CN112426367A - Markable luminous repair material for dentistry and preparation method thereof, adhesive and preparation method thereof, and repair structure - Google Patents
Markable luminous repair material for dentistry and preparation method thereof, adhesive and preparation method thereof, and repair structure Download PDFInfo
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- CN112426367A CN112426367A CN202011453318.7A CN202011453318A CN112426367A CN 112426367 A CN112426367 A CN 112426367A CN 202011453318 A CN202011453318 A CN 202011453318A CN 112426367 A CN112426367 A CN 112426367A
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Images
Classifications
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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
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/884—Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins
- A61K6/887—Compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- A61K6/30—Compositions for temporarily or permanently fixing teeth or palates, e.g. primers for dental adhesives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/70—Preparations for dentistry comprising inorganic additives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/70—Preparations for dentistry comprising inorganic additives
- A61K6/71—Fillers
- A61K6/77—Glass
-
- 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
-
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
- A61K6/833—Glass-ceramic composites
Landscapes
- Health & Medical Sciences (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Plastic & Reconstructive Surgery (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Dental Preparations (AREA)
Abstract
The invention discloses a markable luminous repair material for dentistry and a preparation method thereof, a binder and a preparation method thereof, and a repair structure. The prosthesis prepared by the material has no obvious difference with the conventional false tooth in the daily chewing use process, but under the irradiation of ultraviolet light, the prosthesis can emit obvious fluorescence which is obviously contrasted with the natural tooth. When the prosthesis is damaged or needs to be repaired again due to other reasons, the repairing material can be clearly seen through the irradiation of ultraviolet light, so that the repairing material can be conveniently removed, and the aims of protecting natural teeth and reducing the damage to natural teeth are fulfilled on the premise of completely removing the prosthesis.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the technical field of dental restoration, and particularly relates to a markable luminous restoration material for dentistry, a preparation method of the markable luminous restoration material, a binder, a preparation method of the binder and a restoration structure.
[ background of the invention ]
In the oral cavity service process, the teeth can be damaged or lost to different degrees due to long-time chewing abrasion and oral diseases. The main treatment mode for tooth defect or loss in stomatology is to use dental prosthesis material to repair the defect tooth or lost tooth under the action of binder to restore normal tooth shape and function. In the case that the restored tooth is damaged again due to various reasons during use, a doctor needs to remove the prosthesis and the adhesive completely by the dental drill before restoring the tooth. Clinically, the damage to healthy natural teeth is required to be reduced as much as possible in the tooth restoration process, but because the color of the prosthesis and the color of the adhesive are very similar to that of the natural teeth, how to completely remove the prosthesis and the adhesive in the oral environment without excessively damaging the natural teeth becomes an important problem troubling dentists, and a proper solution is not provided at present.
[ summary of the invention ]
The invention aims to overcome the defects of the prior art and provide a markable luminous restoration material for dentistry, a preparation method, an adhesive, a preparation method and a restoration structure so as to solve the problem that the restoration material, the adhesive and natural teeth are difficult to distinguish in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the markable luminescent repair material for dentistry is prepared by vacuum die pressing of a ceramic material and a first activated luminescent powder material, wherein the mass fraction of the first activated luminescent powder material is 2-30%, and the balance is the ceramic material.
The invention is further improved in that:
preferably, the ceramic material is at least one of alumina ceramic, zirconia ceramic, feldspar ceramic or lithium disilicate glass ceramic; the first activated luminescent powder material is a photoluminescence series short-afterglow ultraviolet excited inorganic material.
Preferably, the grain diameter D50 of the ceramic material is less than or equal to 30 μm, and the grain diameter D50 of the first activated luminescent powder material is less than 1 μm.
The preparation method of the markable luminous restoration material for dentistry comprises the steps of carrying out spherical granulation and homogenization treatment on a ceramic material and a first activated luminous powder material to obtain spherical particles, and carrying out vacuum hot-press molding on the spherical particles to obtain a restoration.
Preferably, the vacuum hot-pressing temperature of the spherical particles is 800-1400 ℃, the pressure is 20-30MPa, and the vacuum degree is more than 0.1 MPa.
