WO2022265129A1 - Bloc de masse dentaire et son procédé de fabrication - Google Patents

Bloc de masse dentaire et son procédé de fabrication Download PDF

Info

Publication number
WO2022265129A1
WO2022265129A1 PCT/KR2021/007510 KR2021007510W WO2022265129A1 WO 2022265129 A1 WO2022265129 A1 WO 2022265129A1 KR 2021007510 W KR2021007510 W KR 2021007510W WO 2022265129 A1 WO2022265129 A1 WO 2022265129A1
Authority
WO
WIPO (PCT)
Prior art keywords
dental
block
gradient
weight
bulk block
Prior art date
Application number
PCT/KR2021/007510
Other languages
English (en)
Korean (ko)
Inventor
임형봉
김용수
Original Assignee
주식회사 하스
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 주식회사 하스 filed Critical 주식회사 하스
Priority to AU2021451277A priority Critical patent/AU2021451277A1/en
Priority to JP2022549869A priority patent/JP2023534777A/ja
Priority to CA3221037A priority patent/CA3221037A1/fr
Priority to BR112023026201A priority patent/BR112023026201A2/pt
Priority to CN202180012222.3A priority patent/CN115996688A/zh
Priority to PCT/KR2021/007510 priority patent/WO2022265129A1/fr
Publication of WO2022265129A1 publication Critical patent/WO2022265129A1/fr

Links

Images

Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00—Dental prostheses; Making same
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00—Dental prostheses; Making same
    • A61C13/08—Artificial teeth; Making same
    • A61C13/083—Porcelain or ceramic 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
    • A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
    • A61K6/833—Glass-ceramic composites
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00—Compositions for glass with special properties

