CN103951191A - Teeth microcrystalline glass compounded of two clinkers and having yellow/white gradient change - Google Patents
Teeth microcrystalline glass compounded of two clinkers and having yellow/white gradient change Download PDFInfo
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- CN103951191A CN103951191A CN201410179282.6A CN201410179282A CN103951191A CN 103951191 A CN103951191 A CN 103951191A CN 201410179282 A CN201410179282 A CN 201410179282A CN 103951191 A CN103951191 A CN 103951191A
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Abstract
The invention discloses teeth microcrystalline glass compounded of two clinkers and having yellow/white gradient change. The teeth microcrystalline glass is prepared by the following processes: firstly, preparing two clinkers of yellow and white colors, and then mixing the white microcrystalline glass clinker with the yellow microcrystalline glass clinker according to a certain ratio; distributing materials according to the requirements; sintering and crystallizing; cooling, trimming, polishing and molding. The degree of yellow color in the appearance of the prepared microcrystalline glass can be changed and regulated according to different material distribution modes, so as to adjust the color and luster of a false tooth. Thus, the color and luster requirements of different teeth can be met.
Description
Technical field
The present invention relates to medically in the devitrified glass of tooth, is specifically the tooth devitrified glass that between a kind of Huang/white, color gradient changes.
Background technology
Devitrified glass has good physical strength, chemical stability, biocompatibility as teeth repairing material, the more and more important effect of performance in clinical medicine.
< < Liaoning University journal (natural science edition) > > periodical third phase Yang Donghui in 2006 discloses the application > > article of a kind of < < devitrified glass on teeth repairing material, its conclusion is: tooth devitrified glass repair materials is started late in China, but it has become one of problem of a joint development in materialogy and medical circle, believe that it can become the preferred material of people on tooth is repaired in the near future.The journal > > of < < Shaanxi Tech Univ periodical the 6th summer phase in 2004, proud, seedling swan goose, Li Yongqiang disclosed the technical study > > article of the toughness reinforcing bio-microcrystal glass material of a kind of < < dental Y-TZP, its conclusion is: prepared devitrified glass has the character such as the strong and chemical stability of the Hao ﹑ density of coking property Gao ﹑ wear resistance is good, substantially meets the performance requriements of biomaterial.Therefore, devitrified glass is feasible as teeth repairing material technically.
But the color and luster of tooth devitrified glass is difficult to meet the requirement of natural tooth at present.After some patients grow permanent teeth, former tooth and artificial tooth color have larger difference, affect attractive in appearance.According to the color and luster of patient's tooth, prepare the devitrified glass that between a kind of Huang/white, color gradient changes, make it meet the color and luster requirement of different teeth.
China Patent Publication No. CN102098979A discloses a kind of formed body of being made by form stable formed material, described material comprises at least one first component and a second component, and second component has different from described the first component painted, and described second component is arranged on the inside of described the first component, form interface, make described interface be presented on curved surface in space; The first component and second component are by dense sintering or porous sintered stupalith or plastic material formed body.The first component and second component formed body in conjunction with time, first with machinery firmly or with binding agent by polycomponent compacting or be bonded to one, 700-800 ℃ by after binder removal at 1200 ℃ of sintering.Due to formed body be by the intermediate molded object of a plurality of different colours first suppress or be bonded to one, then sintering forms, make this technology have following defect: the one, when as dental prosthesis material, because everyone color of teeth is different, even if also there is color distortion in the tooth of same person, this just causes need to preparing the intermediate molded object of not fixing a number in advance, then a plurality of formed bodys graded is as required arranged moulding, complex process is what to be difficult to as dental prosthesis material in reality; The 2nd, the interface between each intermediate molded object is a weak link, the poor compatibility of interface bi-material, cause final molding body interface place to have performance gradient change, just as a bowl breaking, by adhesives, to sintering together with make in advance integral body sintering again, the performance of end product is inhomogeneous.
Summary of the invention
In order to overcome existing tooth devitrified glass complicated process of preparation, the product colour preparing is difficult to meet the technological deficiency that the color and luster of different teeth requires, the invention provides a kind of technique simple possible, color and naturally have the tooth devitrified glass that between Huang/white, color gradient changes, the color of this devitrified glass is closer to grownup's natural tooth color and luster.
