WO2015037788A1 - Procédé de fabrication d'une restauration en céramique préfabriquée et restauration en céramique préfabriquée produite par le procédé pour des services dentaires et vétérinaires - Google Patents

Procédé de fabrication d'une restauration en céramique préfabriquée et restauration en céramique préfabriquée produite par le procédé pour des services dentaires et vétérinaires Download PDF

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Publication number
WO2015037788A1
WO2015037788A1 PCT/KR2013/012096 KR2013012096W WO2015037788A1 WO 2015037788 A1 WO2015037788 A1 WO 2015037788A1 KR 2013012096 W KR2013012096 W KR 2013012096W WO 2015037788 A1 WO2015037788 A1 WO 2015037788A1
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Prior art keywords
polymer
ready
restoration
sintered
dental
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PCT/KR2013/012096
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English (en)
Korean (ko)
Inventor
김용수
전현준
오경식
홍영표
임형기
함덕원
임형봉
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주식회사 하스
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Publication of WO2015037788A1 publication Critical patent/WO2015037788A1/fr

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/15—Compositions characterised by their physical properties
    • A61K6/16—Refractive index
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
    • A61K6/818—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising zirconium oxide
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/884—Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins

Definitions

  • the present invention is to replace a custom-made ceramic restoration made of an all ceramic crown or porcelain laminate method in a dentistry or laboratory with a ready-made ceramic dental restoration of alumina or zirconia
  • Dental restorations include crowns, inlays, onlays, stumps, veneers, and many other precious metal alloys such as gold alloys. Has been used.
  • Dental crowns / veneers are operations that remove caries and cover the teeth with crowns or apply very thin veneers directly to the tooth surface. It is widely used conservatively in place of whole skin for aesthetic improvement of anterior region or repair of posterior region for damaged teeth such as dwarf, fractured tooth, etc. It is possible to reproduce the natural tooth shape, less gingival irritation, and easy to control the appearance of teeth.
  • the ready-made ceramic dental restorations are immediately tried during prosthetic work, and saliva and blood in the tri-in process according to the tooth size selection and cementing position of individual patients. Due to the contamination caused by the adhesion, the adhesive holding force is lowered and cannot be reused.In the case of zirconia, the strength decrease due to the low temperature deterioration occurs during autoclave sterilization to remove the contamination. Do.
  • the applicant of the present invention is a method of manufacturing a ceramic primary tube that can be widely used as a pediatric prosthetic primary tube using zirconia or alumina through Korean Patent Publication No. 10-1071554 Has been proposed.
  • the invention is produced by heating and injection molding raw materials including zirconia or alumina, a polymer and a colorant, and then extracting and degreasing the polymer in the injection molding and barrel processing after sintering, and can be easily manufactured with high aesthetics and biocompatibility. By enabling mass production, manufacturing cost is reduced, so that it can be widely used not only as a kindergarten but also as a material for other dental restorations.
  • the dental restoration manufactured using the above method does not have complete control of the micropores therein, and thus it is not a problem to be used as a temporary dental restoration material for the purpose of short-term treatment such as a primary tube, but it is a three-dimensional material that should be used for a long time.
  • a temporary dental restoration material for the purpose of short-term treatment such as a primary tube
  • it is a three-dimensional material that should be used for a long time.
  • the problem to be solved by the present invention is a dental-veterinary container that can reproduce the shape and aesthetics of natural teeth while being excellent in strength and toughness, so that the dental restoration form can be maintained even after long-term use.
  • the present invention is mixed with a raw material comprising alumina or zirconia forming the skeleton of the dental restoration, a polymer that lowers the viscosity during injection molding to give ductility and a colorant for imparting a color similar or distinct to natural teeth.
  • the raw material preferably contains 80 to 90% by weight of zirconia or alumina, 9 to 19% by weight of the polymer and 0.005 to 5% by weight of the colorant.
  • the polymer preferably includes ethylene vinyl acetate, paraffin wax, low density polyethylene and stearic acid, 7 to 30% by weight ethylene vinyl acetate, 50 to 65% by weight paraffin wax, 15 to 35% by weight low density polyethylene, and stearic acid 1 More preferably, it contains -5 wt%.
  • the colorant is preferably at least one selected from the group consisting of white titanium oxide, red iron oxide, yellow iron oxide and pink erbium oxide.
  • the polymer extraction step is preferably made by stirring the injection molded product at a temperature of 40 ⁇ 90 °C in acetone, N-methylpyrrolidone or a mixed solvent thereof for 1 to 24 hours.
