CN101926734B - Process for improving translucency of CAD/CAM in-ceram zirconia dental materials - Google Patents
Process for improving translucency of CAD/CAM in-ceram zirconia dental materials Download PDFInfo
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- CN101926734B CN101926734B CN2010102204698A CN201010220469A CN101926734B CN 101926734 B CN101926734 B CN 101926734B CN 2010102204698 A CN2010102204698 A CN 2010102204698A CN 201010220469 A CN201010220469 A CN 201010220469A CN 101926734 B CN101926734 B CN 101926734B
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Abstract
The invention provides a process for improving translucency of CAD/CAM in-ceram zirconia dental materials, comprising the following steps: a. preparing nano zirconia powder by reverse coprecipitation; b. adding organic bonds for pelleting; c. carrying out dry pressing under 20-30MPa and carrying out static pressure treatment under 200-250MPa to preform green bodies; d. pumping oxygen when the green bodies are sintered to 200-800 DEG C from room temperature, preserving heat for 30min when the green bodies are sintered to 1250 DEG C, then raising the temperature to the final sintering temperature of 1400-1500 DEG C at a rate of 200 DEG C/h and preserving heat for 2h, thus obtaining the in-ceram zirconia materials with translucency. The invention also provides the in-ceram zirconia materials prepared by the method. With the integral transmittance of visible light of 17.50-18.01%, the in-ceram zirconia materials can meet the requirement of the oral clinical in-ceram restorations for beauty.
Description
Technical field
The present invention relates to a kind of improvement oral cavity CAD/semipermeable technology of the full ceramic material of CAM zirconium oxide, belong to the dental prosthesis field of materials.
Background technology
The development of pfm recovery technique is existing over half a century so far, is to use repair mode the most widely at present.Though metal back layer provides effective intensity, influenced seeing through of incident illumination, dummy lacks stereovision and vigor, can not reproduce the color and luster of natural teeth fully.Along with the raising and the improvement of oral cavity material performance, " not having gold " dummy becomes ideal repair mode in the prosthetic dentistry field.Full porcelain dummy obtains increasing patient and the favor of repairing the doctor because of having excellent biological compatibility and optical property.Compare with metal ceramic prosthesis, full porcelain dummy is formed by multilamellar translucent ceramic material sintering, has refractive index and the scattering coefficient approaching with tissue of tooth, can reproduce color and luster, transparency and the stereovision of natural teeth.Therefore, the aesthetic effect of full porcelain dummy is superior.At present commonly used full porcelain system mainly relies on the full porcelain primer of semi permeability difference to come proof strength, obtains good aesthetic through sintering facing porcelain.The facing porcelain is a trnaslucent materials, and the color of bottom porcelain and light transmission will play conclusive effect to the reproduction of dummy final color.Therefore in order to reach the coupling with the natural teeth color and luster, the transmission performance of primer is one of significant effects factor (J Prosthet Dent 1996; 75:18).
Look back the developing history that full porcelain is repaired. its repairing effect true to nature attractive in appearance is approved by numerous doctors and patient already, and its intensity is the focus that people pay close attention to always.The kind of at present full ceramic material is more; Like leucite, lithio porcelain, aluminium oxide, zirconium oxide etc.; Manufacture method is also had nothing in common with each other; Like osmotic ceramic, hot pressing castable ceramic, porcelain deposition, computer-aided design and area of computer aided making (CAD/CAM) etc., its intensity is also increasingly high, and the reparation indication is also more and more wider.In all full ceramic restoration materials, the highest with the bending strength of the full porcelain of CAD/CAM zirconium dioxide.The CAD/CAM recovery technique is that photoelectron technology, computer technology and automatic control Machining Technology are merged the new technique that is used for Oral Repair, and this technology arises from the seventies in 20th century, but is of limited application, and effect is also unsatisfactory.Along with developing rapidly of electronic computer technology and repair materials, relevant this Study on Technology is more and more, and its application in Oral Repair is also more and more wider.China is the full porcelain recovery technique of Application of CAD/CAM zirconium oxide clinically since 2004.(Sun Feng, etc., the full porcelain of CAD/CAM zirconium oxide was rolled up for 4 phases in the application " Shanghai stomatology " in Oral Repair field in 2006 years 15).