For achieving the above object, tooth devitrified glass of the present invention is prepared from by following methods:
The first step: preparation white micro-crystals glass frit:
The 1.1st step: accurately take in proportion SiO
255-70 part, CaO15-25 part, Na
2o8-15 part, wherein Na
2o is converted into Na
2cO
3after weigh; Mix and pour in stirrer, stir 1 hour;
The 1.2nd step: the powder raw material stirring is poured in the kiln of 1530-1580 ℃, founded 2-4 hour, shrend, takes out post-drying and form white micro-crystals glass frit;
Second step: prepare yellow glass ceramics frit:
The 2.1st step: accurately take in proportion SiO
240-50 part, Al
2o
31-5 part, CaO8-13 part, BaO1-4 part, MgO1-5 part, B
2o
30.3-2 part, Na
2o+K
2o10-15 part, CaF
20.3-2 part, P
2o
51-5 part, ZnO1-5 part, Sb
2o
30.3-1 part, colorant 1-5 part, wherein BaO, Na
2o+K
2o is converted into BaCO
3, Na
2cO
3+ K
2cO
3after weigh, mix and to pour in stirrer, stir 1 hour;
Described colorant is CeO
2and/or TiO
2;
The 2.2nd step: the powder raw material stirring is poured in the kiln of 1500-1550 ℃, founded 2-4 hour, shrend, takes out post-drying and form yellow glass ceramics frit;
The 3rd step: the devitrified glass that between preparation is yellow/white, color gradient changes
The 3.1st step: white micro-crystals glass frit and yellow glass ceramics frit are crushed to respectively below 200 orders, according to the trend that white micro-crystals glass frit proportion of powder reduces gradually, yellow glass ceramics frit powder increases gradually, weigh respectively, mix, stir, form many group mixed powders, the thickness of every layer of frit powder is 2-10mm;
The 3.2nd step: cloth
On forming mould, first lay one deck white micro-crystals glass frit powder, and then lay successively many group mixed powders in the above; While laying many group mixed powders, according to yellow frit proportion of powder principle from less to more in mixed powder, carry out, finally re-lay the yellow glass ceramics frit powder of one deck, the thickness of every layer of powder is 2-10mm;
The 3.3rd step: sintering
By the mixed frit powder sintering processes in crystallization furnace laying: the temperature rise rate with 2-10 ℃/min rises in 1050-1150 ℃ of temperature range, insulation 1-2 hour;
The 4th step: cooling;
The 5th step: trimming, polishing, carry out forming process.
Above-mentioned umber is weight part.
Requirement; Reflectivity ≮ 50% of the white micro-crystals glass of preparing to all wavelengths visible ray; In yellow devitrified glass, to the optimal absorption scope of visible wavelength, be 430-450nm, best is 570-580nm through scope.
Flexural strength ≮ the 80MPa that utilizes material that the present invention is prepared into test on WDW3100 type electronic universal tester, the Vickers' hardness ≮ 5.80GPa (HV testing on FM-700 type microhardness tester
0.5).Can be medically for teeth repairing material.
Advantage of the present invention is:
Positively effect of the present invention is: 1. the present invention founds an existing proportioning and the once sintered method of preparing heterogeneous devitrified glass, make into two kinds of frits respectively proportioning found and be mixed in proportion sintering, make the sintering crystallization treatment temp of two kinds of frits interval consistent, the compatibility while having guaranteed two kinds of frit sintering; If 2. the present invention need to change the color of material, without again founding under Huang, white dichromatism glass ceramics frit prerequisite, by changing the blending ratio of two kinds of frits in mixed powder, just can prepare the tooth devitrified glass of the color that meets the requirements.3. the present invention can be by adjusting the blending ratio of frit composition proportion or two kinds of frit powder of change, can prepare the devitrified glass close to different crowd color of teeth, the factor that preparation technology is pind down is little, and process controllability and strong operability are convenient to promote the use of.4. the present invention is pulverized and mixed the mixed frit of different proportionings, then lays sintering according to the variation tendency of people's color of teeth, and the material property preparing is stablized, and intensity is high, color nature.
Accompanying drawing explanation
Fig. 1 is the microstructure picture of the crystallite glass of example one formula of the present invention.
