CN110317059A - A kind of each uniform layering zirconium oxide porcelain block technology of layer contraction - Google Patents
A kind of each uniform layering zirconium oxide porcelain block technology of layer contraction Download PDFInfo
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- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
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Abstract
The invention belongs to oral cavity material fields, and in particular to a kind of each uniform layering zirconium oxide porcelain block technology of layer contraction.The technical solution of use are as follows: the component and its content in each layer zirconia powder material formula are determined according to required color, each layer zirconium oxide porcelain block includes most bleached bed, transition zone and most dark layer；According to the content of yttrium oxide in each formula, the particle diameter distribution of zirconium oxide and yttrium oxide in most bleached bed and most dark layer formula is adjusted, to guarantee most bleached bed and the sintered shrinking percentage diversity factor < 3 ‰ of most dark layer；By after adjusting most bleached bed and most dark layer mix, obtain transition zone；Most bleached bed, transition zone and most dark layer are successively placed, isostatic pressing, pre-sintering, high temperature sintering by shade sequence, that is, completes preparation.Using technical solution of the present invention, can get it is natural with color, spend and crossed naturally, and the layering zirconium oxide porcelain block that is almost consistent of shrinking percentage thoroughly.
Description
Technical field
The invention belongs to oral cavity material fields, and in particular to a kind of each uniform layering zirconium oxide porcelain block technology of layer contraction.
Background technique
Zirconia ceramics is a kind of bioceramic material, belongs to the scope of green economy, because it is with good biofacies
The advantages that capacitive, excellent mechanical performance and class tooth bulk optics effect true to nature, it is known as 21 century ideal dentures repai material
One of material.
With the improvement of people ' s living standards with the enhancing of health perception, oral artificial tooth repair metallization removal have become development
Trend, All-ceramic restoration obtain the high praise of more and more doctors and patient.But if not carrying out color to All-ceramic material and degree changing thoroughly
Good, color, saturating degree are almost consistent up and down for artificial tooth, very lofty after installation, do not meet pursuit of the people to denture aesthetics.Cause
This, the dyeing of zirconium oxide porcelain block and screening color technology are come into being, and mainly include that external source dyes/hide color and endogenous dyeing/screening color.Outside
It dyes/hides color and refer to that the zirconium oxide porcelain block completed to sintering carries out the modes such as brushing dyeing liquor/screening color liquid and changes zirconium oxide porcelain in source
The color of block and thoroughly degree are difficult to control brushing thickness, color and the transition spent thoroughly depend on operation although easy to operate
The experience of personnel, it is more demanding to operator, and outer brush layer of substance, it can artificially change the thickness of zirconium oxide porcelain block, in turn
Make to have differences between artificial tooth size and in advance measured size, is unfavorable for the operations such as later period installation.And endogenous dyeing/screening color is (pre-
Dye layering) refer to the substance for being previously added in zirconia material powder and adjusting color and spending thoroughly.Although this method can be with
It effectively avoids carrying out the zirconium oxide porcelain block sintered secondary operation problem, but the zirconium oxide porcelain block obtained is still single face
Color and thoroughly degree, can not be presented nature transition effect.
If the zirconia material powder spent using multilayer different colours and thoroughly is compounded, is suppressed, is sintered, although theoretical
On seem can to obtain color and the zirconium oxide porcelain block of degree nature transition, but the in fact, powder formulation used due to every layer thoroughly
It has differences, every layer of porcelain block end sintering shrinkage after being pre-sintered is caused to would also vary from.It is burnt in 1500~1550 DEG C of high temperature
When knot prepares long bridge tooth, it is easy to appear bridge deformation, the zirconium oxide porcelain block for directly resulting in acquisition is scrapped.
In conclusion a kind of technology of preparing of the pre-dyed that shrinking percentage is consistent layering zirconium oxide porcelain block is provided, to oral cavity
The development of material has important practical significance.
Summary of the invention
The zirconium oxide that each interlamellar deformation uniformly, will not occur because of sintering is shunk the object of the present invention is to provide a kind of each layer
Porcelain block technology of preparing.
