CN112374883B - Integrated multicolor dental CAD/CAM zirconia, preparation method thereof and dry pressing die - Google Patents
Integrated multicolor dental CAD/CAM zirconia, preparation method thereof and dry pressing die Download PDFInfo
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- CN112374883B CN112374883B CN202011289080.9A CN202011289080A CN112374883B CN 112374883 B CN112374883 B CN 112374883B CN 202011289080 A CN202011289080 A CN 202011289080A CN 112374883 B CN112374883 B CN 112374883B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/003—Pressing by means acting upon the material via flexible mould wall parts, e.g. by means of inflatable cores, isostatic presses
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B7/00—Moulds; Cores; Mandrels
- B28B7/0097—Press moulds; Press-mould and press-ram assemblies
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
Abstract
The invention provides a multicolor dental CAD/CAM zirconia, a preparation method thereof and a dry pressing die, wherein the dry pressing die comprises at least one layer of isolation diaphragm arranged inside the dry pressing die, the isolation diaphragm divides the inside of the die into at least two independent spaces, and the isolation diaphragm is movably connected with the die. The preparation method can prepare the zirconium oxide material with two or more colors at one time, is simple and is suitable for industrial production.
Description
Technical Field
The invention belongs to the field of inorganic materials, relates to zirconia and a preparation method thereof, and particularly relates to integrated multicolor dental CAD/CAM zirconia, a preparation method thereof and a dry pressing die.
Background
In the dental field, the all-ceramic restoration technology is an ideal choice for oral materials due to good biocompatibility and excellent aesthetic effect, wherein the zirconia ceramic not only has good wear resistance, physical corrosion resistance and biocompatibility, but also has excellent fracture toughness and strength, the mechanical properties of the zirconia ceramic are obviously superior to those of other materials, the problems of insufficient strength and toughness of conventional all-ceramic materials can be solved, and the all-ceramic restoration technology is the focus of attention and research on the oral materials at present. However, because the dental zirconia has higher cost and higher selling price compared with other all-ceramic materials, and because the VITA16 colorimetric plate or the 26-color colorimetric plate is popularized, the denture processing factory needs to stock most of colors of the color or multi-layer color zirconia, and the stock pressure of the denture processing factory is greatly increased.
CN105924163A discloses a zirconia ceramic block and a preparation method thereof, wherein the method comprises the following steps: mechanically mixing white zirconia powder and three kinds of colored powder according to a certain proportion for 10-20 minutes to prepare colored zirconia powder; putting the colored zirconia powder into a die, dry-pressing and molding, and performing static pressure treatment by a static pressure machine to obtain a zirconia ceramic block blank; and placing the zirconia ceramic block blank in a high-temperature furnace for sintering treatment. However, the zirconia prepared by the technology belongs to single-color zirconia, and the integral color variety is not increased, so that the stock pressure of the denture processing factory cannot be reduced.
CN105584161B discloses a light transmission gradient color zirconia material and a preparation process thereof, belonging to the technical field of dental ceramic materials. The light-transmitting gradient colored zirconia material comprises a bottom layer, an intermediate layer A, an intermediate layer B, an intermediate layer C and an upper layer which are arranged in sequence from bottom to top, and is prepared from three powder materials of 3Y-TZP, (3.5-4.5) Y-PSZ and (4.5-6) Y-PSZ and a colorant according to different mass ratios; the preparation process comprises the steps of placing powder materials according to the formula ratio in a die cavity in a layered mode, carrying out dry pressing forming and cold isostatic pressing forming to obtain a blank, then placing the blank in a sintering furnace for presintering, and carrying out cutting and secondary sintering to obtain the light-transmittance gradient colored zirconia material. However, the zirconia prepared by the technology belongs to a single multilayer color, is only subjected to treatment of gradual change color and gradual change transmittance on the basis of the single color, and does not increase the whole color types, so that the stock pressure of the denture manufacturer cannot be reduced.
Disclosure of Invention
In order to solve the technical problems, the invention provides a multicolor dental CAD/CAM zirconia, a preparation method thereof and a dry pressing die.
