CN111499378A - Wet forming process of dental zirconia multilayer gradient ceramic block - Google Patents
Wet forming process of dental zirconia multilayer gradient ceramic block Download PDFInfo
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- CN111499378A CN111499378A CN202010178627.1A CN202010178627A CN111499378A CN 111499378 A CN111499378 A CN 111499378A CN 202010178627 A CN202010178627 A CN 202010178627A CN 111499378 A CN111499378 A CN 111499378A
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 164
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000008569 process Effects 0.000 title claims abstract description 21
- 239000000919 ceramic Substances 0.000 title claims abstract description 19
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 18
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 14
- 238000011068 loading method Methods 0.000 claims abstract description 12
- 238000003825 pressing Methods 0.000 claims abstract description 12
- 230000035699 permeability Effects 0.000 claims abstract description 7
- 238000007599 discharging Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000000465 moulding Methods 0.000 claims abstract description 6
- 238000012545 processing Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 5
- 230000008859 change Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 description 12
- 230000008439 repair process Effects 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004088 simulation Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 235000015895 biscuits Nutrition 0.000 description 1
- 230000001055 chewing effect Effects 0.000 description 1
- 238000003759 clinical diagnosis Methods 0.000 description 1
- 239000011351 dental ceramic Substances 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 210000003074 dental pulp Anatomy 0.000 description 1
- 210000004268 dentin Anatomy 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 201000005299 metal allergy Diseases 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
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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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/15—Compositions characterised by their physical properties
-
- 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
-
- 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
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/26—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor
- B28B1/265—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor pressure being applied on the slip in the filled mould or on the moulded article in the mould, e.g. pneumatically, by compressing slip in a closed mould
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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
- B28B17/00—Details of, or accessories for, apparatus for shaping the material; Auxiliary measures taken in connection with such shaping
- B28B17/02—Conditioning the material prior to shaping
- B28B17/026—Conditioning ceramic materials
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Structural Engineering (AREA)
- Veterinary Medicine (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention discloses a wet forming process of a dental zirconia multilayer gradient porcelain block, which comprises the following steps: s1, preparing three kinds of zirconia with different permeabilities, and grinding the zirconia into fine powdery zirconia; s2, mixing the three kinds of powdery zirconium oxide according to different proportions to obtain powdery gradient mixed zirconium oxide with different degrees of transparency; s3, arranging the zirconium oxide according to the sequence of the permeability from low to high and loading the zirconium oxide into a container; s4, vertically placing a container, and loading the container with the solution to mix the discharged mixed zirconia with the solution; s5, fully rotating the mixed zirconia in the container by adopting a rotating stirring roller to fully mix the mixed zirconia at the same height; s6, pressing the mixed zirconia integrally, and discharging the solution; s7, standing and forming the mixed zirconia; s8, sintering the mixed zirconia to obtain a multilayer gradient ceramic block; and S9, processing and molding the porcelain block. The invention greatly improves the warping and deformation of the product in the sintering process when in use and can perfectly show the aesthetic gradual change effect.
Description
Technical Field
The invention relates to the technical field of dental ceramic production, in particular to a wet forming process of a dental zirconia multilayer gradient ceramic block.
Background
When we refer to oral cavity restoration, the Chinese common people will usually think of "porcelain teeth". The traditional porcelain tooth is a porcelain fused full crown which is formed by using specific metal as a substrate, accumulating porcelain powder outside and sintering at high temperature. Because of the metal substrate, the porcelain with larger brittleness originally can bear certain chewing pressure; also, because the substrate is made of metal, the light transmission and natural aesthetic simulation are limited to a certain extent. Meanwhile, the incompatibility of metal and human body in terms of biocompatibility also makes problems of metal allergy, gum black line and the like inevitable. In recent years, the popularization of nuclear magnetic resonance technology in clinical diagnosis also requires that the existence of metal materials in the body of a patient should be avoided, and the biological materials for repairing human tissues in the future are mainly ceramic and high polymer materials. Under the influence of medical demetalization wave, the dental zirconia repair material can quickly replace a metal repair material due to the superior mechanical and aesthetic properties of the dental zirconia repair material, and becomes the largest part of non-metal repair materials, thereby laying the foundation for the comprehensive development of all-ceramic repair technology.