A markable luminescent binder for dental use, the binder consisting of a resin matrix, a reinforcing filler, a second activated luminescent powder material, tartaric acid and water; the second activated luminescent powder material emits light under ultraviolet irradiation.
Preferably, in the binder, the mass fraction of the resin matrix is 30-60%, the mass fraction of the reinforcing filler is 10-40%, the mass fraction of the second activated luminescent powder (organic) material is 1-10%, the mass fraction of tartaric acid is 5-10%, and the mass fraction of water is 30-50%.
Preferably, the resin matrix is polyacrylic acid or a copolymer of acrylic acid and itaconic acid and maleic acid; glycidyl methacrylate or hydroxyethyl methacrylate is added into the copolymer; the reinforcing filler is glass powder; the second active luminescent material is a photoluminescence series short-afterglow ultraviolet excited high polymer material.
The preparation method of the markable luminous binder for dentistry comprises the steps of mixing selected glass powder materials in proportion, carrying out ball milling, melting the obtained mixture, quenching the mixture into a glass block by water, carrying out ball milling to obtain a reinforcing filler, dispersing the reinforcing filler and a second activated luminous material by ethanol, carrying out surface carboxylation treatment to obtain a luminous mixture A, and uniformly mixing the mixture A, a resin matrix, tartaric acid and water to obtain the markable luminous binder.
Preferably, the repair material and the binder are included.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a markable luminous repair material for dentistry, which is added with a short-afterglow luminous material in conventional ceramic materials and dentistry binders. The prosthesis prepared by the material has no obvious difference with the conventional false tooth in the daily chewing use process, but under the irradiation of ultraviolet light, the prosthesis can emit obvious fluorescence which is obviously contrasted with the natural tooth. When the restoration body is damaged or needs to be restored again due to other reasons, the restoration material can be clearly seen through the irradiation of ultraviolet light, so that the restoration material can be conveniently removed, and the aims of protecting natural teeth and reducing the damage to the natural teeth body are achieved on the premise of completely removing the prosthesis.
The invention also discloses a preparation method of the markable luminous restoration material for dentistry, the preparation method comprises the steps of mixing the ceramic material and the first activating luminous material, performing ball milling uniformly, and performing hot pressing according to a target shape to form a restoration body, and the preparation method is simple and easy to popularize.
The invention discloses a markable luminous binder for dentistry, which is provided with a luminous material, so that a prosthesis using the binder is marked by utilizing the ultraviolet radiation luminous effect, and the prosthesis, the binder and natural teeth can be effectively distinguished in the repair process. The marking material for dental restoration is safe and non-toxic, can provide marks for dentists in the process of removing the dental restoration, and reduces damage to healthy natural teeth.
The invention also discloses a preparation method of the markable luminous binder for dentistry, which is characterized in that all materials are dispersed by ethanol and subjected to surface carboxylation treatment and then uniformly mixed to prepare the binder. According to the actual requirement, the restoration material is acted on the target tooth body by using the adhesive to prepare the markable luminous restoration.
[ description of the drawings ]
FIG. 1 is a photograph of a tooth incorporating a luminescent material according to the present invention;
FIG. 2 is a diagram of the present invention incorporating luminescent materials under UV irradiation;
[ detailed description ] embodiments
The invention is described in further detail below with reference to the accompanying drawings:
in the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, only for the purpose of facilitating description of the present invention and simplifying description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention; the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance; furthermore, unless expressly stated or limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly and encompass, for example, both fixed and removable connections; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases by those skilled in the art.
The invention discloses a markable luminous restoration structure for dentistry and a preparation method thereof, wherein the markable luminous restoration structure is a markable material and comprises a restoration and a binder, and the restoration is bonded on natural teeth through the binder, so that the use amount of the binder is adjusted according to requirements, is the use amount of the restoration in the same way, does not need strict definition, and can firmly bond the restoration on the natural teeth. The prosthesis is provided with a first activated luminescent powder material, and the adhesive is provided with a second activated luminescent powder material. The prosthesis and the binder naturally emit light after being irradiated by ultraviolet rays.