Because the undercapacity of ceramic material, fragility is big, has limited its range of application and dependability, and big quantity research concentrates on and improves full ceramic material intensity and toughness, and the full ceramic material of developing high strength, high tenacity.For improving the intensity of full porcelain primer, often adopt means such as composite ceramics, cause semipermeable decline, optical property and mechanical property can't satisfy and optimize simultaneously.1969, Helmer Diskell reported about the application of zirconia ceramics at biomedical sector, thereby has started the research boom of zirconia ceramics as biomaterial.Zirconia ceramics material has characteristics such as transformation toughening, can solve problems such as conventional full ceramic material intensity and toughness deficiency, and it belongs to bio-inert ceramic class material, is used widely at biomedical sector.In dental prosthetic material was used, PSZ (3Y-TZP) can be widely used in the reparation of leaf-comb, three unit bridges even many units of backteeth bridge because of having higher bending strength and fracture toughness, becomes the dental materials hot research in recent years.
Have good mechanical mechanics property although contain zirconic full porcelain primer, its optical property is relatively poor, and visible light transmissivity is lower, can't satisfy the particularly aesthetic requirement of labial teeth district reparation of dummy.The full porcelain of zirconium oxide (In-Ceram Zirconia) contains the tetragonal zirconia polycrystal of 33wt%, and its semi permeability is poor, and almost the same with metal ceramic prosthesis is opaque material (J Prosthet Dent 2002; 88:4).Therefore the optical property of zirconia ceramics is unsatisfactory; Bao Guangjie; Deng, compound additive to the Zirconia reinforced alumina tooth with ceramic semipermeable influence, " Chinese Tissue Engineering Study and clinical rehabilitation "; 2008 12 27 phases of volume, observe compound additive to the Zirconia reinforced alumina tooth with ceramic semipermeable influence.And the report that can be used for the full ceramic material semi permeability of oral cavity zirconium oxide improved process is not arranged as yet so far.
Summary of the invention
Technical scheme of the present invention has provided a kind of improvement oral cavity CAD/semipermeable technology of the full ceramic material of CAM zirconium oxide.The full ceramic material of zirconium oxide that another technical scheme of the present invention has provided this prepared.
The invention provides a kind of improvement oral cavity CAD/semipermeable technology of the full ceramic material of CAM zirconium oxide, it comprises the steps:
A, the reverse coprecipitation of employing prepare nano zirconium oxide powder;
B, the pelletize of adding organic bond;
C, under the 20-30Mpa condition, dry-pressing formed, handle the preformation base substrate again through the 200-250MPa static pressure;
D, sintering: when the room temperature intensification is sintered to 200-800 ℃, lead to oxygen, be sintered to 1250 ℃, be incubated 30 minutes, rise to final sintering temperature 1400-1550 ℃ then, temperature retention time 2h, heating rate are 200 ℃/h, obtain to have the full ceramic material of semipermeable zirconium oxide.
Wherein, the particle mean size≤40nm of the described powder body of a step.
Wherein, the described organic bond of b step is a polyvinyl alcohol; Described prilling process is a spray drying method.
Further preferably, the described final sintering temperature 1400-1500 of d step ℃.
The step that the reverse coprecipitation that the present invention adopts prepares nanometer 3Y-TZP is: with high-purity Y
2O
3Powder is dissolved in rare nitric acid, heats on the magnetic force heating stirrer, obtains Y (NO
3)
3Crystallization; With presoma zirconates ZrOCl
28H
2O and Y (NO
3)
3Crystallization is heated together and is dissolved in the dehydrated alcohol, filters and removes impurity; Above-mentioned solution branch is packed in the separatory funnel, splash in the 2M excess of ammonia hydrous ethanol solution with 50/min speed, control PH＞9, reaction will be deposited on the bottle,suction and filter, and use the dehydrated alcohol cyclic washing after accomplishing.Filter cake is put into 100 ℃ of oven dry of baking oven 24 hours, calcines after pulverizing and makes nanometer ZrO
2Powder, the powder granularity scope is controlled at 20-40nm.
