CN101870582A - Preparation method of tooth color imitating dental tetragonal polycrystalline zirconia ceramics - Google Patents

Preparation method of tooth color imitating dental tetragonal polycrystalline zirconia ceramics Download PDF

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CN101870582A
CN101870582A CN200910049708A CN200910049708A CN101870582A CN 101870582 A CN101870582 A CN 101870582A CN 200910049708 A CN200910049708 A CN 200910049708A CN 200910049708 A CN200910049708 A CN 200910049708A CN 101870582 A CN101870582 A CN 101870582A
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zirconia ceramics
dental
preparation
tooth color
rare earth
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CN101870582B (en
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高燕
张富强
黄慧
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Ninth Peoples Hospital Shanghai Jiaotong University School of Medicine
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Abstract

The invention relates to a preparation method of tooth color imitating dental tetragonal polycrystalline zirconia ceramics, which specifically comprises the following steps: taking a 3Y-TZP ceramic ingot as the raw material, taking rare earth oxide and transition element oxide as the colorant, adding the colorant and absolute ethyl alcohol into 3Y-TZP, ball milling, adding the 3Y-TZP, the absolute ethyl alcohol and agate ball milling beads into an agate ball milling pot by the mass ratio of 1:1:1, then drying, dry pressing and forming, isopressing and forming; and sintering at normal pressure, cutting and forming to obtain the tooth color imitating dental tetragonal polycrystalline zirconia ceramics. The preparation method of tooth color imitating dental tetragonal polycrystalline zirconia ceramics has the advantages that the chromatic values of 6 types of zirconia ceramics are within the range of natural tooth color, the color stability is good, the mechanical properties are excellent, and a constructed two-stage sintering process is beneficial to industrialized popularization, expands the adaptation disease scope thereof in dental clinical medicine and provides bases for the localization thereof.

