CN106265089B - A kind of dental prosthetic material and preparation method thereof - Google Patents

A kind of dental prosthetic material and preparation method thereof Download PDF

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Publication number
CN106265089B
CN106265089B CN201610717605.1A CN201610717605A CN106265089B CN 106265089 B CN106265089 B CN 106265089B CN 201610717605 A CN201610717605 A CN 201610717605A CN 106265089 B CN106265089 B CN 106265089B
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oxide
dental prosthetic
prosthetic material
powder
zirconium
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CN106265089A (en
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侯超
杜波
战延军
董艳丽
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ZAOZHUANG MUNICIPAL HOSPITAL
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ZAOZHUANG MUNICIPAL HOSPITAL
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/80Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/831Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/80Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/802Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/80Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/802Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
    • A61K6/818Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising zirconium oxide
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/80Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/802Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
    • A61K6/822Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising rare earth metal oxides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/80Preparations for artificial teeth, for filling teeth or for capping teeth
    • A61K6/802Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
    • A61K6/824Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising transition metal oxides

Abstract

The invention discloses a kind of dental prosthetic materials and preparation method thereof, the dental prosthetic material is calculated in mass percent, including following components: cerium oxide 0.6~2%, yttrium oxide 0.8~3%, borax 1~4%, sodium stannate 2~4%, silica 3~5%, aluminium oxide 15~24%, surplus are zirconium oxide.Ceramic tooth elements obtained by the direct injection molding of dental prosthetic material of the invention, tensile strength is big, and linear expansion coefficient is small, and Rockwell hardness is big, yield strength is big, have the characteristics that high rigidity, high intensity and high tenacity, that is, has both good mechanical performance and processing performance, while also there is more preferably corrosion resistance, in addition, ceramic tooth elements obtained by the direct injection molding of dental prosthetic material of the invention are suitable with the tooth bulk refractive index of human body, and more close with the tooth of human body itself, clinical use is more beautiful.