Embodiment
Take below several different devitrified glasses as example further illustrates technical scheme of the present invention
Embodiment mono-
White micro-crystals glass frit is founded and is formed by the raw material of following weight part: SiO
267.5 parts, CaO20 part, Na
2o12.5 part;
Yellow glass ceramics frit is founded and is formed by the raw material of following weight part: SiO
246 parts, Al
2o
33.3 parts, CaO13 part, BaO2 part, MgO3.6 part, B
2o
32 parts, Na
2o+K
2o13 part, CaF
20.6 part, P
2o
54.5 parts, ZnO3 part, Sb
2o
31 part, CeO
21 part, TiO
20.5 part.
Preparation method is as follows:
The first step: preparation white micro-crystals glass frit
1. by above-mentioned weight part, take white frit raw material, mix and pour in stirrer, stir 1 hour; 2. pour in the kiln of 1570 ℃, found 2 hours, shrend, dries, and forms white micro-crystals glass frit;
Second step: prepare yellow glass ceramics frit
1. by above-mentioned weight part, take yellow frit raw material, mix and pour in stirrer, stir 1 hour; 2. pour in the kiln of 1550 ℃, found 2 hours, shrend, dries and forms yellow glass ceramics frit;
The 3rd step: the devitrified glass that between preparation is yellow/white, color gradient changes
(1) white micro-crystals glass frit and yellow glass ceramics frit are crushed to respectively below 200 orders, according to the ratio of 7: 3,5: 5,3: 7, weigh respectively, mix, stir, form three groups of mixed frit powder;
(2) cloth: first lay white micro-crystals glass frit powder on forming mould, and then thereon according to yellow powder ratio principle from less to more in mixed frit powder, lay respectively and mix frit powder end, finally re-lay yellow glass ceramics frit powder, every layer of frit powder thickness is 6mm; That is to say: from the bottom up, be followed successively by white micro-crystals glass frit powder, 7: 3 mixed frit powder, 5: 5 mixed frit powder, 3: 7 mixed frit powder and yellow glass ceramics frit powder,
(3) sintering processes in crystallization furnace: the temperature rise rate with 5 ℃/min rises in 1110 ℃ of temperature ranges, is incubated 1.5 hours;
The 4th step: cooling;
The 5th step: trimming, polishing, carry out forming process, the appearance color of prepared devitrified glass is by presenting graded to Huang in vain.Reflectivity ≮ 50% of the white micro-crystals glass that wherein white praducing frits goes out to all wavelengths visible ray; In the yellow devitrified glass that yellow praducing frits goes out to visible wavelength to see through scope be 580-590nm, CeO in change colorant
2, TiO
2ratio, the scope that sees through of this wavelength changes thereupon, corresponding yellow degree also changes for it.
By the flexural strength of testing on WDW3100 type electronic universal tester in prepared devitrified glass, be 93.1MPa, the Vickers' hardness of testing on FM-700 type microhardness tester is 6.14GPa (HV
0.5), can be medically for teeth repairing material, Fig. 1 is shown in by the microstructure picture of the devitrified glass of preparation.
Microstructure picture from Fig. 1 can be found out: in devitrified glass of the present invention, have two kinds of crystal of A and B, the A crystal crystalline phase that white frit is introduced of serving as reasons wherein, the B crystal crystalline phase that yellow frit is introduced of serving as reasons; After two kinds of frits mix, separate out two kinds of crystal, wherein A, B crystalline phase and glass basis merge mutually, compatible good, pore-free, dense structure.
Embodiment bis-, change blending ratio
The preparation method of embodiment 2 and embodiment 1 are basic identical, different, and the ratio that white micro-crystals glass frit and yellow frit mix is mutually respectively 6: 4,5: 5,4: 6.Reflectivity ≮ 50% of the white micro-crystals glass that white micro-crystals glass frit is prepared to all wavelengths visible ray; In the yellow devitrified glass that yellow glass ceramics frit is prepared, to the optimal absorption scope of visible wavelength, be 430-450nm, best is 570-580nm through scope.
The appearance color of prepared devitrified glass is by presenting graded to Huang in vain.
By the flexural strength of testing on WDW3100 type electronic universal tester in prepared devitrified glass, be 91.9MPa, the Vickers' hardness of testing on FM-700 type microhardness tester is 6.21GPa (HV
0.5), basically identical with the performance of example one.Can be medically for teeth repairing material.
