CN100370963C - Zirconium oxide full-porcelain dental repair material and its preparing method - Google Patents
Zirconium oxide full-porcelain dental repair material and its preparing method Download PDFInfo
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Abstract
The present invention relates to a zirconia full-ceramic dental repairing material and a preparation method thereof, which belongs to the fields of ceramic materials and the preparation thereof. The zirconia full-ceramic dental repairing material is prepared from 86 to 92 wt% of stable tetragonal-phase zirconia with 3.0 to 5.15 wt% of yttrium oxide, 5 to 10 wt% of fluxing agent and 3 to 4 wt% of agglomerant. The fluxing agent is one or more of substances such as boron-aluminum-silicon system glass, hydroxyapatite and beta-wollastonite. The agglomerant is one or more of substances such as polyvinyl alcohol, carboxymethyl cellulose and a polyacrylic acid. In the preparation method, the zirconia full-ceramic dental repairing material is prepared by mixture, granulation, cold isostatic compaction, plastic removal and agglomeration. Compared with the prior art, the zirconia full-ceramic dental repairing material has the advantages of low preparation process cost, high finished size precision, good repetitiveness, stable quality and superior mechanical synthesis property.
Description
Technical field
The invention belongs to ceramic material and preparing technical field thereof, particularly a kind of Zirconium Oxide Whole Porcelain Dentistry Repairment Material and Its Preparation Method.
Background technology
In present dentistry is clinical, repair ceramic material commonly used and mainly contain metal porcelain tooth and full porcelain tooth.
Because metal porcelain tooth has metal strength height, sturdy and durable, advantage such as marginal fit good and the porcelain color and luster is attractive in appearance, corrosion resistance good, self-cleaning action is strong concurrently, so be subjected to odontologist and patient's welcome deeply, application is very general in developed country.Yet it is to be solved that gold-porcelain dummy still has many problems to need, as: the cutting of enamel composition is too many, needs metal casting system; The color and luster not attractive in appearance of metal bottom tire appears in the edge of gold-porcelain dummy sometimes, " neck ring " problem occurs, thereby influences the effect of dummy; And base metal also has etching problem and to the hazardness of human body, life-time service may the deleterious element of stripping in the oral cavity for the metals such as Ni-Cr alloy that generally use at present.Even also there is small number of patients problem hypersensitive in noble metal, if in the long-term implant into body, can be from metal material the stripping metal ion, residual unreacted monomer when stripping is made from macromolecular material has certain hazardness to tissue.
And for full porcelain tooth, pottery has superior functions such as excellent biological compatibility and aesthstic performance, physical and chemical performance is stable, bacterial plaque is difficult for adhering to, thermal conductivity is low, color and luster is stable, incomparable advantage is being arranged aspect the artificial dummy in oral cavity being used as.But the inherent fragility of ceramic material has limited its application in the oral cavity material field.Along with the industrial ceramics development of technology, the full porcelain recovery technique of dentistry also is developed, and the various countries scholar develops and released multiple full porcelain repair system.Difference by manufacturing technology can be divided into: conventional powder slurry porcelain, castable ceramic, machinable ceramic, hot pressed ceramics, glass-infiltrated ceramic.Forming branch by material has: alumina porcelain, glass ceramics, the enhanced feldspar porcelain of leucite.The bending strength of the full ceramic material of dentistry is brought up to hundreds of MPas from tens MPas.But still there is the easy jackknifing of dummy in the full ceramic material of clinical practice at present, repairs problems such as excessive, the full porcelain bridging of required tooth preparation amount junctor is excessive, the pontic span is limited, and the mechanical property of the full ceramic material of dentistry still remains further to be improved.
