CN103641166B - Method for preparing dental colored zirconia powder - Google Patents
Method for preparing dental colored zirconia powder Download PDFInfo
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- CN103641166B CN103641166B CN201310576990.9A CN201310576990A CN103641166B CN 103641166 B CN103641166 B CN 103641166B CN 201310576990 A CN201310576990 A CN 201310576990A CN 103641166 B CN103641166 B CN 103641166B
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Abstract
The invention relates to a method for preparing dental colored zirconia powder, and specifically relates to a method for preparing nanometer zirconia powder. The method comprises: putting zirconia nanometer powder 3Y-TZP with a particle size of 30-50 nm, a coloring agent and a dispersant in a bowl mill to perform long-time ball milling, adding an adhesive into the obtained product, then putting in a bowl mill to perform ball milling for preparing a slurry; and conveying the slurry to a spray drying tower to perform spray granulation processing, so as to obtain the spherical dental colored zirconia powder with an average diameter of 40-85 mu m. The colored zirconia powder prepared by employing the method has the advantages of being regular in shape, less in hard agglomeration, uniform in sintering, and the like; and a dental restoration body prepared after the colored zirconia powder is sintered has the bending strength of 710 MPa or more, has the fracture toughness of 4.8 MPa*m<1/2> or more, has the visible light transmittance of 30% or more, is uniform in coloring, and helps to enable tooth coloring to be simple and practicable.
Description
Technical field
The present invention relates to a kind of preparation method of nano zirconium oxide powder.
Background technology
Current uncoloured dental zirconia material is many arrives ivory white in white, the dentures repai surface made of this zirconia material needs to hide look process, this will make denture prosthesis lose the part transparency, and lack the sense of reality, the requirement of dental clinic to denture prosthesis color cannot be met.If zirconia material self color is adjusted to and intends to repair the lightness of tooth, colourity, saturation ratio are close, dummy will be made to match colors and to become simple, the preparation amount of abutment tooth body can be reduced simultaneously.
Usual zirconia material is painted can two kinds of methods, and one can add coloring oxide in Zirconium powder; Pre-sintered zirconium oxide immerses in the staining fluid containing metal oxide and permeates by another kind method, then sinters.The method of penetration dyeing liquid is simple to operate, but easily produces painted uneven situation, and the impact operated is larger.And coloring oxide is added in zirconia material is produced, and color can be controlled accurately homogeneous, and less on the translucency impact of material, be a kind of more satisfactory color solution.As mentioned Tetragonal polycrystal zirconia (the be called for short 3Y-TZP zirconium white) micro mist that is made up of 3mol% yttrium oxide+97mol% zirconium white in Chinese patent application CN1593371A " a kind of preparation method of dental prosthesis " with ferric oxide or/and cerium oxide mixes, extrusion forming after adding additives granulation, sinter into after making biscuit of ceramics and partially sinter ceramic block, again through CAD/CAM processing, finally do fully sinteredly obtaining denture prosthesis.The dental prosthesis that method disclosed in the document is obtained, physical strength is high, and flexural strength can reach 600-710MPa, fracture toughness property 4-4.8MPam1/2, has certain light transmission, and color can regulate in advance.But be through actual measurement, the dental prosthetic body thickness that the method obtains is that the visible light transmittance rate of the measure sample of 1mm is only 8-10%, finally causes the translucency of denture prosthesis can not meet clinical needs.
Summary of the invention
The present invention aims to provide a kind of method preparing dental coloring zirconia powder, and the physical strength of the dental prosthesis that the colored zirconium oxide powder of gained is made is not less than existing level, but visible light transmittance rate can significantly improve, to meet clinical needs.
Technical scheme of the present invention is: a kind of method preparing dental coloring zirconia powder, comprises the following steps:
Step a, prepares by coprecipitation method the 3Y-TZP zirconia nano-powder that grain diameter is 30-50nm;
Step b, after adding tinting material and dispersion agent, puts into ball mill and carries out milled processed in this zirconia nano-powder, uses mechanical force crumbling method to eliminate hard aggregation; Described tinting material is the mixture of ferric oxide and cerium oxide or the mixture of ferric oxide and bismuth oxide, and wherein the addition of cerium oxide is the 1-4% of this zirconia nano-powder and this tinting material total mass; The addition of ferric oxide is the 0.06-0.15% of this zirconia nano-powder and this tinting material total mass; The addition of bismuth oxide is the 0.05-0.2% of this zirconia nano-powder and this tinting material total mass.
