CN107162603A - A kind of flash sintering method of dental zirconia ceramics - Google Patents
A kind of flash sintering method of dental zirconia ceramics Download PDFInfo
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- CN107162603A CN107162603A CN201710416781.6A CN201710416781A CN107162603A CN 107162603 A CN107162603 A CN 107162603A CN 201710416781 A CN201710416781 A CN 201710416781A CN 107162603 A CN107162603 A CN 107162603A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C13/00—Dental prostheses; Making same
- A61C13/08—Artificial teeth; Making same
- A61C13/083—Porcelain or ceramic teeth
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/15—Compositions characterised by their physical properties
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- 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
- A61K6/818—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising zirconium oxide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Oral & Maxillofacial Surgery (AREA)
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- Composite Materials (AREA)
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- Inorganic Chemistry (AREA)
- Dental Prosthetics (AREA)
- Dental Tools And Instruments Or Auxiliary Dental Instruments (AREA)
Abstract
The invention discloses a kind of flash sintering method of dental zirconia ceramics, it is characterised in that：120 DEG C/min Fast Sintering stove is reached with the programming rate of my company's design, dental material using the 3%molY stabilizing zirconias of the current main flow of dentistry and 5%molY stabilizing zirconias is raw material, material is deacclimatized by the control to sintering method, the 3%molY stabilizing zirconias and 5%molY stabilizing zirconias of the current main flow of dentistry is sintered in 0.5 1.5h while finish, tooth can be made to reach the effect tooth effect (completely material will not be made to spend reduction thoroughly) as traditional 7h 15h sintering methods of the current main flow of dentistry.
Description
Technical field
The present invention relates to the flash sintering method of dental zirconia ceramics, belong to oral cavity material field.
Background technology
The expansion applied recently as zirconium oxide in oral cavity material field, the zirconium oxide dental polishing of existing a variety of brands
Material is listed.There is advantages below compared to baking-ceramic tooth zirconia ceramics:1st, optimal aesthetic effect：Zirconium oxide good in optical property, changes
Learn property stable, the baking-ceramic tooth light translucency pretended out is well relatively true, and is bumped into rear neck unlike other metals can become blacking
Dark pastiness.2nd, optimal biocompatibility：Zirconium oxide thermal conductivity factor is small to be beneficial to dental pulp protection, because tool acid and alkali-resistance inoxidizability is to gum
It is nontoxic it is non-stimulated do not corrode without allergy, its biocompatibility be better than various metals.3rd, optimal precision and marginal fit：Zirconium oxide
Good mechanical property toughness high plasticity is easy to process by force, can guarantee that the accurate and fine edge seal of hat in mould, porcelain tooth is with suffering from
The intraoral abutment of person suits the root of the tooth class incidence of disease after reduction is repaired.
But, current this material of zirconium oxide, because its hardness is excessive, leads to not directly processing.
So as to use following methods on the market at present：Patient teeth is designed in computer using some softwares, it
Afterwards, by not fully sintered zirconia green body, by way of automating 3D cutting processings, it is processed into patient teeth's shape；So
The zirconium oxide of patient teeth's shape is sintered again afterwards, is that patient carries out dental operation by the zirconium oxide after sintering.
Wherein, patient needs first to grind off the tooth of original lesion locations, and doctor could carry out tooth impression-taking, so that according to
Modelling tooth.So as to, whole Zirconium oxide sintering process, all tooth without lesion locations in patient mouthful.At present on the market,
Zirconium oxide sintering needs 7-15h, i.e. in the case that patient at least will be with not some teeth, wait more than 1 day.(often because
For want it is secondary remove clinic the problem of, often want several days) this period, dining is a very painful process.
The patent of zirconium oxide Fast Sintering is had at present, and achieves certain effect.Wu Jia is strong et al. (referring to dental
Zirconium oxide swivel chair formula Fast Sintering stove, the patent No. 201610315918.4) design one it is bright by stepper motor, control keyboard, stove
Complete the sintering furnace of zirconia material the energy Rapid Circulation that body and heating rod are constituted.Tian Wanhong et al. is (referring to one kind oxidation
The improvement of zircon ceramic microwave sintering method and use, the patent No. 201310393378.8) heated in microwave energy heat energy mode,
Helped with carborundum thermosphere material make zirconia ceramics temperature lifted to zirconium oxide can with the temperature of own absorption microwave so that
Zirconia ceramics reaches the temperature of sintering under microwave action, realizes the purpose of Fast Sintering.Two above patent is all changing
Enter to design sintering furnace, reach the purpose of Fast Sintering, have ignored the high-temperature shrinkage speed of zirconia material in itself to density and
The influence of hardness, is extremely difficult to conventional sintering stove to Zirconium oxide sintering effect.
And in dental field, zirconium oxide there must be certain degree thoroughly, just seem consistent with people's tooth, because people's tooth also has one
Fixed degree thoroughly.The zirconium oxide for degree of losing is as stone, it is difficult to be received by dentistry.