For achieving the above object, the technical scheme adopted by the invention is that: a kind of acquisition color, thoroughly degree nature gradual change
Layering zirconium oxide porcelain block method, adjust the partial size of the zirconium oxide and yttrium oxide powder in each layer zirconia powder material formula respectively
The content of distribution and yttrium oxide, until maximum difference degree < 3 ‰ between each layer zirconium oxide shrinking percentage.
Preferably, described method includes following steps:
(1) component and its content in each layer zirconia powder material formula, each layer zirconium oxide are determined according to required color
Porcelain block includes most bleached bed, transition zone and most dark layer；
(2) according to the content of yttrium oxide in each formula, zirconium oxide and oxidation in most bleached bed and most dark layer formula are adjusted
The particle diameter distribution of yttrium powder body is adjusted to the most bleached bed and the sintered shrinking percentage diversity factor < 3 ‰ of most dark layer；
(3) most bleached bed and most dark layer after adjusting step (2) mix, and obtain transition zone；
(4) will most bleached bed, transition zone and most dark layer successively place by shade sequence, isostatic pressing, pre-burning
Knot, high temperature sintering complete preparation.
Preferably, by mass, the formula of most bleached bed are as follows: Zirconium oxide powder 85~95%, yttrium oxide powder 4~
15%, object 0.3~0.4% is coloured.
Preferably, yttria levels are 4%~5% in the most bleached bed.
Preferably, by mass, the formula of most dark layer are as follows: Zirconium oxide powder 92~97%, yttrium oxide powder 3~7%,
Colour object 0.5~0.6%.
Preferably, yttria levels are 3%~4% in the most dark layer.
Preferably, the transition zone is arranged 2~5 layers.
Preferably, the transition zone is arranged 5 layers, and in mass ratio, the formula of each transition zone is respectively most bleached bed: most deep
Chromatograph=2:1,3:2,1:1,2:3,1:2.
Correspondingly, the layering zirconium oxide porcelain block of a kind of color, degree nature gradual change thoroughly, the zirconium oxide porcelain block is by most light
Layer, transition zone and most dark layer three classes zirconia powder material formula are made；By mass, the most light layer formula are as follows: zirconium oxide
Powder 94.7%, yttrium oxide powder 5%, coloring object 0.3%；Zirconium oxide and yttrium oxide powder grain in the most light layer formula
Diameter distribution are as follows: 10~50 μm, accounting 40%；50~150 μm, accounting 50%；150~300 μm, accounting 10%；It is described most dark
The formula of layer are as follows: Zirconium oxide powder 96.5%, yttrium oxide powder 3%, coloring object 0.5%；Oxygen in the most dark layer formula
Change zirconium and yttrium oxide powder particle diameter distribution are as follows: 10~50 μm, accounting 60%；50~150 μm, accounting 30%；It 150~300 μm, accounts for
Than 10%；The formula of the transition zone obtains after being mixed by most bleached bed and most dark layer.
Preferably, the transition zone is arranged 5 layers, and in mass ratio, the formula of each transition zone is respectively most bleached bed: most deep
Chromatograph=2:1,3:2,1:1,2:3,1:2.It should be understood that the formula of this layering zirconium oxide porcelain block provided by the invention is simultaneously
The claimed unique formula of non-present invention.The technical solution provided according to the present invention, when practical operation, can according to need choosing
Suitable shrinking percentage is selected, further according to the anti-formula for selecting zirconium oxide porcelain block of shrinking percentage of selection.As long as utilizing the technology of the present invention side
The anti-formula for selecting acquisition of case, should all fall within the scope of protection of the present invention.