Step c, adds adhesive polyethylene alcohol, puts into ball mill ball milling 2-4 hour, obtain slurry in the product that grinding obtains; Wherein, polyvinyl alcohol addition is the 0.5-3% of this grinding product quality;
Steps d, carries out mist projection granulating process by described slurry transferring to spray-drying tower, obtains distribution of SMD at the spherical dental coloring zirconia powder of 40-85 μm.
The present inventor finds in the research to zirconium white denture prosthesis translucency, and the key factor affecting translucency is porosity after 3Y-TZP zirconia material dense sintering and grain boundary structure.Compare the impact of grain boundary structure on translucency, porosity is larger on scattering of light impact.Porosity is lower translucent higher.Therefore, 3Y-TZP zirconia material must be made to be easy to form the low grain boundary structure of porosity after sintering.The present inventor finds further, and the grain diameter of nano level 3Y-TZP zirconia powder is smaller, and particle surface energy is very big, easily hard aggregation occurs between particle; The textural defect such as the 3Y-TZP Zirconium powder sphericity after this will cause granulation is not high, configuration of surface is irregular, easy generation inside has bubble even broken are the major obstacles that the above-mentioned target of impact is reached.
The present invention prepares the method for dental coloring zirconia powder on the basis of lot of experiments, have selected 3Y-TZP zirconium white that grain diameter is 30-50nm and compound color matching is carried out to dental prosthesis translucency and the less tinting material of Effect on Mechanical Properties, use dispersion agent and the mechanical mill of long period, the hard aggregation that not only can reduce particle can also make tinting material be uniformly distributed simultaneously; The spherical dental coloring zirconia powder made after granulation has regular shape, surface is mellow and full, sphericity is high, good fluidity, processability excellent, hard aggregation is few and sinter the advantages such as even.Experiment proves, spherical dental colored Zirconium powder diameter after zirconia nano-powder selects this particle size range of 30-50nm and granulation is 40-85 μm is complementary within the scope of this, the particle diameter of zirconia nano-powder is less than 30nm, not only produce that difficulty is large, production cost is high, and hard aggregation serious, be difficult to eliminate; The particle diameter of zirconia nano-powder is greater than 50nm, or the particle diameter of spherical dental coloring zirconia powder can not control 40-85 μm of scope, be unfavorable in follow-up sintering process, keeping zirconic internal structure not to be destroyed, and zirconia grains diameter range is controlled at light transmission preferably below 400nm.According to this parameter matching, be easy to form the low cube grain boundary structure of porosity after sintering.Realize the goal of the invention of the present invention's " physical strength of the dental prosthesis that the colored zirconium oxide powder of gained obtains is not less than existing level, but visible light transmittance rate can significantly improve, to meet clinical needs ".
In a preferred embodiment: the ball mill in described step B adopts planetary ball mill, described dispersion agent is ethanol, described zirconia nano-powder and tinting material be ball milling in the mixed solution of ethanol and water, wherein, ethanol accounts for the 10-20% of mixed solution cumulative volume, and the content ratio of this zirconia nano-powder and this tinting material is the 20-50% of this zirconia nano-powder, this tinting material and this mixed solution total mass; The zirconium oxide bead that described planetary ball mill use diameter is 0.3-3mm is as grinding medium, and the ball milling time length is 24-48 hour; Ball mill in described step c still adopts planetary ball mill, is the screen cloth elimination zirconium oxide bead of 0.2mm, obtains described slurry after ball milling 2-4 hour with mesh.
By this ball-milling technology flow process, in the slurry of gained, zirconia nano-powder and tinting material obtain sufficient spheroidization and homogenizing distribution, when being conducive to follow-up extrusion forming, biscuit of ceramics obtains maximum tap density, by improving the density of biscuit of ceramics, follow-up sintering processes can make even dyeing, dental coloring zirconia block that transparency is excellent.
The dental coloring zirconia powder prepared according to the present invention, the relative density of the dental prosthesis that subsequent disposal is obtained reaches 99.65-99.75%, visible light transmittance rate is not less than 30%, and tooth color matching becomes simple.Meanwhile, the physical strength of the dental prosthesis obtained can also be made to improve further, and flexural strength can reach 800-900MPa, fracture toughness property 7-7.5MPam
1/2.Colored zirconium oxide powder preparation manipulation process of the present invention is simple, is easy to scale operation, is conducive to the cost reducing dental prosthesis, benefits more dental patient, meet the pursuit that people become better and approaching perfection day by day to the reparation of high standard Dental Aesthetic.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram of the spherical dental coloring zirconia powder of preparation in embodiment one.