Description

A kind of dental prosthetic material and preparation method thereof
Technical field
The present invention relates to a kind of dental prosthetic materials.Belong to dental care technical field.
Background technique
Oral restoration primarily directed to the treatment work after tooth defect, absence of tooth, such as inlay, complete crown, artificial tooth, It is directed to periodontosis and the treatment of Maxillofacial tissue defect etc. including the use of artificial dummy, is one important point in dentistry Branch.
China because of absence of tooth patient up to total population caused by saprodontia, periodontitis and dent trauma 1 to three/5th / mono-.Therefore, the exploitation for accelerating dental prosthetic material and product releases the pain of millions upon millions of patients, and it is negative to reduce medical expense Load, is undoubtedly very important and the call of social development.
Ceramic material is known as 21 century since its good biocompatibility, structure and color texture are similar to people's tooth Main tooth body dentition defect restoration material.Although having castable ceramic, Glass-Infiltrated-Alumina ceramics, dense multicrystalline oxygen at present Change aluminium ceramics and zirconia ceramics product emerges, and is used in clinic, but the mechanical performance and processing of gained ceramic material Performance tends not to get both, and limits clinical application range, and in addition in clinical use, requirement of the patient to aesthetics is also to get over Come it is higher, then, there is smaller vision difference can meet this requirement for other teeth of prepared product and human body.
Summary of the invention
The purpose of the present invention is to overcome above-mentioned the deficiencies in the prior art, provide a kind of dental prosthetic material.
The present invention also provides the preparation methods of the dental prosthetic material.
To achieve the above object, the present invention adopts the following technical solutions:
A kind of dental prosthetic material, is calculated in mass percent, including following components: cerium oxide 0.6~2%, yttrium oxide 0.8 ~3%, borax 1~4%, sodium stannate 2~4%, silica 3~5%, aluminium oxide 15~24%, surplus is zirconium oxide.
Preferably, including following components: cerium oxide 1~1.5%, yttrium oxide 1.2~2.5%, borax 2~3%, sodium stannate 2.5~3.5%, silica 3.5~4.5%, aluminium oxide 17~22%, surplus is zirconium oxide.
It is further preferred that including following components: cerium oxide 1%, yttrium oxide 2%, borax 3%, sodium stannate 3%, dioxy SiClx 4%, aluminium oxide 20%, surplus are zirconium oxide.
Preferably, the dental prosthetic material is powder, and partial size is 40~50nm.
A kind of preparation method of above-mentioned dental prosthetic material, comprising steps of
(1) zirconium oxychloride is dissolved in ethyl alcohol, cerium oxide, aluminium oxide and yttrium oxide is then added at 60~80 DEG C;
(2) cooling, sodium bicarbonate or potassium bicarbonate solution is added, adds acrylate, it is anti-to be put into high pressure for supersound washing It answers in kettle and is reacted, obtain the first powder after reaction;
(3) by the first powder and borax, sodium stannate and silica mixing and ball milling, 300~450W microwave treatment 20~30 Minute, washing, it is dry to get.
Preferably, in step (1), the mole of zirconium oxychloride is formula ratio zirconium oxide conversion gained, zirconium oxychloride and second The mass volume ratio of alcohol is 1g:40~50mL.
Preferably, in step (2) be cooled to be cooled to 25 DEG C.
Preferably, the additional amount of acrylate is the 0.7~0.9% of zirconium oxychloride quality in step (2).
Preferably, the mass fraction of sodium bicarbonate or saleratus is 2~5% in step (2).
Preferably, the reaction temperature in step (2) be 250~270 DEG C, the reaction time be 3~4 hours, pressure be 4~ 6MPa。
Preferably, the washing in step (3) is to be washed 3~4 times using dehydrated alcohol.
Preferably, the drying in step (3) is freeze-drying.
Above-mentioned dental prosthetic material may be directly applied to injection-molding formed ceramic tooth elements.
Beneficial effects of the present invention:
Dental prosthetic material of the invention also added cerium oxide, yttrium oxide, boron based on zirconium oxide, supplemented by aluminium oxide Sand, sodium stannate and silica.Ceramic tooth elements obtained by the direct injection molding of dental prosthetic material of the invention, tensile strength Greatly, linear expansion coefficient is small, and Rockwell hardness is big, and yield strength is big, has the characteristics that high rigidity, high intensity and high tenacity, that is, has both Good mechanical performance and processing performance, while also there is more preferably corrosion resistance, in addition, dental prosthetic material of the invention is straight It is suitable with the tooth bulk refractive index of human body to connect ceramic tooth elements obtained by injection molding, it is more close with the tooth of human body itself, face Bed use is more beautiful.