The invention has the following advantages:
1, it dyes/hides from common external source unlike color, the present invention uses endogenous dyeing/screening color method, makes to be sintered
The zirconium oxide porcelain block obtained afterwards naturally has the natural color of transition and thoroughly degree, and color keep is consistent inside and outside zirconium oxide, also not
Can as external source dye/hide color, the thickness of zirconium oxide porcelain block can be can increase, so as to cause artificial tooth size with it is expected that size is not united
One the case where；Effect is substantially better than the colouring methods such as general external source brushing, immersion.Have to reach zirconium oxide porcelain block naturally
The natural color of transition and this effect is spent thoroughly, co-pressed, sintering method that present invention employs different zirconium oxide powder multilayers.
And light end, the respective adaptability Zirconium powder formula in dark end are provided, the main difference by adjusting yttria levels
Adjusting the saturating degree of zirconium oxide porcelain block, passing through the type of adjusting coloring object and matching the color for adjusting zirconium oxide porcelain block.Inventor
It has also been found that the content of control coloring object is 1.5% hereinafter, on the one hand can guarantee the color needs of zirconium oxide porcelain block, another party
Shrinking percentage influence in face of zirconium oxide porcelain block also can be ignored.
2 but the zirconium oxide powders of different formulations crystallization process is different when sintering at high temperature, shrinking percentage can also change correspondingly,
Shrinking percentage difference value is once more than a certain range, and bridge will bend, deform, and gently then influences beauty, it is heavy then scrap, can not
It uses.
For this problem, how inventor reduces shrinking percentage if not being conceived to, but creatively proposes a kind of complete
New thinking: how each layer shrinking percentage to be adjusted to unanimously.By a large amount of early-stage study, inventors have found that true in inventor
Recognize Zirconium powder formula in, the shrinking percentage of zirconia ceramics be mainly formulated in yttrium oxide content and zirconium oxide, oxidation
The particle diameter distribution of yttrium powder body controls.Therefore, it after inventor carries out a large number of experiments, finds out under specific yttria levels, aoxidizes
Relationship between zirconium, yttrium oxide particle diameter distribution and shrinking percentage, and completely new technical solution is proposed accordingly: it is (pre- according to actual needs
Precalculated artificial tooth size etc.) the suitable shrinking percentage of selection, zirconium oxide and oxidation in each formula are reversely adjusted further according to shrinking percentage
The particle diameter distribution of yttrium is consistent with controlling zirconia ceramics overall shrinkage.Final obtain naturally has color, spends and cross thoroughly
Naturally, and the layering zirconium oxide porcelain block that is almost consistent of shrinking percentage.
The layering zirconium oxide porcelain block obtained using technical solution of the present invention, no longer needs to carry out secondary manual operation, effectively drops
Low requirement of the dentures repai to operator, alleviates the bottleneck of professional's resource scarcity, saves needed for dentures repai
Time improves the quality of the life of patient.
Specific embodiment
Because of the not identical color of the tooth of human body, there are certain color transitions.And different face
Color corresponds to different zirconia powder material formulas；The general < 1.5% of colored oxide content in formula, to the burning of zirconium oxide porcelain block
Tying shrinking percentage influences can be neglected.
Method core provided by the invention are as follows: by adjusting the particle diameter distribution of Zirconium powder in powder formulation and adjusting
The content of yttrium oxide in formula, so that the shrinking percentage of each layer of zirconium oxide porcelain block is consistent, the generation of zirconium oxide porcelain block is mutually sympathized with when sintering
The contraction of condition, it is final to obtain that sintering post-shrinkage ratio is consistent, zirconium oxide porcelain block of the deformation that bend.Specifically include following step
It is rapid:
(1) each component content in different each layer powder formulations is determined according to required color.
First determine the formula of most bleached bed and most dark layer Zirconium powder.By mass, the formula of most bleached bed are as follows: oxygen
Change zirconium powder 85~95%, yttrium oxide powder 4~15%, coloring object 0.3~0.4%.The formula of most dark layer are as follows: zirconia powder
End 92~97%, yttrium oxide powder 3~7%, coloring object 0.5~0.6%.It is found by a large amount of pre-stage tests, preferred scheme
For in the zirconium oxide powder that most bleached bed uses, yttria levels (mass fraction) are advisable for 4%~5%；Most dark layer uses
Yttria levels be 3%~4% to be advisable.