Adopt spray drying method to add organic bond pelletizes such as polyvinyl alcohol, granule is spherical, and about 50 microns of normal diameter has good flowability, helps obtaining maximum bulk density, improves green density.The main component of Zirconium powder: Y
2O
3, Al
2O
3, SiO
2, Fe
2O
3, Na
2O, the quality percentage composition is respectively: 5.24%, 0.26%, 0.007%, 0.002%, 0.024%.
Wherein, the described dry-pressing formed time of handling with static pressure of c step is 1 minute.Suppress the zirconium oxide base substrate of cylindrical or disc: above-mentioned powder is poured in the ready-formed cylindrical stainless steel mould with funnel; The internal diameter of mould is 15mm; Mould is placed on and adds powder on the agitator, guarantees powder body accumulation uniformity, and powder surface is equal with the mould upper surface; Then mould is put into extrusion forming on the powder compressing machine, pressing speed is slow, can not be overweight when beginning to pressurize, guarantee the abundant discharge of powder air; Prevent blank cracking, 20-30MPa gently pressed 1 minute, with core rod biscuit was ejected, and then the biscuit that obtains was used the rubber finger bag jacket; After the sealing of vacuum pump evacuation, isostatic cool pressing 200-250MPa, 1 minute time; From rubber finger bag, take out base substrate at last, base substrate is an opaque and white, and structure and density are comparatively even.
Wherein, the described sintering process of d step is to be sintered to 1250 ℃ from room temperature, is incubated 30 minutes, is warming up to final sintering temperature 1400-1500 ℃ then, and temperature retention time 2h, heating rate are 200 ℃/h.Concrete sintering process is: base substrate is put into alumina crucible, and with the embedding of aluminium oxide microballon, base substrate is positioned at last 1/3 of crucible; Surface coverage aluminium oxide investment; Place in the high temperature sintering furnace and calcine, sintering schedule is following: under air atmosphere, from 1250 ℃ of room temperature sintering, be incubated 30 minutes; Be warmed up to 1400,1450 or 1500 ℃ then, cool to room temperature with the furnace behind the insulation 2h, heating rate is 200 ℃/h, and logical oxygen obtains to have the full ceramic material of semipermeable zirconium oxide in the 200-800 ℃ of sintering process.
The present invention also provides the oral cavity CAD/full ceramic material of CAM zirconium oxide of this improved process preparation.
Wherein, the visible light integration absorbance of described zirconium oxide primer is 17.50-18.01%.
The optical property of ceramic material is relevant with composition with microstructure, and crystal has heterogeneity, and the coefficient of refraction difference is big more, and the incident scattering of light is many more with absorption, and its semi permeability is poor more.The zirconium oxide coefficient of refraction is 2.20, and the air refraction coefficient is 1.00, and the coefficient of refraction of glassy phase substrate is 1.50, therefore should guarantee the unicity of crystal structure as far as possible for the absorbance that improves zirconia material, reduces the porosity, reaches dense sintering.
Technology of the present invention is accomplished the selection design of granularity through the original Zirconium powder granularity of the synthetic control of reverse coprecipitation, adopts the spray drying method pelletize; Guarantee the flowability of powder, improve the bulk density of green compact, improvement forming technique and sintering process; Reduce the porosity of sintered body; The pressureless sintering condition is issued to complete densification, guarantees the concordance of tetragonal phase zirconium oxide crystal grain, thereby improves the absorbance of the full ceramic material of CAD/CAM zirconium oxide.
