ceramic basal layer. During this second sintering process, the ceramic basal layer and the VITA VM®9 EFFECT LINER within the second slurry would be fused (sintered), while the 8YSZ particles would not be fused due to their high melting temperature, and thereby formed a composite porous layer over the surface of the ceramic article. After the sintering of the composite porous layer, the furnace was cooled down to about 540° C.
  • VZ-A1 to VZ-A5 for composite porous layer having 0.15 ⁇ m-8YSZ
  • VZ-B1 to VZ-B5 for composite porous layer having 1 ⁇ m-8YSZ
  • Comparative samples in which the ceramic samples were treated with conventional methods or coated with other composite powders were also prepared. 6 samples were used in each of the comparative examples.
  • the acid etching processes include HF etching (9.5% HF), hot etching (800 ml of methanol, 200 ml of HCl, and 2 g of FeCl 3 at 80° C.), and chemical etching (3 or 10 drops of HF, 30 ml of HNO 3 , and 60 ml of deionized water).
  • the acid etching was carried out in the fume hood.
  • the sample was washed with water for about 1 minute, and cleaned with 95% alcohol under ultrasonic vibration for about 5 minutes and then oven-dried.
  • These comparative ceramic samples are designated as CE-1 to CE-9 hereinafter.
  • PMMA poly(methyl methacrylate) particles (spherical shape or elliptic shape) was used in place of 8YSZ particles used in Example II, the weight ratios between the VITA VM®9 EFFECT LINER and PMMA particles are summarized in Table 3.
  • the melting temperature of PMMA is about 160° C., which is lower than the melting temperature of the first ceramic material (VITA VM®9 EFFECT LINER).
  • the composite powder containing the VITA VM®9 EFFECT LINER and PMMA was applied on a surface of the ceramic sample and sintered in accordance with steps set forth in Example II.
  • these PMMA particles would be evaporated during the second sintering process due to its low boiling point thereby leaving voids (pores) in the resultant layer.
  • These comparative ceramic samples are designated as CP-A1 to CP-A5 (for composite porous layer having spherical PMMA) and CP-B1 to CP-B5 (for composite porous layer having elliptic PMMA) hereinafter.
  • the average surface roughness (Ra) of each sample was conducted by alpha-step surface profiler (KOSAKA SEF-3500; Mode: ISO 97 (Roughness); Scan distance: 2 mm; Scan rate: 0.2 mm/s; Z-axis: 2000X).
  • HITACHI S-4700 Field emission scanning electron microscope
  • Example V(II) After water storage, the bonded articles from Example V(II) were prepared into tensile test bar (size: 1 ⁇ 1 ⁇ 6 mm 3 ) by a low-speed cutting machine, and the average bonding strength thereof was measured by Micro tensile tester (BISCO).
  • Weight ratios between the first ceramic powder (VITA VM®9 EFFECT LINER) and the second ceramic powder (8YSZ) in the working examples are summarized in Table 1, together with the average surface roughness (Ra) of ceramic samples coated with the composite porous layer prepared in Example II. Also, the average surface roughness (Ra) of comparative ceramic samples from the comparative examples from Example III and the respective treatment thereof are summarized in Table 2. The results are shown as means ⁇ SE of 8 samples for each experimental group.
  • the ceramic samples treated by conventional methods such as acid etching and sandblasting could not substantially increase the surface roughness of the ceramic samples.
  • the surface roughness of ceramic samples treated by HF etching was only about 0.02-0.03 ⁇ m, which was similar to that of the untreated sample from Example I.
  • Chemical etching slightly increased the surface roughness from about 0.02 ⁇ m to about 0.03 to 0.05 ⁇ m.
  • Hot etching was the most effective among the acid etching approaches which increased the surface roughness from about 0.02 ⁇ m to about 0.15 ⁇ m.
  • Sandblasting was more effective than acid etching; however the surface roughness of sandblasted ceramic samples (0.3 ⁇ m) was still unsatisfactory and was much lower than the surface roughness of the ceramic samples according to working examples of the present disclosure.
  • the porous layer formed on the surface of the ceramic sample consists primarily of single component (i.e., the VITA VM®9 EFFECT LINER) because the PMMA particles were evaporated during the sintering process.
  • single component i.e., the VITA VM®9 EFFECT LINER
  • this approach resulted in an increase of surface roughness of the ceramic sample (at least 0.8 ⁇ m) which was commensurate with the working examples provided herein, however, further investigation revealed that this single-component porous layer was not effective in improving the bonding strength of the ceramic samples.
