EP4010300A1 - Ébauche crue de dioxyde de zirconium présentant des gradients de couleur et de translucidité - Google Patents
Ébauche crue de dioxyde de zirconium présentant des gradients de couleur et de transluciditéInfo
- Publication number
- EP4010300A1 EP4010300A1 EP20750276.6A EP20750276A EP4010300A1 EP 4010300 A1 EP4010300 A1 EP 4010300A1 EP 20750276 A EP20750276 A EP 20750276A EP 4010300 A1 EP4010300 A1 EP 4010300A1
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- EP
- European Patent Office
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- Prior art date
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Definitions
- the present invention relates to a sintered shaped body with a color gradient for use in the production of dental restorations and the use of the sintered shaped body for dental restorations.
- Ceramic materials usually have a higher strength, but are more demanding to process for dental restorations when it comes to their precisely fitting manufacture.
- ceramic dental restorations both glass-ceramic and oxide-ceramic materials have established themselves on the market.
- melting processes are usually used, while powder technology pressing and sintering processes are required for oxide-ceramic materials.
- multilayer blocks made of feldspar or leucite ceramics for the dental CAD-CAM application are known. From an aesthetic point of view, these correspond to the appearance of natural teeth, but generally have a strength in the range of 150 to 200 MPa. However, these strengths are less suitable, particularly when it comes to dental restorations with thin walls. On the other hand, high strengths can be achieved with layered zirconia blocks. However, these are usually too opaque to be used as monolithic dental restorations. The use of high-strength zirconium dioxide restorations therefore requires manual post-processing. This can consist in infiltrating the porous frameworks with colored liquids before sintering or the sintered restorations with stains or veneering ceramics are individually adapted in color to the natural tooth color.
- a particular challenge of dental restorations is to create a natural-looking color gradient in the ceramic restoration.
- high demands are placed on dental restorations with regard to their strength, especially their edge strength, their translucency and machinability.
- a first object of the present invention is a sintered molded body with a color gradient for use in the production of dental restorations, obtainable by sintering a press molded body comprising five or more different ceramic powder layers, each powder layer comprising at least two different base powders and the base powders each at least 80 wt .-% zirconium dioxide (ZrCh), the weight information being based on the total weight of the base powder.
- a press molded body comprising five or more different ceramic powder layers, each powder layer comprising at least two different base powders and the base powders each at least 80 wt .-% zirconium dioxide (ZrCh), the weight information being based on the total weight of the base powder.
- a ceramic powder layer consists of at least two distinguishable base powders, preferably three or four distinguishable base powders, the ceramic powder layer preferably being present as a homogeneous mixture of the base powders.
- the ceramic powder layers are preferably arranged in layers one above the other, the respectively adjacent powder layers differing in terms of their chemical composition and / or their physical properties. The differences in the compositions of the individual powder layers can be made through the choice and amount of suitable base powder.
- the ceramic powder layers therefore comprise at least two different base powders. In one embodiment, at least two, preferably at least three, and in particular all ceramic powder layers comprise the same base powder, but in different amounts.
- the ceramic powder layers usually also have organic components, such as pressing aids.
- the share, if any, is limited and should not exceed 10 wt .-% based on the ceramic powder layer.
- one or more of the ceramic powder layers in particular each ceramic powder layer, preferably has at least three base powders, preferably four base powders.
- a press mold body comprising five or more different ceramic powder layers, which are used according to the invention, particular advantages become apparent.
- a good color transition and property transition can be achieved, which is important for dental restorations.
- the artificial tooth necks which are designed in deeper and darker colors, can be adjusted to the lighter incisal and dentin areas of artificial teeth, thereby taking into account the aesthetic and mechanical requirements.
- the sintered molded bodies according to the invention have five powder layers, each powder layer having four different base powders, but each powder layer having different amounts of the respective base powder. It has surprisingly been found that it is particularly effective and inexpensive to work if each ceramic powder layer has four or more base powders. Another object of the present invention is therefore a ceramic powder layer that comprises four or more base powders.
- the base powders to be used according to the invention each comprise at least 80% by weight of zirconium dioxide (ZrCh) and preferably at least 0.02% by weight of Al2O3, the weight data being based on the total weight of the components of the base powder.