Description

A kind of preparation method of tooth color imitating dental tetragonal polycrystalline zirconia ceramics
[technical field]
The present invention relates to the zirconia ceramics technical field, specifically, is a kind of preparation method of tooth color imitating dental tetragonal polycrystalline zirconia ceramics.
[background technology]
The color of ceramic pigment depends mainly on its microtexture, and relevant with microstructure characteristic then is the atomic structure of molecule, ion etc. and mutual influence.Its color depends primarily on ionic structure, electricity price, ionic radius, ligancy and interionic and polarizes mutually; Color is except that outside the Pass having with coloring ion, and is also relevant with the form of carrier, as forming sosoloid, inclusion, spinel etc., can improve the colour stability of colorant; Another factor of decision ceramic pigment color and character is preparation technology and working conditions, and is only reasonable in preparation technology, uses just can make color more reasonable when proper.
Ceramic coloring can adopt that base soil coloring, glaze are painted, painted several method on the painted and glaze under the glaze.Inorganic oxide is a pottery tinting material commonly used.Tinting material is divided into the base substrate tinting material: colorant is mixed in blank forming by a firing.Thereby require this based colorant for the various art breading in the base process, any reaction can not take place; Glaze stains yu: be used to decorate dry body, biscuit or burn till after ceramic whiteware, execute raw glaze thereon and carry out glaze firing again.Requirement must not react with glaze under normal firing temperature, and the while must not flow or grain pattern blurs; Tinting material on the glaze: be used to decorate the surface decoration of product after the glaze firing, require on quite low firing temperature (700～900 ℃) down can be securely attached to glaze, can not infiltrate in the glaze and flow.The clinical porcelain coloring process commonly used of tooth section is a coloring process on base substrate coloring process and the glaze.The base substrate coloring process is by the body porcelain of different colours, and the neck porcelain is through sintering and acquisition, and coloring process obtains by the porcelain powder that dyes outside the dummy surface-coated after glazing on the glaze.Coloring process easily wears away owing to life-time service on the glaze, and makes the color instability.
Pure Y-TZP pottery quality is a white, and its feasible painted approach has two: the first is carry out sintering, hot pressing or HIP sintering or the first thermal treatment of carrying out again behind the sintering under vacuum or the reducing atmosphere under vacuum or the reducing atmosphere in air, because ZrO 2The part oxygen loss forms non-metering ZrO 2-X phase makes Y-TZP be grey black, is referred to as black zirconia in Japan; It two is to add tinting material in Y-TZP, be generally colored ion compound, colloid ion tinting material, coloring of crystal agent of transition element and rare earth element etc., in air or oxidizing atmosphere, burn till, make Y-TZP be colors such as green, blue, yellow, black, purple, brown, light red.
In the Prosthodontics, the reproduction problem of color is an important indicator that influences dummy and tooth objectivity.The color of pure tetragonal zircite ceramic is white in color, and the dummy color of preparing is single, owing to do not possess the fluorescence that natural teeth can embody, is difficult to satisfy clinical requirement to the material color complicacy, so must rely on the facing porcelain to finish.A principle of Oral Repair is the unification that obtains mechanical property and aesthstic performance under the prerequisite that keeps tissue of tooth as far as possible.If the zirconium white substrate crown itself has the color and luster consistent with the natural teeth dentine, in dummy making processes, reduce facing porcelain thickness and still can reach the ideal aesthetic effect, can also reduce tooth simultaneously and be equipped with amount, more help keeping more tissue of tooth.
At present, the tetragonal zircite ceramic of clinical application mainly relies on import, and wherein the TZP of KAVO adds white primitive colour, and one has the substrate crown of 6 kinds of colors; The TZP of LAVA has 7 kinds of colors, and its ceramic briquet presintering realize the individual character reparation by outer dyeing then, but this method technology stability is poor, still lacks the data of long term follow-up aspect colour stability after machining forms unicolor substrate crown.
[summary of the invention]
The objective of the invention is to overcome the problem of tetragonal zircite ceramic intrinsic color, a kind of preparation method of tooth color imitating dental tetragonal polycrystalline zirconia ceramics is provided; Utilize the colour developing effect of rare earth element and transition element, by the blank coloring process, set up the sintering process of the imitative creamy white tetragonal zircite ceramic that is fit to tooth section clinical expansion, prepare the high strength tetragonal zircite ceramic that mates with natural teeth colourity, the tooth color imitating dental tetragonal zirconia ceramics that domesticizes for exploitation provides theoretical foundation.
The objective of the invention is to be achieved through the following technical solutions:
A kind of preparation method of tooth color imitating dental tetragonal polycrystalline zirconia ceramics, concrete steps are:
(1) raw material is the 3Y-TZP ceramic batch, is tinting material with rare earth oxide and transition element oxide compound, and wherein, the massfraction of rare earth oxide is 0.4～1.8%, and the transition element oxide content is 0.01～0.03%;
Described 3Y-TZP full name is a cubic polycrystal zirconia ceramics;
Described rare earth oxide is Pr 6O 11, CeO 2And Er 2O 3
Described transition element oxide compound is MnO 2
(2) tinting material and dehydrated alcohol are joined among the 3Y-TZP, carrying out ball milling, with 3Y-TZP: dehydrated alcohol: agate ball milling pearl is 1: 1: 1 adding in the agate jar by mass ratio, and then carries out drying, carry out dry-pressing formedly after the drying, carry out isostatic pressing again;
Described ball milling is meant to mix behind the moist ball milling 24h of the rotating speed of 200 commentaries on classics/min;
Described drying is meant inserts thermostatic drying chamber, dehydrates 12h under 100 ℃ of conditions, and it is standby to cross 180 mesh sieves then;
Described isostatic pressing is meant at the forming pressure compacted under of 300MPa and pressurize 3min;