There is report to adopt zirconia ceramics can overcome the problems referred to above.Zirconia ceramics has good optical performance, biocompatibility, has antithrombotic and sterilization property; Stable chemical performance, with people's humoral response, acid-alkali-corrosive-resisting is not strong; Zirconia ceramics is owing to distinctive stress-induced phase transformation toughening effect, and its intensity and toughness all are better than traditional feldspar porcelain and aluminium oxide ceramics, becomes the focus that dental materials circle is paid close attention in recent years, is particularly suitable for making the back corona bridge that mechanical performance is had relatively high expectations.But the tetragonal phase zirconium oxide material of at present domestic prepared stabilized with yttrium oxide also exists dimensional accuracy wayward, the shortcoming that mechanical property is low, for example (1) publication number is CN1489988, open day: the Chinese patent of 2004.04.21: Cheap machinable zirconium oxide ceramic dental repairing body and preparation method thereof, its bending strength of zirconia ceramics of preparation is 340～360MPa, and fracture toughness is 2.7～3.MPam
1/2(2) publication number: CN1489987, open day: the Chinese patent of 2004.04.21: polycrystal zirconia ceramics tooth pile material and preparation method thereof, its bending strength of zirconia ceramics tooth pile material of preparation was 600MPa.
Summary of the invention
It is low to the purpose of this invention is to provide a kind of preparation technology's cost, finished size precision height, good reproducibility, steady quality, the good Zirconium Oxide Whole Porcelain Dentistry Repairment Material and Its Preparation Method of mechanical property.
According to above-mentioned purpose, technical scheme of the present invention is:
In addition flux, the binding agent constituent for preparing raw material as dental prosthetic material of phase transformation toughened zirconia pottery-stabilized with yttrium oxide tetragonal phase zirconium oxide pottery that the present invention adopts mechanical property and chemical-biological function admirable, the method for preparing Zirconium oxide full-porcelain dental repair material simultaneously comprises the steps: mixed pelletize, cold isostatic compaction, plastic removal, sintering.
The composition principle of technique scheme is: zirconium oxide has 3 kinds of allotropy structures, i.e. monocline phase m-ZrO
2, cubic phase t-ZrO
2, cube phase c-ZrO
23 kinds of crystal formations are present in different temperature ranges and also can transform mutually, and the transforming relationship between them is as follows:
At ambient temperature, zirconium oxide is with m-ZrO
2Form exist, but when with t-ZrO after suitable stabilizing agent combines
2Also can be present in room temperature.When material is subjected to external force generation micro-crack, the t-ZrO of crack tip
2Crystal is stress induced following to more stable m-ZrO
2Change mutually, volumetric expansion of following and change of shape change the stress field of crack tip, stop the extension of crackle and make cracks can spread need higher external influence load, zirconic stress-induced phase transformation toughening mechanisms that Here it is.
Tend in the process that ceramic material was adjust and reform in sintering, cooling and later stage produce some small defective and crackles on the inside or the surface of porcelain body, and full porcelain dummy bears continuous change size and Orientation in the oral environment midium or long term load, often cause the continuous expansion of micro-crack, can cause full porcelain repairing failure.Zirconia ceramics is owing to have the stress-induced phase transformation toughening mechanisms, and mechanical property improves greatly.
Because the sintering temperature of zirconia ceramics is higher, generally all wants 1600 ℃, is glass hydroxyapatite and β-wollastonite so we introduce flux-boron aluminum silicon in prescription.Wherein boron aluminum silicon is that glass is low-expansion glass, and its composition is: SiO
279～81wt%, Al
2O
32～4wt%, B
2O
311～13wt%, K
2O 5～7wt%, Na
2O 0.5～2wt%.The introducing of flux guarantees to produce abundant liquid phase at hot stage, and the sintering process of being carried out is liquid-phase sintering, makes sintering be able to carry out under 1250～1400 ℃ condition, has saved a large amount of energy.
Technological principle of the present invention is: adopt the dry zirconium dioxide predecessor of vacuum and low temperature Freeze Drying Technique in the mixing granulation, its effect is to make the water sublimed in the mixture and slough, thereby avoided the reunion of zirconium dioxide predecessor particle in the dry run to greatest extent, obtained the zirconium dioxide predecessor of favorable dispersibility.
Because the crown preparation complex process, to the dimension precision requirement height, therefore, the present invention proposes to adopt the method for isostatic compaction to prepare ceramic corona.This is because the isostatic compaction of pottery has following characteristics:
(1) can be shaped complex-shaped, big part and elongated goods that conventional method can not produce and Forming Quality height;
(2) can not increase operation easier and improve briquetting pressure more easily, and the pressure action effect is better than other dry pressing;
(3) because base substrate is respectively even to being stressed, and its density is high and even, bears less and dwindle, size Control precision height, not yielding;
(4) the ceramic member surface smoothing of molding, outward appearance is good;
(5) Mold Making is convenient, and cost is low;
(6) can be less with or without bonding agent;
(7) forming process mechanization degree height can carry out batch manufacturing, good repetitiveness.