Definitions

  • the present invention relates to a dental bulk block that is useful for manufacturing artificial teeth similar to the structural characteristics of natural teeth and has improved machinability, and a method for manufacturing the same.
  • the crown material refers to a prosthetic material that restores parts corresponding to dentin and enamel of a damaged tooth, and may be classified into inlays, onlays, veneers, crowns, and the like, depending on the application area. Since the position where the crown material is restored is the outer surface of the tooth, highly aesthetic properties are required, and high strength is required due to abrasion with the opposing tooth or fracture such as chipping.
  • Existing materials used as crown materials include leucite glass-ceramics, reinforced porcelain or fluorapatite (Ca 5 (PO 4 ) 3 F) crystallized glass, which have excellent aesthetic properties but have low strength. As low as 80 ⁇ 120 MPa, it has a high possibility of fracture. Therefore, research to develop high-strength crown materials of various materials is currently underway.
  • Lithium silicate crystallized glass was developed in 1973 by Marcus P. Borom and Anna M. Turkalo (The Pacific Coast Regional Meeting, The American Ceramic Society, San Francisco, CA, October 31, 1973 (Glass division, No.3-G-73P)). was introduced by
  • the crystalline phase and strength of Li 2 O-Al 2 O 3 -SiO 2 -Li 2 OK 2 OB 2 O 3 -P 2 O 5 based glass were studied for various nucleation and growth heat treatment conditions.
  • the high-temperature lithium disilicate crystal phase was expressed from the low-temperature lithium metasilicate, the strength of 30 to 35 KPS was shown, which is due to the difference in thermal expansion coefficient between the base glass, mother glass, Li 2 SiO 5 , and Li 2 SiO 3 phases. It was because.
  • prosthesis processing by CAD/CAM requires that a prosthesis be fabricated by directly processing a bulk body in a hospital and try it on to the patient as quickly as possible (one-day appointment), so the time delay due to the heat treatment process is economical for patients and users. add difficulty.
  • lithium disilicate crystallized glass materials have limitations in realizing high light transmittance or opalescence similar to natural teeth due to their coarse crystal phase.
  • the existing lithium disilicate crystallized glass material first makes lithium metasilicate crystallized glass with good processability for processing, and after processing, lithium disilicate is formed through secondary crystallization heat treatment to improve strength, At this time, the size of the crystal phase was about 3 ⁇ m or more, and in this state, workability was remarkably poor and only strong parts could be implemented.
  • the present applicant proposed a method for manufacturing crystallized glass including a lithium disilicate crystal phase and a silicate crystal phase with excellent processability by adjusting the crystal size by changing the temperature of the first heat treatment, and has already received a patent (domestic patent registration 10- 1975548). Specifically, 60 to 83% by weight of SiO 2 , 10 to 15% by weight of Li 2 O, 2 to 6% by weight of P 2 O 5 serving as a nucleating agent, increase the glass transition temperature and softening point, and chemical durability of glass.
  • a nano-sized lithium disilicate crystal phase and a silica crystal phase of 5 nm to 2000 nm are generated by the first heat treatment
  • the second heat treatment Disclosed is a method for manufacturing a crystallized glass for teeth comprising a silica crystal phase, characterized in that light transmittance is controlled by heat treatment temperature.
  • No part of a natural tooth is the same color from the neck to the incisal part.
  • the Build-Up method is a method in which powders such as porcelain or zirconia are layered to form colored artificial teeth, and then heat-treated to realize a color similar to that of natural teeth layer by layer. Although it can be imitated, it is completely dependent on the skillful function of the technician, so the reproducibility is poor, and it is not advantageous to the patient because it is impossible to manufacture in an immediate way, and cutting processing such as CAD / CAM There are problems that are difficult to implement with this method.
  • the present invention has been devised to provide a gradation bulk block with improved aesthetics and particularly improved machinability with respect to such a bulk block.
  • the present invention can be used for the manufacture of an artificial tooth restoration material that expresses multi-gradation permeability or physical properties similar to natural teeth so as to have repeatability without the addition of other processes through cutting processing such as CAD / CAM. It is intended to provide a bulk block for
  • the present invention also has improved machinability, which can shorten the time and process of manufacturing an artificial tooth prosthesis, as well as increase the structural stability in terms of force distribution through gradient functionalization of mechanical properties. It is intended to provide a dental bulk block.
  • the present invention is also intended to provide a method for simply manufacturing a dental bulk block that can be used in the manufacture of an artificial tooth restoration material that exhibits multi-gradation permeability or physical properties similar to those of natural teeth.
  • the present invention is also intended to provide a method for easily manufacturing such a dental bulk block into a dental restoration using a processing machine.
  • One embodiment of the present invention is a glass ceramic block including a crystal phase in an amorphous glass matrix, wherein the main crystal phase is lithium disilicate and the additional crystal phase includes eucryptite, and the size of the main crystal phase with respect to depth
  • a dental bulk block which is a functional gradient material having a gradient of , and no interface exists at the point where the gradient value changes in the size of the main crystal phase.
  • the gradient of the size of the main crystal phase may have an average particle diameter in the range of 0.02 ⁇ m to 1.5 ⁇ m.
  • the dental bulk block according to one embodiment of the present invention may also have a light transmittance gradient with respect to depth.
  • the gradient of light transmittance may be within a range of 22 to 35% based on a wavelength of 550 nm.
  • the gradient of light transmittance may vary within a range of less than 0.5 mm with respect to depth.
  • the dental bulk block according to one embodiment of the present invention also has a slope of L * , a * and b * values according to color difference analysis with respect to depth, and the color deviation ( ⁇ E) value changes even within a range of 1.5 mm with respect to depth. It may be
  • a dental bulk block according to a preferred embodiment may have a crystallinity of 40 to 80%.
  • the crystal phase includes 50 to 90 vol.% of lithium disilicate crystal phase and 10 to 40 vol.% of eucryptite crystal phase based on the total volume of the crystal phase. It may be, and another example may be that a lithium phosphate (lithium phosphate) crystal phase is additionally included in a maximum of 5 vol.%.
  • the dental bulk block according to one embodiment of the present invention may also have a gradient of flexural strength with respect to depth.
  • the slope of the flexural strength may be within the range of 210 MPa to 510 MPa.
  • a dental bulk block according to one embodiment of the present invention may be made of a continuous glass matrix.
