阅读说明：本技术 一种义齿贴面的制备方法及由此制备的义齿贴面 (Preparation method of denture overlay and denture overlay prepared by same ) 是由 胡可辉 陆宽 沈震 于 2019-09-17 设计创作，主要内容包括：本公开涉及一种义齿贴面的制备方法及由此制备的义齿贴面。根据本公开的制备方法,可以以简单的方式制备出高精度的义齿贴面,所制备的贴面与患者的牙齿贴合时精度更高。(The present disclosure relates to a method of preparing a denture overlay and a denture overlay prepared thereby. According to the preparation method disclosed by the invention, the high-precision denture veneers can be prepared in a simple manner, and the prepared veneers are higher in precision when being adhered to the teeth of a patient.)

1. A method for preparing a denture overlay, comprising the steps of:

s1: a patient's oral data file is obtained,

s2: generating a generation data file and a veneering data file according to the oral cavity data file,

s3: obtaining a green body of the model and the veneer by using a 3D printer according to the model data file and the veneer data file,

s4: placing the green body of the model and the veneering into a heat preservation box with the temperature of 80-120 ℃ for heat preservation for 0.5-3h,

s5: respectively placing the green bodies of the model and the facing after heat preservation in a furnace at the temperature of 800-1000 ℃ for sintering for 10-100 minutes to respectively obtain the model and the facing of primary sintering,

s6: the veneering of the primary sintering is placed on the primary sintering substitute and secondary sintering is carried out for 5-30 minutes at 900-1000 ℃ to obtain the required veneering of the false tooth.

2. The method of claim 1, wherein

In step S2, the overlay data file is set to: parallel grooves are designed on the side of the veneer, which is attached to the teeth.

3. The method of claim 2, wherein

In step S2, the width between the grooves is 10-100 μm and the depth of the grooves is 1-30 μm.

4. The method of claim 1, wherein

In step S3, the 3D printer used is selected from a photo-curing ceramic 3D printer, an extrusion type ceramic 3D printer, a powder-spread binder-jet ceramic 3D printer, or an ink-jet ceramic 3D printer, and when the green compact is obtained, the 3D printed layer thickness of each layer is not more than 100 μm; the 3D printed layers each have a layer thickness of not more than 50 μm when the veneered green body is obtained.

5. The method of claim 1, wherein

After step S6, the method may further include:

s7: the veneers are dyed once or more times and then sintered for three times at the temperature of 700 ℃ and 900 ℃ for 5 to 10 minutes.

6. The method of claim 1, wherein

In step S3, the 3D printing ceramic paste for making the prototype includes the following components:

10-70 parts of silicon oxide, 10-50 parts of aluminum oxide, 5-15 parts of potassium oxide, 5-15 parts of sodium oxide, 1-10 parts of magnesium oxide, 1-5 parts of yttrium oxide, 5-20 parts of calcium oxide and 10-200 parts of zirconium oxide, wherein the particle diameters of the components are respectively 0.5-100 mu m;

30-90 parts of cross-linking agent, 10-60 parts of solvent, 1-10 parts of dispersant and 0.5-5 parts of catalyst;

the 3D printing ceramic slurry for manufacturing the veneer comprises the following components:

10-70 parts of silicon oxide, 10-50 parts of aluminum oxide, 5-15 parts of potassium oxide, 5-15 parts of sodium oxide, 1-10 parts of magnesium oxide, 1-5 parts of yttrium oxide, 5-20 parts of calcium oxide, 10-200 parts of zirconium oxide and 0.1-10 parts of dyeing auxiliary agent, wherein the particle diameters of the components are 0.5-100 mu m independently;

30-90 parts of cross-linking agent, 10-60 parts of solvent, 1-10 parts of dispersant and 0.5-5 parts of catalyst.

7. The method of claim 6, wherein

In step S3, the 3D printing ceramic paste for making the generational and veneering further comprises, each independently: 0.1 to 50 parts by weight of zirconia having a particle diameter of 1 to 40 nm.

8. The method of claim 6, wherein

In step S3, the paste for making veneering 3D printing ceramic further comprises 0.1-10 parts by weight of an antibacterial material, and the particle size of the antibacterial material is 0.5-10 μm,

wherein the dyeing auxiliary agent is selected from one or more of oxides of Fe, Mn, Zn, Ce, V, In, Er, Dy, Pr, Nd, Sm, Eu and Tb,

the antibacterial material is selected from silver and copper-containing antibacterial material and TiO₂Rare earth elements and one or more of zirconium, manganese, iron, cobalt, nickel, chromium and oxides thereof.

