CN103043910A - Glass ceramic for making dental prosthesis and preparation method thereof - Google Patents
Glass ceramic for making dental prosthesis and preparation method thereof Download PDFInfo
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- CN103043910A CN103043910A CN2012105751084A CN201210575108A CN103043910A CN 103043910 A CN103043910 A CN 103043910A CN 2012105751084 A CN2012105751084 A CN 2012105751084A CN 201210575108 A CN201210575108 A CN 201210575108A CN 103043910 A CN103043910 A CN 103043910A
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Abstract
The invention discloses a glass ceramic for making a dental prosthesis and a preparation method thereof. The glass ceramic comprises the following components in percentage by weight: 56 to 59 percent of SiO2, 28 to 30 percent of Li2CO3, 3.7 to 4.0 percent of K2CO3, 2.7 to 3.0 percent of Al2O3, 2.3 to 2.4 percent of ZrO2, 1.5 to 1.6 percent of CeO2 and 2.5 to 3.0 percent of P2O5. The preparation method of the glass ceramic comprises the following steps of: uniformly mixing and ball-milling the components, and drying after uniformly mixing so as to obtain mixed powder; pouring the mixed powder into a quartz crucible to carry out founding, then pouring molten powder into deionized water and carrying out cold quenching to obtain glass particles; placing the glass particles into an agate jar and carrying out ball milling and drying to obtain glass powder; filling the glass powder into a prefabricated box to carry out cold isostatic pressure forming so as to obtain a glass powder blank; and finally, carrying out two-section crystallization thermal treatment on the glass powder blank to obtain the glass ceramic.
Description
Technical field
The present invention relates to dental glass-ceramic dummy, particularly a kind of glass-ceramic for making dental prosthesis and preparation method thereof.
Background technology
Along with improving constantly of standard of living, people require more and more higher to the visual effect of dental prosthesis.The semipermeability of material is very important on the impact of dummy visual effect.The semipermeability of All-ceramic Dental Material is considered to control the principal element of dummy aesthetic effect, is one of key reference of repair materials selection.This performance to full ceramic restoration material has proposed Secretary, and namely repair materials need possess higher mechanical strength, and is not chipping to bear snap-in force; Must have outstanding optical property on the other hand, can farthest simulate and reproduce the optical signature of natural teeth sclerous tissues.
The low brilliant ceramic material of early stage dentistry take feldspathic china as representative is structurally closer to glass, crystalline component is few, has preferably optical property, the dummy good luster made from this class material, attractive in appearance, but the strength of materials is low, can only be used for finishing material or veneer of anterior tooth.By toughness reinforcing phases such as interpolation white garnet, micas, though improved to a certain extent intensity, but still be confined to the making of labial teeth leaf-comb, veneer.
For expanding the range of application of full ceramic material, under the traditional principles take the function reparation as main purpose instructed, the in the past research of All-ceramic Dental Material mainly concentrated on mechanical property and the high brilliant pottery of preparation that improves material for a long time.Such as dentistry alumina-ceramic and zirconia ceramics, has physical strength the highest in the All-ceramic Dental Material, but the improvement of mechanical property is that to sacrifice optical property be cost, the light transmission of such material is very little, even close to metal, dummy aesthetic property and the emulation made are relatively poor, are not suitable for the aesthetics reparation for labial teeth.
This shows that present commercial full ceramic restoration material still can not satisfy the aesthstic balance unification of repairing the desired mechanical property of principle and optical property of dentistry.
Summary of the invention
One object of the present invention is to provide a kind of glass-ceramic for making dental prosthesis, and it can provide high-mechanical property, also has simultaneously outstanding semi-transparent characteristic and aesthetic effect.
Another object of the present invention is to provide the preparation method of above-mentioned glass-ceramic for making dental prosthesis.
To achieve these goals, the present invention is achieved by the following technical solutions.