- ZrCh zirconium dioxide
- each ceramic powder layer of the press mold body has one or more coloring
- Powder layers adjacent is (neighboring layers), surrounded by a neighboring layer, which has a higher concentration of coloring metal oxides than the intermediate layer.
- Each intermediate layer is preferably from an adjacent layer surrounded, which has a lower concentration of coloring metal oxides.
- Each intermediate layer is particularly preferably surrounded by an adjacent layer which has a lower concentration of coloring metal oxides and a neighboring layer which has a higher concentration of coloring metal oxides.
- the molded body has powder layers in which, starting from an outer powder layer, the concentration of one or more coloring metal oxides increases in layers. This has the particular advantage that a flowing color gradient can be established.
- one or more of the ceramic powder layers of the press mold body preferably all powder layers, have coloring metal oxides in an amount of 0.1 to 2.5% by weight, particularly preferably 0.2 to 2.2 % By weight and especially from 0.2 to 1.5% by weight, each based on the total weight of the powder layer.
- the compression mold body has powder layers in which, starting from an outer powder layer, the concentration of at least one coloring metal oxide increases in layers, preferably up to the opposite outer layer.
- each ceramic powder layer of the molded body has Fe2O3.
- the concentration of Fe2O3 differs in each powder layer.
- Each intermediate layer that is to say each powder layer that is adjacent by two directly adjacent powder layers (neighboring layers), is preferably surrounded by a neighboring layer which has a higher concentration of Fe2O3 than the intermediate layer.
- Each intermediate layer is preferably surrounded by a neighboring layer which has a lower concentration of Fe2O3. It is particularly preferable for each intermediate layer to be surrounded by a neighboring layer which has a lower concentration of Fe2O3 and a neighboring layer which has a higher concentration of Fe2O3.
- the molded body has
- the concentration of Fe2Ü3 increases in layers. This has the particular advantage that a flowing color gradient can be established. In another preferred
- Embodiments of the invention have one or more of the ceramic Powder layers of the press mold body, preferably all powder layers, Fe2O3 in an amount of 0.01 to 0.25% by weight, particularly preferably from 0.02 to 0.2% by weight and especially from 0.1 to 0.18 % By weight, based in each case on the total weight of the powder layer.
- each ceramic powder layer of the press mold body has Er2Ü3.
- the concentration of Er2O3 differs in each powder layer.
- Each intermediate layer that is to say each powder layer which is adjacent by two directly adjacent powder layers (neighboring layers), is preferably surrounded by a neighboring layer which has a higher concentration of Er2O3 than the intermediate layer.
- Each intermediate layer is preferably surrounded by a neighboring layer which has a lower concentration of Er2O3.
- Each intermediate layer is particularly preferably surrounded by a neighboring layer which has a lower concentration of Er2O3 and a neighboring layer which has a higher concentration of Er2O3.
- the molded body has powder layers in which the concentration of Er2O3 increases in layers starting from an outer powder layer.
- This has the particular advantage that a flowing color gradient can be established.
- one or more of the ceramic powder layers of the press mold body, preferably all powder layers have Er2Ü3 in an amount of 0.01 to 1.5% by weight, particularly preferably 0.05 to 1.2% by weight .-% and especially from 0.1 to 0.9% by weight, or 0.2 to 0.5% by weight, each based on the total weight of the powder layer.
- one or more of the powder layers, preferably each powder layer, of the press-molded body have C03O4.
- the amount of CO 3O 4 can usually be in the range from 0.001 to 0.01, particularly preferably from 0.002 to 0.08% by weight and especially from 0.003 to 0.006% by weight, based in each case on the total weight of the powder layer.
- the base powders are suitable for the production of dental restorations and therefore have the necessary properties even in the final sintered state
- zirconium dioxide which is preferably stabilized by yttrium oxide, also ensures a high proportion
- the base powders are chosen so that they are matched to one another in terms of their grain sizes and their sintering behavior, so that sintering defects do not occur during sintering.