9. The method of claim 6, wherein

The cross-linking agent is one or a mixture of acrylic resin, epoxy resin, polymethyl cellulose sodium, polyvinyl alcohol, silica sol, aluminum sol and acrylamide,

the solvent is one or a mixture of water, ethanol, glycol, polyethylene glycol, glycerol, octanol and glycol,

the dispersant is one or a mixture of more of oleic acid, carboxymethyl cellulose, acetic acid, stearic acid amide and a silicon-oxygen coupling agent,

the catalyst is selected from camphorquinone, 2-hydroxy-2-methyl-1-phenyl acetone, 2,4, 6-trimethyl benzoyl-diphenyl phosphine oxide, 2-dimethylamino-2-benzyl-1- [4- (4-morpholinyl) phenyl ] -1-butanone, 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone, methyl benzoylformate, 1-hydroxycyclohexyl phenyl ketone, benzoin dimethyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzoin butyl ether, diphenyl ethyl ketone, alpha-dimethoxy-alpha-phenyl ethyl ketone, aroyl phosphine oxide, bis-benzoylphenyl phosphine oxide, bis-benzoyl phenyl phosphine oxide, methyl ethyl phenyl ether, methyl ethyl phenyl ketone, methyl phenyl methyl benzoate, 1-hydroxy cyclohexyl phenyl ketone, methyl phenyl, Benzophenone, 2, 4-dihydroxybenzophenone, Michler's ketone, thiopropoxythioxanone, isopropylthioxanthone, 2' -azobis (isobutyronitrile), dilauroyl peroxide, tert-butyl peroxybenzoate, benzoyl peroxide, tert-butyl peroxymaleate, tert-butyl cumyl peroxide, and 1, 1-di-tert-butyl peroxycyclohexane.

10. A denture overlay prepared according to the method of manufacture of any one of claims 1 to 9.

Technical Field

The disclosure relates to a ceramic manufacturing process, in particular to a preparation method of a denture overlay and the denture overlay prepared by the same.

Background

With the improvement of living standard, people pay more attention to the health of teeth. In addition to health problems associated with missing teeth, cosmetic care of teeth is also a growing concern. In particular, people who suffer from problems of discoloration of the teeth, such as tetracycline pigmentation teeth, dental fluorosis, etc., also pay more attention to the aesthetic appearance of the teeth.

The false tooth facing is a new tooth beautifying technology, and has excellent beautifying effect on surface defect, stained tooth, discolored tooth, deformed tooth, etc. It can be directly or indirectly covered with repairing material under the condition of preserving living marrow, little or no bruxism, so as to restore normal form of tooth body and improve its colour and lustre.

The existing denture veneering technology comprises a ceramic casting method, a cutting method, a ceramic stacking method, a 3D printing method and the like. However, the preparation methods of the denture overlay in the prior art all have some problems. Wherein, the veneering made by the ceramic casting method is thick and large, the consistency is poor, the period is long, and the product experience is poor. The cutting method is easy to break porcelain and has large material and cutter loss. The manual ceramic stacking period is long, the efficiency is low, the consistency is poor, and the yield is low. The patch of the 3D printing method is made of materials and processes, and the prepared patch cannot have both simulation performance, strength and precision.

Disclosure of Invention

In order to solve the problems of the denture overlay of the prior art, the inventors of the present disclosure propose a new denture overlay manufacturing method and a denture overlay manufactured thereby.

It is an object of the present disclosure to provide a method of preparing a denture overlay.

It is another object of the present disclosure to provide a denture overlay.

According to one embodiment of the present disclosure, there is provided a method of preparing a denture overlay, the method comprising the steps of:

s1: a patient's oral data file is obtained,

s2: generating a generation data file and a veneering data file according to the oral cavity data file,

s3: obtaining a green body of the model and the veneer by using a 3D printer according to the model data file and the veneer data file,

s4: placing the green body of the model and the veneering into a heat preservation box with the temperature of 80-120 ℃ for heat preservation for 0.5-3h,

s5: respectively placing the green bodies of the model and the facing after heat preservation in a furnace at the temperature of 800-1000 ℃ for sintering for 10-100 minutes to respectively obtain the model and the facing of primary sintering,

s6: the veneering of the primary sintering is placed on the primary sintering substitute and secondary sintering is carried out for 5-30 minutes at 900-1000 ℃ to obtain the required veneering of the false tooth.

According to another embodiment of the present disclosure, there is provided a denture overlay prepared according to the method of preparation.

According to the preparation method disclosed by the invention, the high-precision denture veneers can be prepared in a simple manner, and the prepared veneers are higher in precision when being adhered to the teeth of a patient.

Drawings

Fig. 1 is a flow diagram of a method of making according to one embodiment of the present disclosure.

Fig. 2 is a schematic representation of a denture overlay made according to the present disclosure positioned over a replica.

Fig. 3 is an overall schematic view of multiple generations and veneers made according to the present disclosure.