But other recipe ingredients it is identical, only adjustment yttria levels in the case where, yttria levels be 3% with
There are larger difference, shrinking percentage is also not quite similar the saturating degree of 5% formula.If only will simply contain yttrium oxide 3% and 5% to match
The corresponding powder in side puts together, compacting sintering, and not only degree will appear tomography thoroughly, be unable to satisfy beautiful requirement, Er Qiehui
Because there is bridge bending deformation in the difference of shrinking percentage.For degree of solution, color tomography, in most bleached bed and most dark
Several layers of degree, color transition layer thoroughly are set again between layer.The transition zone is generally arranged 2~5 layers.
(2) according to the content of yttrium oxide in each formula, zirconium oxide and oxygen in most bleached bed and most dark layer formula are first adjusted
Change the particle diameter distribution of yttrium, to guarantee that this two layers of powder formulation sintering post-shrinkage ratio is consistent.It then by a certain percentage will most bleached bed
Most dark layer is mixed, and 2~5 layers of transition zone are arranged.
(3) each formula is successively placed into rear, isostatic pressing by required shade；It is then pre-sintered, by normal work
Skill carries out turning sizing, carving milling/slice, then carries out high temperature sintering, that is, completes preparation.
Combined with specific embodiments below, the present invention is further explained.
Embodiment
1, the Zirconium powder formula of most bleached bed and most dark layer is set.In the present embodiment, the Zirconium oxide powder that uses
Purchased from Shanghai Ling Hao metal material Co., Ltd, article No. ZR-2.The formula of most bleached bed is (by mass): Zirconium oxide powder
94.7%, yttrium oxide powder 5%, coloring object 0.3%.The formula of most dark layer is (by mass): Zirconium oxide powder 96.5%,
Yttrium oxide powder 3%, coloring object 0.5%.The coloring object can be erbium chloride, iron chloride, neodymium nitrate, manganese nitrate, metavanadic acid
One of ammonium, cerous nitrate, praseodymium nitrate, cobalt nitrate and nickel nitrate or a variety of mixtures.For convenience of operation, implementation of the invention
It is the coloring object obtained after 6:1:2 is mixed that erbium chloride, iron chloride, manganese nitrate are used in example in mass ratio, and color is tetracycline
Ash.
2, the production of monolith zirconium oxide porcelain block is carried out with the formula of above-mentioned determination, is measured under same recipe, different zirconium oxides
With the shrinking percentage of zirconium oxide porcelain block when yttrium oxide particle diameter distribution.Under above-mentioned same recipe, zirconium oxide and oxygen in formula are adjusted
The particle diameter distribution for changing yttrium measures under each particle diameter distribution after the isostatic pressing of the same terms, pre-sintering, high temperature sintering
Shrinking percentage.The isostatic pressing condition are as follows: pressure maintaining 10min under 150MPa；The pre-sintering condition are as follows: kept the temperature at 1050 DEG C
2h；The high temperature sintering condition are as follows: keep the temperature 2h at 1530 DEG C.Under different particle size distribution, the zirconium oxide of most light layer formula preparation
The shrinking percentage of porcelain block is as shown in table 1；The shrinking percentage of the zirconium oxide porcelain block of most dark layer formula preparation is as shown in table 2.
The shrinking percentage of the most light layer formula of table 1 shows table
The shrinking percentage of the most dark layer formula of table 2 shows table
3, most light layer formula and the shrinking percentage of most dark layer formula are adjusted to consistent.Selection shrinking percentage is similarly
17.70%, 18.70%, 19.03%, 19.35% particle diameter distribution prepares 4 groups of zirconium oxides by the method for layering zirconium oxide porcelain block
Porcelain block, every group sets 3 repetitions, respectively organizes 1,2,3,4.By taking shrinking percentage is similarly 17.70% as an example, that is, most light layer formula
In, the particle diameter distribution of zirconium oxide and yttrium oxide are as follows: 10~50 μm, accounting 40%；50~150 μm, accounting 50%；150~300 μ
M, accounting 10%.In most dark layer formula, the particle diameter distribution of zirconium oxide and yttrium oxide are as follows: 10~50 μm, accounting 60%；50~
150 μm, accounting 30%；150~300 μm, accounting 10%.Remaining organizes other particle diameter distribution and so on.