(3) sintering under normal pressure again, excision forming obtains tooth color imitating dental tetragonal polycrystalline zirconia ceramics then, carries out Performance Evaluation again;
Described sintering process is: the two-part sintering process: just burning temperature is 1100 ℃, and burning temperature eventually is 1350 ℃, is specially first plastic removal: insulation is 2 hours after rising to 700 ℃ with 1 ℃/min heat-up rate, is cooled to room temperature naturally; Two-part sintering schedule again: rise to 1100 ℃ with 5 ℃/min temperature rise rate, be incubated 2 hours, reduce to room temperature with 5 ℃/min cooling rate; Temperature rise rate with 5 ℃/min rises to 1350 ℃ from room temperature subsequently, is incubated and reduces to room temperature with the cooling rate of 5 ℃/min after 2 hours, and sintering is finished.
Compared with prior art, positively effect of the present invention is:
6 kinds of zirconia ceramics colourimetric numbers of the present invention's preparation are in the natural teeth color gamut, colour stability is good, and mechanical property is excellent, and the two-part sintering process of foundation also helps the popularization of industrialization, enlarge it in the clinical indication scope of tooth section, for its production domesticization provides foundation.
[description of drawings]
Fig. 1 process flow sheet of the present invention.
[embodiment]
The preparation method's of a kind of tooth color imitating dental tetragonal polycrystalline zirconia ceramics of the present invention embodiment below is provided.
Embodiment 1
A kind of preparation method of tooth color imitating dental tetragonal polycrystalline zirconia ceramics, concrete steps are:
(1) raw material is the 3Y-TZP ceramic batch, is Pr with the rare earth oxide 6O 11, CeO 2, Er 2O 3With transition element oxide M nO 2Be tinting material, concrete component sees Table 1;
Described 3Y-TZP full name is a cubic polycrystal zirconia ceramics;
(2) tinting material and dehydrated alcohol are joined among the 3Y-TZP, carrying out ball milling, with powder: dehydrated alcohol: agate ball milling pearl is 1: 1: 1 adding in the agate jar by mass ratio, with the moist ball milling 24h of the rotating speed of 200 commentaries on classics/min mixing, and then carries out drying, insert thermostatic drying chamber, dehydrate 12h under 100 ℃ of conditions, it is standby to cross 180 mesh sieves, carries out dry-pressing formed after the drying, carry out isostatic pressing again, at forming pressure compacted under and the pressurize 3min of 300MPa;
(3) sintering under normal pressure again, excision forming obtains tooth color imitating dental tetragonal polycrystalline zirconia ceramics then, carries out Performance Evaluation again;
Described sintering process is: the two-part sintering process: just burning temperature is 1100 ℃, and burning temperature eventually is 1350 ℃, concrete: first plastic removal: insulation is 2 hours after rising to 700 ℃ with 1 ℃/min heat-up rate, is cooled to room temperature naturally; Two-part sintering schedule again: rise to 1100 ℃ with 5 ℃/min temperature rise rate, be incubated 2 hours, reduce to room temperature with 5 ℃/min cooling rate; Temperature rise rate with 5 ℃/min rises to 1350 ℃ from room temperature subsequently, is incubated and reduces to room temperature with the cooling rate of 5 ℃/min after 2 hours, and sintering is finished.
Embodiment 2
A kind of preparation method of tooth color imitating dental tetragonal polycrystalline zirconia ceramics, concrete steps are:
(1) raw material is the 3Y-TZP ceramic batch, is Pr with the rare earth oxide 6O 11, CeO 2, Er 2O 3With transition element oxide M nO 2Be tinting material, concrete component sees Table 1;
Described 3Y-TZP full name is a cubic polycrystal zirconia ceramics;
(2) with the step (2) of embodiment 1;
(3) with the step (3) of embodiment 1.
Embodiment 3
A kind of preparation method of tooth color imitating dental tetragonal polycrystalline zirconia ceramics, concrete steps are:
(1) raw material is the 3Y-TZP ceramic batch, is Pr with the rare earth oxide 6O 11, CeO 2, Er 2O 3With transition element oxide M nO 2Be tinting material, concrete component sees Table 1;
Described 3Y-TZP full name is a cubic polycrystal zirconia ceramics;
(2) with the step (2) of embodiment 1;
(3) with the step (3) of embodiment 1.
Embodiment 4
A kind of preparation method of tooth color imitating dental tetragonal polycrystalline zirconia ceramics, concrete steps are:
(1) raw material is the 3Y-TZP ceramic batch, is Pr with the rare earth oxide 6O 11, CeO 2, Er 2O 3With transition element oxide M nO 2Be tinting material, concrete component sees Table 1;
Described 3Y-TZP full name is a cubic polycrystal zirconia ceramics;
(2) with the step (2) of embodiment 1;
(3) with the step (3) of embodiment 1.
Embodiment 5
A kind of preparation method of tooth color imitating dental tetragonal polycrystalline zirconia ceramics, concrete steps are:
(1) raw material is the 3Y-TZP ceramic batch, is Pr with the rare earth oxide 6O 11, CeO 2, Er 2O 3With transition element oxide M nO 2Be tinting material, concrete component sees Table 1;
Described 3Y-TZP full name is a cubic polycrystal zirconia ceramics;
(2) with the step (2) of embodiment 1;
(3) with the step (3) of embodiment 1.
Embodiment 6
A kind of preparation method of tooth color imitating dental tetragonal polycrystalline zirconia ceramics, concrete steps are:
(1) raw material is the 3Y-TZP ceramic batch, is Pr with the rare earth oxide 6O 11, CeO 2, Er 2O 3With transition element oxide M nO 2Be tinting material, concrete component sees Table 1;
Described 3Y-TZP full name is a cubic polycrystal zirconia ceramics;
(2) with the step (2) of embodiment 1;
(3) with the step (3) of embodiment 1.
Table 1 is the composition table of the painted Y-TZP powder among the embodiment, and table 2 is that the sintering repeatedly of all embodiment is to single factor ANOVA of color parameter influence table as a result; Table 3 is the sintering character parameter list of all embodiment; Table 4 is the mechanical performance parameter table of all embodiment.
Table 1 is the composition of the painted Y-TZP powder among the embodiment
Figure B2009100497085D0000071
Table 2 is repeatedly a sintering to single factor ANOVA of color parameter influence table as a result
Figure B2009100497085D0000072
Table 3 is the sintering character parameter
Figure B2009100497085D0000081
Table 4 is a mechanical performance parameter
The above only is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, without departing from the inventive concept of the premise; can also make some improvements and modifications, these improvements and modifications also should be considered within the scope of protection of the present invention.