Compare with existing Technology, the present invention has following distinguishing feature:
1, the synthetic particle size distribution 20-40nm PSZ of reverse coprecipitation because of having higher surface activity and sintering power, reduces sintering temperature as original powder body.That raw material has is high-purity, ultra-fine, the characteristic of polymolecularity and even particle size distribution.
2, spray drying method pelletize, the powder particle size distribution is even, guarantees the flowability of powder, obtains maximum bulk density, improves the density of green compact.
3, powder body pours into behind the mould on powder compressing machine that 20-30MPa is light to press molding in 1 minute, and biscuit use the rubber finger bag jacket, and the evacuation sealing is afterwards at 1 minute preformation base substrate of the inferior static pressure of 200-250MPa pressure, and blank structure and density are comparatively even.
4, conventional pressureless sintering, final sintering temperature is controlled at 1400-1500 ℃, and heating rate is 200 ℃/h, and its relative density reaches more than 99%, can guarantee basic densification, improves absorbance.
5, through the regulation and control of synthetic selection of raw material and sintering schedule, crystal grain is monophasic tetragonal zircite, even structure behind the sintering.
6, logical oxygen in the low-temperature zone sintering guarantees burnouting fully of organic bond in the pelletize, reduces the introducing of second phase.
Description of drawings
Fig. 1: the section SEM pattern of biscuit, particle size 20-40nm, size distribution is even.
Fig. 2-4: being respectively final sintering temperature is the section SEM figure of 1400 ℃, 1450 ℃, 1500 ℃ sintered bodies, and section does not have obvious pore, and crystal grain is tetragonal zirconia polycrystal.Crystallite dimension raises with temperature and grows up, and grain size is about 200-400nm, is evenly distributed.The crystallite dimension of 1500 ℃ of sintered bodies is obviously bigger, and crystal grain merges, and bigger crystal grain is about 400-600nm, and crystal boundary is obvious.
The specific embodiment
The contrast test of embodiment 1 technology of the present invention and existing technology
Sample performance according to this improved process processing is seen table 1, Cercon porcelain piece is carried out sintering for 1350 ℃ according to the sintering temperature of manufacturer's recommended, and process the sample of the same specification of thick 0.50 ± 0.01mm, as the matched group sample.The result sees table 1:
The optical property and the mechanical property of table 1 oral cavity CAD/full ceramic material of CAM zirconium oxide
Visible by table 1; The full ceramic material of the zirconium oxide of prepared of the present invention is through after controlling powder granularity and sintering temperature; Sintered density, transmitance and three-point bending strength all are higher than Cercon, and at 1400-1500 ℃, the sample relative density that 0.5mm is thick is 99.15-99.39%; Visible light integration transmitance is 17.50-18.01%, can satisfy the optics and the mechanical property requirements of mouth mending material fully.If when temperature surpassed 1500 ℃, excessive grain was grown up, relative density and three-point bending strength descend to some extent.
Above-mentioned description of test; Among the preparation technology of the full ceramic material of zirconium oxide of the present invention, sintering temperature can guarantee higher visible light integration absorbance in 1400-1550 ℃ of scope; And relative density is high; Intensity is big, wherein more preferably with sintering temperature in 1400-1500 ℃ of scope, more can satisfy the semi permeability and the hardness requirement of the full ceramic material of zirconium oxide simultaneously.