Fig. 2 is the scanning electron microscope diagram of spherical dental coloring zirconia powder prepared in embodiment two.
Fig. 3 is the scanning electron microscope diagram of spherical dental coloring zirconia powder prepared in embodiment three.
Fig. 4 is the scanning electron microscope diagram of spherical dental coloring zirconia powder prepared in embodiment four.
Embodiment
One, embodiment one
The 3Y-TZP nano powder that grain diameter is 30-50nm is prepared by coprecipitation method.By this 3Y-TZP zirconia nano-powder and tinting material bismuth oxide (Bi
2o
3) and ferric oxide (Fe
2o
3) mixing, bismuth oxide, ferric oxide and zirconium white (ZrO in obtained mixed powder
2) mass percent be bismuth oxide 0.05%, ferric oxide 0.09%: zirconium white 99.86%.This mixed powder is dropped in planetary ball mill with dispersion agent ethanol together with the mixed solution of deionized water and carries out milled processed, use mechanical force crumbling method to eliminate hard aggregation.Wherein, ethanol accounts for 20% of mixed solution cumulative volume, and the content ratio of this mixed powder is 25% of this mixed powder and this mixed solution total mass.The zirconium oxide bead that planetary ball mill use diameter is 0.3-3mm is as grinding medium, and the ball milling time length is 24 hours.In the product that grinding obtains, add adhesive polyethylene alcohol (PVA), put into the screen cloth elimination zirconium oxide bead that planetary ball mill ball milling is 0.2mm with mesh after 2 hours, obtain slurry; Wherein, polyvinyl alcohol addition is 1% of this grinding product quality.Carry out mist projection granulating process by this slurry transferring to spray-drying tower, obtain distribution of SMD at the spherical dental coloring zirconia powder of 45-70 μm.
The increase of bismuth oxide content, can produce from silvery white to pink coloring effect, the increase of iron oxide content, can produce from Huang to red coloring effect.
Result: can obviously find out from Fig. 1, each particle hard aggregation-free in this colored zirconium oxide powder.The equal globulate of each particle, edge is round and smooth, bubble-free in granule, and without broken particle, most average diameter of particles distribution range is 45 μm-70 μm.
This colored zirconium oxide powder is shaping through 200MPa isostatic cool pressing (CIP), put into electric furnace and sinter 2 hours at 1500 DEG C, obtain the colored zirconium oxide porcelain block sample of 30 × 4 × 3mm.
It is that milk is yellow that the naked eyes of this porcelain block sample see color, to the color of this porcelain block sample at standard white (lightness L
*=92.39, a
*=0.14, b
*=1.62) measure under background.Adopt Japanese Minolta (Minolta) CM-2600d spectral photometric colour measuring meter, standard light source D
65; 10 ° of standard observers; Test probe is contact, and diameter is 3mm; Observation condition is d/8, eliminates specular reflection optical mode.The CIE-1976-Lab colorimeter system that color system adopts International Commission on Illumination (CIE) to recommend.The porcelain block sample lightness L made
*with colourity a
*, b
*for: L*=76.9; A*=1.46; B*=15.2.
Three-point bending resistance method is adopted to make bending strength test, test result to this porcelain block sample: bending strength is 900MPa, and toughness is 7.3MPam
1/2.
Adopt Archimedes (Archimedes) method to measure sintered density and the relative density of this porcelain block sample, the relative density of this porcelain block sample is 99.75%.
This porcelain block sample is made the measure sample that thickness is 1mm, adopts its visible light transmittance rate of spectrophotometer measurement.Light source, test specimen, probe is made point-blank during measurement, regulate hot spot to ensure incident light vertical incidence, first recording light source light intensity (I0), then measure the intensity (I) of light through measure sample, calculate the transmittance of measure sample, T=(I/I0) × 100%.In 400 ~ 800nm visible region every 10nm continuously measured transmittance, obtain the visible ray light transmission integrated of measure sample.Measure after getting average 3 times, the visible light transmittance rate obtaining measure sample is 35.3%.