FIG. 4 is a three-dimensional model of a veneer according to the present disclosure.

FIG. 5 is a three-dimensional model of a generation according to the present disclosure.

FIG. 6 is a photomicrograph of the surface of the bonding side of the veneer according to the present disclosure.

Detailed Description

To make the features and effects of the present invention comprehensible to those having ordinary knowledge in the art, general description and definitions are made with respect to terms and phrases mentioned in the specification and claims. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.

In this document, the terms "comprising," "including," "having," "containing," or any other similar term, are intended to be open-ended franslational phrase (open-ended franslational phrase) and are intended to cover non-exclusive inclusions. For example, a composition or article comprising a plurality of elements is not limited to only those elements recited herein, but may include other elements not expressly listed but generally inherent to such composition or article. In addition, unless expressly stated to the contrary, the term "or" is intended to mean an inclusive "or" rather than an exclusive "or". For example, the condition "a or B" is satisfied in any of the following cases: a is true (or present) and B is false (or not present), a is false (or not present) and B is true (or present), both a and B are true (or present). Furthermore, in this document, the terms "comprising," including, "" having, "" containing, "and" containing "are to be construed as specifically disclosed and to cover both closed and semi-closed conjunctions, such as" consisting of … "and" consisting essentially of ….

All features or conditions defined herein as numerical ranges or percentage ranges are for brevity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to have covered and specifically disclosed all possible subranges and individual numerical values within the ranges, particularly integer numerical values. For example, a description of a range of "1 to 8" should be considered to have specifically disclosed all subranges such as 1 to 7, 2 to 8, 2 to 6, 3 to 6, 4 to 8, 3 to 8, and so on, particularly subranges bounded by all integer values, and should be considered to have specifically disclosed individual values such as 1, 2, 3, 4, 5, 6, 7, 8, and so on, within the range. Unless otherwise indicated, the foregoing explanatory methods apply to all matters contained in the entire disclosure, whether broad or not.

If an amount or other value or parameter is expressed as a range, preferred range, or a list of upper and lower limits, it is to be understood that all ranges subsumed therein for any pair of that range's upper or preferred value and that range's lower or preferred value, whether or not such ranges are separately disclosed, are specifically disclosed herein. Further, when a range of numerical values is recited herein, unless otherwise stated, the range is intended to include the endpoints thereof, and all integers and fractions within the range.

In this context, numerical values should be understood to have the precision of the number of significant digits of the value, provided that the object of the invention is achieved. For example, the number 40.0 should be understood to cover a range from 39.50 to 40.49.

In this document, where Markush group (Markush group) or Option language is used to describe features or examples of the invention, those skilled in the art will recognize that a sub-group of all elements or any individual element within a Markush group or list of options may also be used to describe the invention. For example, if X is described as "selected from the group consisting of₁、X₂And X₃The group "also indicates that X has been fully described as X₁Is claimed with X₁And/or X₂Claim (5). Furthermore, where Markush group or option terms are used to describe features or examples of the invention, those skilled in the art will recognize that any combination of sub-groups of all elements or individual elements within the Markush group or option list can also be used to describe the invention. Accordingly, for example, if X is described as "selected from the group consisting of₁、X₂And X₃Group consisting of "and Y is described as" selected from Y₁、Y₂And Y₃The group "formed indicates that X has been fully described as X₁Or X₂Or X₃And Y is Y₁Or Y₂Or Y₃Claim (5).

The following detailed description is merely exemplary in nature and is not intended to limit the invention or the application thereof. Furthermore, there is no intention to be bound by any theory presented in the preceding prior art or the summary of the invention or the following detailed description or examples.

According to one embodiment of the present disclosure, as shown in fig. 1, there is provided a method of preparing a denture overlay comprising the steps of:

s1: a patient's oral data file is obtained,

s2: generating a generation data file and a veneering data file according to the oral cavity data file,

s3: obtaining a green body of the model and the veneer by using a 3D printer according to the model data file and the veneer data file,

s4: placing the green body of the model and the veneering into a heat preservation box with the temperature of 80-120 ℃ for heat preservation for 0.5-3h,

s5: respectively placing the green bodies of the model and the facing after heat preservation in a furnace at the temperature of 800-1000 ℃ for sintering for 10-100 minutes to respectively obtain the model and the facing of primary sintering,

s6: the veneering of the primary sintering is placed on the primary sintering substitute and secondary sintering is carried out for 5-30 minutes at 900-1000 ℃ to obtain the required veneering of the false tooth.

According to the method, the high-precision denture veneers can be prepared in a simple mode, and the prepared veneers are higher in precision when being adhered to the teeth of a patient. The method has the advantages that the secondary sintering is carried out on the substitute mold, so that the substitute mold plays a supporting role during the secondary sintering, and the finally prepared denture veneering and designing precision is higher.