  • the glass matrix contains 69.0 to 78.0 wt% of SiO 2 , 12.0 to 14.0 wt% of Li 2 O, 5.5 to 10 wt% of Al 2 O 3 , 0.21 to 0.6 wt% of ZnO, and 2.0 to 3.5 wt% of K 2 O. % by weight, 0.3 to 1.0% by weight of Na 2 O, 0.1 to 0.5% by weight of SrO, 0.3 to 1.0% by weight of CaO, 0.1 to 2.0% by weight of La 2 O 3 and 2.0 to 6.0% by weight of P 2 O 5 , Al 2 O 3 /(K 2 O+ZnO) molar ratio may satisfy 1.2 to 2.2.
  • It provides a method for manufacturing a dental bulk block, comprising the step of heat-treating the block at a temperature range of 740 to 850 ° C, giving a temperature gradient in the depth direction of the block.
  • the heat treatment step is performed so that the upper layer of the block is applied at a temperature range of 800 to 850 ° C, and the lower layer of the block is applied at a temperature range of 740 to 760 ° C can
  • the heat treatment may be performed for 1 minute to 40 minutes at an operating temperature of 800 to 1,000 ° C. in a gradient heat treatment furnace.
  • One embodiment of the present invention also comprises the steps of manufacturing a predetermined dental restoration by processing the dental bulk block of the embodiments using a processing machine; and polishing or glazing.
  • glazing may be performed at 730 to 820° C. for 30 seconds to 10 minutes.
  • the glazing may be used for adjusting light transmittance of the processed dental restoration through a heat treatment of at least 825°C. At this time, preferably, glazing may be performed at a temperature of at least 825 ° C. for 1 minute to 20 minutes.
  • the dental bulk block according to the present invention is used for manufacturing artificial tooth restorative materials having multi-gradation light transmittance or physical properties similar to those of natural teeth in a repeatable reproducibility without the addition of other processes through cutting processing such as CAD/CAM. It can be used easily, can shorten the time and process of manufacturing artificial tooth prostheses, and can bring about increased structural stability in terms of force dispersion by functionalization of gradients in mechanical properties, such dental bulk
  • the block has the advantage that it can be manufactured through a simple method of gradient heat treatment using a single glass composition having a specific composition.
  • FIG. 1 is a graph of the results of X-ray diffraction analysis (X-Ray Diffraction) of the bulk block of the present invention.
  • Figure 2 is a scanning electron microscope (SEM) photograph showing the microstructure and crystal phase size by depth of the bulk block of the present invention.
  • Figure 3 is a visible light transmittance measurement graph for 1.5 mm thick slice specimens of the bulk block of the present invention.
  • Figure 4 is a comparative graph of cutting resistance (cutting resistance) for the bulk block of the present invention.
  • Figure 5 is a schematic diagram showing a method for manufacturing a dental bulk block of the present invention as an example.
  • FIG. 6 is a graph showing the particle size of the main crystal phase by depth of a bulk block obtained according to an embodiment of the present invention.
  • FIG. 7 is a graph showing changes in biaxial flexure strength by depth of a bulk block obtained according to an embodiment of the present invention.
  • the dental bulk block of the present invention is a glass ceramic block including a crystal phase in an amorphous glass matrix, wherein the main crystal phase is lithium disilicate and the additional crystal phase includes eucryptite, and the depth of the main crystal phase is It is a functional gradient material that has a gradient and does not have an interface at the point where the gradient value changes in the size of the main crystal phase.
  • main crystal phase is defined as a crystal phase that accounts for at least 50% by weight of the total crystal phase
  • additional crystal phase may be defined as a remaining crystal phase other than the main crystal phase among the total crystal phases.
  • the content of the crystalline phase can be calculated through X-ray diffraction analysis.
  • the ratio F a of the crystalline phase a is quantitatively represented by Equation 1 below.
  • K is the ratio of absolute intensities of two pure polymorphs, I oa /I ob , and is obtained by measuring standard substances.
  • main crystal phase may be defined as set based on the content calculated according to this method.
  • the meaning of 'having a slope of the size of the main crystalline phase with respect to the depth' means that when the size of the main crystalline phase according to the depth of the bulk block is graphed, there is a change slope of the size of the main crystalline phase. That is, it means that the size of the main crystal phase is represented in a gradated form with respect to the depth of the bulk block.
  • the 'change point of the gradient value of the size of the main crystalline phase' means a point at which the gradient value of the change in the size of the main crystalline phase is substantially varied when the size of the main crystalline phase is graphed according to the depth of the bulk block.
  • the meaning of 'substantially fluctuating' may mean a change as a single value, but may also include a substantial change in light of the distribution of the value.
  • the meaning of 'no interface exists at the point of change in the gradient value of the size of the main crystal phase' means that there is no significant interface indicating interlayer separation at the depth point of the bulk block showing the change in the gradient value of the size of the main crystal phase. can be interpreted as That is, it means that the bulk block has a gradient of the size of the main crystal phase in a continuous form without an interface according to depth.
  • 'Functionally Gradient Material (FGM)' refers to a material in which the property of a constituent material continuously changes from one surface to another, and in the present invention, there is practically no interface, but the constituent material In terms of continuously changing properties, the term “gradient functional material” is borrowed.
  • the bulk block is not limited in its shape, and for example, various types of bulk bodies such as block shape, disk shape, ingot shape, cylinder shape, etc. Of course it can be included.
  • the bulk block according to the present invention includes lithium disilicate as a main crystal phase, eucryptite as an additional crystal phase, and lithium phosphate as another additional crystal phase.
  • a graph of XRD analysis results for the bulk block according to a preferred embodiment may be as shown in FIG. 1 .
  • Eucryptite is a lithium aluminum silicate-based (which can be abbreviated as LAS) crystal phase represented by the chemical formula LiAlSiO 4 , and other LAS-based spodumene (LiAlSi 2 O 6 ), orthoclase (LiAlSi 3 O 8 ) or petalite ( Compared to LiAlSi 4 O 8 ), it has low cutting resistance to machining tools due to residual thermal stress. When such a crystalline phase is included, a lower tool wear rate can be exhibited than when only lithium disilicate is present, and when tool resistance is lowered in this way, cutting efficiency can be improved, consumption of milling tools can be minimized, and occurrence during machining can be reduced. chipping (ripping phenomenon) can be minimized.
  • LAS lithium aluminum silicate-based
  • These crystalline phases constituting the bulk block of the present invention can be formed into microcrystals, and have various sizes and size distributions depending on temperature, and various mechanical properties and light transmittance.