The restoration body is composed of a ceramic material, a first activated luminescent powder material with the mass fraction of 2% -30%, and the balance of the ceramic material, and particularly preferably the mass fraction of the first activated luminescent powder material is 10% -15%. The ceramic material is at least one of alumina ceramic, zirconia ceramic, feldspar ceramic and lithium disilicate glass ceramic, and lithium disilicate glass ceramic is preferred. The ceramic material is powder, and the particle size D50 of the ceramic powder is less than 30 mu m. The photoluminescent short-afterglow ultraviolet excited inorganic material is at least one of rare earth doped aluminate, metal doped sulfide and rare earth doped lead-free piezoelectric material, and the rare earth doped aluminate system CaAl2O4Eu, metal-doped sulfide ZnS, Mn/Cu, and rare earth-doped lead-free piezoelectric material (Ba)1-xCax)(Sn0.06Ti0.94)O3、K1-xNaxNbO3、(Bi0.5Na0.5)TiO3Preferably metal doped ZnS: Cu. The particle size of the activated luminescent powder is D50 < 5 μm, preferably D50 < 1 μm.
The preparation method of the prosthesis comprises the following steps:
(1) mixing the selected ceramic material and the first activated luminescent powder material in proportion;
(2) carrying out spherical granulation homogenization treatment on the material obtained in the step (1); ball-milling the mixed ceramic material and luminescent powder into slurry; then adding the slurry into the acidic solution and stirring for 5 hours by matching with a dispersion stirrer; injecting the stirred slurry into a pressure type spray dryer by using a plastic mortar pump to prepare ceramic-luminescent material granulation powder; and roasting the prepared ceramic-luminescent material granulation powder to prepare the ceramic-luminescent material spherical granulation powder.
(3) And (3) carrying out vacuum compression molding on the mixture obtained in the step (2) to obtain the first activated luminescent powder material, wherein the hot pressing temperature is 800-1400 ℃, the pressure is 20-30MPa, and the vacuum degree is more than 0.1 MPa.
The binder for the dental restoration structure comprises 30-60% by mass of a resin matrix, 10-30% by mass of a reinforcing filler, 1-10% by mass of a second activated luminescent powder material, 5-10% by mass of tartaric acid and 20-50% by mass of deionized water.
The resin matrix is polyacrylic acid or a copolymer of acrylic acid, itaconic acid and maleic acid, glycidyl methacrylate or hydroxyethyl methacrylate is added into the copolymer for modification treatment, and glycidyl methacrylate modified polyacrylic acid is preferably added.
The reinforcing filler is glass powder and comprises the following components in percentage by mass: SiO 2257-80 wt%; al (Al)2O311-20 wt%; CaF21-15 wt%; AlPO41 to 8 wt%; na (Na)2AlF61-5 wt%; AlF6Is 1-10 wt%. The grain size D50 of the glass powder is less than 20 μm.
The second activated luminescent powder material is a photoluminescence series short-afterglow ultraviolet excited high molecular material, such as at least one of conjugated polymer materials of polyphenyl, polythiophene, polycarbazole and the like, and polythiophene is preferred. The particle size of the second activated luminescent powder is D50 < 5 μm, and D50 < 1 μm is preferred.
The preparation method of the binder material comprises the following steps:
(1) mixing the selected glass powder materials in proportion, and carrying out high-speed ball milling on the obtained materials in a ball mill to obtain a mixture; the ball milling speed is 800-;
(2) melting the mixture obtained in the step (1) at high temperature to obtain glass liquid, and then quenching the glass liquid into distilled water to obtain glass fragments; the high-temperature melting temperature is controlled to be 1300 ℃ and 1550 ℃, and the heat preservation time is 30 min.
(3) Crushing and ball-milling the glass fragments obtained in the step (2) to obtain glass powder; the ball milling speed is 800-;
(4) mixing the glass powder obtained in the step (3) with a second activated luminescent powder material according to a ratio to obtain mixed powder, dispersing the mixed powder in ethanol, placing the dispersed mixed powder in a carboxylation beaker containing anhydrous ethanol saturated liquid of succinic anhydride, shaking the mixed powder by a shaking table for more than 4 hours, and carrying out surface carboxylation treatment at the treatment temperature of 60 ℃ to obtain a mixture A of the surface carboxylated luminescent powder and glass;
(5) and (4) uniformly mixing the mixture A obtained in the step (4) with a resin matrix, tartaric acid and deionized water according to a ratio to prepare the markable binder material for the dental restoration.
