CN109734446A - A kind of preparation method of zirconia ceramics dummy - Google Patents
A kind of preparation method of zirconia ceramics dummy Download PDFInfo
- Publication number
- CN109734446A CN109734446A CN201910057962.3A CN201910057962A CN109734446A CN 109734446 A CN109734446 A CN 109734446A CN 201910057962 A CN201910057962 A CN 201910057962A CN 109734446 A CN109734446 A CN 109734446A
- Authority
- CN
- China
- Prior art keywords
- preparation
- dummy
- zirconia
- sintering
- molding
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to Ceramic restorations preparation technical fields, more particularly to a kind of preparation method of zirconia ceramics dummy, a kind of preparation method of zirconia ceramics dummy provided by the invention, the following steps are included: by zirconia sol, solvent and dispersant, successively formed, be pre-sintered and CAM processing, obtain molding dummy；The molding dummy is sintered, zirconia ceramics dummy is obtained；The dispersed phase of the zirconia sol is zirconium oxide and stabilizer.The present invention makes the consistency of zirconium oxide prosthesis reach 99.3% or more by utilizing the tetragonal phase of stabilizer stabilizing zirconia by pre-sintering and sintering, makes it have the lower porosity, preferable surface smoothness；Meanwhile flexural strength >=800MPa of the zirconia ceramics dummy.
Description
Technical field
The present invention relates to Ceramic restorations preparation technical field more particularly to a kind of preparation sides of zirconia ceramics dummy
Method.
Background technique
With work as pre-ceramic recovery technique rapid development, All-ceramic material by feat of its own good biocompatibility,
A series of speciality such as corrosion resistance, dielectricity, thermal stability and excellent aesthetic effect, become the research emphasis of people.
Wherein zirconia ceramics due to become with high tenacity, high-flexural strength and wearability repaired currently used for ceramics it is best complete
One of ceramic material.
But the zirconia ceramics repair materials porosity with higher in the prior art, can have transparency, surface light
The problems such as cleanliness is inadequate.To solve the above-mentioned problems, people generally use cubic zirconia crystal phase and repair as zirconia ceramics
Multiple material, but the zirconium oxide of above-mentioned cubic phase can reduce the flexural strength of ceramic repair materials, and it is special to weaken zirconium oxide institute
The crystal transition played the role of hinders crack propagation.Therefore, how pottery is improved while guaranteeing Ceramic restorations flexural strength
The surface smoothness of Porcelain veneer, there are no relevant records in the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of zirconia ceramics dummy, utilize the preparation method system
Standby obtained Ceramic restorations have the lower porosity, higher surface smoothness and preferable flexural strength.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of preparation methods of zirconia ceramics dummy, comprising the following steps:
By zirconia sol, solvent and dispersant, successively formed, be pre-sintered and CAM processing, obtain molding repair
Complex；
The molding dummy is sintered, zirconia ceramics dummy is obtained；
The dispersed phase of the zirconia sol is zirconium oxide and stabilizer.
Preferably, the stabilizer is one or more of yttrium oxide, cerium oxide and magnesia.
Preferably, the mass ratio of zirconium oxide and stabilizer is (93~96): (4~7) in the zirconia sol.
Preferably, the diameter of the colloidal solid of the zirconia sol is≤30nm.
Preferably, the dispersing agent is organic acid, acylate, ammonium hydroxide, tetramethylammonium hydroxide, polyvinyl lactam and gathers
One or more of ethylene glycol.
Preferably, described be blended under conditions of ball milling carries out；
The ratio of grinding media to material of the ball milling is (8~12): 1, the revolving speed of the ball milling is 100~300 revs/min, the ball milling
Time be 2~4 hours.
Preferably, the molding pressure is 0.5~30MPa, and the molding time is 3~30 minutes.
It preferably, further include that obtained biscuit is dried after the molding；
The relative humidity of the drying is 40~80%, and the temperature of the drying is 50~200 DEG C, the time of the drying
It is 10~80 hours.
Preferably, the temperature of the pre-sintering is 700~1000 DEG C, and the time of the pre-sintering is 50~100 hours.
Preferably, the temperature of the sintering is 1200~1450 DEG C, and the time of the sintering is 2~3 hours.