(1) a kind of glass-ceramic for making dental prosthesis is characterized in that, comprises the component of following mass percent: 56～59% SiO
2, 28～30% Li
2CO
3, 3.7～4.0% K
2CO
3, 2.7～3.0% Al
2O
3, 2.3～2.4% ZrO
2, 1.5～1.6% CeO
2, and 2.5～3.0% P
2O
5
The component of the optimization mass percent of technique scheme is: 58% SiO
2, 29% Li
2CO
3, 3.7% K
2CO
3, 2.8% Al
2O
3, 2.4% ZrO
2, 1.5% CeO
2, 2.6% P
2O
5
(2) for the preparation method of the glass-ceramic of making dental prosthesis, it is characterized in that, may further comprise the steps: take by weighing each component according to mass percent, with each component mixing ball milling, mix post-drying, get mixed powder; Mixed powder is poured in the quartz crucible again, founded 1.5～2h for 1400～1500 ℃, then, will melt slurry and pour in the deionized water, cold quenching obtains glass particle; Glass particle is placed agate jar, ball milling, drying gets glass powder; The cold isostatic compaction in the prefabricated flask of then glass powder being packed into gets the glass powder base substrate; At last the glass powder base substrate is carried out the two-part crystallization and thermal treatment, get final product.
In the technique scheme, described two-part crystallization and thermal treatment is 700 ℃/5h and 900 ℃/5h.
(3) glass-ceramic of above-mentioned preparation is for the preparation of the method for dental prosthesis, it is characterized in that, use dentistry hot pressing casting machine described glass-ceramic is carried out the hot pressing casting, wherein: hot pressing temperature 900-1000 ℃, die casting pressure 3.5-4.5bar, die casting time 4-6min, soaking time 12-18min.
The glass-ceramic that is used for making dental prosthesis of the present invention's preparation, principal crystalline phase is two lithium silicate (Li
2Si
2O
5), contain in addition a small amount of lithium metasilicate (Li
2SiO
3) and Trilithium phosphate (Li
3PO
4).The crystal formation interlocking microstructure of two bar-shaped lithium silicates can Effective Raise material resistance to crack extension ability.Its three-point bending strength is 308MPa, satisfies dental material ISO required standard.Main crystalline phase composition two lithium silicate crystal (Li
2Si
2O
5), its optical refractive index is 1.55, and glass matrix (1.50) is very approaching, can form good optical match with glass matrix, greatly reduces the scattering process to incident beam.Thereby two lithium silicate glass-ceramic of the present invention can keep preferably semipermeability, and its TP value (Translucency parameter) is 20.6, and are good with natural teeth sclerous tissues semipermeability coupling.
Description of drawings
Below in conjunction with the drawings and specific embodiments the present invention is described in further details.
Fig. 1 is X-ray diffraction analysis (XRD) figure of the glass-ceramic of embodiment 1 preparation.
Fig. 2 is the micro-structure diagram of the glass-ceramic of embodiment 1 preparation.
Fig. 3 is X-ray diffraction analysis (XRD) figure of the glass-ceramic of embodiment 2 preparations.
Fig. 4 is the micro-structure diagram of the glass-ceramic of embodiment 2 preparations.
Fig. 5 is X-ray diffraction analysis (XRD) figure of the glass-ceramic of embodiment 3 preparations.
Fig. 6 is the micro-structure diagram of the glass-ceramic of embodiment 3 preparations.
Fig. 7 is X-ray diffraction analysis (XRD) figure of the glass-ceramic of embodiment 4 preparations.
Fig. 8 is the micro-structure diagram of the glass-ceramic of embodiment 4 preparations.
Fig. 9 is for utilizing the dental all-ceramics dummy figure of the glass-ceramic making of implementing 1 preparation.
Embodiment
Embodiment 1:
Take by weighing according to mass ratio: 58% SiO
2, 29% Li
2CO
3, 3.7% K
2CO
3, 2.8% Al
2O
3, 2.4% ZrO
2, 1.5% CeO
2And 2.6% P
2O
5It is for subsequent use to amount to the 500g batching.
Above-mentioned batching is mixed rear ball milling 8h, put into baking oven after mixing, 80 ℃ of oven dry 24h get mixed powder.
Quartz crucible places the resistance furnace preheating, mixed powder is poured in the quartz crucible of preheating, is warming up to 1480 ℃ with 10 ℃/min speed, found 2h for 1480 ℃ in the program-controlled resistor stove, then resulting molten slurry is poured into rapidly in the deionized water, cold quenching obtains glass particle.