The present invention, is just intended to greatly reduce patient's pain time and (so that patient can just treat and finish on the same day, is gone without secondary
Clinic) while, it is ensured that the saturating degree of its zirconium oxide tooth, make it consistent with people's tooth.
The content of the invention
The technical problems to be solved by the invention are the flash sintering method of dental zirconia ceramics, and this method was both real
The Fast Sintering of existing 3%mol-5%molY stabilizing zirconia teeth；It can reach again being burnt slowly with conventional sintering stove 7h-15h
Effect so that reach oral cavity field can repair purpose.
The technical scheme is that：
The tooth of the 3%mol-5%molY stabilizing zirconias of the current main flow of dentistry is as raw material, by sintering method
Control deacclimatize material, reach with normally sinter effect.The program total duration 0.5-1.5h, especially 0.75h-
1.3h。
The flash sintering method of dental zirconia ceramics as described above, the preparation of the zirconia ceramics complete crown tooth,
Specially：
Turning is carried out to the 3%mol-5%molY stabilizing zirconia porcelain block of the current main flow of dentistry, standard film (15*8* is obtained
3mm) and tooth.Heating and cooling program is set first, 1000-1200 DEG C is risen to 120 DEG C/min speed, it is then quick by furnace bottom
Lower, place tooth, 1530-1550 DEG C is risen to 7-17 DEG C/min heating rate, be incubated 10-30min.After cooling,
Take out tooth.
Flash sintering method as described above, heating rate and soaking time after stove are entered by adjusting standard film, with point
The change of the light transmittance of light photometer D65 test of light source teeth.
Advantage of the invention is that：The Fast Sintering of zirconia ceramics is the method achieve, 1-1.5h is foreshortened to, compared
The 7-15h of conventional sintering, because the shortening of time, patient can finish in same day treatment, if arrangement of time is appropriate, even without
Delay the dining on the same day.Sintering effect is consistent with conventional sintering simultaneously, reaches the requirement of aesthetic orthopaedics.And have energy consumption
Small, equipment is simple, many advantages, such as with low cost.
Embodiment
The flash sintering method of the present invention is further described below in conjunction with specific embodiment：
Embodiment 1
Turning is carried out to the 3%mol stabilizing zirconia porcelain block of the current main flow of dentistry, standard film and backteeth complete crown is obtained.Point
It is not sintered with conventional sintering stove and fast-burning furnace.Fast-burning furnace rises to 1200 DEG C with 100 DEG C/min speed, then with 10 DEG C/min
Heating rate rise to 1550 DEG C, be incubated 20min, tooth and standard film taken out after cooling；Conventional sintering stove is with 10 DEG C/min's
Speed rises to 900 DEG C, and after 900 DEG C are incubated 30min, 1550 DEG C are warming up to 5 DEG C of speed per minute, in 1550 DEG C of insulations
120min, takes out tooth and standard film after cooling.
Standard film is tested with spectrophotometer D65 light sources degree of progress respectively, Vickers hardness is tested with hardometer, measures
Degree is 42%, Vickers hardness 1496 thoroughly；Conventional sintering stove sintering standard film spends 42%, Vickers hardness 1504 thoroughly.Both data bases
This is consistent.Backteeth complete crown outward appearance is sintered without any difference with ordinary sinter stove.
Embodiment 2
Turning is carried out to the 5%mol stabilizing zirconia porcelain block porcelain block of the current main flow of public dentistry, standard film is obtained and backteeth is complete
Hat.It is sintered respectively with conventional sintering stove and fast-burning furnace.Fast-burning furnace rises to 1200 DEG C with 120 DEG C/min speed, then with 7
DEG C/min heating rate rises to 1530 DEG C, 25min is incubated, tooth and standard film are taken out after cooling；Conventional sintering stove with 5 DEG C/
Min speed rises to 900 DEG C, after 900 DEG C are incubated 30min, 1530 DEG C is warming up to 3 DEG C of speed per minute, at 1530 DEG C
120min is incubated, tooth and standard film are taken out after cooling.
Standard film is tested with spectrophotometer D65 light sources degree of progress, Vickers hardness is tested with hardometer, measures fast burning
Degree is 49%, Vickers hardness 1461 to zirconium oxide thoroughly；Conventional sintering stove sintering standard film spends 49%, Vickers hardness 1452 thoroughly.Both
Data are basically identical.Backteeth complete crown outward appearance is sintered without any difference with ordinary sinter stove.
Claims (5)
1. a kind of flash sintering method of dental zirconia ceramics, it is characterised in that：With the 3%mol- of the current main flow of dentistry
The dental material of 5%molY stabilizing zirconias is raw material, deacclimatizes material by the control to sintering method, dentistry is led at present
The 3%mol-5%molY stabilizing zirconias of stream can be sintered in 0.5-1.5h and finished, and not reduce above-mentioned zirconia material
Saturating degree.