Isostatic compaction has the high advantage of compact density, thereby the density of ceramic product is greater than 6.0/cm behind the assurance sintering
3
It is little that the molding blank sintering shrinks, and total linear shrinkage ratio is 10～15%, is out of shape for a short time, guaranteed the product size precision.
According to above-mentioned purpose and composition, technological principle, the concrete technical scheme of the present invention is:
The preparation raw material chemical composition (weight %) of this material is: contain the tetragonal phase zirconium oxide 86～92% of 3.0～5.15% stabilized with yttrium oxide, flux 5～10%, binding agent 3～4%.
Flux described in the preparation raw material is that boron aluminum silicon is one or more in glass, hydroxyapatite, the β-wollastonite.
Described boron aluminum silicon is that glass is low-expansion glass, and its chemical composition (weight %) is: SiO
279～81%, Al
2O
32～4%, B
2O
311～13%, K
2O 5～7%, Na
2O 0.5～2%.
Binding agent described in the preparation raw material is one or more in polyvinyl alcohol, carboxymethyl cellulose, the polyacrylic acid.
The preparation method of above-mentioned Zirconium oxide full-porcelain dental repair material comprises following concrete steps:
(1), mixed pelletize: the tetragonal phase zirconium oxide powder body, flux, binding agent and an amount of ball-milling additive deionized water that with particle diameter 0.2～0.4 μ m are stabilized with yttrium oxide earlier join in the fire ball grinding machine together, mixed ball milling 15～30min, vacuum and low temperature lyophilization predecessor then, vacuum freeze drier is used in described vacuum and low temperature lyophilization, vacuum is 2～10Pa, temperature obtains the granule of particle diameter 0.5～1 μ m less than-40～-50 ℃.
(2), cold isostatic compaction: the granule of above-mentioned institute expense is packed in the mould, wait the static pressure operation then.Briquetting pressure is 100～200MPa, and the dwell time is 5～20min.
(3), plastic removal: the base substrate that above-mentioned isostatic compaction obtains is put into Muffle furnace, speed with 40～80 ℃/h is warming up to 600～800 ℃, and insulation 1～3h naturally cools to room temperature then, remove the organic binder bond in the base substrate, obtain the biscuit of Zirconium oxide full-porcelain dental repair material.
(4), sintering: the biscuit of the Zirconium oxide full-porcelain dental repair material of above-mentioned defat is placed in the high temperature furnace, speed with 50～150 ℃/h is warming up to sintering temperature, temperature range is 1250～1400 ℃, is incubated 1～3h under this temperature, and the speed with 150～200 ℃/h is cooled to room temperature then.
It is low that the present invention compared with prior art has preparation technology's cost, finished size precision height, good reproducibility, steady quality, the good advantage of mechanical property.The comprehensive mechanical property of prepared Zirconium oxide full-porcelain dental repair material is good: bending strength 1000～1300MPa, fracture toughness is up to 15MPam
1/2, elastic modelling quantity 130～150MPa, Vickers hardness 1250～1400MPa.
Description of drawings
Accompanying drawing 1 is the quiet photo of scanning electricity * 7200 of the prepared biscuit fracture of the invention process example.Accompanying drawing 2 is the quiet photo of scanning electricity * 7200 of the prepared sintered body fracture of the invention process example.
The specific embodiment
The chemical composition of the used preparation raw material of Zirconium oxide full-porcelain dental repair material adopts preparation method of the present invention according to the present invention, has prepared 7 batches of Zirconium oxide full-porcelain dental repair materials.Wherein, table 1 is the chemical composition table of the used preparation raw material of Zirconium oxide full-porcelain dental repair material of the present invention, table 2 is the processing step and the process parameter table of Zirconium oxide full-porcelain dental repair material preparation method of the present invention, and table 3 is compared with the prior art routine performance comparison table for Zirconium oxide full-porcelain dental repair material embodiment of the present invention.Wherein, sequence number 1-7# is the embodiment of the invention, 8-9# is the prior art Comparative Examples, being respectively (1) publication number is ℃ N1489988, open day: the Chinese patent of 2004.04.21: Cheap machinable zirconium oxide ceramic dental repairing body and preparation method thereof, (2) publication number: CN1489987, open day: the Chinese patent of 2004.04.21: polycrystal zirconia ceramics tooth pile material and preparation method thereof.