4, according to the most light layer formula and most dark layer formula after adjusting, the formula of transition zone is determined.In mass ratio, respectively
Group transition zone mass ratio be respectively most bleached bed: most dark layer=2:1,3:2,1:1,2:3,1:2, will most light layer formula and
Most dark layer formula is mixed, and obtains backing powder formula 1,2,3,4,5 respectively.Because most bleached bed and most dark interlayer have defined
The shrinking percentage difference of the maximum difference degree of shrinking percentage, the sintering shrinkage of the transition zone of preparation and most bleached bed, most dark interlayer
Degree does not exceed the value, to guarantee that the layering zirconium oxide porcelain block shrinking percentage finally obtained is consistent.
5, by the sequence of most bleached bed, transition zone 1, transition zone 2, transition zone 3, transition zone 4, transition zone 5, most dark layer,
It is sequentially placed each layer powder, by method isostatic pressing, pre-sintering, the high temperature sintering of step 2, that is, obtains the zirconium oxide porcelain of each group
Block.The zirconium oxide porcelain block shrinking percentage diversity factor is measured, and visual inspection is spent thoroughly and the transient condition of color.Step 2 is pressed simultaneously
Method, the light zirconium oxide porcelain block and 4 groups of monoliths of 4 groups of monoliths are prepared again respectively with formula and the particle diameter distribution of organizing 1,2,3,4
Dark zirconium oxide porcelain block, the light transmittance of each group light color zirconium oxide porcelain block and dark zirconium oxide porcelain block is detected, and detects
The three-point bending resistance intensity (being carried out referring to GB30356-2013) of each group dark color zirconium oxide porcelain block.The results are shown in Table 3.
3 each group effect of table shows table
Claims (10)
1. a kind of method for being layered zirconium oxide porcelain block for obtaining color, degree nature gradual change thoroughly, it is characterised in that: adjust each layer respectively
The particle diameter distribution of zirconium oxide and yttrium oxide powder in zirconia powder material formula and the content of yttrium oxide, until each layer zirconium oxide porcelain block
Maximum difference degree < 3 ‰ between shrinking percentage.
2. the method according to claim 1 that be layered zirconium oxide porcelain block for obtaining color, degree nature gradual change thoroughly, feature exist
In: include the following steps:
(1) component and its content in each layer zirconia powder material formula are determined according to required color, each layer zirconium oxide includes
Most bleached bed, transition zone and most dark layer；
(2) according to the content of yttrium oxide in each formula, zirconium oxide and oxidation yttrium powder in most bleached bed and most dark layer formula are adjusted
The particle diameter distribution of body is adjusted to the most bleached bed and the sintered shrinking percentage diversity factor < 3 ‰ of most dark layer；
(3) most bleached bed and most dark layer after adjusting step (2) mix, and obtain transition zone；
(4) will most bleached bed, transition zone and most dark layer successively place by shade sequence, isostatic pressing, pre-sintering, height
Temperature sintering, that is, complete preparation.
3. the method according to claim 2 that be layered zirconium oxide porcelain block for obtaining color, degree nature gradual change thoroughly, feature exist
In: by mass, the formula of the most bleached bed are as follows: Zirconium oxide powder 85~95%, yttrium oxide powder 4~15%, coloring object
0.3~0.4%.
4. the method according to claim 3 that be layered zirconium oxide porcelain block for obtaining color, degree nature gradual change thoroughly, feature exist
In: yttria levels are 4%~5% in the most bleached bed.