The present invention provides a kind of preparation methods of zirconia ceramics dummy, comprising the following steps: by zirconia sol,
Solvent and dispersant, successively formed, be pre-sintered and CAM processing, obtain molding dummy；By the molding dummy
It is sintered, obtains zirconia ceramics dummy；The dispersed phase of the zirconia sol is zirconium oxide and stabilizer.The present invention is logical
The tetragonal phase of stabilizer stabilizing zirconia is crossed, and reaches the consistency of zirconium oxide prosthesis by pre-sintering and sintering
99.3% or more, make it have the lower porosity, preferable surface smoothness；Meanwhile the zirconia ceramics dummy
Flexural strength >=800MPa.
Specific embodiment
The present invention provides a kind of preparation methods of zirconia ceramics dummy, comprising the following steps:
By zirconia sol, solvent and dispersant, successively formed, be pre-sintered and CAM processing, obtain molding repair
Complex；
The molding dummy is sintered, zirconia ceramics dummy is obtained；
The dispersed phase of the zirconia sol is zirconium oxide and stabilizer.
In the present invention, if without specified otherwise, all raw material components are commercial product well known to those skilled in the art.
The present invention will successively be formed zirconia sol, solvent and dispersant, be pre-sintered and CAM processing, be obtained
To molding dummy.In the present invention, the dispersed phase of the zirconia sol is zirconium oxide and stabilizer；In the present invention, institute
Stating stabilizer is preferably one or more of yttrium oxide, cerium oxide and magnesia；When the stabilizer is above-mentioned specific choice
In it is two or more when, proportion no any special restriction of the present invention to the specific substance is mixed by any proportion
Conjunction.In the present invention, the mass ratio of zirconium oxide and stabilizer is preferably (93~96) in the zirconia sol: (4~
7), more preferably (94~95): (5~6).
In the present invention, the decentralized medium of the zirconia sol is preferably water, dispersed phase in the zirconia sol
Mass concentration is preferably 1~30%, and more preferably 3~5%, most preferably 5%.
In the present invention, the partial size of the colloidal solid of the zirconia sol preferably≤30nm, more preferably≤15nm,
Most preferably≤8nm.
In the present invention, the solvent is preferably one or more of water, ethyl alcohol and propyl alcohol；When the solvent is above-mentioned
When two or more in specific choice, proportion no any special restriction of the present invention to the specific substance, by arbitrarily matching
Than being mixed.
In the present invention, the dispersing agent is preferably organic acid, acylate, ammonium hydroxide, tetramethylammonium hydroxide, polyethylene
One or more of amide and polyethylene glycol；The organic acid is preferably oleic acid, citric acid or acrylic acid；The acylate
The corresponding salt of preferably above-mentioned organic acid；When the dispersing agent be above-mentioned specific choice in it is two or more when, the present invention is to institute
The no any special restriction of proportion for stating specific substance, is mixed by any proportion.
In the present invention, the mass ratio of the zirconia sol and dispersing agent is preferably (95~100): 1, preferably (96
~98): 1.
In the present invention, the solid content for the slurry that zirconia sol, solvent and dispersant obtain is preferably 40~
50wt%, more preferably 42~48wt%, most preferably 44~46wt%.
The present invention does not have any special restriction to the order by merging of the zirconia sol, solvent and dispersing agent, uses
Order by merging well known to those skilled in the art.
In the present invention, the pH value of the slurry obtained after the zirconia sol, solvent and dispersant is preferably 5~
11, more preferably 6~10, most preferably 8~9.
In the present invention, the mixed mode is preferably ball milling；In the present invention, the material of the abrading-ball of the ball milling is excellent
It is selected as zirconium oxide；The ratio of grinding media to material of the ball milling is preferably (8~12): 1, more preferably (9~11): 1；The revolving speed of the ball milling is excellent
It is selected as 100~300 revs/min, more preferably 150~250 revs/min；The time of the ball milling is preferably 2~4 hours, more excellent
It is selected as 2.5~3.5 hours.
After the completion of ball milling, the present invention preferably carries out de-bubble to obtained ball milling material；In the present invention, the de-bubble is preferred
The slurry after ball milling to be vacuum-treated to remove the bubble in slurry；The vacuum degree of the vacuum processing preferably-
0.1MPa。
In the present invention, the molding pressure is preferably 0.5~30MPa, more preferably 5~25MPa, most preferably 10
~20MPa；The molding time is preferably 3~30 minutes, more preferably 5~10 minutes, most preferably 8 minutes.