Table 1 is the chemical composition table (weight %) of the used preparation raw material of Zirconium oxide full-porcelain dental repair material of the present invention
| Sequence number | Mean diameter μ m | The tetragonal phase zirconium oxide of stabilized with yttrium oxide | Flux | Binding agent | ||||||||||
| Yittrium oxide % | Zirconium oxide % | Boron aluminum silicon is glass % | SiO 2 | Al 2O 3 | B 2O 3 | K 2O | Na 2O | Hydroxyapatite % | β-wollastonite % | Polyvinyl alcohol % | Carboxymethyl cellulose % | Polypropylene % | ||
| 1 | 0.3 | 3.00 | 40+51 | 2 | 79 | 3 | 11 | 5 | 2 | 4 | 3 | |||
| 2 | 0.2 | 4.15 | 40+48 | 4 | 80 | 2 | 12 | 5 | 1 | 4 | 4 | |||
| 3 | 0.4 | 5.15 | 40+46 | 5 | 5 | 2 | 2 | |||||||
| 4 | 0.4 | 5.15 | 40+52 | 5 | 79 | 2 | 13 | 5.5 | 0.5 | 3 | ||||
| 5 | 0.3 | 3.00 | 40+47 | 10 | 1 | 1 | 1 | |||||||
| 6 | 0.2 | 4.15 | 40+49 | 8 | 1 | 2 | ||||||||
| 7 | 0.4 | 4.15 | 40+50 | 2 | 80 | 3 | 11 | 5 | 1 | 2 | 2 | 2 | 2 | |
Table 2 is the processing step and the process parameter table of Zirconium oxide full-porcelain dental repair material preparation method of the present invention
| Sequence number | Mixing granulation | Cold isostatic compaction | Plastic removal | Sintering | |||||||||
| Ball milling time min | Vacuum Pa | Temperature ℃ | Footpath μ m | Briquetting pressure MPa | Dwell time min | Programming rate ℃/h | Intensification temperature ℃ | Temperature retention time h | Programming rate ℃/h | Intensification degree temperature ℃ | Temperature retention time h | Cooling rate ℃/h | |
| 1 | 15 | 2 | -40 | 0.5 | 200 | 5 | 40 | 600 | 3 | 50 | 1250 | 3 | 200 |
| 2 | 20 | 5 | -45 | 0.8 | 160 | 10 | 50 | 700 | 2 | 100 | 1350 | 2 | 175 |
| 3 | 30 | 10 | -50 | 1 | 100 | 20 | 80 | 800 | 1 | 150 | 1400 | 1 | 150 |
| 4 | 25 | 8 | -46 | 0.5 | 150 | 10 | 70 | 800 | 1 | 150 | 1400 | 2 | 200 |
| 5 | 15 | 9 | -48 | 0.7 | 170 | 10 | 80 | 700 | 2 | 100 | 1300 | 1 | 170 |
| 6 | 20 | 7 | -40 | 0.8 | 120 | 20 | 40 | 750 | 2 | 120 | 1250 | 1.5 | 180 |
| 7 | 30 | 6 | -50 | 0.6 | 150 | 10 | 50 | 650 | 1 | 80 | 1400 | 1.5 | 160 |
Table 3 is compared with the prior art routine performance comparison table for Zirconium oxide full-porcelain dental repair material embodiment of the present invention
| Sequence number | Rupture strength MPa | Fracture toughness MPam 0.5 | Elastic modelling quantity MPa | Vickers hardness MPa |
| 1 | 1120 | 13.1 | 134 | 1324 |
| 2 | 1184 | 14.4 | 145 | 1380 |
| 3 | 1323 | 13.5 | 137 | 1354 |
| 4 | 1003 | 11.7 | 130 | 1250 |
| 5 | 1143 | 12.1 | 131 | 1276 |
| 6 | 1200 | 15.0 | 150 | 1400 |
| 7 | 1178 | 13.4 | 141 | 1380 |
| 8 | 340-360 | 2.7-3.5 | ||
| 9 | 600 | 13 | 140 | 1050~1200 |
Claims (3)
1. a Zirconium oxide full-porcelain dental repair material is characterized in that the constituent (weight %) of the preparation raw material of this material is: contain the tetragonal phase zirconium oxide 86～92% of 3.0～5.15% stabilized with yttrium oxide, flux 5～10%, binding agent 3～4%; Described flux is that boron aluminum silicon is one or more in glass, hydroxyapatite, the β-wollastonite; Described boron aluminum silicon is that glass is low-expansion glass, and its chemical composition (weight %) is: SiO
279～81%, Al
2O
32～4%, B
2O
311～13%, K
2O 5～7%, Na
2O 0.5～2%.