Example 1
The lithium disilicate glass ceramic powder with the mass fraction of 95 percent and the metal-doped ZnS and Cu material with the mass fraction of 5 percent are used for preparing a first activated luminescent powder material:
(1) mixing the lithium disilicate glass ceramic powder with a metal-doped ZnS-Cu material in a ratio;
(2) ball-milling the mixed ceramic material and luminescent powder into slurry; then adding the slurry into the acidic solution and stirring for 5 hours by matching with a dispersion stirrer; injecting the stirred slurry into a pressure type spray dryer by using a plastic mortar pump to prepare ceramic-luminescent material granulation powder; and roasting the prepared ceramic-luminescent material granulation powder to prepare the ceramic-luminescent material spherical granulation powder.
(3) And carrying out vacuum hot-pressing molding on the obtained mixture, wherein the hot-pressing temperature is 1000 ℃, the pressure is 30MPa, and the vacuum degree is 0.15 MPa. The obtained bulk ceramic material can emit fluorescence when irradiated by ultraviolet rays and can be used as a marking material for dental restoration.
Referring to fig. 1, a picture of a tooth added with a luminescent material under daily illumination and fig. 2, a picture of the tooth added with the luminescent material of the embodiment, it can be seen from the picture that the prosthesis added with the luminescent material has no difference with the common tooth under the daily illumination, and under the irradiation of ultraviolet radiation, the difference between the prosthesis and the body can be clearly seen.
Example 2
Preparing a markable binder material for dental restoration by using 40% by mass of glycidyl methacrylate modified polyacrylic acid copolymer, 20% by mass of reinforcing filler, 1% by mass of polythiophene material, 5% by mass of tartaric acid and 34% by mass of deionized water:
(1) preparing a reinforcing filler according to the component content shown in the following table 1, taking the raw material components for proportioning, mixing the raw materials according to the proportion, and then carrying out high-speed ball milling on the raw materials in a ball mill at the ball milling speed of 1800r/min for 14h to obtain a mixture;
table 1 example 2 reinforcing filler ingredient content formulation
| Components | Mass content wt% |
| SiO2 | 60 |
| Al2O3 | 15 |
| CaF2 | 10 |
| AlPO4 | 2 |
| Na2AlF6 | 3 |
| AlF6 | 10 |
(2) Melting the obtained mixture at 1450 ℃ to obtain glass liquid, preserving the temperature for 30min, and quenching the glass liquid into distilled water to obtain glass fragments;
(3) crushing and ball-milling the obtained glass fragments to obtain glass powder;
(4) mixing the obtained glass powder and polythiophene materials according to a ratio, heating and stirring in absolute ethyl alcohol for 30min at a heating temperature of 60 ℃ to obtain a luminescent powder-glass mixture;
(5) the obtained mixture is uniformly mixed with resin matrix, tartaric acid and deionized water according to a proportion to prepare the binder material with a marking function, and the binder material can be used for dental restoration.
Example 3
The first activated phosphor material from example 1 and the markable binder material from example 2 were mixed together to produce a repaired structure.
Example 4
98 percent of alumina ceramic powder and 2 percent of metal-doped CaAl2O4Preparing a first activated luminescent powder material by using a Eu material:
(1) alumina ceramic powder and metal-doped CaAl2O4Mixing the materials E in proportion;
(2) ball-milling the mixed ceramic material and luminescent powder into slurry; then adding the slurry into the acidic solution and stirring for 5 hours by matching with a dispersion stirrer; injecting the stirred slurry into a pressure type spray dryer by using a plastic mortar pump to prepare ceramic-luminescent material granulation powder; and roasting the prepared ceramic-luminescent material granulation powder to prepare the ceramic-luminescent material spherical granulation powder.