  • the degreasing step is a process of heat treatment for 6 to 48 hours at a temperature of 500 ⁇ 1200 °C extracted injection part of the polymer, the step of atmospheric pressure sintering 1200 ⁇ 1650 degreasing body from which the polymer is removed It is made of a heat treatment for 6 to 48 hours at a temperature of °C, the degreasing step and atmospheric pressure sintering step is preferably made continuously in one furnace.
  • the pressure sintering step is preferably made of a process of heat-treating the pressure-sintered sintered body for 6 to 24 hours at a temperature of 1200 ⁇ 1650 °C under pressure of 500 ⁇ 1500 bar.
  • the step of heat-treating the pressure-sintered sintered body is preferably made of a process of heat-treating the pressure-sintered body at 500 ⁇ 1500 °C, more preferably made in a state of being cut off from the outside air.
  • the present invention also provides a dental-veterinary ready-made ceramic dental restoration produced by the above method.
  • the ceramic dental restoration of the present invention can reproduce the shape of the natural teeth without implementing ceramic material build-up or CADCAM by implementing the shape, light transmittance and aesthetics of the natural teeth in alumina or zirconia dental restorations.
  • the strength and toughness properties are superior to those of general ceramic lamination methods, so that even after long-term use, the dental restoration form can be maintained as it is, and it can be easily manufactured using injection molding and mass production is possible. It can be widely used as a dental restoration because it is reduced and inexpensive.
  • alumina or zirconia is injection molded to produce preformed dental restorations and preformed tri-in dental restorations, thereby reducing the duration of treatment and reducing the burden on the cost of treatment through immediate modification or rework during the procedure.
  • the ready-made tri-in dental restoration of the present invention can be produced in a variety of colors, such as pink (pink), blue (black), black (black) is easy to secure identification and remove the contamination by saliva and blood poetic It is possible to prevent contamination and improve adhesive strength of the male moldable dental restorations, and to easily secure the size and cementing position of dental restorations for each patient and to maintain high strength and toughness by eliminating the autoclave sterilization process of dental restorations.
  • FIG. 1 is a manufacturing process diagram of a ready-made ceramic dental restoration in accordance with a preferred embodiment of the present invention.
  • FIG. 2 is a view for explaining a process in which the degreasing process and the sintering process of the present invention are performed in-situ in one furnace.
  • FIG. 3 is a view for explaining the pressure sintering process of the present invention.
  • the present invention relates to a method of manufacturing a ready-made ceramic dental restoration and to a dental-veterinary ready-made ceramic dental restoration prepared by such a method, the method of manufacturing a ready-made ceramic dental restoration is alumina or zirconia forming the skeleton of the dental restoration Mixing raw materials including a polymer that lowers the viscosity during injection molding to give ductility and a colorant for imparting a color similar to or distinct from natural teeth; Heating the raw materials such that the polymers contained in the mixed raw materials have ductility; Injection molding the heated raw material; A polymer extraction step of lowering brittleness and ductility of the injection-molded extrudate; Degreasing to completely remove the polymer component from the injection from which some of the polymer is extracted by the polymer extraction; Atmospheric sintering the degreasing body from which the polymer component has been removed to improve mechanical properties; Pressure sintering the atmospherically sintered sintered compact to improve light transmittance and mechanical properties; Heat-treating
  • the present invention proposes a prosthetic ceramic dental restoration for prosthesis, which can meet the esthetics and strength at the same time, can be mass-produced, can improve the quality stability of the product, and can be easily manufactured by injection molding.
  • Figure 1 shows the manufacturing process of the ready-made ceramic dental restoration in accordance with a preferred embodiment of the present invention.
  • Method for manufacturing a ready-made ceramic dental restoration is to give a similar or distinctive color to the alumina or zirconia forming the skeleton of the dental restoration, the polymer and the softness to lower the viscosity during injection molding and give a softness Mixing the raw materials including the colorant (S10); Heating the raw materials such that the polymer contained in the mixed raw materials has ductility (S20); Injection molding the heated raw material (S30); Polymer extraction step (S40) to lower the brittleness and ductility of the injection-molded injection molding; Degreasing to completely remove the polymer component from the injection part in which some of the polymer is extracted by the polymer extraction (S50); Atmospheric sintering the degreased body from which the polymer component has been removed to improve mechanical properties (S60); Pressure sintering the atmospherically sintered sintered compact to improve light transmittance and mechanical properties (S70); Heat-treating the pressure-sintered sintered compact for decarbur