2. Zirconium oxide full-porcelain dental repair material according to claim 1 is characterized in that preparing the binding agent described in the raw material and is in polyvinyl alcohol, carboxymethyl cellulose, the polyacrylic acid one or more.
3. the preparation method of Zirconium oxide full-porcelain dental repair material according to claim 1 is characterized in that this method comprises following concrete steps:
(1), mixed pelletize: tetragonal phase zirconium oxide powder body, flux, binding agent and an amount of ball-milling additive deionized water with stabilized with yttrium oxide joins in the fire ball grinding machine together earlier, mixed ball milling 15～30min, vacuum and low temperature lyophilization predecessor then, vacuum freeze drier is used in described vacuum and low temperature lyophilization, vacuum is 2～10Pa, temperature obtains the granule of particle diameter 0.5～1 μ m less than-40～-50 ℃;
(2), cold isostatic compaction: the granule of above-mentioned institute expense is packed in the mould, wait the static pressure operation then, briquetting pressure is 100～200MPa, and the dwell time is 5～20min;
(3), plastic removal: the base substrate that above-mentioned isostatic compaction obtains is put into Muffle furnace, speed with 40～80 ℃/h is warming up to 600～800 ℃, and insulation 1～3h naturally cools to room temperature then, remove the organic binder bond in the base substrate, obtain the biscuit of Zirconium oxide full-porcelain dental repair material;
(4), sintering: the biscuit of the Zirconium oxide full-porcelain dental repair material of above-mentioned plastic removal is placed in the high temperature furnace, speed with 50～150 ℃/h is warming up to sintering temperature, temperature range is 1250～1400 ℃, is incubated 1～3h under this temperature, and the speed with 150～200 ℃/h is cooled to room temperature then.
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| CN105669190A (en) * | 2016-03-03 | 2016-06-15 | 刘佩佩 | High-strength zirconia ceramic material for dental restoration and preparation method thereof |
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| CN107162603A (en) * | 2017-06-06 | 2017-09-15 | 爱迪特（秦皇岛）科技股份有限公司 | A kind of flash sintering method of dental zirconia ceramics |
| CN108101503A (en) * | 2017-12-08 | 2018-06-01 | 郑州搜趣信息技术有限公司 | High ceramic composite of a kind of intensity and its preparation method and application |
| CN107935623B (en) * | 2017-12-14 | 2021-01-12 | 苏州新汉盛精密陶瓷科技有限公司 | Wear-resistant ceramic material and preparation method and application thereof |
| CN112250438B (en) * | 2020-10-16 | 2022-11-25 | 江西德锆美瓷有限公司 | Preparation method of high-uniformity zirconia ceramic block for all-ceramic false tooth and product thereof |
| CN112239359A (en) * | 2020-10-21 | 2021-01-19 | 青岛理工大学 | 3D printing zirconia-based dental ceramic and preparation method thereof |
| CN114394830B (en) * | 2021-12-28 | 2023-06-09 | 中红外激光研究院(江苏)有限公司 | Preparation method of high-strength zirconia ceramic |
| CN114409430B (en) * | 2022-01-04 | 2022-11-04 | 北京劲松口腔医院投资管理有限公司 | All-ceramic prosthesis and preparation process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1489987A (en) * | 2003-09-05 | 2004-04-21 | 清华大学 | Polycrystal zirconium oxide ceramic dental material and preparation thereof |
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| CN1489987A (en) * | 2003-09-05 | 2004-04-21 | 清华大学 | Polycrystal zirconium oxide ceramic dental material and preparation thereof |
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