The preparation of embodiment 2 oral cavity CADs of the present invention/full ceramic material of CAM zirconium oxide
Pass through ZrOCl
28H
2O adopts reverse coprecipitation to make nanometer ZrO
2Powder: at first with high-purity Y
2O
3Powder is dissolved in the rare nitric acid of 2M, heats on the magnetic force heating stirrer, obtains Y (NO
3)
3Crystallization; With presoma zirconates ZrOCl
28H
2O and Y (NO
3)
3Crystallization is heated together and is dissolved in the dehydrated alcohol, is mixed with the 0.3M alcoholic solution, filters and removes impurity; Above-mentioned solution branch is packed in the separatory funnel, splash in the 2M excess of ammonia hydrous ethanol solution with 50/min speed, control PH＞9, reaction will be deposited on the bottle,suction and filter, and use the dehydrated alcohol cyclic washing after accomplishing.Filter cake is put into 100 ℃ of oven dry of baking oven 24 hours, calcines after pulverizing and makes nanometer ZrO
2Powder, the powder granularity scope is controlled at 20-40nm, adopts spray drying method to add organic bond pelletizes such as polyvinyl alcohol, and granule is spherical, about 50 microns ± 10 microns of normal diameter.The above-mentioned Zirconium powder of 0.48g is poured in the cylindrical die of prefabricated internal diameter 15mm, and light pressure of 20-30MPa became disk in 1 minute on powder compressing machine, and the test specimen of preparation is used the rubber finger bag jacket, after the evacuation sealing, and isostatic cool pressing 200MPa, 1 minute time.Base substrate is put into alumina crucible, uses the alumina balls embedding, places in the high temperature sintering furnace and calcines, and under air atmosphere, is sintered to 1250 ℃ from room temperature, is incubated 30 minutes; Be warmed up to 1400 ℃ then, cool to room temperature with the furnace behind the insulation 2h, heating rate is 200 ℃/h, logical oxygen in the 200-800 ℃ of sintering process.The disk test specimen carries out step by step sanding and polishing to minute surface with diamond polishing cream (25 μ m, 10 μ m, 5 μ m, 1 μ m).The disk specification is thick 0.50 ± 0.01mm, and totally 5 samples supply to measure visible light integration absorbance.Make 3 cylinder specimens with the 5.70g powder body as stated above, measure sintered density.
The measuring method of sintered density and relative density: adopt the Archimedes method to measure the sintered density of porcelain piece.Computing formula is following:
W
D: the dry weight of sintering test specimen.After cylinder specimen placed 80 ℃ of dry 24h of baking oven, analytical balance weighing test specimen dry weight.
W
SS: the buoyant weight of sintering test specimen.Test specimen is put into boiling water boils 1h, be cooled to room temperature after, the buoyant weight of the saturated test specimen of weighing in water.
W
S: the weight in wet base of sintering test specimen.Test specimen is taken out from water, wipe test specimen surface redundant moisture, rapidly the aerial weight in wet base of the saturated test specimen of weighing.
ρ
W: the density (0.9982g/cm of water under 20 ℃ of room temperatures
3).
Each test specimen is measured 3 times, averages.
The computing formula of relative density is following:
D＝ρ/ρ
0×100％
ρ
0Solid density (6.10g/cm for tetragonal zircite (3Y-TZP)
3).
The measuring method of visible light integration absorbance: adopt spectrophotometer to measure, light source, disk test specimen, spectrophotometer are popped one's head in point-blank, guarantee incident illumination vertical incidence, the light intensity (I of first recording light source through regulating hot spot
0), measuring light is passed the intensity (I) of test specimen to be measured again, calculates the approximate absorbance of test specimen, and formula is: T=(I/I
0) * 100%.Every at the 400-780nm visible region at a distance from 10nm continuous measurement absorbance, obtain the visible light integration absorbance of test specimen.The measuring light spot diameter is 4mm, and each test specimen is measured and got average 3 times.
The zirconium oxide test specimen sintered density that this embodiment obtains is 6.0626 ± 0.0071g/cm
3, relative density reaches 99.39%, reaches densification basically, and visible light integration absorbance is 17.50 ± 0.47%.Scanning electron microscope section observation crystal is tetragonal zircite crystal grain, and crystallite dimension 200-300nm is evenly distributed, and sintered body is fine and close, does not see tangible hole.
Wherein, the preparation of described nano zirconium oxide powder also can be adopted other method preparation, as: Yin Wanzhong, etc., the reverse precipitation legal system is equipped with the dentistry nano zirconium oxide powder, modern stomatology magazine, 2006 the 20th the 3rd phases of volume, reported method.
