CN105622096A - Color gradient zirconia material and preparation method thereof - Google Patents
Color gradient zirconia material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a color gradient zirconia material and a preparation method thereof and belongs to the technical field of dental ceramic materials. The zirconia material adopts a three-layer structure comprising a bottom layer, a middle layer and an outer layer; the three-layer structure is made of the following raw materials in percentage by mass: 70-99 percent of nano zirconia powder, 0.5-20 percent of iron oxide and 0.5-20 percent of erbium oxide. The preparation method comprises the following steps: respectively mixing the nano zirconia powder, the iron oxide and the erbium oxide according to different proportions, and then putting at different positions in a die cavity, so as to obtain the color gradient zirconia material through dry-pressing forming, isostatic forming, pre-sintering, cutting and secondary sintering. The color gradient zirconia material provided by the invention solves the problems of single zirconia ceramic color and tedious and complicated internal dyeing process and is not needed to be internally dyed in the preparation process; corresponding color of zirconium blocks are only needed to be selected after a doctor determines the color and are directly put into a sintering furnace to be sintered after being cut, so that not only is the color distribution rule of natural teeth satisfied, but also the process is simplified.
Description
Technical field
The present invention relates to a kind of color gradients zirconia material and preparation method thereof, belong to ceramic material for dental applications technical field.
Background technology
Zirconia ceramics is owing to having higher bending strength and fracture toughness, become a kind of important structural ceramics, again because it is found that zirconia ceramics has good bio-intermiscibility, also there is excellent stability, as wear-resistant and corrosion-resistant etc., it is possible to the intensity solving to exist in full ceramic dental repairing body is low, the problem of poor toughness, therefore dental field it is widely used in, but zirconia ceramics presents white more, and color is single, it is impossible to meet the COLOR COMPOSITION THROUGH DISTRIBUTION rule of nature tooth. It addition, at present the kind of zirconia ceramics is more, its saturating property differs, and as general, high saturating and super etc. and with same dyeing liquor, its colouring effect carried out during interior dye is also different, causes the loaded down with trivial details and complicated of operation. Therefore, it is necessary to the preparation method of zirconia ceramics is studied.
Summary of the invention
It is an object of the invention to provide a kind of color gradients zirconia material, the problem solving zirconia ceramics color dyer's sequence very complicated single, interior, while meeting nature tooth distribution of color rule, technical process have also been obtained simplification, present invention simultaneously provides its preparation method.
Color gradients zirconia material of the present invention, including bottom, intermediate layer and outer layer three-decker, three-decker is made by the raw material of following mass percent:
Nano zirconium oxide powder 70-99
Ferrum oxide 0.5-20
Erbia 0.5-20.
Wherein, the relative density of zirconia material is 0.992-0.998.
The preparation method of color gradients zirconia material of the present invention, comprises the following steps:
(1) dispensing:
Nano zirconium oxide powder, ferrum oxide, Erbia are mixed into three parts by different ratio respectively;
(2) packing compact forming:
By step (1) is sequentially placed into respectively the diverse location in film chamber by the powder of different proportion mixing, after dry-pressing formed, obtain base substrate;
(3) sintering;
Put into after the base substrate obtained in step (2) is carried out vacuum packaging in cold isostatic press and carry out isostatic pressing, then it is placed in Muffle furnace and carries out presintering, adopt CAD/CAM system to carry out double sintering again after cutting, obtain color gradients zirconia material.
Wherein, it is preferred that technical scheme is as follows:
In step (1), nano zirconium oxide powder accounts for 70-99wt%, and ferrum oxide accounts for 0.5-30wt%, and Erbia accounts for 0.5-30wt%.
In step (2), dry-pressing formed pressure is 60-100MPa.
In step (3), isostatic pressing pressure is 200-300MPa.
In step (3), pre-sintering temperature is 900-1050 DEG C, and double sintering temperature is 1450-1550 DEG C.