  • the polymer preferably includes ethylene vinyl acetate (EVA), paraffin wax, low density polyethylene (LDPE) and stearic acid, and based on the total weight of the polymer It is more preferable to contain 7-30 wt% of vinyl acetate, 50-65 wt% of paraffin wax, 15-35 wt% of low density polyethylene, and 1-5 wt% of stearic acid.
  • EVA ethylene vinyl acetate
  • LDPE low density polyethylene
  • stearic acid stearic acid
  • the colorant is to impart a color similar to or distinct from natural teeth, and is an inorganic colorant, such as white titanium oxide (TiO 2 ), red iron oxide (Fe 2 O 3 ), yellow iron oxide (Fe 2 O 3 ), and pink erbium oxide (Er). 2 O 3 ) or a mixture of two or more thereof is preferable.
  • an inorganic colorant such as white titanium oxide (TiO 2 ), red iron oxide (Fe 2 O 3 ), yellow iron oxide (Fe 2 O 3 ), and pink erbium oxide (Er). 2 O 3 ) or a mixture of two or more thereof is preferable.
  • Titanium oxide has a white color to give a color very similar to that of natural teeth. It is very different from natural teeth and can be applied as a tri-in dental restoration.
  • the tri-in tooth restoration is used for the preliminary test work performed before the pre-molded dental restoration work, which can be implemented in various colors such as pink, blue, and black, so that the color can be clearly distinguished from natural teeth.
  • a grinding process may be added to secure and refine the size uniformity of the raw material particles, and the grinding may use a wet ball milling process.
  • the ball milling process is performed by charging raw material ceramic (alumina or zirconia), polymer and colorant into a ball milling machine, mixing a solvent such as water or alcohol, and then rotating the ball mill at a constant speed.
  • Raw material particles are mechanically ground and uniformly mixed.
  • the balls used for ball milling may use balls made of ceramics such as zirconia or alumina, and the balls may be all the same size or may be used with balls having two or more sizes.
  • the milling time for example, the size of the ball 1 ⁇ 30 mm, the rotational speed of the ball mill 50 ⁇ 500 rpm, milling time It can be set in the range of 1 to 48 hours.
  • the raw material is pulverized into fine-sized particles and has a spherical uniform particle size distribution.
  • the mixed raw material is heated to a temperature of 40 to 180 ° C. for 1 to 12 hours, and the water contained in the raw material (water or alcohol component used as a solvent in the wet ball milling process) is removed by heating, and the polymer Is lowered to be softer to facilitate the injection molding process.
  • water contained in the raw material water or alcohol component used as a solvent in the wet ball milling process
  • the raw material is injected into the injection molding machine, and the injection molding, the injection temperature is preferably 130 ⁇ 200 °C, the injection molding process is a well known process, so a detailed description thereof will be omitted.
  • the injection molded product in such an injection molding process is very brittle and requires great care during operation. Accordingly, in order to smoothly process and improve the quality of the product, a process for reducing the brittleness and ductility of the injection molded injection molded product is required. do.
  • a solvent such as acetone, N-methylpyrollidone or a mixture thereof, which can dissolve the polymer component.
  • a degreasing process is performed to completely remove the polymer component from the injection product in which a part of the polymer is extracted by the polymer extraction process, and the degreasing process is performed at 500 to 1200 ° C., preferably at 600 to 1000 ° C. for 6 to 48 hours. It consists of a process of heat treatment.
  • the polymer component remaining in the injection molding may form bubbles in the sintering process described below, which may act as a factor of deteriorating the mechanical properties of the sintered body, and may generate voids or fine cracks in the sintered body. You can.
  • the injection product from which the polymer is removed by the polymer extraction and degreasing process has a low brittleness as compared with the injection molding immediately after injection molding, while the ductility increases, which may deform the product during the prosthetic operation.
  • the degreased body from which the polymer of the degreasing process is removed is subjected to atmospheric pressure sintering.
  • the atmospheric pressure sintering process is performed to improve the mechanical properties of the degreased body. Heat treatment for ⁇ 48 hours.
  • the degreasing process and atmospheric pressure sintering process should be performed continuously in one furnace (furnace, as described below) to ensure the process efficiency.
  • FIG. 2 is a view illustrating a process in which a degreasing process and a sintering process are performed in-situ in one furnace.
  • the temperature increase rate is preferably 1 ⁇ 50 °C / min, when the temperature increase rate exceeds 50 °C / min thermal stress may act on the injection molding by a sudden temperature change, if the time is less than 1 °C / minute long There is a disadvantage in that productivity is low.
  • the temperature of the furnace is raised to a target atmospheric pressure sintering temperature of 1200 ⁇ 1650 °C (t3 section of Figure 2) and the temperature increase rate at this time is preferably 5 ⁇ 50 °C / min, the temperature increase rate is 50 °C