In the present invention, the molding detailed process is preferably to inject the slurry after the de-bubble in porous mold,
When green body reaches certain thickness, applies pressure forming, obtain biscuit；The porous mold is preferably nano aperture；The present invention
There is no any special restriction to the thickness, obtains respective thickness according to actual needs.
After molding, obtained biscuit is dried in the present invention；In the present invention, the relative humidity of the drying is preferably
40~80%, more preferably 50~70%, most preferably 55~65%；The temperature of the drying is preferably 50~200 DEG C, more excellent
It is selected as 80~150 DEG C；The time of the drying is preferably 10~80 hours, and more preferably 30~40 hours.
In the present invention, the temperature of the pre-sintering is preferably 700~1000 DEG C, more preferably 800~950 DEG C, optimal
It is selected as 900 DEG C；The time of the pre-sintering is preferably 50~100 hours, more preferably 70~90 hours, most preferably 75~85
Hour.
In the present invention, the pre-sintering preferably carries out in normal pressure-sintered furnace.
The present invention processes no any special restriction to the CAM, is processed using CAM well known to those skilled in the art
It carries out, and is processed into required shape.
In the present invention, the temperature of the sintering is preferably 1200~1450 DEG C, more preferably 1250~1400 DEG C, optimal
It is selected as 1300~1350 DEG C；The time of the sintering is preferably 2~3 hours, and more preferably 2.2~2.8 hours, most preferably
2.4~2.6 hours.
In the present invention, the sintering preferably carries out in hot pressing furnace or hot isostatic pressing furnace.
In order to further illustrate the present invention, below with reference to embodiment to the system of zirconia ceramics dummy provided by the invention
Preparation Method is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
It is 8nm by 100g partial size, zirconia sol that mass concentration be 5% (mass ratio of zirconium oxide and yttrium oxide is 93:
7), ethyl alcohol, the mixing of 1g oleic acid, obtain the slurry that solid content is 45%；It is to carry out ball milling in 10:1 addition ball mill according to ball material
(revolving speed of ball milling is 200 revs/min, and the time is 3 hours), obtains mixed slurry；
After the mixed slurry is carried out de-bubble processing at -0.1MPa, the slurry after de-bubble is injected into ready receive
In the porous mold of metre hole diameter, at 30MPa, compression moulding after pressure maintaining 20min obtains biscuit；
It is 40% in relative humidity, after temperature dries the biscuit 60 hours under conditions of being 60 DEG C, is put into normal pressure burning
It in freezing of a furnace, is pre-sintered 70 hours at 900 DEG C, carries out CAM processing after the completion of being pre-sintered, obtain molding dummy；By the molding
Dummy places into hot pressing furnace, after being sintered 2h at 1280 DEG C, obtains zirconia ceramics dummy.The zirconia ceramics reparation
The consistency of body is 99.4%, and particle size is 15~80nm, the porosity 0.01%, flexural strength 1100MPa.
Embodiment 2
It is 25nm by 500g partial size, (mass ratio of zirconium oxide and cerium oxide is the zirconia sol that mass concentration is 3%
95:5), ethyl alcohol, the mixing of 5.5g oleic acid, obtain the slurry that solid content is 48%；According to material ball ratio be 10:1 be added ball mill in into
Row ball milling (revolving speed of ball milling is 150 revs/min, and the time is 3 hours), obtains mixed slurry；
After the mixed slurry is carried out de-bubble processing at -0.1MPa, the slurry after de-bubble is injected into ready receive
In the porous mold of metre hole diameter, at 10MPa, compression moulding after 25min obtains biscuit；
It is 50% in relative humidity, temperature is put into normal pressure after the biscuit is dried 80 hours under conditions of being 80 DEG C
CAM processing is carried out after being pre-sintered 80h in sintering furnace, at 950 DEG C, obtains molding dummy；The molding dummy is placed into
In hot pressing furnace, after being sintered 2h at 1350 DEG C, zirconia ceramics dummy is obtained.The consistency of the zirconia ceramics dummy is
99.5%, particle size is 40~60nm, the porosity 0.01%, flexural strength 950MPa.