Embodiment tri-, change blending ratio and fabric thickness is prepared devitrified glass simultaneously
The preparation method of embodiment 3 and embodiment 1 are basic identical, different is, the ratio that white micro-crystals glass frit and yellow glass ceramics frit mix is mutually respectively 8: 2,6: 4,5: 5,4: 6,2: 8, and the thickness that white micro-crystals glass frit powder, yellow glass ceramics frit powder, each mixed microcrystalline glass frit powder are laid is 4mm.Reflectivity ≮ 50% of the white micro-crystals glass that white praducing frits goes out to all wavelengths visible ray; In the yellow devitrified glass that yellow praducing frits goes out, to the optimal absorption scope of visible wavelength, be 430-450nm, best is 570-580nm through scope.
The appearance color of prepared devitrified glass is by presenting graded to Huang in vain, and the variation of gradient color is milder.
By the flexural strength of testing on WDW3100 type electronic universal tester in prepared devitrified glass, be 94.7MPa, the Vickers' hardness of testing on FM-700 type microhardness tester is 6.16GPa (HV
0.5), can be medically for teeth repairing material.
From above-mentioned three embodiment, can find out: no matter the present invention is by changing the proportioning of each component two kinds of glass ceramics frits, or the ratio of mutually mixing by changing white micro-crystals glass frit and yellow frit, or change blending ratio and fabric thickness simultaneously, the devitrified glass performance preparing does not have great change, it is little that this has also confirmed the factor that preparation technology of the present invention pind down, process controllability and strong operability, be convenient to promote the use of.
Umber in embodiment is weight part.
Claims (2)
1. the tooth devitrified glass that between the compound Huang of two kinds of frits/white, color gradient changes, is characterized in that, it is prepared from by following methods:
The first step: preparation white micro-crystals glass frit:
The 1.1st step: accurately take in proportion SiO
255-70 part, CaO15-25 part, Na
2o8-15 part, wherein Na
2o is converted into Na
2cO
3after weigh; Mix and pour in stirrer, stir 1 hour;
The 1.2nd step: the powder raw material stirring is poured in the kiln of 1530-1580 ℃, founded 2-4 hour, shrend, takes out post-drying and form white micro-crystals glass frit;
Second step: prepare yellow glass ceramics frit:
The 2.1st step: accurately take in proportion SiO
240-50 part, Al
2o
31-5 part, CaO8-13 part, BaO1-4 part, MgO1-5 part, B
2o
30.3-2 part, Na
2o+K
2o10-15 part, CaF
20.3-2 part, P
2o
51-5 part, ZnO1-5 part, Sb
2o
30.3-1 part, colorant 1-5 part, wherein BaO, Na
2o+K
2o is converted into BaCO
3, Na
2cO
3+ K
2cO
3after weigh, mix and to pour in stirrer, stir 1 hour;
Described colorant is CeO
2and/or TiO
2;
The 2.2nd step: the powder raw material stirring is poured in the kiln of 1500-1550 ℃, founded 2-4 hour, shrend, takes out post-drying and form yellow glass ceramics frit;
The 3rd step: the devitrified glass that between preparation is yellow/white, color gradient changes
The 3.1st step: white micro-crystals glass frit and yellow glass ceramics frit are crushed to respectively below 200 orders, according to the trend that white micro-crystals glass frit proportion of powder reduces gradually, yellow glass ceramics frit powder increases gradually, weigh respectively, mix, stir, form many group mixed powders, the thickness of every layer of frit powder is 2-10mm;
The 3.2nd step: cloth
On forming mould, first lay one deck white micro-crystals glass frit powder, and then lay successively many group mixed powders in the above; While laying many group mixed powders, according to yellow frit proportion of powder principle from less to more in mixed powder, carry out, finally re-lay the yellow glass ceramics frit powder of one deck, the thickness of every layer of powder is 2-10mm;
The 3.3rd step: sintering
By the mixed frit powder sintering processes in crystallization furnace laying: the temperature rise rate with 2-10 ℃/min rises in 1050-1150 ℃ of temperature range, insulation 1-2 hour;
The 4th step: cooling;
The 5th step: trimming, polishing, carry out forming process;
Above-mentioned umber is weight part.