2. the flash sintering method of dental zirconia ceramics as claimed in claim 1, it is characterised in that：Tooth room temperature-
At 1200 DEG C, heating rate is 80 DEG C/min-120 DEG C/min, greatly shortens the sintering furnace heating and cooling time.
3. the flash sintering method of dental zirconia ceramics as claimed in claim 1 or 2, it is characterised in that：In 1200-1550
Heating rate cannot be below 17 DEG C/min (especially 17 DEG C/min-7 DEG C/min is optimum temperature rise speed), the process in the range of DEG C
For this Material shrinkage process of zirconium oxide, too fast heating can make zirconium oxide tooth can serious degree of losing, influence the aesthetics of tooth
Effect.
4. the flash sintering method of dental zirconia ceramics as claimed in claim 1, it is characterised in that：Tooth is in 1530-
During 1550 DEG C of highest temperatures, soaking time is：10min-30min.
5. by the way that as described in claim 2,3, this heating mode first quick and back slow goes to cater to this ceramic material of zirconium oxide
High-temperature shrinkage process, reach i.e. quick, ensure the saturating degree of zirconium oxide tooth again, so as to ensure the aesthetic effect of tooth.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019166938A1 (en) | 2018-02-28 | 2019-09-06 | 3M Innovative Properties Company | Process for producing a dental zirconia article with a fast sintering process |
| CN110790572A (en) * | 2019-12-11 | 2020-02-14 | 深圳市家鸿口腔医疗股份有限公司 | Zirconia dental crown and preparation method and application thereof |
| KR20200022348A (en) | 2018-08-22 | 2020-03-03 | 소후 인코포레이티드 | Zirconia mill blank for dental cutting and machining and preparing method thereof |
| KR20200090640A (en) | 2019-01-21 | 2020-07-29 | 소후 인코포레이티드 | High permeable zirconia blank capable of sintering at high speed |
| WO2020178712A1 (en) | 2019-03-04 | 2020-09-10 | 3M Innovative Properties Company | Process for producing a colored dental zirconia article |
| EP4008699A1 (en) * | 2019-08-01 | 2022-06-08 | Kuraray Noritake Dental Inc. | Method for producing zirconia sintered compact |
| EP4079702A4 (en) * | 2019-12-20 | 2024-01-24 | Kuraray Noritake Dental Inc. | Method for producing zirconia sintered compact |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019166938A1 (en) | 2018-02-28 | 2019-09-06 | 3M Innovative Properties Company | Process for producing a dental zirconia article with a fast sintering process |
| US20210093517A1 (en) * | 2018-02-28 | 2021-04-01 | 3M Innovative Properties Company | Process for producing a dental zirconia article with a fast sintering process |
| KR20240116433A (en) | 2018-08-22 | 2024-07-29 | 소후 인코포레이티드 | Zirconia mill blank for dental cutting and machining and preparing method thereof |
| KR20200022348A (en) | 2018-08-22 | 2020-03-03 | 소후 인코포레이티드 | Zirconia mill blank for dental cutting and machining and preparing method thereof |
| EP3636621A2 (en) | 2018-08-22 | 2020-04-15 | Shofu Inc. | Zirconia mill blank for dental cutting and machining and preparing method thereof |
| US11986362B2 (en) | 2018-08-22 | 2024-05-21 | Shofu Inc. | Zirconia mill blank for dental cutting and machining and preparing method thereof |
| EP3712121A1 (en) | 2019-01-21 | 2020-09-23 | Shofu Inc. | High permeable zirconia blank capable of sintering at high speed |
| KR20200090640A (en) | 2019-01-21 | 2020-07-29 | 소후 인코포레이티드 | High permeable zirconia blank capable of sintering at high speed |
| WO2020178712A1 (en) | 2019-03-04 | 2020-09-10 | 3M Innovative Properties Company | Process for producing a colored dental zirconia article |
| CN113508100A (en) * | 2019-03-04 | 2021-10-15 | 3M创新有限公司 | Method for preparing colored dental zirconia articles |
| CN113508100B (en) * | 2019-03-04 | 2023-09-29 | 3M创新有限公司 | Method for preparing a coloured dental zirconia article |
| EP4008699A1 (en) * | 2019-08-01 | 2022-06-08 | Kuraray Noritake Dental Inc. | Method for producing zirconia sintered compact |
| EP4008699A4 (en) * | 2019-08-01 | 2023-08-30 | Kuraray Noritake Dental Inc. | Method for producing zirconia sintered compact |
| CN110790572A (en) * | 2019-12-11 | 2020-02-14 | 深圳市家鸿口腔医疗股份有限公司 | Zirconia dental crown and preparation method and application thereof |
| EP4079702A4 (en) * | 2019-12-20 | 2024-01-24 | Kuraray Noritake Dental Inc. | Method for producing zirconia sintered compact |
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