Embodiment 3
It is 15nm by 100g partial size, (mass ratio of zirconium oxide and magnesia is the zirconia sol that mass concentration is 10%
95:5), ethyl alcohol, the mixing of 1g oleic acid, obtain the slurry that solid content is 50%, and the pH for adjusting slurry is 3；It is 10:1 according to material ball ratio
It is added in ball mill and carries out ball milling (revolving speed of ball milling is 150 revs/min, and the time is 3.5 hours), obtain mixed slurry；
After the mixed slurry is carried out de-bubble processing at -0.1MPa, the slurry after de-bubble is injected into ready receive
In the porous mold of metre hole diameter, at 5MPa, compression moulding after 30min obtains biscuit；
It is 50% in relative humidity, after the biscuit is dried 60 hours under conditions of being 75 DEG C by temperature, is put into often
It presses in sintering furnace, carries out CAM processing after 72h is pre-sintered at 880 DEG C, obtain molding dummy；By the molding dummy, then put
Enter in hot pressing furnace, after being sintered 2.5h at 1310 DEG C, obtains zirconia ceramics dummy.The densification of the zirconia ceramics dummy
Degree is 99.5%, and particle size is 50~90nm, the porosity 0.01%；Flexural strength is 890MPa.
As seen from the above embodiment, the consistency of zirconium oxide prosthesis provided by the invention reaches 99.3% or more, has
The lower porosity (0.01%), preferable surface smoothness；Meanwhile the flexural strength of the zirconia ceramics dummy >=
800MPa。
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications should also regard
For protection scope of the present invention.
Claims (10)
1. a kind of preparation method of zirconia ceramics dummy, comprising the following steps:
By zirconia sol, solvent and dispersant, successively formed, be pre-sintered and CAM processing, obtain molding repair
Body；
The molding dummy is sintered, zirconia ceramics dummy is obtained；
The dispersed phase of the zirconia sol is zirconium oxide and stabilizer.
2. preparation method as described in claim 1, which is characterized in that the stabilizer is yttrium oxide, cerium oxide and magnesia
One or more of.
3. preparation method as claimed in claim 2, which is characterized in that the matter of zirconium oxide and stabilizer in the zirconia sol
Amount is than being (93~96): (4~7).
4. preparation method as claimed in claim 1 or 3, which is characterized in that the diameter of the colloidal solid of the zirconia sol
≤30nm。
5. preparation method as described in claim 1, which is characterized in that the dispersing agent be organic acid, acylate, ammonium hydroxide,
One or more of tetramethylammonium hydroxide, polyvinyl lactam and polyethylene glycol.
6. preparation method as described in claim 1, which is characterized in that described be blended under conditions of ball milling carries out；
The ratio of grinding media to material of the ball milling is (8~12): 1, the revolving speed of the ball milling is 100~300 revs/min, the ball milling when
Between be 2~4 hours.
7. preparation method as described in claim 1, which is characterized in that the molding pressure be 0.5~30MPa, it is described at
The time of type is 3~30 minutes.
8. preparation method as claimed in claim 1 or 7, which is characterized in that further include after the molding to obtained biscuit into
Row drying；
The relative humidity of the drying is 40~80%, and the temperature of the drying is 50~200 DEG C, and the time of the drying is 10
~80 hours.
9. preparation method as described in claim 1, which is characterized in that the temperature of the pre-sintering is 700~1000 DEG C, described
The time of pre-sintering is 50~100 hours.