- an individual coloring and translucency can be achieved in each ceramic powder layer, which in turn is selected in such a way that it leads to a continuous and stepless color gradient with the adjacent powder layers, if any.
- the base powders comprise Al2O3 in an amount of 0.02 to 0.6% by weight, particularly preferably 0.03 to 0.4% by weight and especially 0.04 to 0.3% by weight %, preferably 0.04 to 0.2% by weight or 0.03 to 0.1 or 0.02 to 0.08% by weight, based in each case on the total weight of the base powder.
- yttrium oxide or erbium oxide is advantageous for phase stabilization of the zirconium dioxide ceramics in the sintered state.
- At least one, preferably at least two or three of the base powders, in particular all of the base powders, comprise yttrium oxide (Y2O3) and / or erbium oxide (Er203), preferably in an amount of at least 3% by weight, in particular at least 5% by weight % or at least 6% by weight and in particular from 3.0 to 11% by weight, especially from 5 to 10% by weight, preferably from 4.5 to 11% by weight, especially from 6 to 10% by weight. -%, each based on the total weight of the constituents of the base powder.
- Y2O3 yttrium oxide
- Er203 erbium oxide
- At least one of the base powders preferably at least two or at least three of the base powders, has coloring metal oxides.
- these coloring metal oxides can be selected from the group consisting of iron oxide (Fe 2 O 3), cobalt oxide (CO 3 O 4) and erbium oxide (Er 2 O 3).
- Individual tooth colors can be created by adding the coloring metal oxides.
- At least one of the base powders preferably at least two or at least three of the base powders, contains zirconium dioxide, optionally together with hafnium dioxide, in an amount of at least 89% by weight, preferably in an amount of 89 to 98% by weight , in particular from 90 to 96% by weight, based in each case on the total weight of the constituents of the base powder.
- the base powders can contain zirconium dioxide and hafnium dioxide, preferably in a weight ratio of ZrÜ2 to HfÜ2 of 25: 1 to 98: 1, in particular 30: 1 to 90: 1 and especially 50: 1 to 90: 1.
- the powder layers contain a base powder A which contains 92 to 96% by weight of zirconium dioxide, 0.02 to 0.4% by weight, preferably 0.02 to 0.1% by weight of aluminum oxide, 3.5 to 6.5 wt .-%, or 5.0 to 10 wt .-%, preferably 5.0 to 9.5 wt .-% yttrium oxide and 0.02 to 0.1 wt .-% cobalt oxide, the Weight data are based on the total weight of the base powder A.
- the powder layers have a base powder B which contains 85 to 93% by weight of zirconium dioxide, 0.02 to 0.4% by weight, preferably 0.02 to 0.1% by weight of aluminum oxide and 7 , 5 to 11% by weight of erbium oxide, the weight data being based on the total weight of the base powder B.
- the powder layers have a base powder C which contains 90 to 94% by weight of zirconium dioxide, 0.02 to 0.4% by weight, preferably 0.02 to 0.1% by weight of aluminum oxide and 5.5 up to 8.0% by weight, or 6.5 to 10% by weight, preferably 6.5 to 9.5% by weight, yttrium oxide, the weight data in each case being based on the total weight of the base powder
- the powder layers have a base powder D which contains 90 to 94% by weight of zirconium dioxide, 0.02 to 0.4% by weight, preferably 0.02 to 0.1% by weight Aluminum oxide, 5.5 to 8.0% by weight, or 6.5 to 10% by weight, preferably 6.5 to 9.5% by weight yttrium oxide and 0.1 to 0.3% by weight Has iron oxide, the weight data being based in each case on the total weight of the base powder
- At least one base powder preferably all base powders, additionally contain organic constituents, preferably in an amount of 3 to 6% by weight, in particular in an amount of 4 to 5% by weight.
- Organic ingredients come in particular Binders and pressing auxiliaries in question, which can be easily removed thermally in the debinding step.
- Suitable binders for zirconium dioxide sintering powder are known to the person skilled in the art. This includes, for example, polyvinyl alcohol (PVA).
- the base powders preferably have a bulk density below 1.2 g / cm 3 .