The human tooth comprises a multi-layer structure of dental pulp, dentin, enamel and the like from inside to outside, and the tooth structure is determined to be a gradient structure, which is directly reflected that the tooth appearance is gradually changed from top to bottom in color and transmittance. The existing middle and low-end dental zirconia all-ceramic repair material is a single homogeneous material and cannot well simulate the aesthetic and mechanical effects of gradual change of layers. In addition, the mechanical property and aesthetic light transmittance of the zirconia material are the relationship that fish and bear paw cannot be obtained to a certain extent, and the problem of how to properly combine the mechanical property and the aesthetic property to realize the best simulation effect is also the problem faced by the prior homogeneous zirconia repair material. In order to solve the problems, some denture scientific research institutions and enterprises at home and abroad are beginning to develop gradient gradual change dental zirconia repair materials, and corresponding 3D multilayer gradual change dental zirconia ceramic block products are also produced, so that the materials become the most advanced dental zirconia repair materials at present. However, new use problems occur along with the 3D multi-layer gradient dental zirconia product, for example, the mismatch of shrinkage rates between different materials will cause warpage deformation in the denture manufacturing process, and the natural aesthetic simulation degree is affected by obvious color distinction of the transition interface.
The production process of the dental zirconia ceramic block at present adopts a traditional powder dry pressing forming process without exception, and the multilayer gradient ceramic block adopts a dry pressing forming process after layering and powder spreading. This results in a distinct interface between the layers, which is not conducive to the display of continuous transitional and gradual aesthetic properties, and a sudden change in composition between the layers will also result in a sudden change in shrinkage during the sintering of the ceramic block, thereby causing some degree of warping or deformation of the final restoration.
Disclosure of Invention
In order to overcome the problems, the invention provides a dental zirconia multilayer gradient porcelain block wet forming process.
The technical scheme of the invention provides a dental zirconia multilayer gradient porcelain block wet forming process, which is characterized by comprising the following steps:
s1, preparing three kinds of zirconia with different permeabilities, and grinding the zirconia into fine powdery zirconia;
s2, mixing the three kinds of powdery zirconium oxide according to different proportions to obtain powdery gradient mixed zirconium oxide with different degrees of transparency;
s3, arranging and loading the powdery gradient mixed zirconia into a container according to the sequence of transparency from low to high;
s4, vertically placing a container, and loading the container with the solution to mix the discharged mixed zirconia with the solution;
s5, fully rotating the mixed zirconia in the container by adopting a rotating stirring roller to fully mix the mixed zirconia at the same height;
s6, pressing the mixed zirconia integrally, and discharging the solution;
s7, standing and forming the mixed zirconia;
s8, sintering the mixed zirconia to obtain a multilayer gradient ceramic block;
and S9, processing and molding the porcelain block.
Further, in the step S6, the pressure is 56-66MPa, and the pressure maintaining time is 75-85S.
Further, in the step S8, a drying process is performed first, and then sintering is performed, wherein the drying temperature is 60 to 77 ℃, the drying time is 65 to 75min, the sintering temperature is 1300 to 1400 ℃, and the heat preservation time is 125 to 140 min.
The invention has the beneficial effects that: the wet forming process of the dental zirconia multilayer gradient gradually-changed ceramic block thoroughly abandons the traditional powder dry pressing forming process, adopts the wet forming process, widens the interface between layers due to the mutual diffusion of raw material slurry, forms a slowly and continuously-transitional interface, greatly improves the warping and deformation of the product in the sintering process when in use, and can perfectly show the aesthetic gradually-changed effect; the density distribution unevenness caused by the stress gradient among the powder bodies in the powder body dry pressing forming is avoided, the integral uniformity of the ceramic biscuit is greatly improved compared with the powder body dry pressing forming, the consistency and the reliability of the ceramic block are obviously improved, and the warping and the deformation of the product in the sintering process are greatly improved when the product is used. On the other hand, the interface between layers is widened due to the mutual diffusion of the raw material slurry, a slow continuous transition interface is formed, a clear interface formed by a powder dry pressing process is avoided, and the aesthetic gradual change effect is perfectly displayed.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1:
the invention discloses a wet forming process of a dental zirconia multilayer gradient porcelain block, which is characterized by comprising the following steps of:
s1, preparing three kinds of zirconia with different permeabilities, and grinding the zirconia into fine powdery zirconia;
s2, mixing the three kinds of powdery zirconium oxide according to different proportions to obtain powdery gradient mixed zirconium oxide with different degrees of transparency;
s3, arranging and loading the powdery gradient mixed zirconia into a container according to the sequence of transparency from low to high;
s4, vertically placing a container, and loading the container with the solution to mix the discharged mixed zirconia with the solution;
s5, fully rotating the mixed zirconia in the container by adopting a rotating stirring roller to fully mix the mixed zirconia at the same height;
s6, integrally pressing the mixed zirconia, and discharging the solution, wherein the pressure is 56MPa, and the pressure maintaining time is 85S;
s7, standing and forming the mixed zirconia;
s8, firstly, drying, and then sintering, wherein the drying temperature is 60 ℃, the drying time is 75min, the sintering temperature is 1400 ℃, the heat preservation time is 140min, and the mixed zirconia is sintered to obtain a multilayer gradient ceramic block;
and S9, processing and molding the porcelain block.