Specific embodiment
Below with reference to embodiment, the present invention will be further elaborated, it should explanation, following the description merely to It explains the present invention, its content is not defined.
Embodiment 1:
A kind of dental prosthetic material, is calculated in mass percent, including following components: cerium oxide 0.6%, yttrium oxide 0.8%, Borax 1%, sodium stannate 2%, silica 3%, aluminium oxide 15%, surplus are zirconium oxide.The dental prosthetic material is powder, Partial size is 40nm.
A kind of preparation method of above-mentioned dental prosthetic material, comprising steps of
(1) by zirconium oxychloride, (its mole is formula ratio zirconium oxide conversion gained, the quality volume of zirconium oxychloride and ethyl alcohol Than being dissolved in ethyl alcohol for 1g:40~50mL), cerium oxide, aluminium oxide and yttrium oxide are then added at 60 DEG C;
(2) 25 DEG C are cooled to, sodium bicarbonate or potassium bicarbonate solution that mass fraction is 2% is added, adds acrylic acid Ester the 0.7% of zirconium oxychloride quality (additional amount be), supersound washing are put into autoclave and are reacted that (reaction temperature is 250 DEG C, the reaction time is 3 hours, pressure 4MPa), the first powder is obtained after reaction;
(3) 300W microwave treatment 20 minutes, anhydrous by the first powder and borax, sodium stannate and silica mixing and ball milling Ethanol washing 3 times, freeze-drying to get.
Embodiment 2:
A kind of dental prosthetic material, is calculated in mass percent, including following components: cerium oxide 2%, yttrium oxide 3%, borax 4%, sodium stannate 4%, silica 5%, aluminium oxide 24%, surplus is zirconium oxide.The dental prosthetic material is powder, partial size For 50nm.
A kind of preparation method of above-mentioned dental prosthetic material, comprising steps of
(1) by zirconium oxychloride, (its mole is formula ratio zirconium oxide conversion gained, the quality volume of zirconium oxychloride and ethyl alcohol Than being dissolved in ethyl alcohol for 1g:40~50mL), cerium oxide, aluminium oxide and yttrium oxide are then added at 80 DEG C;
(2) 25 DEG C are cooled to, sodium bicarbonate or potassium bicarbonate solution that mass fraction is 5% is added, adds acrylic acid Ester the 0.9% of zirconium oxychloride quality (additional amount be), supersound washing are put into autoclave and are reacted that (reaction temperature is 270 DEG C, the reaction time is 4 hours, pressure 6MPa), the first powder is obtained after reaction;
(3) 450W microwave treatment 30 minutes, anhydrous by the first powder and borax, sodium stannate and silica mixing and ball milling Ethanol washing 4 times, freeze-drying to get.
Embodiment 3:
A kind of dental prosthetic material, is calculated in mass percent, including following components: it is preferred, including following components: oxidation Cerium 1%, yttrium oxide 1.2%, borax 2%, sodium stannate 2.5%, silica 3.5%, aluminium oxide 17%, surplus are zirconium oxide. The dental prosthetic material is powder, partial size 40nm.
A kind of preparation method of above-mentioned dental prosthetic material, comprising steps of
(1) by zirconium oxychloride, (its mole is formula ratio zirconium oxide conversion gained, the quality volume of zirconium oxychloride and ethyl alcohol Than being dissolved in ethyl alcohol for 1g:40~50mL), cerium oxide, aluminium oxide and yttrium oxide are then added at 60 DEG C;
(2) 25 DEG C are cooled to, sodium bicarbonate or potassium bicarbonate solution that mass fraction is 2% is added, adds acrylic acid Ester the 0.7% of zirconium oxychloride quality (additional amount be), supersound washing are put into autoclave and are reacted that (reaction temperature is 250 DEG C, the reaction time is 3 hours, pressure 4MPa), the first powder is obtained after reaction;
(3) 300W microwave treatment 20 minutes, anhydrous by the first powder and borax, sodium stannate and silica mixing and ball milling Ethanol washing 3 times, freeze-drying to get.
Embodiment 4:
A kind of dental prosthetic material, is calculated in mass percent, including following components: cerium oxide 1.5%, yttrium oxide 2.5%, Borax 3%, sodium stannate 3.5%, silica 4.5%, aluminium oxide 22%, surplus are zirconium oxide.The dental prosthetic material is powder Body, partial size 50nm.
A kind of preparation method of above-mentioned dental prosthetic material, comprising steps of
(1) by zirconium oxychloride, (its mole is formula ratio zirconium oxide conversion gained, the quality volume of zirconium oxychloride and ethyl alcohol Than being dissolved in ethyl alcohol for 1g:40~50mL), cerium oxide, aluminium oxide and yttrium oxide are then added at 80 DEG C;