(3) And carrying out vacuum hot-pressing molding on the obtained mixture, wherein the hot-pressing temperature is 800 ℃, the pressure is 20MPa, and the vacuum degree is 0.2 MPa. The obtained bulk ceramic material can emit fluorescence when irradiated by ultraviolet rays and can be used as a marking material for dental restoration.
Example 5
Preparing a marking adhesive material for dental restoration by using 30 mass percent of hydroxyethyl methacrylate modified acrylic copolymer, 30 mass percent of reinforcing filler, 10 mass percent of polyphenyl material, 10 mass percent of tartaric acid and 20 mass percent of deionized water:
(1) preparing a reinforcing filler according to the component content shown in the following table 2, taking the raw material components for proportioning, mixing the raw materials in proportion, and then carrying out high-speed ball milling on the raw materials in a ball mill at the ball milling speed of 1500r/min for 2h to obtain a mixture;
table 2 example 5 reinforcing filler ingredient content formulation
(2) Melting the obtained mixture at 1550 ℃ to obtain glass liquid, preserving the temperature for 30min, and quenching the glass liquid into distilled water to obtain glass fragments;
(3) crushing and ball-milling the obtained glass fragments to obtain glass powder;
(4) mixing the obtained glass powder and a polyphenyl material according to a ratio, heating and stirring in absolute ethyl alcohol for 30min at the heating temperature of 60 ℃ to obtain a luminescent powder-glass mixture;
(5) the obtained mixture is uniformly mixed with resin matrix, tartaric acid and deionized water according to a proportion to prepare the binder material with a marking function, and the binder material can be used for dental restoration.
Example 6
The first activated phosphor material from example 4 and the markable binder material from example 5 were mixed together to produce a repaired structure.
Example 7
Preparing a first activated luminescent powder material from 70 mass percent of zirconia ceramic powder and 30 mass percent of metal-doped ZnS: Mn material:
(1) mixing zirconia ceramic powder and metal-doped ZnS: Mn material in proportion;
(2) ball-milling the mixed ceramic material and luminescent powder into slurry; then adding the slurry into the acidic solution and stirring for 5 hours by matching with a dispersion stirrer; injecting the stirred slurry into a pressure type spray dryer by using a plastic mortar pump to prepare ceramic-luminescent material granulation powder; and roasting the prepared ceramic-luminescent material granulation powder to prepare the ceramic-luminescent material spherical granulation powder.
(3) And carrying out vacuum hot-pressing molding on the obtained mixture, wherein the hot-pressing temperature is 1400 ℃, the pressure is 25MPa, and the vacuum degree is 0.15 MPa. The obtained bulk ceramic material can emit fluorescence when irradiated by ultraviolet rays and can be used as a marking material for dental restoration.
Example 8
Preparing a markable binder material for dental restoration by using a copolymer of acrylic acid and itaconic acid with the mass fraction of 34%, a reinforcing filler with the mass fraction of 10%, a polycarbazole material with the mass fraction of 1%, tartaric acid with the mass fraction of 5% and deionized water with the mass fraction of 50%:
(1) preparing a reinforcing filler according to the component content shown in the following table 3, taking the raw material components for proportioning, mixing the raw materials in proportion, and then carrying out high-speed ball milling on the raw materials in a ball mill at the ball milling speed of 2000r/min for 16h to obtain a mixture;
table 3 example 8 reinforcing filler ingredient content formulation
| Components | Mass content wt% |
| SiO2 | 80 |
| Al2O3 | 11 |
| CaF2 | 6 |
| AlPO4 | 1 |
| Na2AlF6 | 1 |
| AlF6 | 1 |
(2) Melting the obtained mixture at 1300 ℃ to obtain glass liquid, preserving the heat for 30min, and quenching the glass liquid into distilled water to obtain glass fragments;
(3) crushing and ball-milling the obtained glass fragments to obtain glass powder;
(4) mixing the obtained glass powder and a polycarbazole material according to a ratio, heating and stirring in absolute ethyl alcohol for 30min at a heating temperature of 60 ℃ to obtain a luminescent powder-glass mixture;
(5) the obtained mixture is uniformly mixed with resin matrix, tartaric acid and deionized water according to a proportion to prepare the binder material with a marking function, and the binder material can be used for dental restoration.