Example 2:
the invention discloses a wet forming process of a dental zirconia multilayer gradient porcelain block, which is characterized by comprising the following steps of:
s1, preparing three kinds of zirconia with different permeabilities, and grinding the zirconia into fine powdery zirconia;
s2, mixing the three kinds of powdery zirconium oxide according to different proportions to obtain powdery gradient mixed zirconium oxide with different degrees of transparency;
s3, arranging and loading the powdery gradient mixed zirconia into a container according to the sequence of transparency from low to high;
s4, vertically placing a container, and loading the container with the solution to mix the discharged mixed zirconia with the solution;
s5, fully rotating the mixed zirconia in the container by adopting a rotating stirring roller to fully mix the mixed zirconia at the same height;
s6, integrally pressing the mixed zirconia, and discharging the solution, wherein the pressure is 66MPa, and the pressure maintaining time is 85S;
s7, standing and forming the mixed zirconia;
s8, firstly, drying, and then sintering, wherein the drying temperature is 77 ℃, the drying time is 65min, the sintering temperature is 1300 ℃, the heat preservation time is 125min, and the mixed zirconia is sintered to obtain a multilayer gradient ceramic block;
and S9, processing and molding the porcelain block.
Example 3:
the invention discloses a wet forming process of a dental zirconia multilayer gradient porcelain block, which is characterized by comprising the following steps of:
s1, preparing three kinds of zirconia with different permeabilities, and grinding the zirconia into fine powdery zirconia;
s2, mixing the three kinds of powdery zirconium oxide according to different proportions to obtain powdery gradient mixed zirconium oxide with different degrees of transparency;
s3, arranging and loading the powdery gradient mixed zirconia into a container according to the sequence of transparency from low to high;
s4, vertically placing a container, and loading the container with the solution to mix the discharged mixed zirconia with the solution;
s5, fully rotating the mixed zirconia in the container by adopting a rotating stirring roller to fully mix the mixed zirconia at the same height;
s6, integrally pressing the mixed zirconia, and discharging the solution, wherein the pressure is 61MPa, and the pressure maintaining time is 80S;
s7, standing and forming the mixed zirconia;
s8, firstly, drying, and then sintering, wherein the drying temperature is 71 ℃, the drying time is 70min, the sintering temperature is 1350 ℃, the heat preservation time is 138min, and the mixed zirconia is sintered to obtain a multilayer gradient ceramic block;
and S9, processing and molding the porcelain block.
The above embodiment is only one embodiment of the present invention, and the description thereof is specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (3)
1. A dental zirconia multilayer gradient porcelain block wet forming process is characterized by comprising the following steps:
s1, preparing three kinds of zirconia with different permeabilities, and grinding the zirconia into fine powdery zirconia;
s2, mixing the three kinds of powdery zirconium oxide according to different proportions to obtain powdery gradient mixed zirconium oxide with different degrees of transparency;
s3, arranging and loading the powdery gradient mixed zirconia into a container according to the sequence of transparency from low to high;
s4, vertically placing a container, and loading the container with the solution to mix the discharged mixed zirconia with the solution;
s5, fully rotating the mixed zirconia in the container by adopting a rotating stirring roller to fully mix the mixed zirconia at the same height;
s6, pressing the mixed zirconia integrally, and discharging the solution;
s7, standing and forming the mixed zirconia;
s8, sintering the mixed zirconia to obtain a multilayer gradient ceramic block;
and S9, processing and molding the porcelain block.
2. The dental zirconia multilayer gradient porcelain block wet forming process according to claim 1, which is characterized in that: in the step S6, the pressure is 56-66MPa, and the pressure maintaining time is 75-85S.
3. The dental zirconia multilayer gradient porcelain block wet forming process according to claim 1, which is characterized in that: in the step S8, a drying process is firstly carried out, and then sintering is carried out, wherein the drying temperature is 60-77 ℃, the drying time is 65-75 min, the sintering temperature is 1300-1400 ℃, and the heat preservation time is 125-140 min.
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