Beneficial effects of the present invention is as follows:
The relative density of the zirconia material that the present invention prepares is 0.992-0.998, its preparation process is without interior dye, have only to select after being determined color by doctor the zirconium block of respective color, directly it is put in sintering furnace after CAD/CAM carving and milling machine is cut and is sintered, both the distribution of color rule having met nature tooth in turn simplify technical process, and its application market is extensive.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
Color gradients zirconia material, including bottom, intermediate layer and outer layer three-decker, bottom is made up of the nano zirconium oxide powder of 70wt%, the ferrum oxide of 20wt% and the Erbia of 2wt%, intermediate layer is made up of the nano zirconium oxide powder of 80wt%, the ferrum oxide of 18.5wt% and the Erbia of 1.5wt%, and outer layer is made up of the nano zirconium oxide powder of 90wt%, the ferrum oxide of 9wt% and the Erbia of 1wt%.
Preparation method is as follows:
(1) dispensing:
A) weigh the nano zirconium oxide powder of 70wt%, the ferrum oxide of 20wt%, 2wt% Erbia mix;
B) weigh the nano zirconium oxide powder of 80wt%, the ferrum oxide of 18.5wt%, 1.5wt% Erbia mix;
C) weigh the nano zirconium oxide powder of 90wt%, the ferrum oxide of 9wt%, 1wt% Erbia mix;
(2) packing compact forming:
The mixed powder prepared in step a), step b), step c) is from bottom to top sequentially placed in die cavity, carries out dry-pressing formed under 60MPa; Obtain base substrate;
(3) sintering;
Put in cold isostatic press after the base substrate obtained in step (2) is carried out vacuum packaging, isostatic pressing is carried out under 250MPa, then it is placed in Muffle furnace, presintering is carried out at 960 DEG C, CAD/CAM system is adopted to carry out double sintering again at 1480 DEG C after cutting, obtaining color gradients zirconia material, its relative density is 0.992.
Embodiment 2
Color gradients zirconia material, including bottom, intermediate layer and outer layer three-decker, bottom is made up of the nano zirconium oxide powder of 75wt%, the ferrum oxide of 20wt% and the Erbia of 5wt%, intermediate layer is made up of the nano zirconium oxide powder of 85wt%, the ferrum oxide of 10.5wt% and the Erbia of 4.5wt%, and outer layer is made up of the nano zirconium oxide powder of 95wt%, the ferrum oxide of 3.5wt% and the Erbia of 1.5wt%.
Preparation method is as follows:
(1) dispensing:
A) weigh the nano zirconium oxide powder of 75wt%, the ferrum oxide of 20wt%, 5wt% Erbia mix;
B) weigh the nano zirconium oxide powder of 85wt%, the ferrum oxide of 10.5wt%, 4.5wt% Erbia mix;
C) weigh the nano zirconium oxide powder of 95wt%, the ferrum oxide of 3.5wt%, 1.5wt% Erbia mix;
(2) packing compact forming:
The mixed powder prepared in step a), step b), step c) is from bottom to top sequentially placed in die cavity, carries out dry-pressing formed under 60MPa; Obtain base substrate;
(3) sintering;
Put in cold isostatic press after the base substrate obtained in step (2) is carried out vacuum packaging, isostatic pressing is carried out under 250MPa, then it is placed in Muffle furnace, presintering is carried out at 960 DEG C, CAD/CAM system is adopted to carry out double sintering again at 1480 DEG C after cutting, obtaining color gradients zirconia material, its relative density is 0.993.
Embodiment 3
Color gradients zirconia material, including bottom, intermediate layer and outer layer three-decker, bottom is made up of the nano zirconium oxide powder of 80wt%, the ferrum oxide of 12wt% and the Erbia of 8wt%, intermediate layer is made up of the nano zirconium oxide powder of 90wt%, the ferrum oxide of 5.5wt% and the Erbia of 4.5wt%, and outer layer is made up of the nano zirconium oxide powder of 96wt%, the ferrum oxide of 2.5wt% and the Erbia of 1.5wt%.