  • the bulk block can implement gradated light transmittance and mechanical properties with respect to depth. Moreover, since there is no interface at the point where the gradient value of the main crystal phase changes, interlayer bonding is not required, and the problem of layer separation during cutting can be solved. In addition, it is possible to provide an artificial tooth prosthesis with increased structural stability in terms of force dissipation due to such inclined functionalization.
  • the gradient of the size of the main crystal phase may be implemented within the range of 0.02 ⁇ m to 1.5 ⁇ m in average particle diameter.
  • FIG. 2 shows a scanning electron microscope (SEM) picture of the dental bulk block of the present invention.
  • SEM scanning electron microscope
  • the average size of the crystalline particles can be derived from the SEM picture obtained in this way. Specifically, by drawing a diagonal line or a random straight line on the SEM picture and dividing the number of crystal phases that the straight line passes by the length of the straight line, considering the magnification, the linear intercept It can be obtained according to the method.
  • the bulk block of the present invention is an inclined functional material, and as this functional inclined material is applied to cutting processing, for example, CAD / CAM processing, etc. under the same processing conditions, machinability is considered, and permeability usable clinically, such as artificial tooth restoration materials, is In terms of expression, it may be preferable that the average particle diameter of the gradient of the main crystal phase is in the range of 0.02 ⁇ m to 1.5 ⁇ m.
  • the dental bulk block of the present invention has a gradient of light transmittance with respect to depth according to the gradient of the size of the main crystal phase.
  • the gradient of light transmittance may be in the range of 22 to 35% based on the wavelength of 550 nm.
  • UV-visible spectrometer UV-2401PC, Shimadzu, Japan
  • the dental bulk block of the present invention does not have an interface at the point where the gradient value of the main crystal phase changes. It can be confirmed that it changes even within the range of 1.5 mm for .
  • the surface of the specimen is cleaned using ethanol and UV-visible spectrometer (UV-2401PC, Shimadzu , Japan).
  • UV-visible spectrometer UV-2401PC, Shimadzu , Japan
  • the measurement wavelength range was 300-800 nm
  • the slit width was 2.0 nm. It can be seen from the results of FIG. 3 that there is a difference in transmittance for the slice specimens having a thickness of 1.5 mm.
  • each specimen corresponds to a specimen by depth in Table 1 below.
  • the dental bulk block of the present invention also has a gradient in the shade, specifically, with respect to depth, it has a gradient of L * , a * and b * values according to color difference analysis. As described above, the dental bulk block of the present invention does not have an interface at the point where the gradient value of the main crystal phase changes. there is.
  • the dental bulk block In order to measure the color of the dental bulk block according to the present invention, it is cut to about 1.5 mm in the depth direction where the transparency decreases, and then the surface of the specimen is cleaned with ethanol and UV-visible spectrometer (UV-2401PC, Shimadzu , Japan). At this time, the measurement wavelength range was 380-780 nm, and the slit width was 2.0 nm. After setting a baseline using a reference sample, the reflectance of the specimen was measured to obtain an L * a * b * colorimetric system. The measured L * a * b * value was repeated three times to reduce the error, and then the average value was used. Using these three values, ⁇ E representing the difference in color was obtained.
  • ⁇ E value of the two specimens is 0, it means that there is no difference in color, and a value between 0 and 2 means that there is a very slight difference in color.
  • Values of 2 to 4 mean that color differences are noticeably distinct, and values of 4 to 6 mean that color differences are readily distinguishable.
  • a value of 6 to 12 means that the color difference remains very much, and a value of 12 or more means that the color difference remains very much.
  • the dental bulk block which is an inclined function material that has a gradient of the size of the crystal phase and does not have an interface at the point where the gradient value of the main crystal phase changes
  • the color deviation ( ⁇ E) with respect to the depth for the slice specimens with a thickness of 1.5 mm is It can be confirmed from the results of Table 2 below that 1.4 to 1.6 appear. This result can be seen as meaning that the color deviation ( ⁇ E) value changes even within the range of 1.5 mm for depth, that is, a gradient shade with a different color appears even at this thickness.
  • the dental bulk block of the present invention has a gradient of flexural strength depending on the depth.
  • the flexural strength gradient may be in the range of 210 MPa to 510 MPa.
  • the dental bulk block of the present invention may preferably have a crystallinity of 40 to 80% in consideration of the aspect and processability capable of implementing functional gradients of various physical properties as described above.
  • 'crystallinity' may be defined as the ratio of the crystalline phase to the amorphous glass matrix, which can be obtained through various methods, in one embodiment of the present invention, through an X-ray diffractometer. This is an automatically calculated value.
  • the dental bulk block of the present invention is a glass ceramic in which a crystal phase is precipitated in a continuous amorphous glass matrix, and includes a crystal phase including lithium disilicate as a main crystal phase and eucryptite as an additional crystal phase, It is possible to obtain a functional gradient material having a gradient of the size of the main crystal phase and no interface at the point where the gradient value of the size of the main crystal phase changes.
  • the crystal phase may preferably include 50 to 90 vol.% of the lithium disilicate crystal phase and 10 to 40 vol.% of the eucryptite crystal phase, which is an additional crystal phase, based on the total volume of the crystal phase,
  • lithium phosphate is included as an additional crystalline phase, it may be preferable that the content not exceed 5 vol.% at most.
  • the eucryptite crystal phase may serve to improve cutting machinability of glass ceramics having lithium disilicate as the main crystal phase, but if the content thereof is excessively increased, the strength may be reduced. Therefore, considering processability and strength, it may be preferable that the content of eucryptite in the crystal phase is 10 to 40 vol.% based on the volume of the entire crystal phase.
  • continuous glass matrix may be defined as the fact that no interlayer interface exists in the glass matrix and the composition constituting the glass matrix is the same in the entire block.
  • a preferred glass matrix is specifically SiO 2 69.0-78.0 wt%, Li 2 O 12.0-14.0 wt%, Al 2 O 3 5.5-10 wt%, ZnO 0.21-0.6 wt%, K 2 O 2.0-3.5 wt%, Na 2 O 0.3 ⁇ 1.0% by weight, SrO 0.1 ⁇ 0.5% by weight, CaO 0.3 ⁇ 1.0% by weight, La 2 O 3 0.1 ⁇ 2.0% by weight and P 2 O 5 2.0 ⁇ 6.0% by weight, including Al 2 O 3 / (K 2 O + ZnO) molar ratio may satisfy 1.2 to 2.2.
  • the glass composition precipitates a crystal phase in an amorphous glass matrix through crystal nucleation and crystal growth heat treatment to generate crystallization. That is, crystal nuclei start to form at a minimum of 500 ° C and crystal growth occurs while raising the temperature, and this crystal growth shows the lowest light transmittance when used as an artificial tooth at a maximum of 850 ° C. That is, the light transmittance gradually decreases from the temperature at which the crystal grows up to a maximum of 850 ° C. When focusing on this crystal growth, if it is implemented in one bulk block, it can imitate the multi gradation of natural teeth. do.