One of the purposes of the invention is to provide an integrated multicolor dental CAD/CAM zirconia dry pressing mold, wherein the dry pressing mold comprises at least one isolation diaphragm arranged inside the dry pressing mold, the isolation diaphragm divides the inside of the mold into at least two independent spaces, and the isolation diaphragm is movably connected with the mold.
In the invention, the number of the membranes in the dry pressing die can be adjusted according to the number of colors required by the zirconia.
As the preferable technical scheme of the invention, the isolation diaphragm is made of any one of stainless steel, polyvinyl chloride, polypropylene or organic glass.
In the invention, the isolation diaphragm is made of materials which are not limited to the above materials, and materials which have certain rigidity and small friction with zirconia powder can be used for preparing the isolation diaphragm.
Preferably, the dry-pressing mold comprises a circular dry-pressing mold or a rectangular dry-pressing mold.
In the invention, the shape of the dry pressing die is not limited to the above shape, and dies with other shapes, such as triangle, ellipse or combined graph, can be selected according to the requirement of the product.
Preferably, the size of the isolation diaphragm is the radius length of the inner cavity of the circular dry pressing die or any side length of the inner cavity of the rectangular dry pressing die.
The second purpose of the invention is to provide a preparation method of the dental CAD/CAM zirconia with integrated multicolor, which comprises the following steps:
placing powder of at least two kinds of color zirconia into the dry pressing mould of claim 1 or 2, removing the isolating membrane, performing dry pressing treatment, and performing cold isostatic pressing treatment and presintering treatment in sequence to obtain the integrated multicolor dental CAD/CAM zirconia.
In a preferred embodiment of the present invention, the pressure of the dry pressing is 3 to 15MPa, such as 4MPa, 5MPa, 6MPa, 7MPa, 8MPa, 9MPa, 10MPa, 11MPa, 12MPa, 13MPa or 14MPa, but the pressure is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
In a preferred embodiment of the present invention, the time of the dry pressing treatment is 5 to 30 seconds, such as 8 seconds, 10 seconds, 12 seconds, 15 seconds, 18 seconds, 20 seconds, 22 seconds, 25 seconds, or 28 seconds, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
In a preferred embodiment of the present invention, the cold isostatic pressing treatment is performed at a molding pressure of 80 to 270MPa, such as 90MPa, 100MPa, 120MPa, 150MPa, 180MPa, 200MPa, 220MPa or 250MPa, but the pressure is not limited to the above values, and other values not listed in the above range are also applicable.
In a preferred embodiment of the present invention, the cold isostatic pressing process has a dwell time of 60 to 200 seconds, such as 70 seconds, 80 seconds, 90 seconds, 100 seconds, 110 seconds, 120 seconds, 130 seconds, 140 seconds, 150 seconds, 160 seconds, 170 seconds, 180 seconds, 190 seconds, etc., but the dwell time is not limited to the recited values, and other values not recited in the range of values are also applicable.
In a preferred embodiment of the present invention, the temperature of the pre-sintering treatment is 800 to 1100 ℃, for example 850 ℃, 900 ℃, 950 ℃, 1000 ℃ or 1050 ℃, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
Preferably, the time of the pre-sintering treatment is 90-180min, such as 100min, 110min, 120min, 130min, 140min, 150min, 160min or 170min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
In a preferred embodiment of the present invention, the method for preparing the integrally multicolor dental CAD/CAM zirconia comprises:
placing powder of at least two kinds of color zirconia into the dry pressing die of claim 1 or 2, removing the isolation diaphragm, and then performing dry pressing treatment, wherein the pressure of the dry pressing treatment is 3-15 MPa and the time is 5-30 s; and sequentially carrying out cold isostatic pressing treatment and presintering treatment, wherein the forming pressure of the cold isostatic pressing treatment is 80-270 MPa, the pressure maintaining time is 60-200 s, the temperature of the presintering treatment is 800-1100 ℃, and the time is 90-180min, so that the integrated multicolor dental CAD/CAM zirconia is obtained.
The invention also aims to provide an integrated multicolor dental CAD/CAM zirconia, which is prepared by the preparation method.