According to an embodiment of the present disclosure, in step S1, obtaining the oral cavity data file of the patient may be performed by: including but not limited to oral cavity internal scanning, oral cavity plaster model scanning, three-dimensional software direct modeling, and scanning the silica gel membrane after the silica gel is turned over.

According to an embodiment of the present disclosure, in step S2, the overlay data file is set to: parallel grooves are designed on the side of the veneer, which is attached to the teeth.

According to this method, the adhesive force at the time of the denture attachment can be increased.

According to one embodiment of the present disclosure, in step S2, the width between grooves is 10 to 100 μm and the depth of the grooves is 1 to 30 μm.

At such a specific width and depth, the fitting and separation between the replica and the facing after the secondary sintering can be made smoother.

According to an embodiment of the present disclosure, in step S3, the 3D printer used is selected from a photo-curing ceramic 3D printer, an extrusion type ceramic 3D printer, a powder-spread binder-jetting ceramic 3D printer, or an ink-jetting ceramic 3D printer, and when the green compact is obtained, the 3D printed layer thickness of each layer is not more than 100 μm; the 3D printed layers each have a layer thickness of not more than 50 μm when the veneered green body is obtained.

With such an arrangement, a suitable green body for the prototype and the facing can be obtained better, and the accuracy of the facing after sintering can be improved.

According to an embodiment of the present disclosure, the preparation method may further include, after step S6:

s7: the veneers are dyed once or more times and then sintered for three times at the temperature of 700 ℃ and 900 ℃ for 5 to 10 minutes.

According to the steps, the veneers with more beautiful appearances can be obtained, and after two times of sintering, the veneers can not deform when being sintered for three times.

According to one embodiment of the present disclosure, in step S3, the 3D printing ceramic paste for making the prototype includes the following components:

10-70 parts of silicon oxide, 10-50 parts of aluminum oxide, 5-15 parts of potassium oxide, 5-15 parts of sodium oxide, 1-10 parts of magnesium oxide, 1-5 parts of yttrium oxide, 5-20 parts of calcium oxide and 10-200 parts of zirconium oxide, wherein the particle diameters of the components are respectively 0.5-100 mu m;

30-90 parts of cross-linking agent, 10-60 parts of solvent, 1-10 parts of dispersant and 0.5-5 parts of catalyst;

the 3D printing ceramic slurry for manufacturing the veneer comprises the following components:

10-70 parts of silicon oxide, 10-50 parts of aluminum oxide, 5-15 parts of potassium oxide, 5-15 parts of sodium oxide, 1-10 parts of magnesium oxide, 1-5 parts of yttrium oxide, 5-20 parts of calcium oxide, 10-200 parts of zirconium oxide and 0.1-10 parts of dyeing auxiliary agent, wherein the particle diameters of the components are 0.5-100 mu m independently;

30-90 parts of cross-linking agent, 10-60 parts of solvent, 1-10 parts of dispersant and 0.5-5 parts of catalyst.

In the case of using the 3D printing ceramic slurry of such components, particularly, since a specific combination of components is selected, the volume shrinkage rate of the ceramic after sintering can be better controlled, thereby improving the accuracy in the application of the veneer to a tooth.

According to an embodiment of the present disclosure, in step S3, the 3D printing ceramic paste for making the generative and veneering further comprises, each independently: 0.1-50 parts by weight of zirconia having a particle size of 1-40 nm;

the nano-grade (1-40nm particle size) zirconia can better adjust the volume shrinkage of the sintered ceramic, thereby improving the precision of the veneering and the tooth fitting of the application.

According to one embodiment of the present disclosure, the 3D printing ceramic paste for fabricating a veneer further includes 0.1 to 10 parts by weight of an antibacterial material, and the particle size of the antibacterial material is 0.5 to 10 μm at step S3,

wherein the dyeing auxiliary agent is selected from one or more of oxides of Fe, Mn, Zn, Ce, V, In, Er, Dy, Pr, Nd, Sm, Eu and Tb,

the antibacterial material is selected from silver and copper-containing antibacterial material and TiO₂Rare earth elements and one or more of zirconium, manganese, iron, cobalt, nickel, chromium and oxides thereof.

The antibacterial material containing silver and copper is an antibacterial material known in the art, such as an inorganic or organic antibacterial material containing silver ions, copper ions, such as silver sulfate, silver nitrate, copper sulfate, etc.

The antibacterial material has low grain diameter (0.5-10 μm), and can also adjust the volume shrinkage of the sintered ceramic to a certain extent, thereby improving the precision of the veneering and the tooth veneering of the application,

further, the inventors have also found that when the above-described 3D printing ceramic paste for making the replica and the 3D printing ceramic paste for making the facing are used, it is possible to prevent the replica and the facing from being sintered together at the time of secondary sintering,

when the 3D printing ceramic paste for making the veneer includes the above components and satisfies the above particle size, it can be more advantageously dyed and sintered multiple times.