Preparation method is as follows:
(1) dispensing:
A) weigh the nano zirconium oxide powder of 80wt%, the ferrum oxide of 12wt%, 8wt% Erbia mix;
B) weigh the nano zirconium oxide powder of 90wt%, the ferrum oxide of 5.5wt%, 4.5wt% Erbia mix;
C) weigh the nano zirconium oxide powder of 96wt%, the ferrum oxide of 2.5wt%, 1.5wt% Erbia mix;
(2) packing compact forming:
The mixed powder prepared in step a), step b), step c) is from bottom to top sequentially placed in die cavity, carries out dry-pressing formed under 60MPa; Obtain base substrate;
(3) sintering;
Put in cold isostatic press after the base substrate obtained in step (2) is carried out vacuum packaging, isostatic pressing is carried out under 250MPa, then it is placed in Muffle furnace, presintering is carried out at 960 DEG C, CAD/CAM system is adopted to carry out double sintering again at 1480 DEG C after cutting, obtaining color gradients zirconia material, its relative density is 0.996.
Embodiment 4
Color gradients zirconia material, including bottom, intermediate layer and outer layer three-decker, bottom is made up of the nano zirconium oxide powder of 85wt%, the ferrum oxide of 4wt% and the Erbia of 11wt%, intermediate layer is made up of the nano zirconium oxide powder of 95wt%, the ferrum oxide of 1wt% and the Erbia of 4wt%, and outer layer is made up of the nano zirconium oxide powder of 98wt%, the ferrum oxide of 1.5wt% and the Erbia of 0.5wt%.
Preparation method is as follows:
(1) dispensing:
A) weigh the nano zirconium oxide powder of 85wt%, the ferrum oxide of 4wt%, 11wt% Erbia mix;
B) weigh the nano zirconium oxide powder of 95wt%, the ferrum oxide of 1wt%, 4wt% Erbia mix;
C) weigh the nano zirconium oxide powder of 98wt%, the ferrum oxide of 1.5wt%, 0.5wt% Erbia mix;
(2) packing compact forming:
The mixed powder prepared in step a), step b), step c) is from bottom to top sequentially placed in die cavity, carries out dry-pressing formed under 60MPa; Obtain base substrate;
(3) sintering;
Put in cold isostatic press after the base substrate obtained in step (2) is carried out vacuum packaging, isostatic pressing is carried out under 250MPa, then it is placed in Muffle furnace, presintering is carried out at 960 DEG C, CAD/CAM system is adopted to carry out double sintering again at 1480 DEG C after cutting, obtaining color gradients zirconia material, its relative density is 0.998.
Embodiment 5
Color gradients zirconia material, including bottom, intermediate layer and outer layer three-decker, bottom is made up of the nano zirconium oxide powder of 75wt%, the ferrum oxide of 20wt% and the Erbia of 5wt%, intermediate layer is made up of the nano zirconium oxide powder of 85wt%, the ferrum oxide of 10.5wt% and the Erbia of 4.5wt%, and outer layer is made up of the nano zirconium oxide powder of 95wt%, the ferrum oxide of 3.5wt% and the Erbia of 1.5wt%.
Preparation method is as follows:
(1) dispensing:
A) weigh the nano zirconium oxide powder of 75wt%, the ferrum oxide of 20wt%, 5wt% Erbia mix;
B) weigh the nano zirconium oxide powder of 85wt%, the ferrum oxide of 10.5wt%, 4.5wt% Erbia mix;
C) weigh the nano zirconium oxide powder of 95wt%, the ferrum oxide of 3.5wt%, 1.5wt% Erbia mix;
(2) packing compact forming:
The mixed powder prepared in step a), step b), step c) is from bottom to top sequentially placed in die cavity, carries out dry-pressing formed under 75MPa; Obtain base substrate;
(3) sintering;
Put in cold isostatic press after the base substrate obtained in step (2) is carried out vacuum packaging, isostatic pressing is carried out under 280MPa, then it is placed in Muffle furnace, presintering is carried out at 960 DEG C, CAD/CAM system is adopted to carry out double sintering again at 1480 DEG C after cutting, obtaining color gradients zirconia material, its relative density is 0.995.
Above example can not limit the present invention, and the technical staff of the industry is it will be clearly understood that without departing from preparation method of the present invention when, it is also possible to the present invention makes improvement and extension, and these improve and extension also should in the protection category of the present invention.