Compared with the prior art, the invention at least has the following beneficial effects:
the invention provides a multicolor dental CAD/CAM zirconia, a preparation method thereof and a dry pressing die.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a preparation method of integrated multicolor dental CAD/CAM zirconia, which comprises the following steps:
preparing required colored zirconia powder according to color formulas of A2 color and A3 color of VITA16 color, placing the colored zirconia powder in a rectangular dry pressing die, removing the isolating membrane, performing dry pressing treatment, and sequentially performing cold isostatic pressing treatment and presintering treatment to obtain the multicolor dental CAD/CAM zirconia;
the dry pressing treatment conditions are that the dry pressing pressure is 3MPa, and the dry pressing time is 5s.
The cold isostatic pressing treatment conditions are that the cold isostatic pressing pressure is 270MPa, and the pressure is maintained for 100s.
The presintering treatment is carried out under the conditions that the presintering temperature is 1100 ℃ and the presintering time is 90min.
The dry pressing die used in the embodiment comprises an isolation diaphragm made of stainless steel and arranged at the short side length inside the dry pressing die, the isolation diaphragm divides the inside of the die into two independent spaces, and the isolation diaphragm is movably connected with the die.
Example 2
The embodiment provides a preparation method of integrated multicolor dental CAD/CAM zirconia, which comprises the following steps:
preparing required colored zirconia powder according to a color formula of B1 color, B2 color, C1 color and C3 color of VITA16 color, placing the colored zirconia powder in a circular dry pressing die, removing the isolating membrane, performing dry pressing treatment, and sequentially performing cold isostatic pressing treatment and presintering treatment to obtain the multicolor dental CAD/CAM zirconia;
the dry pressing treatment conditions are that the dry pressing pressure is 5MPa, and the dry pressing time is 10s.
The cold isostatic pressing treatment conditions are that the cold isostatic pressing pressure is 190MPa, and the pressure is maintained for 120s.
The presintering treatment conditions are that the presintering temperature is 900 ℃ and the presintering time is 120min.
The dry pressing die used in the embodiment comprises four organic glass isolation diaphragms with the radius lengths, which are arranged inside the dry pressing die, wherein the isolation diaphragms divide the inside of the die into four independent spaces, and are movably connected with the die.
Example 3
The embodiment provides a preparation method of integrated multicolor dental CAD/CAM zirconia, which comprises the following steps:
preparing required colored zirconia powder according to a color formula of A1 color of VITA16 color, B2 color of VITA26 color and 2M3 color of VITA26 color, placing the colored zirconia powder in a circular dry pressing die, removing the isolating membrane, performing dry pressing treatment, and sequentially performing cold isostatic pressing treatment and presintering treatment to obtain the dental CAD/CAM zirconia with multicolor bodies;
the dry pressing treatment conditions are that the dry pressing pressure is 6MPa, and the dry pressing time is 20s.
The cold isostatic pressing treatment conditions are that the cold isostatic pressing pressure is 170MPa, and the pressure is maintained for 90s.
The presintering treatment conditions are that the presintering temperature is 980 ℃ and the presintering time is 134min.
The dry pressing die used in the embodiment comprises a polyvinyl chloride isolation diaphragm arranged inside the dry pressing die and having three radii, the isolation diaphragm divides the inside of the die into three independent spaces, and the isolation diaphragm is movably connected with the die.
Example 4
The embodiment provides a preparation method of integrated multicolor dental CAD/CAM zirconia, which comprises the following steps:
preparing required colored zirconia powder according to a 6-layer color gradient color formula of A1 of VITA16 color and 3M2 of VITA26 color, placing the colored zirconia powder in a rectangular dry pressing die, removing the isolating membrane, performing dry pressing treatment, and sequentially performing cold isostatic pressing treatment and presintering treatment to obtain the multi-color dental CAD/CAM zirconia;
the dry pressing treatment conditions are that the dry pressing pressure is 7MPa, and the dry pressing time is 25s.
The cold isostatic pressing treatment conditions are that the cold isostatic pressing pressure is 210MPa, and the pressure is kept for 145s.