The preparation of embodiment 3 oral cavity CADs of the present invention/full ceramic material of CAM zirconium oxide
Final sintering temperature is 1450 ℃ in the sintering schedule, and other conditions and technology are with embodiment 2.The zirconium oxide test specimen sintered density that this embodiment obtains is 6.0627 ± 0.0074g/cm
3, relative density reaches 99.39%, reaches densification basically, and visible light integration absorbance is 17.83 ± 0.16%.Scanning electron microscope section observation crystal is tetragonal zircite crystal grain, and crystallite dimension 200-400nm is evenly distributed, and sintered body is fine and close, does not see tangible hole.
The preparation of embodiment 4 oral cavity CADs of the present invention/full ceramic material of CAM zirconium oxide
Final sintering temperature is 1500 ℃ in the sintering, and other conditions and technology are with embodiment 2.The zirconium oxide test specimen sintered density that this embodiment obtains is 6.0481 ± 0.0045g/cm
3, relative density reaches 99.15%, reaches densification basically, and visible light integration absorbance is 18.01 ± 0.07%.Scanning electron microscope section observation crystal is tetragonal zircite crystal grain, and crystallite dimension is obviously bigger, and crystal grain merges, and bigger crystal grain is about 400-600nm, and crystal boundary is obvious.
In sum, the full ceramic material visible light of zirconium oxide of the present invention integration absorbance can reach 17.50-18.01%, can satisfy the demand attractive in appearance of the full porcelain dummy of clinical oral.
Claims (8)
1. improve oral cavity CAD/semipermeable technology of the full ceramic material of CAM zirconium oxide for one kind, it comprises the steps:
A, the reverse coprecipitation of employing prepare nanometer 3Y-TZP: with high-purity Y
2O
3Powder is dissolved in rare nitric acid, heats on the magnetic force heating stirrer, obtains Y (NO
3)
3Crystallization; With presoma zirconates ZrOCl
28H
2O and Y (NO
3)
3Crystallization is heated together and is dissolved in the dehydrated alcohol, filters and removes impurity; Above-mentioned solution branch is packed in the separatory funnel, splash in the 2M excess of ammonia hydrous ethanol solution with 50/min speed, control PH＞9, reaction will be deposited on the bottle,suction and filter, and use the dehydrated alcohol cyclic washing after accomplishing; Filter cake is put into 100 ℃ of oven dry of baking oven 24 hours, calcines after pulverizing and makes nanometer ZrO
2Powder, the powder granularity scope is controlled at 20-40nm;
B, the pelletize of adding organic bond;
C, under the 20-30Mpa condition, dry-pressing formed, handle the preformation base substrate again through the 200-250MPa static pressure;
D, sintering: when room temperature is sintered to 200-800 ℃, lead to oxygen, be sintered to 1250 ℃, be incubated 30 minutes, rise to final sintering temperature 1400-1550 ℃ then, temperature retention time 2h, heating rate are 200 ℃/h, obtain to have the full ceramic material of semipermeable zirconium oxide.
2. technology according to claim 1 is characterized in that: the particle mean size≤40nm of the described powder body of a step.
3. technology according to claim 1 is characterized in that: the described organic bond of b step is a polyvinyl alcohol; Described prilling process is a spray drying method.
4. according to claim 1 or 3 described technologies, it is characterized in that: the described particle diameter of b step is 50 microns ± 10 microns.
5. technology according to claim 1 is characterized in that: the described dry-pressing formed time of handling with static pressure of c step is 1 minute.
6. technology according to claim 1 is characterized in that: the described final sintering temperature 1400-1500 of d step ℃.
7. the oral cavity CAD of any described prepared of claim 1-6/full ceramic material of CAM zirconium oxide.
8. the full ceramic material of zirconium oxide according to claim 7 is characterized in that: the visible light integration absorbance of described zirconium oxide primer is 17.50-18.01%.
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