- base powders which have an average granulate size D 50 of 35 ⁇ m to 85 ⁇ m, preferably 40 ⁇ m to 80 ⁇ m and in particular 50 ⁇ m to 70 ⁇ m or 40 to 60 ⁇ m.
- the granulate powders are measured dry using laser diffraction using a Cilas granulometer.
- the inorganic constituents of the base powder that is to say after removal of the organic constituents such as binders, etc., usually have a particle size D 50 of 0.1 to 1 ⁇ m, preferably 0.2 ⁇ m to 0.8 ⁇ m and in particular 0.2 ⁇ m to 0.7 pm, measured by means of laser diffraction. It was found that the particle sizes make a positive contribution to sintering and, in particular, to the color transitions between the individual powder layers.
- the press mold body to be sintered according to the invention can be obtained by arranging five or more ceramic powder layers one on top of the other.
- the layers can be arranged, for example, in a cylindrical container with the formation of slices or disks.
- the powder layers can be uniaxially pressed after each layer application. This can be done, for example, by a press ram, but only pre-consolidation takes place.
- the uniaxial pressing of the layers perpendicular to the layer surface is preferably carried out at a pressure of 10 to 20 MPa, in particular 12 to 15 MPa.
- the pressing of the ceramic powder layers, arranged one above the other in layers takes place by pressing initially uniaxially and perpendicular to the layer surface, preferably with the formation of a precompacted press-molded body with a density below 2.8 g / cm 3 , preferably with a Density in the range from 2.5 to 2.7 g / cm 3 , for example 2.65 g / cm 3 .
- the uniaxial precompaction can lead to a better and more intimate mixing and thus a more uniform transition between the layers.
- the pressing for the production of the press mold body takes place isostatically, with the isostatic pressing preferably taking place after uniaxial precompression, with the formation of a press mold body with a density below 3.4 g / cm 3 , in particular a density of 2 , 80 to 3.15 g / cm 3 , especially with a density of 2.85 to 3.10 g / cm 3 .
- the isostatic pressing is preferably carried out after all the layers of the molded press body have been arranged. Suitable pressures for isostatic pressing are usually in the range from 500 to 10,000 bar, preferably in the range from 800 to 8000 bar, for example 1000 to 7000 bar or 1000 to 3000 bar.
- the thickness of the individual powder layers of the press mold body can vary. In a preferred embodiment, at least two of the ceramic powder layers differ in terms of their thickness. At least two of the ceramic powder layers of the press mold body preferably have a thickness difference of at least 5%.
- the molded bodies can be in the form of cylindrical, circular disks with diameters in the range from 50 to 200 mm, for example 75 to 150 mm.
- the total thickness of the cylindrical disks can for example be in the range from 8 to 40 mm, preferably from 10 to 30 mm, especially from 13 to 25 mm.
- the dimensions relate to the press mold body in the unsintered state.
- At least one of the outer ceramic powder layers preferably both outer ceramic powder layers of the press mold body has a greater thickness than a ceramic powder layer lying between the outer ceramic powder layers.
- the above-described layer structure with at least one thicker outer layer has proven to be advantageous, since this represents a suitable structure for processing in CAD / CAM systems or other subtractive processing methods.
- the compression mold body comprises five ceramic powder layers, the first powder layer 20 to 30%, preferably 22 to 28%, the second powder layer 10 to 20%, preferably 12 to 18%, the third powder layer 15 to 25%, preferably 17 to 23%, the fourth powder layer 10 to 20%, preferably 12 to 18% and the fifth powder layer 20 to 30%, preferably 22 to 28% of the total thickness of the powder layers arranged one above the other and with the proviso that the total thickness is 100% supplemented.
- sintering takes place at a temperature in the range from 950 to 1100 ° C., preferably from 980 to 1050 ° C., with the formation of a pre-sintered ceramic molded body (white body).
- a pre-sintered ceramic molded body white body
- the sintering takes place over a period of time which is sufficient to remove the binders present and to give the press-molded body sufficient strength for processing by subtractive processes.
- the pre-sintered and debonded molded bodies are referred to as white bodies.