The presintering treatment conditions are that the presintering temperature is 1000 ℃ and the presintering time is 156min.
The dry pressing die used in the embodiment comprises an isolation diaphragm which is arranged on the polypropylene with the length of the long edge inside the dry pressing die, the isolation diaphragm divides the inside of the die into two independent spaces, and the isolation diaphragm is movably connected with the die.
The strength of the dental CAD/CAM zirconia prepared in examples 1 to 4 was measured, and the results are shown in table 1.
TABLE 1
| Three point bending strength/MPa | |
| Example 1 | 1000 |
| Example 2 | 1100 |
| Example 3 | 1150 |
| Example 4 | 600-1100 |
The hardness of the dental CAD/CAM zirconia prepared in examples 1 to 4 was measured, and the results are shown in table 2.
TABLE 2
| Vickers hardness/HV 10 | |
| Example 1 | 1415 |
| Example 2 | 1380 |
| Example 3 | 1467 |
| Example 4 | 1435-1496 |
The transmittance of the dental CAD/CAM zirconia prepared in examples 1-4 was measured, and the results are shown in Table 3.
TABLE 3
| Transmittance (a) | |
| Example 1 | 42 |
| Example 2 | 39 |
| Example 3 | 44 |
| Example 4 | 43-57 |
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (8)
1. A method for preparing a multi-color dental CAD/CAM zirconia integrated with a plurality of colors, the method comprising:
placing powder of at least two kinds of colored zirconia into a dry pressing die, wherein the dry pressing die comprises at least one layer of isolation diaphragm arranged inside the dry pressing die, the isolation diaphragm divides the inside of the die into at least two independent spaces, and the isolation diaphragm is movably connected with the die; the dry pressing die comprises a round dry pressing die or a rectangular dry pressing die; the isolation diaphragm is made of any one of stainless steel, polyvinyl chloride, polypropylene or organic glass; the size of the isolation diaphragm is the radius length of the inner cavity of the circular dry pressing die or any side length of the inner cavity of the rectangular dry pressing die;
and removing the isolating membrane, carrying out dry pressing treatment, and sequentially carrying out cold isostatic pressing treatment and presintering treatment to obtain the integrated multicolor CAD/CAM zirconia for dentistry.
2. The method according to claim 1, wherein the pressure of the dry pressing is 3 to 15 MPa.
3. The method of claim 1, wherein the dry pressing is carried out for 5 to 30 seconds.
4. The method according to claim 1, wherein the isostatic cool pressing is carried out at a molding pressure of 80 to 270 MPa.
5. The production method according to claim 1, wherein the cold isostatic pressing treatment is carried out for a dwell time of 60 to 200 s.
6. The method for preparing a polycarbonate resin composition according to claim 1, wherein the temperature of the pre-sintering treatment is 800 to 1100 ℃.
7. The method for preparing a polyurethane foam according to claim 1, wherein the time for the pre-sintering treatment is 90 to 180min.
8. An integrally multicolored dental CAD/CAM zirconia, wherein the dental CAD/CAM zirconia is prepared by the preparation method according to any one of claims 1 to 7.
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| WO2006095254A2 (en) * | 2005-03-09 | 2006-09-14 | Mira Di Algeri Maris | Isostatic pressing means |
| CN105856387A (en) * | 2015-01-19 | 2016-08-17 | 辽宁爱尔创生物材料有限公司 | Manufacturing method for zirconium dioxide ceramic green-pressing |
| CN107175747B (en) * | 2017-05-12 | 2020-04-07 | 爱迪特（秦皇岛）科技股份有限公司 | Dental zirconia repair material with uniform transition of strength and color and preparation method thereof |
| CN111152333A (en) * | 2018-11-08 | 2020-05-15 | 唐安泰 | Cold isostatic pressing method based on rigid mold and application thereof |
| CN110587783A (en) * | 2019-09-11 | 2019-12-20 | 中国科学院上海硅酸盐研究所 | Silicon carbide ceramic upper pressure head of high-temperature bending resistance testing machine and preparation method and die thereof |
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