  • the temperature increase rate is 50 °C
  • thermal stress may act on the degreasing body due to a sudden temperature change, and in the case of less than 5 ° C / min, it takes a long time to have a disadvantage in decreasing productivity.
  • the sintering temperature is considered in consideration of the diffusion of particles, necking (necking) between the particles If the sintering temperature is too high, the mechanical properties may be degraded due to excessive growth of the particles, and if the sintering temperature is too low, the characteristics of the sintered body may be deteriorated due to incomplete sintering.
  • the microstructure, particle size, and the like of the sintered body are different depending on the sintering temperature. This is because surface diffusion is dominant when the sintering temperature is low, while lattice diffusion and grain boundary diffusion are performed when the sintering temperature is high.
  • the sintering time is more than 48 hours, it is not only economically difficult to expect more sintering effects because energy consumption is high, and when the sintering time is less than 6 hours, the characteristics of the sintered body may be poor due to incomplete sintering.
  • the furnace is cooled, and the cooling of the furnace may be naturally cooled by cutting off the power of the heating means, or may be cooled by artificially setting a temperature drop rate (for example, 10 ° C./minute).
  • the atmospheric pressure sintered sintered body is sintered again in a pressurized state to improve the mechanical properties and light transmittance of the sintered body.
  • the pressure sintering is carried out by applying hot isostatic pressing (HIP), and heat treatment at 1200 ⁇ 1650 °C, preferably 1200 ⁇ 1500 °C under a pressure of 500 ⁇ 1500 bar for 6 to 24 hours .
  • HIP hot isostatic pressing
  • Figure 3 is a view for explaining the pressure sintering process, it will be described in detail with reference to this, first charging the pressure-sintered sintered body into the furnace and then using the heating means and pressure apparatus provided in the furnace temperature of the furnace It raises to 1200-1650 degreeC which is target pressure sintering temperature (t1 section of FIG. 3).
  • the pressure is preferably 500 to 1500 bar, and the temperature increase rate is preferably 5 to 50 ° C./min.
  • the temperature increase rate exceeds 50 ° C./min, thermal stress may act on the sintered body by a sudden temperature change. In the case of less than 5 °C / min has a disadvantage that takes a long time productivity is lowered.
  • the sintering temperature is the most suitable temperature to produce a high-density sintered body while suppressing grain growth Range.
  • the furnace is cooled (t3 section in FIG. 3), and the cooling of the furnace is to naturally cool by cutting off the power of the heating means or artificially set a temperature drop rate (for example, 10 ° C / min). It can also cool.
  • a temperature drop rate for example, 10 ° C / min.
  • Pressurized sintering is performed under high pressure to suppress the temperature rise of the sintered product, so that uniform quality can be obtained in the cross-sectional, length, and width directions, and a pressurized sintered product having a smooth surface at a density of 100% is obtained. It is possible to obtain a dental restoration, such as a veneer with a flat plate with no relief.
  • the pressure sintered body is heat-treated at 500 to 1500 ° C. for the decarburization and light transmission reproduction of the pressure-sintered pressure sintered body.
  • decarburization occurs at the surface of the sintered body, and the hardness of the core is maintained while the toughness of the surface is increased.
  • the change in the properties of the ceramic depending on the content is caused by the higher hardness of the ceramic and the higher tensile strength of the ceramic.
  • the ratio of oxygen is increased by the penetration of external air during the decarburization heat treatment, the surface decarburization of the sintered body is not performed smoothly, so it is preferable to perform the decarburization heat treatment in a state in which the external air is blocked.
  • the outer surface of the sintered body is polished to give glossiness and barrel processing is carried out for 12 to 72 hours to remove fine burrs.
  • the barrel processing is to put the object to be treated in a rotating container and rotate with the abrasive.
  • As a finishing method for polishing it is generally used for burr removal, corner trimming, surface finishing, or gloss finishing, and this barrel processing is well known in the art, and thus description thereof is omitted.
  • the ready-made ceramic dental restoration of the present invention prepared as described above is particularly suitable for the manufacture of crowns or veneers, and has a three-dimensional three-dimensional conformational crown or thin plate shape without a separate manufacturing process through injection molding and pressure sintering. Since the veneer shape can be implemented, the manufacturing process can be shortened, thereby reducing manufacturing time and cost.
  • Custom dental dental restorations manufactured by ceramic crowns or porcelain laminates in conventional dental or laboratory can be replaced with ready-made ceramic dental restorations of alumina or zirconia according to the present invention. Or it can be widely used as a veterinary dental restoration.