Example 9
The first activated phosphor material from example 7 and the markable binder material from example 8 were mixed together to produce a repaired structure.
Example 10
90% of feldspar ceramic powder and 10% of (Ba)1-xCax)(Sn0.06Ti0.94)O3The material as the first activated luminescent powder material:
(1) feldspar ceramic powder and metal doped (Ba)1-xCax)(Sn0.06Ti0.94)O3Mixing the materials in proportion;
(2) ball-milling the mixed ceramic material and the first activated luminescent powder material into slurry; then adding the slurry into the acidic solution and stirring for 5 hours by matching with a dispersion stirrer; injecting the stirred slurry into a pressure type spray dryer by using a plastic mortar pump to prepare ceramic-luminescent material granulation powder; and roasting the prepared ceramic-luminescent material granulation powder to prepare the ceramic-luminescent material spherical granulation powder.
(3) And carrying out vacuum hot-pressing molding on the obtained mixture, wherein the hot-pressing temperature is 900 ℃, the pressure is 22MPa, and the vacuum degree is 0.15 MPa. The obtained bulk ceramic material can emit fluorescence when irradiated by ultraviolet rays and can be used as a marking material for dental restoration.
Example 11
Preparing a markable binder material for dental restoration by using a copolymer of acrylic acid and maleic acid with the mass fraction of 40%, a reinforcing filler with the mass fraction of 17%, a mixed material of polyphenyl and polythiophene with the mass fraction of 5%, tartaric acid with the mass fraction of 8% and deionized water with the mass fraction of 30%:
(1) preparing a reinforcing filler according to the component content shown in the following table 4, taking the raw material components for proportioning, mixing the raw materials in proportion, and then carrying out high-speed ball milling on the raw materials in a ball mill at the ball milling speed of 800r/min for 10h to obtain a mixture;
table 4 example 11 reinforcing filler ingredient content formulation
(2) Melting the obtained mixture at 1400 ℃ to obtain glass liquid, preserving the heat for 30min, and quenching the glass liquid into distilled water to obtain glass fragments;
(3) crushing and ball-milling the obtained glass fragments to obtain glass powder;
(4) mixing the obtained glass powder and polythiophene materials according to a ratio, heating and stirring in absolute ethyl alcohol for 30min at a heating temperature of 60 ℃ to obtain a luminescent powder-glass mixture;
(5) the obtained mixture is uniformly mixed with resin matrix, tartaric acid and deionized water according to a proportion to prepare the binder material with a marking function, and the binder material can be used for dental restoration.
Example 12
The first activated phosphor material from example 10 and the markable binder material from example 11 were mixed together to produce a repaired structure.
Example 13
80 mass percent of mixed ceramic powder of alumina ceramic and zirconia ceramic, and 20 mass percent of K1-xNaxNbO3Preparing a first activated luminescent powder material:
(1) mixing ceramic powder with K1-xNaxNbO3Mixing the materials in proportion;
(2) ball-milling the mixed ceramic material and luminescent powder into slurry; then adding the slurry into the acidic solution and stirring for 5 hours by matching with a dispersion stirrer; injecting the stirred slurry into a pressure type spray dryer by using a plastic mortar pump to prepare ceramic-luminescent material granulation powder; and roasting the prepared ceramic-luminescent material granulation powder to prepare the ceramic-luminescent material spherical granulation powder.
(3) And carrying out vacuum hot-pressing molding on the obtained mixture, wherein the hot-pressing temperature is 1200 ℃, the pressure is 28MPa, and the vacuum degree is 0.2 MPa. The obtained bulk ceramic material can emit fluorescence when irradiated by ultraviolet rays and can be used as a marking material for dental restoration.