According to one embodiment of the present disclosure, wherein,

the cross-linking agent is one or a mixture of acrylic resin, epoxy resin, polymethyl cellulose, silica sol, aluminum sol and acrylamide,

the solvent is one or a mixture of water, ethanol, glycol, polyethylene glycol, glycerol, octanol and glycol,

the dispersant is one or a mixture of more of oleic acid, carboxymethyl cellulose, acetic acid, stearic acid amide and a silicon-oxygen coupling agent,

the catalyst is selected from camphorquinone, 2-hydroxy-2-methyl-1-phenyl acetone, 2,4, 6-trimethyl benzoyl-diphenyl phosphine oxide, 2-dimethylamino-2-benzyl-1- [4- (4-morpholinyl) phenyl ] -1-butanone, 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone, methyl benzoylformate, 1-hydroxycyclohexyl phenyl ketone, benzoin dimethyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzoin butyl ether, diphenyl ethyl ketone, alpha-dimethoxy-alpha-phenyl ethyl ketone, aroyl phosphine oxide, bis-benzoylphenyl phosphine oxide, bis-benzoyl phenyl phosphine oxide, methyl ethyl phenyl ether, methyl ethyl phenyl ketone, methyl phenyl methyl benzoate, 1-hydroxy cyclohexyl phenyl ketone, methyl phenyl, Benzophenone, 2, 4-dihydroxybenzophenone, Michler's ketone, thiopropoxythioxanone, isopropylthioxanthone, 2' -azobis (isobutyronitrile), dilauroyl peroxide, tert-butyl peroxybenzoate, benzoyl peroxide, tert-butyl peroxymaleate, tert-butyl cumyl peroxide, and 1, 1-di-tert-butyl peroxycyclohexane.

The substitute and veneer prepared by using the specific components can better realize the technical effects of the disclosure: namely, the facing material has high precision, simple and convenient processing and beautiful appearance.

According to another embodiment of the present disclosure, as shown in fig. 2, there is provided a denture overlay prepared according to the preparation method. Wherein, fig. 2 is a schematic view of the denture overlay positioned on the replica.

Examples

Example 1: preparation of moulding pulp and facing pulp

Preparing mixed porcelain powder A: mixing 70g of silicon oxide with the particle size of 10 mu m, 10g of aluminum oxide, 5g of potassium oxide, 5g of sodium oxide, 1g of magnesium oxide, 1g of yttrium oxide, 5g of calcium oxide and 10g of zirconium oxide by a ball mill for 2 hours;

preparing mixed porcelain powder B: 70g of silicon oxide with a particle size of 10 μm, 10g of aluminum oxide, 5g of potassium oxide, 5g of sodium oxide, 1g of magnesium oxide, 1g of yttrium oxide, 5g of calcium oxide, 10g of zirconium oxide, 1g of iron oxide, TiO₂2g, mixing for 2 hours by using a ball mill;

preparing a ready-mixed solution: mixing 50g of cross-linking agent acrylic resin, 40g of solvent ethylene glycol, 8g of dispersant oleic acid and 2g of catalyst 2-hydroxy-2-methyl-1-phenyl acetone, and stirring at room temperature overnight;

mixing 250g of mixed porcelain powder A and 100g of premixed solution, placing the mixture in a ball mill for ball milling for 3h, standing the mixture for 24h, and then defoaming the mixture for 20min in vacuum by using a defoaming machine to obtain uniformly and stably dispersed slurry for preparing a prototype.

And mixing 250g of the mixed porcelain powder B with 100g of the pre-mixed liquid, placing the mixture in a ball mill for ball milling for 3h, standing the mixture for 24h, and then defoaming the mixture for 20min in vacuum by using a defoaming machine to obtain uniformly and stably dispersed slurry for preparing veneers.

Example 2

Preparing mixed porcelain powder A: mixing 50g of silicon oxide with particle size of 2 μm, 40g of aluminum oxide, 10g of potassium oxide, 5g of sodium oxide, 1g of magnesium oxide, 1g of yttrium oxide, 5g of calcium oxide, 50g of zirconium oxide, and 5g of zirconium oxide with particle size of 20nm by ball mill for 1.5 h;

preparing mixed porcelain powder B: 50g of silicon oxide with a particle size of 2 μm, 40g of aluminum oxide, 10g of potassium oxide, 5g of sodium oxide, 1g of magnesium oxide, 1g of yttrium oxide, 5g of calcium oxide, 50g of zirconium oxide, 1g of iron oxide, TiO₂2g of zirconia with the particle size of 20nm is mixed for 1.5h by a ball mill;

preparing a ready-mixed solution: mixing 60g of a cross-linking agent silica sol, 30g of solvent octanol, 5g of dispersant carboxymethyl cellulose and 5g of catalyst dilauroyl peroxide, and stirring at room temperature overnight;

mixing 250g of mixed porcelain powder A and 100g of premixed solution, placing the mixture in a ball mill for ball milling for 3h, standing the mixture for 24h, and then defoaming the mixture for 15min in vacuum by using a defoaming machine to obtain uniformly and stably dispersed slurry for preparing a prototype.