10. preparation method as described in claim 1, which is characterized in that the temperature of the sintering is 1200~1450 DEG C, described
The time of sintering is 2~3 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910057962.3A CN109734446A (en) | 2019-01-22 | 2019-01-22 | A kind of preparation method of zirconia ceramics dummy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910057962.3A CN109734446A (en) | 2019-01-22 | 2019-01-22 | A kind of preparation method of zirconia ceramics dummy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109734446A true CN109734446A (en) | 2019-05-10 |
Family
ID=66365687
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910057962.3A Pending CN109734446A (en) | 2019-01-22 | 2019-01-22 | A kind of preparation method of zirconia ceramics dummy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109734446A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0194191A1 (en) * | 1985-03-01 | 1986-09-10 | Rhone-Poulenc Chimie | Stabilized zirconia, process for its preparation and its use in ceramic compositions |
| CN101863659A (en) * | 2010-06-11 | 2010-10-20 | 广东工业大学 | Method for preparing stabilized zirconia superfine powder by stirring ball-milling reaction |
| 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 |
| CN103641472A (en) * | 2013-11-14 | 2014-03-19 | 厦门惠方生物科技有限公司 | Method for preparing coloring semipermeable zirconia presintered body |
| WO2018033800A1 (en) * | 2016-08-18 | 2018-02-22 | Ivoclar Vivadent Ag | Metal oxide ceramic nanomaterials and methods of making and using same |
| CN108703890A (en) * | 2018-04-22 | 2018-10-26 | 杭州而然科技有限公司 | A kind of screening color zirconium oxide prosthesis |
-
2019
- 2019-01-22 CN CN201910057962.3A patent/CN109734446A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0194191A1 (en) * | 1985-03-01 | 1986-09-10 | Rhone-Poulenc Chimie | Stabilized zirconia, process for its preparation and its use in ceramic compositions |
| CN101863659A (en) * | 2010-06-11 | 2010-10-20 | 广东工业大学 | Method for preparing stabilized zirconia superfine powder by stirring ball-milling reaction |
| 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 |
| CN103641472A (en) * | 2013-11-14 | 2014-03-19 | 厦门惠方生物科技有限公司 | Method for preparing coloring semipermeable zirconia presintered body |
| WO2018033800A1 (en) * | 2016-08-18 | 2018-02-22 | Ivoclar Vivadent Ag | Metal oxide ceramic nanomaterials and methods of making and using same |
| CN108703890A (en) * | 2018-04-22 | 2018-10-26 | 杭州而然科技有限公司 | A kind of screening color zirconium oxide prosthesis |
Non-Patent Citations (1)
| Title |
|---|
| 陈安勇等: "CAD/CAM全氧化锆嵌体修复的临床应用", 《中外医学研究》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108748611B (en) | Method for forming ceramic body | |
| KR101276616B1 (en) | Manufacturing method of dental zirconia block with shade gradient | |
| CN107721424B (en) | Method for preparing YAG transparent ceramic by gel casting | |
| JP6359400B2 (en) | Method for producing translucent zirconia sintered body, translucent zirconia sintered body obtained by the production method, and pre-sintered calcined body for producing translucent zirconia sintered body | |
| CN108516818A (en) | A method of YAG crystalline ceramics is prepared based on improved Isobam gel rubber systems | |
| CN104671781B (en) | Preparation method of sky-blue zirconia ceramic | |
| CN112661504B (en) | Preparation method of zirconia dental material | |
| CN110128115A (en) | A kind of method that flash burning prepares oxide eutectic ceramics | |
| CN109095921B (en) | Zirconia ceramic bone implantation prosthesis and preparation method thereof | |
| Jayaseelan et al. | High‐strength porous alumina ceramics by the pulse electric current sintering technique | |
| CN103708830A (en) | Dental colored zirconia ceramic material and its preparation method | |
| CN112851342A (en) | Zirconia ceramic material and preparation method and application thereof | |
| Zhang et al. | Ammonium citrate assisted surface modification and gel casting of YAG transparent ceramics | |
| CN106431360A (en) | Material for dental restoration and method for preparing dental restoration | |
| JPS61261274A (en) | Method of forming powder | |
| CN114656260A (en) | Preparation method and application of medical high-permeability zirconia ceramic sintered body | |
| CN109734446A (en) | A kind of preparation method of zirconia ceramics dummy | |
| CN109516813B (en) | Method for preparing high-light-transmittance AlON transparent ceramic by direct water injection molding | |
| JP2008019144A (en) | Manufacturing method of ceramic composite material containing zirconia | |
| CN104446498B (en) | Manufacturing method of transparent aluminum nitride ceramics | |
| KR101416654B1 (en) | recycling method of residual dental zirconia block through slip casting process | |
| Liu et al. | Pressureless sintering behavior of injection molded alumina ceramics | |
| CN114133270B (en) | Hollow flat plate ceramic filter membrane and preparation method thereof | |
| CN108529673A (en) | The method for producing zirconium dioxide nanometer powder using zirconium dioxide sintering waste material | |
| CN113105216A (en) | Injection-molded zirconium-aluminum composite ceramic and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190510 |