  • FIG. 4 is a microscopic photograph illustrating the surface morphology of the composite porous layer the ceramic sample of example VZ-A5 (hereinafter, VZ-A5 sample). As could be seen in FIG. 4 , there are pluralities of white particles dispersed within the composite porous layer. Analysis with energy dispersive spectrometer (EDS) confirmed that these white particles were 8YSZ particles.
  • EDS energy dispersive spectrometer
  • the ceramic samples were bonded with various resin adhesives (PANAVIATM, RELYXTM U100, or RELYXTM ARC) and underwent water storage (WS) for 1 day or 30 days; the microscopic photographs illustrating the cross-sectional structures of these bonded ceramic samples were provided in FIG. 5 (VZ-A5 sample), FIG. 6 (VZ-B5 sample), and FIGS. 7-8 (comparative samples).
  • resin adhesives PANAVIATM, RELYXTM U100, or RELYXTM ARC
  • WS water storage
  • Test bars were prepared from the ceramic/resin bonded articles to elucidate the bonding strength between the ceramic and resin adhesive; the results are summarized in Table 3 and shown as means ⁇ SE of 8 samples for each experimental group. Most bonded articles formed from comparative ceramic samples broke during the preparation of the test bar; these bonded articles are designated as F (failure) in Table 3.
  • VZ-A5/resin bonded articles exhibited a bonding strength of at least 20 MPa.
  • the VZ-A5/RELYXTM U100 bonded article exhibited a bonding strength of at least 35 MPa, which was suitable for clinical application.
  • the bonding strength after 30 days of water storage was increased as compared with the bonding strength after 1 day of water storage. This was probably due to the self-polymerization of the resin adhesive during the 30 days of water storage.
  • VZ-B5 sample also exhibited increased surface roughness, in comparison with untreated ceramic sample.
  • cracks were observed in the VZ-B5/resin bonded articles.
  • cracks indicated by arrow head
  • All VZ-B5/resin bonded articles broke during the preparation of the test bar, which coincided with the above-mentioned findings in microscopic observation.
  • the sandblasted ceramic sample from example CE-10 (CE-10 sample, hereinbelow) was bonded with PANAVIATM resin adhesive, and no crack was observed after water storage for one day ( FIG. 7( c )) and 30 days ( FIG. 7( d )).
  • the bonding strength of the CE-10/PANAVIA bonded article was 35.60 MPa; however, it was noted that the standard error of this group was quite large ( ⁇ 10.77), which reflected the finding that the bonding strengths of the samples in this group notably varied from one another.
  • the CE-10/PANAVIA bonded articles, after 30 days of water storage failed to give the test bars; suggesting that the long-term water storage may deteriorate the bonding between the CE-10 sample and the PANAVIA resin.
  • test bars were obtained from groups subjected to 30 days of water storage but not from groups subjected to 1 day of water storage.
  • the coating of a composite porous layer comprising 0.15 ⁇ m of 8YSZ particles is effective in increasing both the surface roughness of the ceramic article and the bonding strength between the ceramic article and the resin adhesive.
  • the coating of a composite porous layer comprising 1 ⁇ m of 8YSZ particles (VZ-B5 sample) or single-component porous layer comprising spherical (CP-A5) or elliptic (CP-B5) PMMA particles fails to increase the bonding strength albeit the increase in surface roughness is observed.
  • Other conventional surface treatments including acid etching and sandblasting fail to increase either the surface roughness or the bonding strength to an extent sufficient for clinical application.
  • embodiments of the present disclosure provide an easy-to-manufacture ceramic article with an increased surface roughness and thus an improved bonding strength, as well as a corresponding method for manufacturing it. Accordingly, the present disclosure facilitates the clinical application of all-ceramic material made of high-strength ceramics such as zirconium oxide and aluminum oxide.
  • the present ceramic article provides sufficient wettability to allow the penetration of resin adhesive into the pores of the composite porous layer, thereby increasing the bonding strength.
  • the composite porous layer itself exhibits sufficient bonding strength with the ceramic body on which it is coated so that the composite porous layer would not break away from the ceramic body.
  • the present composite porous layer is thin enough such that it would not substantially increase the occlusal height after being inserted.

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US20170156827A1 (en) * 2014-08-20 2017-06-08 Brandie Carter Winged pontic and related method
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