Two, embodiment two
The 3Y-TZP nano powder that grain diameter is 30-50nm is prepared by coprecipitation method.By this 3Y-TZP zirconia nano-powder and tinting material bismuth oxide (Bi
2o
3) and ferric oxide (Fe
2o
3) mixing, bismuth oxide, ferric oxide and zirconium white (ZrO in obtained mixed powder
2) mass percent be bismuth oxide 0.05%, ferric oxide 0.05%: zirconium white 99.9%.This mixed powder is dropped in planetary ball mill with dispersion agent ethanol together with the mixed solution of deionized water and carries out milled processed, use mechanical force crumbling method to eliminate hard aggregation.Wherein, ethanol accounts for 15% of mixed solution cumulative volume, and the content ratio of this mixed powder is 20% of this mixed powder and this mixed solution total mass.The zirconium oxide bead that planetary ball mill use diameter is 0.3-3mm is as grinding medium, and the ball milling time length is 30 hours.In the product that grinding obtains, add adhesive polyethylene alcohol (PVA), put into the screen cloth elimination zirconium oxide bead that planetary ball mill ball milling is 0.2mm with mesh after 3 hours, obtain slurry; Wherein, polyvinyl alcohol addition is 1.5% of this grinding product quality.Carry out mist projection granulating process by this slurry transferring to spray-drying tower, obtain distribution of SMD at the spherical dental coloring zirconia powder of 40-50 μm.
Result: obviously can find out each particle hard aggregation-free in this colored zirconium oxide powder from Fig. 2, particle balling preparation shape, edge is round and smooth, the particle of bubble-free, nothing fragmentation in granule, most average diameter of particles distribution range is 40 μm-50 μm.
By shaping through the CIP of 200MPa for this colored zirconium oxide powder, put into electric furnace and sinter 2 hours at 1500 DEG C, obtain the colored zirconium oxide porcelain block sample of acquisition 30 × 4 × 3mm.It is yellowish that porcelain block sample naked eyes see color, and use aforesaid method and apparatus to detect, this porcelain block sample lightness L* and colourity a*, b* are: L*=78.8; A*=1.6; B*=10.8; The bending strength of porcelain block sample is 860MPa, and toughness is 7.5MPam1/2.The relative density of this porcelain block sample is 99.65%.The thickness that this porcelain block sample is made is the sample of 1mm, and recording visible light transmittance rate is 33.4%.
Three, embodiment three
The 3Y-TZP nano powder that grain diameter is 30-50nm is prepared by coprecipitation method.By this 3Y-TZP zirconia nano-powder and tinting material cerium oxide (Ce
2o
3) and ferric oxide (Fe
2o
3) mixing, cerium oxide, ferric oxide and zirconium white (ZrO in obtained mixed powder
2) mass percent be cerium oxide 3%, ferric oxide 0.09%: zirconium white 96.91%.This mixed powder is dropped in planetary ball mill with dispersion agent ethanol together with the mixed solution of deionized water and carries out milled processed, use mechanical force crumbling method to eliminate hard aggregation.Wherein, ethanol accounts for 10% of mixed solution cumulative volume, and the content ratio of this mixed powder is 30% of this mixed powder and this mixed solution total mass.The zirconium oxide bead that planetary ball mill use diameter is 0.3-3mm is as grinding medium, and the ball milling time length is 35 hours.In the product that grinding obtains, add adhesive polyethylene alcohol (PVA), put into the screen cloth elimination zirconium oxide bead that planetary ball mill ball milling is 0.2mm with mesh after 2 hours, obtain slurry; Wherein, polyvinyl alcohol addition is 2% of this grinding product quality.Carry out mist projection granulating process by this slurry transferring to spray-drying tower, obtain distribution of SMD at the spherical dental coloring zirconia powder of 48-80 μm.
The increase of cerium-oxide contents, can produce the coloring effect from yellowish to orange, and the increase of iron oxide content can produce from Huang to red coloring effect.
Result: obviously can find out each particle hard aggregation-free in this colored zirconium oxide powder from Fig. 3, particle balling preparation shape, edge is round and smooth, the particle of bubble-free, nothing fragmentation in granule, most average diameter of particles distribution range is 48 μm-80 μm.
By shaping through the CIP of 200MPa for this colored zirconium oxide powder, put into electric furnace and sinter 2 hours at 1500 DEG C, obtain the colored zirconium oxide porcelain block sample of 30 × 4 × 3mm.It is yellow that these porcelain block sample naked eyes see color, uses the measuring method described in embodiment 1 and equipment, records this porcelain block sample lightness L* and colourity a*, b* are: L*=70.6; A*=4.5; B*=24.5; This porcelain block sample bending strength is 800MPa, and toughness is 7.0MPam1/2.Relative density is 99.68%.The thickness that this porcelain block sample is made is the visible light transmittance rate of the sample of 1mm is 33.1%.