The glass particle that obtains is placed agate jar ball milling 12h, and drying gets glass powder; With the glass powder prefabricated flask of packing into, carry out isostatic cool pressing and process, pressure 250MPa forms base substrate.Above-mentioned base substrate is carried out crystallization and thermal treatment, begin to be warming up to 700 ℃ from room temperature, 10 ℃/min of temperature rise rate, 700 ℃ of degree insulations were warming up to 900 ℃ after 5 hours, were incubated after 5 hours, and furnace cooling is namely finished the preparation of glass-ceramic.
Simulation dental prosthesis making processes, use dentistry hot pressing casting machine above-mentioned glass-ceramic is carried out hot pressing casting (950 ℃ of hot pressing temperatures, die casting pressure 4bar, die casting time 5min, soaking time 15min) test specimen is respectively tested in making, and each test specimen is carried out crystalline phase composition, three-point bending strength and semipermeability analysis.
The result shows that the principal crystalline phase of glass-ceramic is two lithium silicate (Li
2Si
2O
5), contain in addition a small amount of lithium metasilicate (Li
2SiO
3) and Trilithium phosphate (Li
3PO
4).Three-point bending strength is 308MPa, satisfies dental material ISO required standard, and semipermeability TP value is 20.61.
Take by weighing according to mass ratio: 59% SiO
2, 28.2% Li
2CO
3, 3.7% K
2CO
3, 2.7% Al
2O
3, 2.3% ZrO
2, 1.6% CeO
2, 2.5% P
2O
5It is for subsequent use to amount to the 500g batching.
Above-mentioned batching is mixed rear ball milling 8h, put into baking oven after mixing, 80 ℃ of oven dry 24h get mixed powder.
Quartz crucible places the resistance furnace preheating, mixed powder is poured in the quartz crucible of preheating, is warming up to 1500 ℃ with 10 ℃/min speed, found 1.5h for 1500 ℃ in the program-controlled resistor stove, then resulting molten slurry is poured into rapidly in the deionized water, cold quenching obtains glass particle.
The glass particle that obtains is placed agate jar ball milling 12h, and drying gets glass powder; With the glass powder prefabricated flask of packing into, carry out isostatic cool pressing and process, pressure 250MPa forms base substrate.Above-mentioned base substrate is carried out crystallization and thermal treatment, begin to be warming up to 700 ℃ from room temperature, 10 ℃/min of temperature rise rate, 700 ℃ of degree insulations were warming up to 900 ℃ after 5 hours, were incubated after 5 hours, and furnace cooling is namely finished the preparation of glass-ceramic.
Simulation dental prosthesis making processes, use dentistry hot pressing casting machine above-mentioned glass-ceramic is carried out hot pressing casting (950 ℃ of hot pressing temperatures, die casting pressure 4bar, die casting time 5min, soaking time 15min) test specimen is respectively tested in making, and each test specimen is carried out crystalline phase composition, three-point bending strength and semipermeability analysis.
The result shows that the principal crystalline phase of glass-ceramic is two lithium silicate (Li
2Si
2O
5), contain in addition a small amount of lithium metasilicate (Li
2SiO
3) and Trilithium phosphate (Li
3PO
4).Three-point bending strength is 297MPa, satisfies dental material ISO required standard, and semipermeability TP value (Translucency parameter) is 20.82.
Embodiment 3:
Take by weighing according to mass ratio: 58% SiO
2, 29% Li
2CO
3, 3.8% K
2CO
3, 2.7% AL
2O
3, 2.4% ZrO
2, 1.5% CeO
2, 2.6% P
2O
5It is for subsequent use to amount to the 500g batching.
Above-mentioned batching is mixed rear ball milling 8h, put into baking oven after mixing, 80 ℃ of oven dry 24h get mixed powder.
Quartz crucible places the resistance furnace preheating, mixed powder is poured in the quartz crucible of preheating, is warming up to 1450 ℃ with 10 ℃/min speed, found 2h for 1450 ℃ in the program-controlled resistor stove, then resulting molten slurry is poured into rapidly in the deionized water, cold quenching obtains glass particle.
The glass particle that obtains is placed agate jar ball milling 12h, and drying gets glass powder; With the glass powder prefabricated flask of packing into, carry out isostatic cool pressing and process, pressure 250MPa forms base substrate.Above-mentioned base substrate is carried out crystallization and thermal treatment, begin to be warming up to 700 ℃ from room temperature, 10 ℃/min of temperature rise rate, 700 ℃ of degree insulations were warming up to 900 ℃ after 5 hours, were incubated after 5 hours, and furnace cooling is namely finished the preparation of glass-ceramic.