2. a method of preparing the tooth devitrified glass that between the compound Huang of two kinds of frits/white, color gradient changes, is characterized in that, method is as follows:
The first step: preparation white micro-crystals glass frit:
The 1.1st step: accurately take in proportion SiO
255-70 part, CaO15-25 part, Na
2o8-15 part, wherein Na
2o is converted into Na
2cO
3after weigh; Mix and pour in stirrer, stir 1 hour;
The 1.2nd step: the powder raw material stirring is poured in the kiln of 1530-1580 ℃, founded 2-4 hour, shrend, takes out post-drying and form white micro-crystals glass frit;
Second step: prepare yellow glass ceramics frit:
The 2.1st step: accurately take in proportion SiO
240-50 part, Al
2o
31-5 part, CaO8-13 part, BaO1-4 part, MgO1-5 part, B
2o
30.3-2 part, Na
2o+K
2o10-15 part, CaF
20.3-2 part, P
2o
51-5 part, ZnO1-5 part, Sb
2o
30.3-1 part, colorant 1-5 part, wherein BaO, Na
2o+K
2o is converted into BaCO
3, Na
2cO
3+ K
2cO
3after weigh, mix and to pour in stirrer, stir 1 hour;
Described colorant is CeO
2and/or TiO
2;
The 2.2nd step: the powder raw material stirring is poured in the kiln of 1500-1550 ℃, founded 2-4 hour, shrend, takes out post-drying and form yellow glass ceramics frit;
The 3rd step: the devitrified glass that between preparation is yellow/white, color gradient changes
The 3.1st step: white micro-crystals glass frit and yellow glass ceramics frit are crushed to respectively below 200 orders, according to the trend that white micro-crystals glass frit proportion of powder reduces gradually, yellow glass ceramics frit powder increases gradually, weigh respectively, mix, stir, form many group mixed powders, the thickness of every layer of frit powder is 2-10mm;
The 3.2nd step: cloth
On forming mould, first lay one deck white micro-crystals glass frit powder, and then lay successively many group mixed powders in the above; While laying many group mixed powders, according to yellow frit proportion of powder principle from less to more in mixed powder, carry out, finally re-lay the yellow glass ceramics frit powder of one deck, the thickness of every layer of powder is 2-10mm;
The 3.3rd step: sintering
By the mixed frit powder sintering processes in crystallization furnace laying: the temperature rise rate with 2-10 ℃/min rises in 1050-1150 ℃ of temperature range, insulation 1-2 hour;
The 4th step: cooling;
The 5th step: trimming, polishing, carry out forming process;
Above-mentioned umber is weight part.
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CN201410179282.6A CN103951191B (en) | 2014-04-29 | 2014-04-29 | The tooth devitrified glass of color gradient change between the Huang of two kinds of frit compounds/white |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112408800A (en) * | 2020-11-25 | 2021-02-26 | 江西璞晶新材料股份有限公司 | Method for preparing marble-like colored microcrystalline glass by using ceramic pigment |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1349944A (en) * | 2001-12-18 | 2002-05-22 | 清华大学 | Tinct adjustable stomatic bioactive divitrified glass and its prepn |
US20080044488A1 (en) * | 2004-05-29 | 2008-02-21 | Jose Zimmer | Nano Glass Powder and Use Thereof, in Particular Multicomponent Glass Powder with a Mean Particle Size of Less Than 1 µm |
CN103429546A (en) * | 2010-12-17 | 2013-12-04 | 义获嘉伟瓦登特公司 | Production of shaped dental parts composed of porous glass |
-
2014
- 2014-04-29 CN CN201410179282.6A patent/CN103951191B/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1349944A (en) * | 2001-12-18 | 2002-05-22 | 清华大学 | Tinct adjustable stomatic bioactive divitrified glass and its prepn |
US20080044488A1 (en) * | 2004-05-29 | 2008-02-21 | Jose Zimmer | Nano Glass Powder and Use Thereof, in Particular Multicomponent Glass Powder with a Mean Particle Size of Less Than 1 µm |
CN103429546A (en) * | 2010-12-17 | 2013-12-04 | 义获嘉伟瓦登特公司 | Production of shaped dental parts composed of porous glass |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112408800A (en) * | 2020-11-25 | 2021-02-26 | 江西璞晶新材料股份有限公司 | Method for preparing marble-like colored microcrystalline glass by using ceramic pigment |
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