Four, embodiment four
The 3Y-TZP zirconia nano-powder that grain diameter is 30-50nm is prepared by coprecipitation method.By this 3Y-TZP zirconia nano-powder and tinting material cerium oxide (Ce
2o
3) and ferric oxide (Fe
2o
3) mixing, cerium oxide, ferric oxide and zirconium white (ZrO in obtained mixed powder
2) mass percent be cerium oxide 4%, ferric oxide 0.12%: zirconium white 95.88%.This mixed powder is dropped in planetary ball mill with dispersion agent ethanol together with the mixed solution of deionized water and carries out milled processed, use mechanical force crumbling method to eliminate hard aggregation.Wherein, ethanol accounts for 12% of mixed solution cumulative volume, and the content ratio of this mixed powder is 50% of this mixed powder and this mixed solution total mass.The zirconium oxide bead that planetary ball mill use diameter is 0.3-3mm is as grinding medium, and the ball milling time length is 48 hours.In the product that grinding obtains, add adhesive polyethylene alcohol (PVA), put into the screen cloth elimination zirconium oxide bead that planetary ball mill ball milling is 0.2mm with mesh after 4 hours, obtain slurry; Wherein, polyvinyl alcohol addition is 0.5% of this grinding product quality.Carry out mist projection granulating process by this slurry transferring to spray-drying tower, obtain distribution of SMD at the spherical dental coloring zirconia powder of 50-85 μm.
Result: obviously can find out each particle hard aggregation-free in this colored zirconium oxide powder from Fig. 4, particle balling preparation shape, edge is round and smooth, the particle of bubble-free, nothing fragmentation in granule, average diameter of particles distribution range is 50 μm-85 μm.
By shaping through the CIP of 200MPa for this spherical dental colored Zirconium powder, put into electric furnace and sinter 2 hours at 1500 DEG C, obtain the colored zirconium oxide porcelain block sample of 30 × 4 × 3mm.It is yellow that these porcelain block sample naked eyes see color, uses the measuring method described in embodiment 1 and equipment, records this porcelain block sample lightness L* and colourity a*, b* are: L*=72.8; A*=4.0; B*=22.3; This porcelain block sample bending strength is 810MPa, and toughness is 7.2MPam1/2.Relative density is 99.65%.The thickness that this porcelain block sample is made is the visible light transmittance rate of the sample of 1mm is 31.1%.
The above, be only present pre-ferred embodiments, do not limit scope of the invention process with this, and equivalence change and the modification done according to technical scheme of the present invention and description, all should belong to the scope that the present invention is contained.
Claims (1)
1. prepare a method for dental coloring zirconia powder, comprise the following steps:
Step a, prepares by coprecipitation method the 3Y-TZP zirconia nano-powder that grain diameter is 30-50nm;
Step b, after adding tinting material and dispersion agent, puts into ball mill and carries out milled processed in this zirconia nano-powder, uses mechanical force crumbling method to eliminate hard aggregation; Described tinting material is the mixture of ferric oxide and cerium oxide or the mixture of ferric oxide and bismuth oxide, and wherein the addition of cerium oxide is the 1-4% of this zirconia nano-powder and this tinting material total mass; The addition of ferric oxide is the 0.06-0.15% of this zirconia nano-powder and this tinting material total mass; The addition of bismuth oxide is the 0.05-0.2% of this zirconia nano-powder and this tinting material total mass; Ball mill adopts planetary ball mill, described dispersion agent is ethanol, described zirconia nano-powder and tinting material be ball milling in the mixed solution of ethanol and deionized water, wherein, ethanol accounts for the 10-20% of mixed solution cumulative volume, and the content ratio of this zirconia nano-powder and this tinting material is the 20-50% of this zirconia nano-powder, this tinting material and this mixed solution total mass; The zirconium oxide bead that described planetary ball mill use diameter is 0.3-3mm is as grinding medium, and the ball milling time length is 24-48 hour;
Step c, adds adhesive polyethylene alcohol, puts into ball mill ball milling 2-4 hour, obtain slurry in the product that grinding obtains; Wherein, polyvinyl alcohol addition is the 0.5-3% of this grinding product quality; Ball mill still adopts planetary ball mill, is the screen cloth elimination zirconium oxide bead of 0.2mm, obtains described slurry after ball milling 2-4 hour with mesh;
Steps d, carries out mist projection granulating process by described slurry transferring to spray-drying tower, obtains distribution of SMD at the spherical dental coloring zirconia powder of 40-85 μm.
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