Simulation dental prosthesis making processes, use dentistry hot pressing casting machine above-mentioned glass-ceramic is carried out hot pressing casting (950 ℃ of hot pressing temperatures, die casting pressure 4bar, die casting time 5min, soaking time 15min) test specimen is respectively tested in making, and each test specimen is carried out crystalline phase composition, three-point bending strength and semipermeability analysis.
The result shows that the principal crystalline phase of glass-ceramic is two lithium silicate (Li
2Si
2O
5), contain in addition a small amount of lithium metasilicate (Li
2SiO
3) and Trilithium phosphate (Li
3PO
4).Three-point bending strength is 301MPa, satisfies dental material ISO required standard, and semipermeability TP value (Translucency parameter) is 20.75.
Embodiment 4:
Take by weighing according to mass ratio: 57% SiO
2, 30% Li
2CO
3, 3.7% K
2CO
3, 2.8% AL
2O
3, 2.4% ZrO
2, 1.5% CeO
2, 2.6% P
2O
5It is for subsequent use to amount to the 500g batching.
Above-mentioned batching is mixed rear ball milling 8h, put into baking oven after mixing, 80 ℃ of oven dry 24h get mixed powder.
Quartz crucible places the resistance furnace preheating, mixed powder is poured in the quartz crucible of preheating, is warming up to 1400 ℃ with 10 ℃/min speed, found 2h for 1400 ℃ in the program-controlled resistor stove, then resulting molten slurry is poured into rapidly in the deionized water, cold quenching obtains glass particle.
The glass particle that obtains is placed agate jar ball milling 12h, and drying gets glass powder; With the glass powder prefabricated flask of packing into, carry out isostatic cool pressing and process, pressure 250MPa forms base substrate.Above-mentioned base substrate is carried out crystallization and thermal treatment, begin to be warming up to 700 ℃ from room temperature, 10 ℃/min of temperature rise rate, 700 ℃ of degree insulations were warming up to 900 ℃ after 5 hours, were incubated after 5 hours, and furnace cooling is namely finished the preparation of glass-ceramic.
Simulation dental prosthesis making processes, use dentistry hot pressing casting machine above-mentioned glass-ceramic is carried out hot pressing casting (950 ℃ of hot pressing temperatures, die casting pressure 4bar, die casting time 5min, soaking time 15min) test specimen is respectively tested in making, and each test specimen is carried out crystalline phase composition, three-point bending strength and semipermeability analysis.
The result shows that the principal crystalline phase of glass-ceramic is two lithium silicate (Li
2Si
2O
5), contain in addition a small amount of lithium metasilicate (Li
2SiO
3) and Trilithium phosphate (Li
3PO
4).Three-point bending strength is 311MPa, and semipermeability TP value (Translucency parameter) is 20.64.
Although below by reference to the accompanying drawings embodiment of the present invention are described, the present invention is not limited to above-mentioned specific embodiments, and above-mentioned specific embodiments only is schematic, guiding, rather than restrictive.Those of ordinary skill in the art in the situation that does not break away from the scope that claim of the present invention protects, can also make a variety of forms under the enlightenment of this specification sheets, these all belong to the row of the present invention's protection.
Claims (5)
1. a glass-ceramic that is used for making dental prosthesis is characterized in that, comprises the component of following mass percent: 56～59% SiO
2, 28～30% Li
2CO
3, 3.7～4.0% K
2CO
3, 2.7～3.0% Al
2O
3, 2.3～2.4% ZrO
2, 1.5～1.6% CeO
2, and 2.5～3.0% P
2O
5
2. the glass-ceramic for making dental prosthesis according to claim 1 is characterized in that, comprises the component of following mass percent: 58% SiO
2, 29% Li
2CO
3, 3.7% K
2CO
3, 2.8% Al
2O
3, 2.4% ZrO
2, 1.5% CeO
2, 2.6% P
2O
5
3. the preparation method of the glass-ceramic for making dental prosthesis according to claim 1 and 2 is characterized in that, may further comprise the steps: take by weighing each component according to mass percent, with each component mixing ball milling, mix post-drying, get mixed powder; Mixed powder is poured in the quartz crucible again, founded 1.5～2h for 1400～1500 ℃, then, will melt slurry and pour in the deionized water, cold quenching obtains glass particle; Glass particle is placed agate jar, ball milling, drying gets glass powder; The cold isostatic compaction in the prefabricated flask of then glass powder being packed into gets the glass powder base substrate; At last the glass powder base substrate is carried out the two-part crystallization and thermal treatment, get final product.