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  • Health & Medical Sciences (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Epidemiology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Ceramic Engineering (AREA)
  • Plastic & Reconstructive Surgery (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Dental Prosthetics (AREA)
  • Dental Preparations (AREA)
  • Dental Tools And Instruments Or Auxiliary Dental Instruments (AREA)

Abstract

La présente invention concerne : un procédé de fabrication d'une restauration en céramique préfabriquée par remplacement d'une restauration en céramique sur mesure, qui est fabriquée par un procédé de couronne toute céramique ou de stratifié porcelaine dans une clinique dentaire ou un laboratoire de dentisterie, par une restauration céramique préfabriquée en alumine ou en zircone, ce qui permet l'essayage de la prothèse et la pose de dent provisoire immédiate ; et une restauration en céramique préfabriquée pour des services dentaires et vétérinaires fabriqués par le procédé. La restauration en céramique préfabriquée de la présente invention peut reproduire la forme d'une dent naturelle telle qu'elle est, peut conserver la forme de la restauration opérée même si elle est utilisée pendant longtemps, est facile à fabriquer, réduit les coûts de fabrication, réduit la durée du traitement et la charge financière médicale d'un patient par le biais d'un travail ou d'une réfection correctif immédiat pendant une opération, favorise la prévention de la contamination et l'amélioration de l'adhésion, permet d'obtenir une taille de restauration pour chaque patient et la fixation aisée de la position de cimentation, et peut maintenir une résistance et une dureté élevées.
PCT/KR2013/012096 2013-09-10 2013-12-24 Procédé de fabrication d'une restauration en céramique préfabriquée et restauration en céramique préfabriquée produite par le procédé pour des services dentaires et vétérinaires WO2015037788A1 (fr)

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KR1020130108612A KR101676610B1 (ko) 2013-09-10 2013-09-10 기성형 세라믹 치아수복물의 제조방법
KR10-2013-0108612 2013-09-10

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11523888B2 (en) 2016-10-07 2022-12-13 3M Innovative Properties Company Ceramic dental restorations made by additive manufacturing

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20210100861A (ko) 2020-02-07 2021-08-18 부산대학교 산학협력단 치아 수복용 조성물의 제조 방법

Citations (5)

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JP2000086333A (ja) * 1998-09-11 2000-03-28 Asahi Optical Co Ltd 高強度リン酸カルシウム系セラミックスの製造方法および高強度リン酸カルシウム系セラミックス
US20020010063A1 (en) * 1997-11-10 2002-01-24 Marcel Schweiger Process for the preparation of shaped translucent lithium disilicate glass ceramic products
US20050127544A1 (en) * 1998-06-12 2005-06-16 Dmitri Brodkin High-strength dental restorations
JP2010105884A (ja) * 2008-10-31 2010-05-13 Tosoh Corp 高靭性で透光性のアルミナ焼結体及びその製造方法並びに用途
KR101071554B1 (ko) * 2010-04-06 2011-10-10 주식회사 하스 세라믹 유치관 제조방법 및 이에 의해 제조된 세라믹 유치관

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Publication number Priority date Publication date Assignee Title
US6648638B2 (en) * 2001-12-28 2003-11-18 3M Innovative Properties Company Orthodontic appliances including polycrystalline alumina-based ceramic material, kits, and methods

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020010063A1 (en) * 1997-11-10 2002-01-24 Marcel Schweiger Process for the preparation of shaped translucent lithium disilicate glass ceramic products
US20050127544A1 (en) * 1998-06-12 2005-06-16 Dmitri Brodkin High-strength dental restorations
JP2000086333A (ja) * 1998-09-11 2000-03-28 Asahi Optical Co Ltd 高強度リン酸カルシウム系セラミックスの製造方法および高強度リン酸カルシウム系セラミックス
JP2010105884A (ja) * 2008-10-31 2010-05-13 Tosoh Corp 高靭性で透光性のアルミナ焼結体及びその製造方法並びに用途
KR101071554B1 (ko) * 2010-04-06 2011-10-10 주식회사 하스 세라믹 유치관 제조방법 및 이에 의해 제조된 세라믹 유치관

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11523888B2 (en) 2016-10-07 2022-12-13 3M Innovative Properties Company Ceramic dental restorations made by additive manufacturing

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