And mixing 250g of the mixed porcelain powder B with 100g of the pre-mixed liquid, placing the mixture in a ball mill for ball milling for 3h, standing the mixture for 24h, and then defoaming the mixture for 15min in vacuum by using a defoaming machine to obtain uniformly and stably dispersed slurry for preparing veneers.

Example 3

Preparing mixed porcelain powder A: mixing 50g of silicon oxide with particle size of 2 μm, 40g of aluminum oxide, 10g of potassium oxide, 5g of sodium oxide, 5g of magnesium oxide, 3g of yttrium oxide, 5g of calcium oxide, 100g of zirconium oxide, and 10g of zirconium oxide with particle size of 40nm by ball mill for 2 h;

preparing mixed porcelain powder B: 50g of silicon oxide with a particle size of 2 μm, 40g of aluminum oxide, 10g of potassium oxide, 5g of sodium oxide, 5g of magnesium oxide, 3g of yttrium oxide, 5g of calcium oxide, 100g of zirconium oxide, 1g of iron oxide, TiO₂2g of zirconia with the particle size of 40nm and 10g of zirconia are mixed for 2 hours by a ball mill;

preparing a ready-mixed solution: 75g of cross-linking agent, polymethyl cellulose, 15g of solvent water, 6g of dispersant acetic acid and 4g of catalyst, 2' -azobis (isobutyronitrile), were mixed and stirred at room temperature overnight;

and mixing 230g of the mixed porcelain powder A and 100g of the pre-mixed liquid, placing the mixture in a ball mill for ball milling for 3h, standing the mixture for 24h, and then defoaming the mixture for 15min in vacuum by using a defoaming machine to obtain uniformly and stably dispersed slurry for preparing the model-replacing paste.

And mixing 230g of the mixed porcelain powder B with 100g of the pre-mixed liquid, placing the mixture in a ball mill for ball milling for 3h, standing the mixture for 24h, and then defoaming the mixture for 15min in vacuum by using a defoaming machine to obtain uniformly and stably dispersed slurry for preparing the veneering.

Example 4

Preparing mixed porcelain powder A: mixing 10g of silicon oxide with a particle size of 0.5 μm, 10g of aluminum oxide, 15g of potassium oxide, 15g of sodium oxide, 10g of magnesium oxide, 5g of yttrium oxide, 10g of calcium oxide, 200g of zirconium oxide and 50g of zirconium oxide with a particle size of 30nm by a ball mill for 2 h;

preparing mixed porcelain powder B: mixing 10g of silicon oxide with a particle size of 0.5 μm, 10g of aluminum oxide, 15g of potassium oxide, 15g of sodium oxide, 10g of magnesium oxide, 5g of yttrium oxide, 10g of calcium oxide, 200g of zirconium oxide, 1g of manganese oxide, 2g of silver sulfate and 50g of zirconium oxide with a particle size of 30nm by using a ball mill for 2 hours;

preparing a ready-mixed solution: mixing 80g of cross-linking agent polymethyl cellulose, 10g of solvent water, 9g of dispersing agent acetic acid and 1g of catalyst camphorquinone, and stirring at room temperature overnight;

and mixing 200g of mixed porcelain powder A and 100g of pre-mixed liquid, placing the mixture in a ball mill for ball milling for 3h, standing the mixture for 24h, and then defoaming the mixture for 15min in vacuum by using a defoaming machine to obtain uniformly and stably dispersed slurry for preparing a prototype.

And mixing 200g of the mixed porcelain powder B and 100g of the pre-mixed liquid, placing the mixture in a ball mill for ball milling for 3h, standing the mixture for 24h, and then defoaming the mixture for 15min in vacuum by using a defoaming machine to obtain uniformly and stably dispersed slurry for preparing veneers.

Example 5: preparation of substitute and veneer

The method comprises the steps of carrying out oral cavity scanning through a three-dimensional scanner instrument to obtain a patient oral cavity data file, generating a generation data file consistent with a tooth model of a patient through the oral cavity data file, designing a veneer according to the generation data file, wherein the inner side of the veneer is completely attached to the outer surface of a tooth to be repaired, the thickness of the veneer is 0.2mm, and patterns are designed on the inner side of the veneer and the tooth attachment surface to increase the adhesive force after the veneer is attached. Wherein the pattern structure on the inner side of the veneer is designed into parallel transverse stripes, the width of the transverse stripes is 25 μm, and the groove depth of the transverse stripes is 30 μm.