  • the present invention SiO 2 69.0 ⁇ 78.0% by weight, Li 2 O 12.0 ⁇ 14.0% by weight, Al 2 O 3 5.5 ⁇ 10% by weight, ZnO 0.21 ⁇ 0.6% by weight, K 2 O 2.0 ⁇ 3.5% by weight, Na 2 O 0.3 ⁇ 1.0% by weight, SrO 0.1 ⁇ 0.5% by weight, CaO 0.3 ⁇ 1.0% by weight, La 2 O 3 0.1 ⁇ 2.0% by weight and P 2 O 5 2.0 ⁇ 6.0% by weight, including Al 2 O 3 / (K 2 O +ZnO)
  • the molar ratio is 1.2 to 2.2, including melting a glass composition, forming and cooling in a mold, and annealing at a set rate for 20 minutes to 2 hours from 480 ° C to 250 ° C. Manufacturing a shaped block; and
  • It provides a method for manufacturing a dental bulk block, comprising the step of heat-treating the block at a temperature range of 740 to 850 ° C, giving a temperature gradient in the depth direction of the block.
  • the glass composition can exhibit characteristics in which the light transmittance of the material is different depending on the heat treatment temperature range.
  • heat treatment When heat treatment is uniformly applied to the entire block, it shows constant light transmittance.
  • multi gradation of physical properties or light transmittance can be expressed in one block.
  • a bulk block In the case of a bulk block, it is used as a workpiece for machining such as CAD/CAM processing.
  • heat is applied with a temperature gradient in the depth direction when the block is heat-treated, so that light transmittance and strength are improved. It can be manufactured as a multi-gradation bulk block.
  • Conventional crystallized glass generally has a coarse crystal size, making it difficult to control light transmittance and hard to process due to its strong strength.
  • the glass composition adopted in the present invention it is possible to form microcrystals, which have various sizes and size distributions depending on temperature. While showing a variety of physical properties and light transmittance, reflecting this, a block is manufactured from one glass composition and then heat-treated by giving a temperature gradient, so that the mechanical properties and light transmittance of one bulk block can be improved. It has become possible to embody it to become a multi-gradation.
  • the meaning of 'the step of heat treatment by giving a temperature gradient in the depth direction of the block' means that the temperature gradient can be sequentially increased from the bottom to the top in the depth direction of the block, as well as partially reducing the temperature difference. Temperature gradients in a given manner are also acceptable.
  • the selection of the temperature gradient method can be changed according to the characteristics of the patient's natural teeth requiring the prosthetic prosthesis or according to the unique characteristics of the part of the tooth requiring the prosthesis.
  • the heat treatment step is performed so that the upper layer of the block is applied in a temperature range of 800 to 850 ° C, and the lower layer of the block is applied in a temperature range of 740 to 760 ° C. It may be preferable to carry out for 1 minute to 40 minutes under an operating temperature of 800 to 1,000 °C in a furnace (furnace).
  • the physical properties of natural teeth have a high flexural strength of enamel, which is the surface layer, and a low strength of dentin inside it, which plays a role in absorbing and dispersing external forces.
  • mechanical properties, mechanical properties Particularly, it is possible to produce an inclined function material having a gradient in flexural strength, so that it can reproduce very similarly to the physical properties of natural teeth.
  • Manufacturing a dental restoration using the dental bulk block obtained according to the present invention can expect a significant improvement in terms of processability. processing to produce a predetermined dental restoration; and polishing or glazing.
  • the dental restoration includes all crowns, inlays, onlays, veneers, abutments, and the like, of course.
  • the glazing may be performed at 730 to 820° C. for 30 seconds to 10 minutes, and in this case, it may be a typical finishing heat treatment step in which there is little change in light transmittance by heat treatment. Glazing is usually performed within a range that does not change the inherent light transmittance of the bulk block, and during the glazing heat treatment, surface healing can increase the strength by 50% or more.
  • the glazing in the manufacturing method of a dental restoration using a bulk block according to the present invention, may be used for adjusting the light transmittance of the processed dental restoration through a heat treatment of at least 825 ° C. . That is, glazing can be used for the purpose of adjusting the brightness by reducing the light transmittance in the final finishing step after manufacturing a dental restoration by processing the bulk block.
  • a dental restoration by machining using a bulk block by a processor or a user
  • the light transmittance is unintentionally changed to a high level.
  • a conventional lithium disilicate-based bulk block After the block is discarded, a bulk block that satisfies the desired light transmittance is reprocessed through a predetermined heat treatment from the bulk block, and then the bulk block is processed into a dental restoration.
  • the bulk block according to the present invention it is a specific bulk block having a fine crystalline phase, and since it can express the characteristics of adjusting the light transmittance according to the heat treatment temperature, it does not require reprocessing and finishes the processed product as a dental restoration.
  • the step of performing glazing under predetermined conditions the light transmittance can be easily adjusted again. Thus, it is possible to shield colored teeth generated during processing with dental restorations in a simple way through glazing.
  • Glazing for this application is preferably carried out at a temperature of at least 825° C. for 1 to 20 minutes.
  • a glass ceramic block comprising a crystal phase in a glass matrix of which the main crystal phase is lithium disilicate and the additional crystal phase includes eucryptite, has a gradient of the size of the main crystal with respect to the depth, and the size of the main crystal
  • the dental bulk block (this invention), which is an inclined functional material that does not have an interface at the gradient value change point of (2514485H17, Norton, USA) was rotated at 250 RPM and the cutting time was measured.
  • Cutting resistance (%) was calculated from each cutting time value obtained in this way. Specifically, the cutting time obtained for a general lithium disilicate block was set as 100%, and the cutting time was converted into a relative percentage. This was calculated as each cutting resistance value.
  • the general lithium disilicate block had the highest cutting resistance, followed by lithium alumino silicate (LAS) crystallized glass and zirconia-reinforced crystallized glass, and the block according to the present invention had significantly lower cutting resistance. showed cutting resistance. From these results, it can be predicted that the glass ceramic block of the present invention is the most machinable, which is due to the inclusion of eucryptite as an additional crystal phase.
  • LAS lithium alumino silicate
  • a specific embodiment of the present invention is, first, SiO 2 69.0 ⁇ 78.0% by weight, Li 2 O 12.0 ⁇ 14.0% by weight, Al 2 O 3 5.5 ⁇ 10% by weight, ZnO 0.21 ⁇ 0.6% by weight, K 2 O 2.0 ⁇ 3.5 % by weight, 0.3 to 1.0% by weight of Na 2 O, 0.1 to 0.5% by weight of SrO, 0.3 to 1.0% by weight of CaO, 0.1 to 2.0% by weight of La 2 O 3 and 2.0 to 6.0% by weight of P 2 O 5 , Al 2 O 3 /(K 2 O + ZnO)