- the sintering to produce the white body takes place over a period of more than 30 minutes, preferably more than 1 hour, in particular more than 20 hours or more than 50 hours, for example 60 to 200 hours or 70 to 150 hours.
- the pre-sintered ceramic shaped body is processed by subtractive processes and then preferably to be finally sintered in a further step.
- the sintering shrinkage is usually taken into account.
- the Vickers hardness of one outer layer differs from the Vickers hardness of the opposite outer layer.
- the difference in Vickers hardness is preferably at least 5%, more preferably at least 10%, in particular at least 15% or at least 20%, in each case based on the outer layer with the lower hardness.
- the Vickers hardness [HV2] according to DIN EN 843 of the outer layer with the lower Vickers hardness is preferably in the range from 45 to 60, particularly preferably from 50 to 59.
- the Vickers hardness [HV2] according to DIN EN 843 of the outer layer with the higher Vickers hardness is preferably above 60 and especially in the range from 61 to 80, particularly preferably from 65 to 75.
- the final sintering usually takes place at temperatures above 1350 ° C, preferably above 1400 ° C, especially in the range from 1420 ° C to 1600 ° C or 1450 ° C to 1550 ° C.
- the sintering time for the final sintering usually takes place over a period of more than 4 minutes, preferably more than 5 minutes, in particular in the range from 5 to 120 minutes.
- the moldings according to the invention can be used in particular in the dental field. Here they are characterized by high edge strength in dental restorations, an excellent structure and high 3-point flexural strength.
- the ceramic molded bodies of the present invention are therefore preferably dental restorations, such as, for example, inlays, onlays, crowns, bridges, veneers and veneers or abutments for implants.
- Another object of the present invention is the use of the ceramic molded body according to the invention for dental restorations or for the production of dental restorations.
- Another object of the present invention is a
- a method for producing a sintered shaped body with a color gradient for use in the production of dental restorations comprising the steps: a) mixing at least two, preferably at least three, different base powders to produce five or more different ceramic powder layer mixtures; b) Layer-by-layer arrangement of the various ceramic powder layer mixtures obtained in step a) to form ceramic powder layers arranged one above the other; c) Uniaxial pressing of the ceramic powder layers perpendicular to the powder layer surface to form a pre-compacted press mold body; d) Isostatic pressing of the uniaxially pre-compressed compression mold body in step c); and e) sintering the shaped body obtained in step d) to form a ceramic shaped body, the ceramic powder layers each having a composition different from one another and wherein each ceramic powder layer comprises a mixture of at least two, preferably at least three different base powders and the base powders each at least 80 % By weight ZrÜ2, the weight information being based on the total weight of the base powder.
- Another object of the present invention is a sintered molded body with a layer structure and color gradient for use in the production of dental restorations, wherein the molded body has at least two, preferably at least three different ceramic powder layers and each layer consists of at least three or four different base powders, wherein each base powder has at least 80% by weight of ceramic oxides, the weight data in each case being based on the total weight of the base powder.
- the ceramic powder layers preferably have ceramic oxides as defined above.
- the base powders to be used each correspond to the base powders defined above.
- Table 1 shows 4 base powders A to D which are used for the compositions of the ceramic powder layers.
- the granulate size Dso of the base powder is in the range from 40 to 80 ⁇ m.
- the inorganic constituents of the base powder have a particle size D 50 of 0.2 to 0.7 ⁇ m.
- the weight data relate in each case to the total weight of the powder composition.
- Table 1 The weight data relate in each case to the total weight of the powder composition.
- the arrangements of the layers listed in Table 2 below show the composition of each individual ceramic powder layer in the molded body.
- the molded bodies are intended for use in the production of dental restorations, so that the layer compositions are designed according to the position in the tooth.
- the compositions of the powder layers are formed from the base powders by varying the proportions in order to obtain an ideal color gradient.
- the composition of each powder layer is achieved by homogeneously mixing the base powders in the specified amounts.
- the powders are then placed in layers in a cylindrical press mold with a diameter of 100 mm and a layer thickness of 18 mm is set.
- the powder layers are pre-pressed uniaxially at a pressure of 13 MPa perpendicular to the layer surface and then isostatically pressed at a pressure of 2000 bar.