(2) 25 DEG C are cooled to, sodium bicarbonate or potassium bicarbonate solution that mass fraction is 5% is added, adds acrylic acid Ester the 0.9% of zirconium oxychloride quality (additional amount be), supersound washing are put into autoclave and are reacted that (reaction temperature is 270 DEG C, the reaction time is 4 hours, pressure 6MPa), the first powder is obtained after reaction;
(3) 450W microwave treatment 30 minutes, anhydrous by the first powder and borax, sodium stannate and silica mixing and ball milling Ethanol washing 4 times, freeze-drying to get.
Embodiment 5:
A kind of dental prosthetic material, is calculated in mass percent, including following components: cerium oxide 1%, yttrium oxide 2%, borax 3%, sodium stannate 3%, silica 4%, aluminium oxide 20%, surplus is zirconium oxide.The dental prosthetic material is powder, partial size For 50nm.
A kind of preparation method of above-mentioned dental prosthetic material, comprising steps of
(1) by zirconium oxychloride, (its mole is formula ratio zirconium oxide conversion gained, the quality volume of zirconium oxychloride and ethyl alcohol Than being dissolved in ethyl alcohol for 1g:40~50mL), cerium oxide, aluminium oxide and yttrium oxide are then added at 70 DEG C;
(2) 25 DEG C are cooled to, sodium bicarbonate or potassium bicarbonate solution that mass fraction is 4% is added, adds acrylic acid Ester the 0.8% of zirconium oxychloride quality (additional amount be), supersound washing are put into autoclave and are reacted that (reaction temperature is 260 DEG C, the reaction time is 3 hours, pressure 5MPa), the first powder is obtained after reaction;
(3) 400W microwave treatment 25 minutes, anhydrous by the first powder and borax, sodium stannate and silica mixing and ball milling Ethanol washing 4 times, freeze-drying to get.
Comparative example:
A kind of dental prosthetic material, is calculated in mass percent, including following components: yttrium oxide 2%, and aluminium oxide 20% is remaining Amount is zirconium oxide.Preparation method is as follows:
(1) by zirconium oxychloride, (its mole is formula ratio zirconium oxide conversion gained, the quality volume of zirconium oxychloride and ethyl alcohol Than being dissolved in ethyl alcohol for 1g:40~50mL), yttrium oxide and aluminium oxide are then added at 70 DEG C;
(2) 25 DEG C are cooled to, sodium bicarbonate or potassium bicarbonate solution that mass fraction is 4% is added, adds acrylic acid Ester the 0.8% of zirconium oxychloride quality (additional amount be), supersound washing are put into autoclave and are reacted that (reaction temperature is 260 DEG C, the reaction time be 3 hours, pressure 5MPa), dehydrated alcohol wash 4 times, freeze-drying to get.
Test example
The dental prosthetic material of Examples 1 to 5 and comparative example is directly applied into injection molding using identical method Ceramic tooth elements.
1, Mechanics Performance Testing
The detection such as tensile strength, thermal expansion coefficient, Rockwell hardness, yield strength has been carried out, the results are shown in Table 1.
1. mechanical experimental results table of table
From table 1, it could be assumed that, ceramic tooth elements obtained by the dental prosthetic material of Examples 1 to 5, tensile strength is big, line The coefficient of expansion is small, and Rockwell hardness is big, and yield strength is big, show dental prosthetic material of the invention have high rigidity, high intensity and The features such as high tenacity.
2, corrosion resistance is tested
The test of artificial saliva corrosion weight loss is carried out, testing result is shown in Table 2.
2. corrosion resistance test result of table
It will be apparent that ceramic tooth elements obtained by the dental prosthetic material of Examples 1 to 5 have more preferably corrosion resistance.
3, index of refraction is tested
Refractive index is measured using Nereid section automatic Abbe refractometer (constant temperature) on WAY-ZT at room temperature, the results are shown in Table 3.
3. refraction index test result of table
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Comparative example
Refractive index 2.2648 2.2768 2.2682 2.2735 2.2701 1.3598
100 person-times of statistics through applicant's acquisition, the tooth ontology mean refractive index of human body is 2.27 or so, Examples 1 to 5 It is suitable with the tooth bulk refractive index of human body, it is more close with the tooth of human body itself, and comparative example and other tooth differences are more Obviously, beauty is influenced.
Above-mentioned, although specific embodiments of the present invention have been described, not to the limit of the scope of the present invention System, based on the technical solutions of the present invention, those skilled in the art do not need to make the creative labor can make it is each Kind modification or deformation are still within protection scope of the present invention.