  • the glass composition satisfying the molar ratio of 1.2 to 2.2 is weighed and mixed.
  • Al 2 O 3 When Al 2 O 3 is added to silicate glass, it enters the tetrahedral site and acts as a glass former, increasing the viscosity and reducing the mobility of ions.
  • K 2 O, ZnO, CaO, and LaO lower viscosity and increase ion mobility.
  • an increase in modifiers such as ZnO increases the mobility of ions, and when an excess of SiO 2 is included, minor crystal phases such as eucryptite are precipitated in the glass matrix along with lithium disilicate, the main crystal phase. do.
  • an Al 2 O 3 /(K 2 O+ZnO) molar ratio of 1.2 to 2.2 may be preferable in providing the bulk block of the present invention including eucryptite as an additional crystalline phase.
  • Li 2 CO 3 may be added instead of Li 2 O, and carbon dioxide (CO 2 ), which is a carbon (C) component of Li 2 CO 3 , is released as a gas during the glass melting process.
  • CO 2 carbon dioxide
  • K 2 CO 3 and Na 2 CO 3 may be added instead of K 2 O and Na 2 O in alkali oxides, and carbon dioxide ( CO 2 ) is released as a gas in the melting process of glass and escapes.
  • Ball milling uses a dry mixing process, and a ball milling process or the like can be used as the dry mixing process.
  • a ball milling process or the like can be used as the dry mixing process.
  • starting materials are charged into a ball milling machine, and the ball milling machine is rotated at a constant speed to mechanically grind and mix the starting materials uniformly.
  • Balls used in the ball mill may be balls made of a ceramic material such as zirconia or alumina, and balls having the same size or at least two different sizes may be used. Considering the target particle size, adjust the ball size, milling time, and rotation speed per minute of the ball mill.
  • the ball size may be set in the range of about 1 mm to 30 mm, and the rotational speed of the ball mill may be set in the range of about 50 to 500 rpm.
  • Ball milling is preferably performed for 1 to 48 hours in consideration of the target particle size.
  • the starting material is pulverized into finely sized particles, has a uniform particle size, and is uniformly mixed at the same time.
  • the mixed starting materials are placed in a melting furnace, and the melting furnace containing the starting materials is heated to melt the starting materials.
  • melting means that the starting material is changed into a viscous material state of a liquid state rather than a solid state.
  • the melting furnace is preferably made of a material having a high melting point, high strength, and a low contact angle to suppress the sticking of the melt.
  • platinum (Pt) diamond-like-carbon (DLC), chamotte
  • It is preferably a melting furnace made of the same material or coated with a material such as platinum (Pt) or diamond-like-carbon (DLC).
  • Melting is preferably performed for 1 to 12 hours at 1,400 to 2,000 ° C. and atmospheric pressure. If the melting temperature is less than 1,400 ° C, the starting material may not be melted yet, and if the melting temperature exceeds 2,000 ° C, it is not economical because excessive energy consumption is required. Do. In addition, if the melting time is too short, the starting material may not be sufficiently melted, and if the melting time is too long, excessive energy consumption is required, which is not economical.
  • the temperature increase rate of the melting furnace is preferably about 5 to 50°C/min. If the temperature increase rate of the melting furnace is too slow, it takes a long time to reduce productivity.
  • melting is preferably performed in an oxidizing atmosphere such as oxygen (O 2 ) or air.
  • the melt is poured into a predetermined molding mold to obtain a crystallized glass for teeth in a desired shape and size.
  • the forming mold is preferably made of a material that has a high melting point, high strength, and a low contact angle to suppress the sticking of the glass melt.
  • it is made of a material such as graphite or carbon, In order to prevent this, it is preferable to preheat to 200 ⁇ 300 °C and pour the melt into the molding mold.
  • the melt contained in the molding mold is molded and cooled, it may be desirable to undergo an annealing step at a set rate for 20 minutes to 2 hours from 480 ° C to 250 ° C after the cooling process.
  • the slow cooling step reduces the stress deviation in the molded product, preferably, so that the stress does not exist, and has a desirable effect on controlling the size of the crystal phase and improving the homogeneity of the crystal distribution in the subsequent crystallization step. , thereby ultimately obtaining the desired functional gradient material.
  • the speed set here may be preferably 2.3 to 14 ° C / min in terms of sufficient slow cooling.
  • the molded article that has undergone the slow cooling process is transferred to a crystallization heat treatment sintering furnace to form nuclei and grow crystals to manufacture a desired crystallized glass.
  • FIG. 5 schematically shows a method of performing crystallization heat treatment by giving a temperature gradient according to the present invention.
  • the upper end is heat treated at a high temperature (High temperature) and the lower part is heat treated by giving a temperature gradient to perform low temperature heat treatment.
  • the heat treatment step by giving a temperature gradient is not limited to a specific device and method, but can be performed in a gradient heat treatment furnace as an example, and considering the heat treatment temperature, the operating temperature is 900 to 900 It may be preferred to operate under 1,100°C.
  • the light transmittance from the high temperature part to the low temperature part has a high transmittance and a gradient
  • the flexural strength shows an aspect with a low flexural strength and a gradient. This is because the size of the crystals in the crystallized glass can be controlled with temperature.
  • the crystal phase generated after heat treatment with a temperature gradient includes lithium disilicate as a main crystal phase and eucryptite as an additional crystal phase, and may have a size gradient of 0.02 ⁇ m to 1.5 ⁇ m in average particle size.
  • the present invention is useful for manufacturing artificial teeth similar to the structural characteristics of natural teeth, and particularly relates to a dental bulk block with improved machinability and a method for manufacturing the same.
  • the dental bulk block according to the present invention is used for manufacturing artificial tooth restorative materials having multi-gradation light transmittance or physical properties similar to those of natural teeth in a repeatable reproducibility without the addition of other processes through cutting processing such as CAD/CAM. It can be used easily, can shorten the time and process of manufacturing artificial tooth prostheses, and can bring about increased structural stability in terms of force dispersion by functionalization of gradients in mechanical properties, such dental bulk
  • the block has the advantage that it can be manufactured through a simple method of gradient heat treatment using a single glass composition having a specific composition.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Engineering (AREA)
  • Epidemiology (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Dentistry (AREA)
  • Plastic & Reconstructive Surgery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Glass Compositions (AREA)
  • Dental Preparations (AREA)
  • Dental Prosthetics (AREA)