4. the preparation method of the glass-ceramic for making dental prosthesis according to claim 3 is characterized in that described two-part crystallization and thermal treatment is 700 ℃/5h and 900 ℃/5h.
5. the glass-ceramic of claim 3 preparation is for the preparation of the method for dental prosthesis, it is characterized in that, use dentistry hot pressing casting machine described glass-ceramic is carried out the hot pressing casting, wherein: hot pressing temperature 900-1000 ℃, die casting pressure 3.5-4.5bar, die casting time 4-6min, soaking time 12-18min.
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|---|---|---|---|
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553339A (en) * | 2013-09-30 | 2014-02-05 | 西安交通大学 | Lithium disilicate microcrystalline glass material prepared by using hybrid reaction sintering method and method |
| CN104909571A (en) * | 2015-05-14 | 2015-09-16 | 西安交通大学 | Preparation method for dental lithium silicate microcrystalline glass |
| CN105731807A (en) * | 2016-02-01 | 2016-07-06 | 中国人民解放军第四军医大学 | Method for preparing dental restoration material lithium disilicate glass ceramic by means of adhesive |
| CN108751721A (en) * | 2018-06-15 | 2018-11-06 | 中国人民解放军第四军医大学 | A kind of lithium bisilicate glass ceramics and its preparation method and application for dental zirconium oxide surface decorations porcelain |
| CN113060937A (en) * | 2021-04-08 | 2021-07-02 | 辽宁西纳瓦口腔瓷块科技有限公司 | Lithium metasilicate microcrystalline glass and preparation method and application thereof |
| CN114728838A (en) * | 2020-08-21 | 2022-07-08 | Ａｇｃ株式会社 | Chemically strengthened glass and glass ceramics, and methods for producing them |
| CN115531605A (en) * | 2022-10-28 | 2022-12-30 | 深圳玉汝成口腔材料有限公司 | Dental glass ceramic restoration and preparation method thereof |
| CN116265410A (en) * | 2022-01-20 | 2023-06-20 | 洛阳北苑新材料技术有限公司 | Preparation method of glass ceramic with gradually changed transmittance and color |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553339A (en) * | 2013-09-30 | 2014-02-05 | 西安交通大学 | Lithium disilicate microcrystalline glass material prepared by using hybrid reaction sintering method and method |
| CN103553339B (en) * | 2013-09-30 | 2015-08-05 | 西安交通大学 | Lithium bisilicate microcrystal glass material prepared by hybrid reaction sintering process and method thereof |
| CN104909571A (en) * | 2015-05-14 | 2015-09-16 | 西安交通大学 | Preparation method for dental lithium silicate microcrystalline glass |
| CN105731807A (en) * | 2016-02-01 | 2016-07-06 | 中国人民解放军第四军医大学 | Method for preparing dental restoration material lithium disilicate glass ceramic by means of adhesive |
| CN108751721A (en) * | 2018-06-15 | 2018-11-06 | 中国人民解放军第四军医大学 | A kind of lithium bisilicate glass ceramics and its preparation method and application for dental zirconium oxide surface decorations porcelain |
| CN114728838A (en) * | 2020-08-21 | 2022-07-08 | Ａｇｃ株式会社 | Chemically strengthened glass and glass ceramics, and methods for producing them |
| CN113060937A (en) * | 2021-04-08 | 2021-07-02 | 辽宁西纳瓦口腔瓷块科技有限公司 | Lithium metasilicate microcrystalline glass and preparation method and application thereof |
| CN116265410A (en) * | 2022-01-20 | 2023-06-20 | 洛阳北苑新材料技术有限公司 | Preparation method of glass ceramic with gradually changed transmittance and color |
| CN115531605A (en) * | 2022-10-28 | 2022-12-30 | 深圳玉汝成口腔材料有限公司 | Dental glass ceramic restoration and preparation method thereof |
| CN115531605B (en) * | 2022-10-28 | 2023-09-12 | 深圳玉汝成口腔材料有限公司 | Dental glass ceramic prosthesis and preparation method thereof |
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Application publication date: 20130417 |
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