Claims (7)

1. a kind of dental prosthetic material, which is characterized in that be calculated in mass percent, including following components: cerium oxide 0.6~2%, Yttrium oxide 0.8~3%, borax 1~4%, sodium stannate 2~4%, silica 3~5%, aluminium oxide 15~24%, surplus are zirconium oxide; The dental prosthetic material is powder, and partial size is 40~50nm;Preparation method, comprising steps of
(1) zirconium oxychloride is dissolved in ethyl alcohol, cerium oxide, aluminium oxide and yttrium oxide is then added at 60~80 DEG C;
(2) cooling, sodium bicarbonate or potassium bicarbonate solution is added, adds acrylate, supersound washing is put into autoclave In reacted, after reaction the first powder;
(3) by the first powder and borax, sodium stannate and silica mixing and ball milling, 300~450W microwave treatment 20~30 minutes, Washing, it is dry to get;
Reaction temperature in step (2) is 250~270 DEG C, and the reaction time is 3~4 hours, and pressure is 4~6MPa.
2. a kind of dental prosthetic material according to claim 1, which is characterized in that including following components: cerium oxide 1~ 1.5%, yttrium oxide 1.2~2.5%, borax 2~3%, sodium stannate 2.5~3.5%, silica 3.5~4.5%, aluminium oxide 17~ 22%, surplus is zirconium oxide;The dental prosthetic material is powder, and partial size is 40~50nm;Preparation method, comprising steps of
(1) zirconium oxychloride is dissolved in ethyl alcohol, cerium oxide, aluminium oxide and yttrium oxide is then added at 60~80 DEG C;
(2) cooling, sodium bicarbonate or potassium bicarbonate solution is added, adds acrylate, supersound washing is put into autoclave In reacted, after reaction the first powder;
(3) by the first powder and borax, sodium stannate and silica mixing and ball milling, 300~450W microwave treatment 20~30 minutes, Washing, it is dry to get;
Reaction temperature in step (2) is 250~270 DEG C, and the reaction time is 3~4 hours, and pressure is 4~6MPa.
3. a kind of dental prosthetic material according to claim 1, which is characterized in that including following components: cerium oxide 1%, oxygen Change yttrium 2%, borax 3%, sodium stannate 3%, silica 4%, aluminium oxide 20%, surplus is zirconium oxide;The dental prosthetic material is powder Body, partial size are 40~50nm;Preparation method, comprising steps of
(1) zirconium oxychloride is dissolved in ethyl alcohol, cerium oxide, aluminium oxide and yttrium oxide is then added at 60~80 DEG C;
(2) cooling, sodium bicarbonate or potassium bicarbonate solution is added, adds acrylate, supersound washing is put into autoclave In reacted, after reaction the first powder;
(3) by the first powder and borax, sodium stannate and silica mixing and ball milling, 300~450W microwave treatment 20~30 minutes, Washing, it is dry to get;
Reaction temperature in step (2) is 250~270 DEG C, and the reaction time is 3~4 hours, and pressure is 4~6MPa.
4. a kind of dental prosthetic material described in any one of claim 1 to 3, which is characterized in that in step (1), oxygen The mole of zirconium chloride is obtained by the conversion of formula ratio zirconium oxide, and the mass volume ratio of zirconium oxychloride and ethyl alcohol is 1g:40~50mL.
5. a kind of dental prosthetic material described in any one of claim 1 to 3, which is characterized in that propylene in step (2) The additional amount of acid esters is the 0.7~0.9% of zirconium oxychloride quality.
6. a kind of dental prosthetic material described in any one of claim 1 to 3, which is characterized in that carbonic acid in step (2) The mass fraction of hydrogen sodium or saleratus is 2~5%.
7. a kind of dental prosthetic material described in any one of claim 1 to 3, which is characterized in that washing in step (3) It washs to use dehydrated alcohol to wash 3~4 times;Dry is freeze-drying.
CN201610717605.1A 2016-08-24 2016-08-24 A kind of dental prosthetic material and preparation method thereof Expired - Fee Related CN106265089B (en)

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CN106904961A (en) * 2017-02-21 2017-06-30 朱军 A kind of dental prosthetic material and preparation method thereof
CN106693045A (en) * 2017-02-21 2017-05-24 朱军 High-bending-strength oral cavity repair material and preparation method thereof
CN112979309A (en) * 2021-02-07 2021-06-18 刘美顺 Ceramic material for oral restoration and preparation method thereof

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