Claims (7)
1. a color gradients zirconia material, including bottom, intermediate layer and outer layer three-decker, it is characterised in that: three-decker is made by the raw material of following mass percent:
Nano zirconium oxide powder 70-99%
Ferrum oxide 0.5-20%
Erbia 0.5-20%.
2. color gradients zirconia material according to claim 1, it is characterised in that: the relative density of zirconia material is 0.992-0.998.
3. the preparation method of the color gradients zirconia material described in a claim 1 or 2, it is characterised in that: comprise the following steps:
(1) dispensing:
Nano zirconium oxide powder, ferrum oxide, Erbia are mixed into three parts by different ratio respectively;
(2) packing compact forming:
By step (1) is sequentially placed into respectively the diverse location in film chamber by the powder of different proportion mixing, after dry-pressing formed, obtain base substrate;
(3) sintering;
Put into after the base substrate obtained in step (2) is carried out vacuum packaging in cold isostatic press and carry out isostatic pressing, then through presintering, cutting and double sintering, obtain color gradients zirconia material.
4. the preparation method of color gradients zirconia material according to claim 3, it is characterised in that: in step (2), dry-pressing formed pressure is 60-100MPa.
5. the preparation method of color gradients zirconia material according to claim 3, it is characterised in that: in step (3), isostatic pressing pressure is 200-300MPa.
6. the preparation method of color gradients zirconia material according to claim 3, it is characterised in that: in step (3), pre-sintering temperature is 900-1050 DEG C.
7. the preparation method of color gradients zirconia material according to claim 3, it is characterised in that: in step (3), double sintering temperature is 1450-1550 DEG C.
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| EP3400929A1 (en) | 2017-05-12 | 2018-11-14 | Aidite (Qinhuangdao) Technology Co.Ltd. | Dental zirconia restoration material with uniform transition of strength and color, and preparation method thereof |
| US10264690B2 (en) | 2016-09-01 | 2019-04-16 | Apple Inc. | Ceramic sintering for uniform color for a housing of an electronic device |
| US10463125B2 (en) | 2015-03-08 | 2019-11-05 | Apple Inc. | Co-molded ceramic and polymer structure |
| US10624217B2 (en) | 2016-09-21 | 2020-04-14 | Apple Inc. | Yttria-sensitized zirconia |
| US10703680B2 (en) | 2015-05-25 | 2020-07-07 | Apple Inc. | Fiber-reinforced ceramic matrix composite for electronic devices |
| US11088718B2 (en) | 2016-09-06 | 2021-08-10 | Apple Inc. | Multi-colored ceramic housings for an electronic device |
| US11104616B2 (en) | 2015-09-30 | 2021-08-31 | Apple Inc. | Ceramic having a residual compressive stress for use in electronic devices |
| CN113461421A (en) * | 2021-07-30 | 2021-10-01 | 北京大学口腔医学院 | Laminated zirconia dental ceramic material and preparation method thereof |
| US11604514B2 (en) | 2016-04-14 | 2023-03-14 | Apple Inc. | Substrate having a visually imperceptible texture for providing variable coefficients of friction between objects |
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| CN104844200A (en) * | 2015-04-30 | 2015-08-19 | 浙江大学 | Multiple-oxide-doped gradient-color zirconia dental prosthesis and preparation method thereof |
| CN104909745A (en) * | 2015-06-23 | 2015-09-16 | 成都贝施美生物科技有限公司 | Preparation method for uniform gradient-colour zirconium oxide porcelain blocks |
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| CN103058655A (en) * | 2013-01-18 | 2013-04-24 | 秦皇岛爱迪特高技术陶瓷有限公司 | Gradient transparent zirconium oxide dental ceramic and preparation method thereof |
| CN104844200A (en) * | 2015-04-30 | 2015-08-19 | 浙江大学 | Multiple-oxide-doped gradient-color zirconia dental prosthesis and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US10463125B2 (en) | 2015-03-08 | 2019-11-05 | Apple Inc. | Co-molded ceramic and polymer structure |
| US10703680B2 (en) | 2015-05-25 | 2020-07-07 | Apple Inc. | Fiber-reinforced ceramic matrix composite for electronic devices |
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