- the ceramic powder layers are arranged so that layer 1 (cutting edge) 25%, layer 2 (dentin / cutting edge) 15%, layer 3 (dentin) 20%, layer 4 (dentin / neck) 15% and layer 5 ( Neck) makes up 25% of the total thickness of the die body.
- FIG. 1 shows, by way of example, dental restorations that are obtained from the exemplary ceramic molded body.
- the layer transitions and color transitions are fluid.
- the restorations show excellent edge strength and stability. Reworking and readjusting the tooth color is not necessary.
- the optimal structure and the composition of the layers shows a largely homogeneous shrinkage over all layers during sintering. This is particularly advantageous for precisely fitting the dental restorations, since costly reworking can be largely avoided.
- the hardness of the ceramic can be optimally adjusted by the layer structure.
- the Vickers hardness is measured after furnace firing on the top (light layer, cutting edge) and on the bottom (dark layer, tooth neck) of an exemplary disc.
- the white body density and thus also the Vickers hardness on the underside is always greater than on the top.
- Table 3 shows the determined values:
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Abstract
L'invention concerne un moulage fritté à gradient de couleur destiné à être utilisé dans la fabrication de restaurations dentaires, pouvant être obtenues par frittage d'un élément moulé par compression comprenant au moins cinq couches différentes de poudre céramique, chaque couche de poudre comprenant au moins deux poudres de base différentes et chaque poudre de base contenant au moins 80 % en poids de ZrO2, chaque proportion en poids se rapportant au poids total de la poudre de base.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP19190778.1A EP3772498A1 (fr) | 2019-08-08 | 2019-08-08 | Procédé de fabrication d'un lingot en dioxyde de zirconium à dégradé de couleurs et translucidité |
EP19190774.0A EP3772497A1 (fr) | 2019-08-08 | 2019-08-08 | Lingot de zircone à dégradé de couleur ou de translucidité |
PCT/EP2020/072048 WO2021023791A1 (fr) | 2019-08-08 | 2020-08-05 | Ébauche crue de dioxyde de zirconium présentant des gradients de couleur et de translucidité |
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EP4010300A1 true EP4010300A1 (fr) | 2022-06-15 |
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EP20750276.6A Pending EP4010300A1 (fr) | 2019-08-08 | 2020-08-05 | Ébauche crue de dioxyde de zirconium présentant des gradients de couleur et de translucidité |
EP20750275.8A Pending EP4010299A1 (fr) | 2019-08-08 | 2020-08-05 | Procédé de fabrication d'une ébauche crue de dioxyde de zirconium avec des gradients de couleur et de translucidité |
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EP20750275.8A Pending EP4010299A1 (fr) | 2019-08-08 | 2020-08-05 | Procédé de fabrication d'une ébauche crue de dioxyde de zirconium avec des gradients de couleur et de translucidité |
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US (2) | US20220273403A1 (fr) |
EP (2) | EP4010300A1 (fr) |
JP (2) | JP2022544088A (fr) |
WO (2) | WO2021023791A1 (fr) |
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US11672632B2 (en) | 2020-10-05 | 2023-06-13 | Pritidenta Gmbh | Multi-layered zirconia dental blank with reverse layers, process for its preparation and uses thereof |