5. the method according to claim 2 that be layered zirconium oxide porcelain block for obtaining color, degree nature gradual change thoroughly, feature exist
In: by mass, the formula of the most dark layer are as follows: Zirconium oxide powder 92~97%, yttrium oxide powder 3~7%, coloring object
0.5~0.6%.
6. the method according to claim 5 that be layered zirconium oxide porcelain block for obtaining color, degree nature gradual change thoroughly, feature exist
In: yttria levels are 3%~4% in the most dark layer.
7. the method according to claim 2 that be layered zirconium oxide porcelain block for obtaining color, degree nature gradual change thoroughly, feature exist
In: the transition zone is arranged 2~5 layers.
8. the method according to claim 7 that be layered zirconium oxide porcelain block for obtaining color, degree nature gradual change thoroughly, feature exist
In: the transition zone is arranged 5 layers, and in mass ratio, the formula of each transition zone is respectively most bleached bed: most dark layer=2:1,3:
2、1:1、2:3、1:2。
9. the layering zirconium oxide porcelain block of a kind of color, degree nature gradual change thoroughly, it is characterised in that: the zirconium oxide porcelain block is by most light
Layer, transition zone and most dark layer three classes zirconia powder material formula are made；By mass, the most light layer formula are as follows: zirconium oxide
Powder 94.7%, yttrium oxide powder 5%, coloring object 0.3%；Zirconium oxide and yttrium oxide powder grain in the most light layer formula
Diameter distribution are as follows: 10~50 μm, accounting 40%；50~150 μm, accounting 50%；150~300 μm, accounting 10%；
The formula of the most dark layer are as follows: Zirconium oxide powder 96.5%, yttrium oxide powder 3%, coloring object 0.5%；It is described most deep
Zirconium oxide and yttrium oxide powder particle diameter distribution in chromatograph formula are as follows: 10~50 μm, accounting 60%；50~150 μm, accounting
30%；150~300 μm, accounting 10%；
The formula of the transition zone obtains after being mixed by most bleached bed and most dark layer.
10. the layering zirconium oxide porcelain block of a kind of color according to claim 9, degree nature gradual change thoroughly, it is characterised in that: institute
State transition zone be arranged 5 layers, in mass ratio, the formula of each transition zone is respectively most bleached bed: most dark layer=2:1,3:2,1:1,
2:3、1:2。
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112723885A (en) * | 2021-01-27 | 2021-04-30 | 湖南柯盛新材料有限公司 | Zirconia-based ceramic back plate and preparation method and application thereof |
| CN113336544A (en) * | 2021-06-30 | 2021-09-03 | 蓝思科技股份有限公司 | Multicolor ceramic cover plate and preparation method thereof |
| CN113402282A (en) * | 2021-07-30 | 2021-09-17 | 广东工业大学 | Bionic human bone based on 3D printing and manufacturing method thereof |
| CN113666753A (en) * | 2021-07-30 | 2021-11-19 | 广东工业大学 | Bionic human bone based on digital light processing molding technology and preparation method |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1593371A (en) * | 2004-06-28 | 2005-03-16 | 李石保 | Dental dummy preparation method |
| US20110027742A1 (en) * | 2008-04-09 | 2011-02-03 | Tosoh Corporation | Translucent zirconia sintered body, process for producing the same, and use of the same |
| CN102228408A (en) * | 2011-07-04 | 2011-11-02 | 辽宁爱尔创生物材料有限公司 | Light transmission gradually changed zirconium oxide material for dental surgery and preparation process thereof |
| CN102285795A (en) * | 2011-05-30 | 2011-12-21 | 北京大学口腔医学院 | Dental compound-color cuttable zirconia ceramic and preparation method thereof |
| 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 |