Example 14
Preparing a marked adhesive material for dental restoration by using 60 mass percent of glycidyl methacrylate modified acrylic copolymer, 10 mass percent of reinforcing filler, 4 mass percent of a mixture material of thiophene and polycarbazole, 6 mass percent of tartaric acid and 20 mass percent of deionized water:
(1) preparing a reinforcing filler according to the component content shown in the following table 5, taking the raw material components for proportioning, mixing the raw materials in proportion, and then carrying out high-speed ball milling on the raw materials in a ball mill at the ball milling speed of 1000r/min for 5h to obtain a mixture;
table 5 example 14 reinforcing filler ingredient content formulation
| Components | Mass content wt% |
| SiO2 | 65 |
| Al2O3 | 20 |
| CaF2 | 2 |
| AlPO4 | 5 |
| Na2AlF6 | 1 |
| AlF6 | 7 |
(2) Melting the obtained mixture at 1350 deg.C to obtain glass liquid, maintaining the temperature for 30min, and quenching the glass liquid into distilled water to obtain glass fragments;
(3) crushing and ball-milling the obtained glass fragments to obtain glass powder;
(4) mixing the obtained glass powder and polythiophene materials according to a ratio, heating and stirring in absolute ethyl alcohol for 30min at a heating temperature of 60 ℃ to obtain a luminescent powder-glass mixture;
(5) the obtained mixture is uniformly mixed with resin matrix, tartaric acid and deionized water according to a proportion to prepare the binder material with a marking function, and the binder material can be used for dental restoration.
Example 15
The first activated phosphor material from example 13 and the markable binder material from example 14 were mixed together to produce a repaired structure.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The markable luminescent repair material for dentistry is characterized by being prepared by vacuum die pressing of a ceramic material and a first activated luminescent powder material, wherein the mass fraction of the first activated luminescent powder material is 2-30%, and the balance is the ceramic material.
2. The markable luminescent restoration material for dentistry according to claim 1, wherein the ceramic material is at least one of alumina ceramic, zirconia ceramic, feldspathic ceramic or lithium disilicate glass ceramic; the first activated luminescent powder material is a photoluminescence series short-afterglow ultraviolet excited inorganic material.
3. The markable luminescent restoration material for dentistry according to claim 1, wherein the ceramic material has a particle size D50 ≤ 30 μm, and the first activated luminescent powder material has a particle size D50 ≤ 1 μm.
4. A method for preparing a markable luminescent restoration material for dentistry as claimed in any of claims 1 to 3, wherein the ceramic material and the first activated luminescent powder material are subjected to spherical granulation and homogenization treatment to obtain spherical particles, and the spherical particles are subjected to vacuum hot-press molding to obtain the restoration.
5. The method as claimed in claim 4, wherein the spherical particles have a vacuum hot pressing temperature of 800-1400 ℃, a pressure of 20-30MPa, and a vacuum degree of > 0.1 MPa.
6. A markable luminescent binder for dental use, characterized in that the binder consists of a resin matrix, a reinforcing filler, a second activated luminescent powder material, tartaric acid and water; the second activated luminescent powder material emits light under ultraviolet irradiation.
7. The markable luminescent binder for dentistry according to claim 6, wherein the binder has a mass fraction of the resin matrix of 30-60%, a mass fraction of the reinforcing filler of 10-40%, a mass fraction of the second activated luminescent powder (organic) material of 1-10%, a mass fraction of tartaric acid of 5-10% and a mass fraction of water of 30-50%.
8. The markable luminescent binder for dentistry according to claim 6 wherein the resin matrix is polyacrylic acid or a copolymer of acrylic acid with itaconic acid, maleic acid; glycidyl methacrylate or hydroxyethyl methacrylate is added into the copolymer; the reinforcing filler is glass powder; the second active luminescent material is a photoluminescence series short-afterglow ultraviolet excited high polymer material.
9. A method for preparing a markable luminescent binder for dentistry as claimed in any one of claims 6 to 9, wherein the markable luminescent binder is prepared by mixing and ball milling selected glass powder materials in proportion, melting the obtained mixture, quenching the melted mixture into glass blocks, ball milling the glass blocks to prepare reinforcing fillers, dispersing the reinforcing fillers and the second activated luminescent material by ethanol, performing surface carboxylation treatment to obtain a markable luminescent binder a, and uniformly mixing the mixture a, the resin matrix, tartaric acid and water.
10. A markable luminescent restoration for dental use, comprising a restorative material according to claim 1 and a binder according to claim 5.
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