CN113461421B (zh) * | 2021-07-30 | 2022-02-01 | 北京大学口腔医学院 | 一种叠层氧化锆牙科陶瓷材料及其制备方法 |
US11771534B2 (en) * | 2021-12-22 | 2023-10-03 | Franz Collection Inc. | Apparatus and method for three-dimensional laminating a ceramic denture in a color-and-transmittance variable manner |
DE102022104741A1 (de) * | 2022-02-28 | 2023-09-14 | Bredent Gmbh & Co. Kg | Vorrichtung und Verfahren zur Mischung von Bestandteilen eines keramischen Ausgangsstoffes |
JP2024064856A (ja) | 2022-10-28 | 2024-05-14 | 株式会社松風 | 安定化剤濃度のΔSP(m)の最大値が0.5未満であるジルコニア被切削体 |
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US8173562B2 (en) * | 2006-05-23 | 2012-05-08 | Ivoclar Vivadent Ag | Shaded zirconia ceramics |
CN102285795A (zh) * | 2011-05-30 | 2011-12-21 | 北京大学口腔医学院 | 牙科复色可切削氧化锆陶瓷及制备方法 |
JP6392203B2 (ja) * | 2012-04-16 | 2018-09-19 | ヴィタ ツァーンファブリーク ハー. ラオテル ゲーエムベーハー ウント コー カーゲー | 少なくとも2つの層を有する非緻密焼結セラミック成形体の製造プロセス |
KR101324467B1 (ko) * | 2012-06-12 | 2013-11-06 | (주)에큐세라 | 다양한 색상과 투광성이 있는 기능성 지르코니아 블록 |
EP2909029A1 (fr) * | 2012-10-17 | 2015-08-26 | 3M Innovative Properties Company | Bloc de fraisage à zircone dentaire à plusieurs sections, procédé de fabrication et utilisation de celui-ci |
CN103058655B (zh) * | 2013-01-18 | 2014-09-10 | 秦皇岛爱迪特高技术陶瓷有限公司 | 一种梯度透明性氧化锆牙科陶瓷及其制备方法 |
KR101276616B1 (ko) * | 2013-03-05 | 2013-06-19 | 주식회사 디맥스 | 색상 구배를 갖는 인공치아용 지르코니아 블록의 제조방법 |
US10231807B2 (en) * | 2013-05-10 | 2019-03-19 | Kuraray Noritake Dental Inc. | Zirconia sintered body, zirconia composition, zirconia pre-sintered body and preparing method thereof, and dental prosthesis |
EP2829251B1 (fr) * | 2013-07-22 | 2019-04-10 | Ivoclar Vivadent AG | Contrôle de la cinétique de frittage de céramiques oxydées |
KR101601948B1 (ko) * | 2014-09-16 | 2016-03-10 | 주식회사 하스 | 강도, 투광성,색상 구배를 지닌 치과용 지르코니아 블록 및 이의 제조방법 |
CN104844200A (zh) * | 2015-04-30 | 2015-08-19 | 浙江大学 | 多种氧化物掺杂的渐变色氧化锆牙科修复体及其制备方法 |
JP6917679B2 (ja) * | 2016-02-19 | 2021-08-11 | 株式会社松風 | 色調再現性が高い多層構造歯科切削加工用セラミックスブランク |
DE102016106370A1 (de) * | 2016-03-23 | 2017-09-28 | Degudent Gmbh | Verfahren zur Herstellung eines eingefärbten Rohlings sowie Rohling |
EP3108849B1 (fr) * | 2016-04-25 | 2019-04-24 | 3M Innovative Properties Company | Ébauche pour fraisage dentaire à zircone multicouche et procédé de production |
CN107175747B (zh) * | 2017-05-12 | 2020-04-07 | 爱迪特(秦皇岛)科技股份有限公司 | 强度、颜色均匀过渡的牙科氧化锆修复材料及其制备方法 |
-
2020
- 2020-08-05 US US17/632,539 patent/US20220273403A1/en active Pending
- 2020-08-05 US US17/632,534 patent/US20220289632A1/en active Pending
- 2020-08-05 EP EP20750276.6A patent/EP4010300A1/fr active Pending
- 2020-08-05 WO PCT/EP2020/072048 patent/WO2021023791A1/fr unknown
- 2020-08-05 JP JP2022506828A patent/JP2022544088A/ja active Pending
- 2020-08-05 WO PCT/EP2020/072044 patent/WO2021023788A1/fr unknown
- 2020-08-05 JP JP2022506827A patent/JP2022543125A/ja active Pending
- 2020-08-05 EP EP20750275.8A patent/EP4010299A1/fr active Pending
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JP2022543125A (ja) | 2022-10-07 |
JP2022544088A (ja) | 2022-10-17 |
EP4010299A1 (fr) | 2022-06-15 |
US20220273403A1 (en) | 2022-09-01 |
US20220289632A1 (en) | 2022-09-15 |
WO2021023788A1 (fr) | 2021-02-11 |
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