Claims (10)

1. the preparation method of a tooth color imitating dental tetragonal polycrystalline zirconia ceramics is characterized in that, concrete steps are:
(1) raw material is the cubic polycrystal zirconia ceramics blank, is tinting material with rare earth oxide and transition element oxide compound, and wherein, the massfraction of rare earth oxide is 0.4～1.8%, and the transition element oxide content is 0.01～0.03%;
(2) tinting material and dehydrated alcohol are added cubic polycrystal zirconia ceramics in, carrying out ball milling, with cubic polycrystal zirconia ceramics: dehydrated alcohol: agate ball milling pearl is 1: 1: 1 adding in the agate jar by mass ratio, and then carry out drying, carry out dry-pressing formedly after the drying, carry out isostatic pressing again;
(3) sintering under normal pressure again, excision forming obtains tooth color imitating dental tetragonal polycrystalline zirconia ceramics then.
2. the preparation method of a kind of tooth color imitating dental tetragonal polycrystalline zirconia ceramics as claimed in claim 1 is characterized in that, in described step (1), described rare earth oxide is Pr 6O 11, CeO 2And Er 2O 3
3. the preparation method of a kind of tooth color imitating dental tetragonal polycrystalline zirconia ceramics as claimed in claim 1 is characterized in that, in described step (1), described transition element oxide compound is MnO 2
4. the preparation method of a kind of tooth color imitating dental tetragonal polycrystalline zirconia ceramics as claimed in claim 1 is characterized in that, in described step (1), the massfraction of rare earth oxide and transition element oxide compound component is respectively Pr 6O 11Be 0.005%, CeO 2Be 0.4%, Er 2O 3Be 0.4%, MnO 2Be 0.03%.
5. the preparation method of a kind of tooth color imitating dental tetragonal polycrystalline zirconia ceramics as claimed in claim 1 is characterized in that, in described step (1), the massfraction of rare earth oxide and transition element oxide compound component is respectively Pr 6O 11Be 0.02%, CeO 2Be 0.6%, Er 2O 3Be 0.3%, MnO 2Be 0.02%.
6. the preparation method of a kind of tooth color imitating dental tetragonal polycrystalline zirconia ceramics as claimed in claim 1 is characterized in that, in described step (1), the massfraction of rare earth oxide and transition element oxide compound component is respectively Pr 6O 11Be 0.04%, CeO 2Be 0.8%, Er 2O 3Be 0.6%, MnO 2Be 0.02%.
7. the preparation method of a kind of tooth color imitating dental tetragonal polycrystalline zirconia ceramics as claimed in claim 1 is characterized in that, in described step (1), the massfraction of rare earth oxide and transition element oxide compound component is respectively Pr 6O 11Be 0.02%, CeO 2Be 1%, Er 2O 3Be 0.6%, MnO 2Be 0.02%.
8. the preparation method of a kind of tooth color imitating dental tetragonal polycrystalline zirconia ceramics as claimed in claim 1 is characterized in that, in described step (1), the massfraction of rare earth oxide and transition element oxide compound component is respectively Pr 6O 11Be 0.01%, CeO 2Be 0.8%, Er 2O 3Be 0.5%, MnO 2Be 0.01%.
9. the preparation method of a kind of tooth color imitating dental tetragonal polycrystalline zirconia ceramics as claimed in claim 1 is characterized in that, in described step (1), the massfraction of rare earth oxide and transition element oxide compound component is respectively Pr 6O 11Be 0.015%, CeO 2Be 0.2%, Er 2O 3Be 0.2%, MnO 2Be 0.03%.
10. the preparation method of a kind of tooth color imitating dental tetragonal polycrystalline zirconia ceramics as claimed in claim 1, it is characterized in that, in described step (3), described sintering process is: the two-part sintering process: just burning temperature is 1100 ℃, burning temperature eventually is 1350 ℃, be specially first plastic removal: insulation is 2 hours after rising to 700 ℃ with 1 ℃/min heat-up rate, is cooled to room temperature naturally; Two-part sintering schedule again: rise to 1100 ℃ with 5 ℃/min temperature rise rate, be incubated 2 hours, reduce to room temperature with 5 ℃/min cooling rate; Temperature rise rate with 5 ℃/min rises to 1350 ℃ from room temperature subsequently, is incubated and reduces to room temperature with the cooling rate of 5 ℃/min after 2 hours, and sintering is finished.
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