Abstract

La présente invention divulgue un bloc de masse dentaire pour la coupe, le bloc de masse dentaire étant un bloc de vitrocéramique comprenant une phase cristalline dans une matrice de verre amorphe, la phase cristalline principale étant du disilicate de lithium, et de l'eucryptite étant en outre inclus en tant que phase cristalline supplémentaire. Le bloc de masse dentaire est un matériau à gradient fonctionnel qui présente un gradient de la taille de la phase cristalline principale par rapport à la profondeur, et dans lequel aucune interface n'est présente à des points au niveau desquels la valeur de gradient de la taille de cristal principale change. Le bloc de masse dentaire est utile pour fabriquer une prothèse dentaire artificielle qui est similaire à une dent naturelle, la phase cristalline supplémentaire d'eucryptite facilite le traitement mécanique du bloc de masse dentaire par rapport au cas où seul le disilicate de lithium est présent, et le bloc de masse dentaire réduit non seulement le temps nécessaire à la fabrication de la prothèse dentaire artificielle, mais peut également procurer l'effet d'une stabilité structurelle accrue en termes de distribution de forces en raison de la fonctionnalisation par gradient des propriétés mécaniques.
PCT/KR2021/007510 2021-06-15 2021-06-15 Bloc de masse dentaire et son procédé de fabrication WO2022265129A1 (fr)

Priority Applications (6)

Application Number Priority Date Filing Date Title
AU2021451277A AU2021451277A1 (en) 2021-06-15 2021-06-15 Dental bulk block, and method for manufacturing same
JP2022549869A JP2023534777A (ja) 2021-06-15 2021-06-15 歯科用バルクブロック及びその製造方法
CA3221037A CA3221037A1 (fr) 2021-06-15 2021-06-15 Bloc de masse dentaire et son procede de fabrication
BR112023026201A BR112023026201A2 (pt) 2021-06-15 2021-06-15 Bloco de massa dentário e método para fabricar o mesmo
CN202180012222.3A CN115996688A (zh) 2021-06-15 2021-06-15 牙科用块体及其制造方法
PCT/KR2021/007510 WO2022265129A1 (fr) 2021-06-15 2021-06-15 Bloc de masse dentaire et son procédé de fabrication

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/KR2021/007510 WO2022265129A1 (fr) 2021-06-15 2021-06-15 Bloc de masse dentaire et son procédé de fabrication

Publications (1)

Publication Number Publication Date
WO2022265129A1 true WO2022265129A1 (fr) 2022-12-22

Family

ID=84526573

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/KR2021/007510 WO2022265129A1 (fr) 2021-06-15 2021-06-15 Bloc de masse dentaire et son procédé de fabrication

Country Status (6)