FIG. 5 is a three-dimensional model of the generational model generated after scanning.

FIG. 4 is a three-dimensional model of a veneer according to a prototype design.

The slurry for prototyping/surfacing prepared in example 1 was then used, using an AutoCera-M model 3D printer, Ten-dimensional technologies, Inc. of Beijing, at a slice thickness of 25 μ M, 30mW/cm²And respectively preparing a prototype green body and a veneered green body under the parameters of exposure power and single-layer curing time of 10 s. And then, cleaning the printed veneers and residual slurry on the surfaces of the substituted green bodies, placing the veneers and the substituted green bodies into an ultraviolet lamp box for sterilization, and then placing the veneers and the substituted green bodies into a 100-DEG C heat preservation box for heat preservation for 1 hour.

Then, respectively putting the green bodies subjected to heat preservation into a porcelain oven for primary sintering, and taking out the green bodies; wherein the primary sintering temperature is 800 ℃, and the sintering time is 60 min.

And then placing the veneers obtained after the primary sintering on the mould substitutes after the primary sintering, and carrying out secondary sintering for 5min at the temperature of 1000 ℃.

And polishing after secondary sintering to obtain the denture veneer prepared by the invention.

FIG. 3 is a schematic overall view of the prepared multi-particle model and the veneers.

Examples 6 to 8

A denture overlay was prepared in the same manner as in example 5, except that the paste for the model/overlay prepared in examples 2 to 4 was used, and a high-precision extrusion type 3D printer of the shin source gagagagao was used instead of the auto cera-M model 3D printer of beijing ten-dimensional science and technology ltd (which is a photo-curing type 3D printer), and the inner pattern structure of the overlay was designed as parallel cross-stripes having a width of 100 μ M and a groove depth of 10 μ M.

Fig. 6 is a photomicrograph of the surface of the adhesive side of the facing.

Comparative example 1

A denture overlay was prepared in the same manner as in example 5, except that the secondary sintering step was not performed, and direct polishing was performed.

Comparative example 2

Except that the sintering step (including primary sintering and secondary sintering) was modified to: the denture overlay was prepared in the same manner as in example 5, except that the overlaid green body after heat preservation was directly placed on the green substitute body and sintered at a temperature of 1000 c for 30 minutes (and then further polished).

Comparative example 3

A denture overlay was prepared in the same manner as in example 5, except that the inner pattern structure of the overlay was designed as parallel cross-hatching with a width of 50 μm and a groove depth of 50 μm.

Comparative example 4:

a substitute/veneer paste was prepared in the same manner as in example 1, except that 10g of zirconia having a particle size of 10 μm was not added at the time of preparing mixed porcelain powders A and B, and 50g of carboxymethyl cellulose was used instead of 50g of acrylic resin at the time of preparing a pre-mix, and then a denture veneer was prepared in the same manner as in examples 6 to 8 using this paste instead of the paste of example 1.

Comparative example 5:

a dummy overlay was prepared in the same manner as in example 1, except that potassium oxide was not added at the time of preparing mixed porcelain powders a and B, and 50g of polyvinyl alcohol was used instead of 50g of acrylic resin at the time of preparing a pre-mix, and then a denture overlay was prepared in the same manner as in examples 6 to 8 using the paste instead of the paste of example 1.

Comparative example 6:

a substitute/veneer paste was prepared in the same manner as in example 1, except that no sodium oxide was added at the time of preparing mixed porcelain powders a and B, and then a denture veneer was prepared in the same manner as in example 5, using this paste instead of the paste of example 1.

Comparative example 7:

a dummy/veneer paste was prepared in the same manner as in example 1, except that 5g of ethylene glycol solvent was added to the preparation pre-mix solution instead of 40g of ethylene glycol solvent, and then a denture veneer was prepared in the same manner as in example 5 using the paste instead of the paste of example 1.