| CN103121840A (en) * | 2012-03-23 | 2013-05-29 | 中新棠国业（北京）科技有限责任公司 | Preparation of multilayer semitransparent zirconia full-porcelain dental repair material |
| CN107108373A (en) * | 2014-12-26 | 2017-08-29 | 可乐丽则武齿科株式会社 | Zirconia composition, zirconium oxide pre-burning body and zirconia sintered body and gear division product |
| CN109771064A (en) * | 2019-02-27 | 2019-05-21 | 深圳市翔通光电技术有限公司 | The artificial tooth and preparation method thereof that a kind of intensity, permeability and color successively change |
-
2019
- 2019-07-09 CN CN201910613983.9A patent/CN110317059B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1593371A (en) * | 2004-06-28 | 2005-03-16 | 李石保 | Dental dummy preparation method |
| US20110027742A1 (en) * | 2008-04-09 | 2011-02-03 | Tosoh Corporation | Translucent zirconia sintered body, process for producing the same, and use of the same |
| CN102285795A (en) * | 2011-05-30 | 2011-12-21 | 北京大学口腔医学院 | Dental compound-color cuttable zirconia ceramic and preparation method thereof |
| CN102228408A (en) * | 2011-07-04 | 2011-11-02 | 辽宁爱尔创生物材料有限公司 | Light transmission gradually changed zirconium oxide material for dental surgery and preparation process thereof |
| CN103121840A (en) * | 2012-03-23 | 2013-05-29 | 中新棠国业（北京）科技有限责任公司 | Preparation of multilayer semitransparent zirconia full-porcelain dental repair material |
| 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 |
| CN107108373A (en) * | 2014-12-26 | 2017-08-29 | 可乐丽则武齿科株式会社 | Zirconia composition, zirconium oxide pre-burning body and zirconia sintered body and gear division product |
| CN109771064A (en) * | 2019-02-27 | 2019-05-21 | 深圳市翔通光电技术有限公司 | The artificial tooth and preparation method thereof that a kind of intensity, permeability and color successively change |
Non-Patent Citations (1)
| Title |
|---|
| 李石保等: "制备高性能氧化锆陶瓷牙科修复体的初步研究", 《口腔医学研究》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114430629A (en) * | 2020-10-29 | 2022-05-03 | Oppo广东移动通信有限公司 | Ceramic shell, method for preparing ceramic shell and electronic equipment |
| CN112723885A (en) * | 2021-01-27 | 2021-04-30 | 湖南柯盛新材料有限公司 | Zirconia-based ceramic back plate and preparation method and application thereof |
| CN113336544A (en) * | 2021-06-30 | 2021-09-03 | 蓝思科技股份有限公司 | Multicolor ceramic cover plate and preparation method thereof |
| CN113402282A (en) * | 2021-07-30 | 2021-09-17 | 广东工业大学 | Bionic human bone based on 3D printing and manufacturing method thereof |
| CN113666753A (en) * | 2021-07-30 | 2021-11-19 | 广东工业大学 | Bionic human bone based on digital light processing molding technology and preparation method |
| CN113666753B (en) * | 2021-07-30 | 2023-12-26 | 广东工业大学 | Bionic human bone based on digital light processing molding technology and preparation method thereof |
| CN115159978A (en) * | 2022-05-25 | 2022-10-11 | 辽宁爱尔创生物材料有限公司 | Multilayer zirconia ceramic, preparation method and application |
| CN115159978B (en) * | 2022-05-25 | 2023-11-07 | 辽宁爱尔创生物材料有限公司 | Multilayer zirconia ceramic, preparation method and application |
| CN115353380A (en) * | 2022-08-10 | 2022-11-18 | 深圳玉汝成口腔材料有限公司 | Multilayer ceramic block, preparation method of multilayer ceramic block and false tooth |
| CN115745600A (en) * | 2022-11-23 | 2023-03-07 | 辽宁爱尔创生物材料有限公司 | Multilayer dental material and preparation method thereof |
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Denomination of invention: A Layered Zirconia Ceramic Block Technology with Uniform Shrinkage of Each Layer Effective date of registration: 20230728 Granted publication date: 20210706 Pledgee: Industrial Bank Limited by Share Ltd. Chengdu branch Pledgor: CHENGDU BESMILE MEDICAL TECHNOLOGY Corp.,Ltd. Registration number: Y2023980050334 |