Country Link
JP (1) JP2023534777A (fr)
CN (1) CN115996688A (fr)
AU (1) AU2021451277A1 (fr)
BR (1) BR112023026201A2 (fr)
CA (1) CA3221037A1 (fr)
WO (1) WO2022265129A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20150137573A (ko) * 2014-05-30 2015-12-09 한국세라믹기술원 결정화 글라스-세라믹스 치과 재료의 제조방법
US20180099900A1 (en) * 2016-10-07 2018-04-12 Dentsply Sirona Inc. Lithium silicate glass ceramic
WO2020073254A1 (fr) * 2018-10-10 2020-04-16 Schott Glass Technologies (Suzhou) Co. Ltd. Article en vitrocéramique ultramince et procédé de fabrication d'un article en vitrocéramique ultramince
CN111018356A (zh) * 2019-12-30 2020-04-17 深圳市东丽华科技有限公司 一种高晶体含量的微晶玻璃及其制备方法
KR102246195B1 (ko) * 2019-05-29 2021-04-29 주식회사 하스 절삭가공을 위한 치과용 벌크 블록 및 그 제조방법

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5507981A (en) * 1994-05-31 1996-04-16 Tel Ventures, Inc. Method for molding dental restorations
JP2001288027A (ja) * 2000-02-24 2001-10-16 Tec Ventures Inc 歯科修復物の形成方法及び関連の装置
US7955159B2 (en) * 2003-08-07 2011-06-07 Ivoclar Vivadent Ag Machining of ceramic materials
DE102011084501B3 (de) * 2011-10-14 2013-03-21 Schott Ag Röntgenopakes bariumfreies Glas und dessen Verwendung
KR101796196B1 (ko) * 2015-08-26 2017-11-13 주식회사 하스 상부구조물이 연결된 치과용 결정화 유리 블록 및 이의 제조방법
EP3696149A1 (fr) * 2019-02-14 2020-08-19 Ivoclar Vivadent AG Vitrocéramique fluorescente et verres contenant du cérium et de l'étain

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20150137573A (ko) * 2014-05-30 2015-12-09 한국세라믹기술원 결정화 글라스-세라믹스 치과 재료의 제조방법
US20180099900A1 (en) * 2016-10-07 2018-04-12 Dentsply Sirona Inc. Lithium silicate glass ceramic
WO2020073254A1 (fr) * 2018-10-10 2020-04-16 Schott Glass Technologies (Suzhou) Co. Ltd. Article en vitrocéramique ultramince et procédé de fabrication d'un article en vitrocéramique ultramince
KR102246195B1 (ko) * 2019-05-29 2021-04-29 주식회사 하스 절삭가공을 위한 치과용 벌크 블록 및 그 제조방법
CN111018356A (zh) * 2019-12-30 2020-04-17 深圳市东丽华科技有限公司 一种高晶体含量的微晶玻璃及其制备方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JUNG SEOK-KI, KIM DAE WOON, LEE JEONGYOL, RAMASAMY SELVAPONPRIYA, KIM HYUN SIK, RYU JAE JUN, SHIM JI SUK: "Modulation of Lithium Disilicate Translucency through Heat Treatment", MATERIALS, vol. 14, no. 9, 1 January 2021 (2021-01-01), pages 1 - 10, XP093007761, DOI: 10.3390/ma14092094 *

Also Published As

Publication number Publication date
JP2023534777A (ja) 2023-08-14
CA3221037A1 (fr) 2022-12-22
AU2021451277A1 (en) 2023-12-21
CN115996688A (zh) 2023-04-21
BR112023026201A2 (pt) 2024-03-05

Similar Documents

Publication Publication Date Title
WO2020241974A1 (fr) Bloc dentaire brut pour usinage et son procédé de fabrication
WO2022065560A1 (fr) Bloc dentaire en vrac pour la coupe et son procédé de fabrication
KR102641760B1 (ko) 치과용 벌크 블록 및 그 제조방법
WO2022265129A1 (fr) Bloc de masse dentaire et son procédé de fabrication
WO2022250184A1 (fr) Bloc dentaire en vrac pour usinage par découpe et son procédé de fabrication
WO2023008650A1 (fr) Bloc de masse dentaire et son procédé de fabrication
WO2022250185A1 (fr) Bloc de masse dentaire pour usinage et son procédé de fabrication
WO2022065559A1 (fr) Bloc de masse dentaire pour usinage et procédé de fabrication associé
KR102582076B1 (ko) 절삭가공을 위한 치과용 벌크 블록 및 그 제조방법
KR102582075B1 (ko) 절삭가공을 위한 치과용 벌크 블록 및 그 제조방법
WO2023146227A1 (fr) Ébauche de grande surface pour la fabrication d'une prothèse et son procédé de fabrication
WO2022250183A1 (fr) Bloc dentaire en vrac à découper et son procédé de fabrication
TWI838766B (zh) 牙科用塊體及其製造方法
WO2022270973A1 (fr) Bloc en vrac pour fabrication de prothèse dentaire
KR20220160941A (ko) 절삭가공을 위한 치과용 벌크 블록 및 그 제조방법

Legal Events

Date Code Title Description
ENP Entry into the national phase

Ref document number: 2022549869

Country of ref document: JP

Kind code of ref document: A

121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 21946140

Country of ref document: EP

Kind code of ref document: A1

WWE Wipo information: entry into national phase

Ref document number: 3221037

Country of ref document: CA

WWE Wipo information: entry into national phase

Ref document number: 2021451277

Country of ref document: AU

Ref document number: AU2021451277

Country of ref document: AU

REG Reference to national code

Ref country code: BR

Ref legal event code: B01A

Ref document number: 112023026201

Country of ref document: BR

ENP Entry into the national phase

Ref document number: 2021451277

Country of ref document: AU

Date of ref document: 20210615

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

ENP Entry into the national phase

Ref document number: 112023026201

Country of ref document: BR

Kind code of ref document: A2

Effective date: 20231212