Experimental example 1: overlay structure defect testing

The veneers prepared in examples 5-8 and comparative examples 1-7 were scanned using an ultrasonic flaw detector and the results are shown in Table 1. The test was used to evaluate the strength of the overlay. The evaluation criteria were:

and (3) excellent: crack defect less than 1

Medium: crack defect of 1-2

Difference: crack defect is more than 3

Experimental example 2: overlay accuracy test

The veneers prepared in examples 5-8 and comparative examples 1-7 were subjected to 3D data scanning using a three dimensional scanning instrument and the results were compared to the data for the original veneer design and are listed in table 1. The accuracy of the facing was evaluated using this test. The evaluation criteria were:

and (3) excellent: the size difference is less than 20 mu m

Medium: the size difference was 50 μm

Difference: the size difference is more than 50 mu m

Experimental example 3: test of surface Release

The veneers prepared in examples 5-8 and comparative examples 2-7 were removed from the mold insert by conventional methods to test their mold release properties. This test was used to evaluate the releasability of the facing, i.e., whether the facing was easily removed from the alternative after sintering. The results are shown in Table 1. The evaluation criteria were:

and (3) excellent: the veneers can be easily taken down by hands

Medium: the adhesive surface can be removed with tweezers without causing visible damage to the outer side and the adhesive side of the adhesive surface

Difference: after removal, there was visible damage to the appearance side or the adhesive side of the overlay, or the overlay could not be removed.

Experimental example 4: test for adhesion of veneers

The veneer was bonded to a model using a dental light-curable adhesive, and then the adhesiveness was examined using a peel test method. This test was used to evaluate the effect of the overlay structure on the adhesion of the overlay. That is, how well the veneer adheres to the patient's teeth when removed from the model. Here, the patient's teeth are replaced with a substitute type. The results are shown in Table 1. The evaluation criteria were:

and (3) excellent: peel strength greater than 50N/cm, or failure to peel (i.e., damaged prior to peeling)

Medium: the peel strength is more than 40N/cm and less than or equal to 50N/cm

Difference: the peeling force is less than 40N/cm

Experimental example 5: overlay appearance and dyeability testing

The veneers prepared in examples 5 to 8 and comparative examples 1 to 7 were subjected to transmittance test using a BNOT transmittance tester of the tenzhen nikko optical precision technology ltd to characterize the appearance and dyeing properties thereof by the method described in the specification, and the results are shown in table 1. The appearance of the veneer was evaluated using this test. The evaluation criteria were:

and (3) excellent: the transmittance is 30-60%;

medium: less than 30%;

difference: greater than 60%.

TABLE 1

	Structure of the product	Accuracy of measurement	Releasability from mold	Adhesion Property	Appearance and dyeability
						Example 5	Superior food	Superior food	Superior food	Superior food	Superior food
Example 6	Superior food	Superior food	Superior food	Superior food	Superior food
						Example 7	Superior food	Superior food	Superior food	Superior food	Superior food
Example 8	Superior food	Superior food	Superior food	Superior food	Superior food
						Comparative example 1	Medium and high grade	Difference (D)	-	Difference (D)	Superior food
Comparative example 2	Superior food	Superior food	Difference (D)	Superior food	Superior food
						Comparative example 3	Superior food	Superior food	Medium and high grade	Difference (D)	Superior food
Comparative example 4	Difference (D)	Superior food	Difference (D)	Superior food	Superior food
						Comparative example 5	Superior food	Superior food	Superior food	Superior food	Difference (D)
Comparative example 6	Difference (D)	Superior food	Superior food	Superior food	Difference (D)
						Comparative example 7	Difference (D)	Superior food	Superior food	Superior food	Superior food

As can be seen from table 1 above, denture overlays can be prepared with high precision and without internal defects according to embodiments of the present disclosure.

In comparative example 1 in which the secondary sintering was not performed, the denture overlay had poor accuracy and severe deformation, and was difficult to use as an overlay product even after the subsequent processing, and the mechanical strength of the overlay was slightly poor.

In comparative example 2 in which the primary sintering was not performed, the parting and the facing sintering could not be separated, and the product could not be used.

In comparative example 3, the releasability of the facing was slightly poor after the secondary sintering, and the adhesion was poor.

In comparative example 4, the finished veneer had poor strength and also had poor mold release properties.

In comparative example 5, the finished overlay had poor transparency, resulting in an unacceptable appearance.

In comparative example 6, the coating had many pores in the interior and the coating had poor coloring properties.

In comparative example 7, the coating had many cracks.

The above embodiments are merely exemplary in nature and are not intended to limit the claimed embodiments or the application or uses of such embodiments. In this document, the term "exemplary" represents "as an example, instance, or illustration. Any exemplary embodiment herein is not necessarily to be construed as preferred or advantageous over other embodiments.

In addition, while at least one exemplary embodiment or comparative example has been presented in the foregoing detailed description, it should be appreciated that a vast number of variations are possible. It should also be appreciated that the embodiments described herein are not intended to limit the scope, applicability, or configuration of the claimed subject matter in any way. Rather, the foregoing implementations will provide those of ordinary skill in the art with a convenient road map for implementing the described embodiment or embodiments. Further, various changes may be made in the function and arrangement of elements without departing from the scope defined in the claims, which includes known equivalents and all foreseeable equivalents at the time of filing this patent application.