CN101219894A - Process for manufacturing zirconium oxide/lanthanum phosphoric acid full porcelain oral cavity body material which can be cut - Google Patents
Process for manufacturing zirconium oxide/lanthanum phosphoric acid full porcelain oral cavity body material which can be cut Download PDFInfo
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- CN101219894A CN101219894A CNA2008100324166A CN200810032416A CN101219894A CN 101219894 A CN101219894 A CN 101219894A CN A2008100324166 A CNA2008100324166 A CN A2008100324166A CN 200810032416 A CN200810032416 A CN 200810032416A CN 101219894 A CN101219894 A CN 101219894A
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Abstract
The invention relates to a method for preparing an all-ceramic oral cavity repairing composite material with machinable zirconia/lanthanum phosphate, belonging to a field of inorganic composite material preparation. The method of the invention is essentially characterized by adjusting the strength and toughness of compound ceramic of zirconia and lanthanum phosphate through controlling the content of zirconia and lanthanum phosphate; the preparation technology of the invention comprises the following processes: lanthanum phosphate powders are prepared; mixture powders of yttrium oxide, lanthanum phosphate and zirconia are prepared by a certain mass ratio; isostatic pressing and sintering is carried out for the mixture under 150 to 250MPa and 1,500 to 1,650 DEG C respectively; and finally the dental composite ceramic material with machinable zirconia and lanthanum phosphate of the invention is obtained. The composite of the invention is suitable for all-ceramic dental repair of oral cavity clinic.
Description
Technical field:
The present invention relates to a kind of machinable zirconium white/lanthanum phosphoric acid full porcelain mouth mending material preparation methods, belong to the inorganic composite materials manufacturing process technology field.
Background technology:
Along with the raising of people's standard of living and quality, the generation of mishap in the daily life, Oral Repair becomes and becomes more and more important.Present dental material develops into a large amount of use metallic substance, resin material and stupalith from originally animal teeth.Full ceramic dental repairing body is compared with metal and polymer dental prosthesis, can have the refraction close with tissue of tooth, scattering coefficient, can reproduce the transparency of natural teeth, color and luster.In addition, stupalith chemical stability height, good biocompatibility, thermal expansivity and tissue of tooth are close, do not degrade in oral environment, and polishing and glazed porcelain facing are bright and clean, and bacterial plaque is difficult for adhering to, and is a kind of ideal dental prosthetic material.
The zirconia ceramics excellent biological compatibility, it not only is used widely as the femoral head replacement material, also gazed at as dental prosthetic material, zirconia ceramics as dental prosthetic material have corrosion-resistant, chemical stability good, toughness is heat conductivity high, the lowest in the stupalith and advantage such as attractive in appearance under the no sensitization, room temperature.But zirconia ceramics intensity height reaches more than the 800MPa, is difficult to carry out ground finish at dental CAD/CAM (computer aided design (CAD) and manufacturing), and ground finish cost height has also limited its clinical application.
The phosphate base biological ceramics has excellent biological compatibility, is applied in the reparation of tooth, bone etc. with in replacing gradually.Lanthanum, molybdenum, fluorochemical synergy suppress enamel decalcification, have the anti-dental caries effect.
The present full ceramic dental repairing body of machinable of main usefulness clinically: the alumina-ceramic (In-Ceram) of feldspathic porcelain (Vita and Celay), mica-based glass-ceramic (Dicor) and glass infiltration.But preceding two kinds of materials exist intensity low (about 200MPa) and poor toughness, cause in clinical experiment mortality higher, limit its application, are preced with as the Dicor molar.Although adopt glass osmose process sintering to obtain the In-Ceram porcelain hat of higher-strength (about 341MPa), the toughness deficiency only limits to leaf-comb and labial teeth reparation, and technology is also too complicated.Porcelain-fused-to-metal resto-ration, utilize metal base to strengthen the intensity of pottery, along with going deep into of clinical application research, engender that metallic corrosion variable color, high thermal conductivity painted to gum, metal cause dentin hypersensitiveness, dummy neck aesthetic property is not good enough and a few patients makes problems such as pottery bursts apart to metal alloy intermediate ion allergy, golden porcelain bonding force are relatively weak, porcelain-fused-to-metal resto-ration easily produces stress concentration.
Summary of the invention:
The object of the present invention is to provide a kind of machinable zirconium white/lanthanum phosphoric acid full porcelain mouth mending material preparation methods.
For achieving the above object, the present invention adopts following technical scheme:
A kind of machinable zirconium white/lanthanum phosphoric acid full porcelain mouth mending material preparation methods is characterized in that in the control material content of weak phase lanthanum orthophosphate and can undergo phase transition the content of toughness reinforcing tetragonal phase zirconium oxide; And lanthanum orthophosphate is uniformly distributed in the zirconium white, this method includes following processing step:
A. the preparation of pure phosphoric acid lanthanum powder: the mol ratio by La: P is 1: 1, the lanthanum trioxide of particle diameter≤0.2um, purity＞99.9% is slowly added by in the water-reducible phosphoric acid water body lotion of deionization, after reaction is finished with reaction product with deionized water rinsing to the filtered liquid pH value near 7.Dry powder with Rotary Evaporators,, obtain lanthanum phosphate powder 900-1100 ℃ of calcining 2 hours;
B. mixed powder preparation: is 0: 10 with yttrium oxide, the above-mentioned lanthanum phosphate powder that makes and zirconium white by mass ratio: 90-5: carry out batch mixing, wherein Y in the zirconium white at 45: 50
2O
3And ZrO
2Mol ratio be 3: 97; With batch mixing: agate ball: the mass ratio of ethanol=1: 1.2: 0.8 is packed in the urethane ball grinder, carries out ball milling with 150-250 rev/min rotating speed, and the ball milling time is 16-24 hour, discharging then, oven dry; Siccative after the oven dry is crossed 60 mesh standard sieves, the gained powder is put into alumina crucible, and place in the globars electric furnace, under air atmosphere, calcine, calcining temperature is 1200-1300 ℃, and is incubated 1-3 hour; The gained powder is again with batch mixing: agate ball: the mass ratio of ethanol=1: 1.2: 0.8 is packed in the urethane ball grinder, carry out ball milling with 150-250 rev/min rotating speed, the ball milling time is 16-24 hour, discharging then, oven dry, and lanthanum orthophosphate/Zirconium powder finally is uniformly mixed;
C. composite ceramics preparation: above-mentioned mixed phosphate lanthanum/Zirconium powder is packed in the oil resistant plastics mould, at the inferior static pressure of 150-250Mpa pressure, then the gained base substrate is put into alumina crucible, and place in the silicon molybdenum rod furnace, calcine under air atmosphere, calcining temperature is 1500-1650 ℃, and is incubated 1-3 hour, obtain zirconium white/lanthanum orthophosphate composite ceramic material, be machinable zirconium white/lanthanum phosphoric acid full porcelain mouth mending material material.
Above-mentioned machinable zirconium white/lanthanum phosphoric acid full porcelain mouth mending material preparation methods, it is characterized in that the sintering condition that described composite ceramics prepares: calcining temperature is 1600 ℃, soaking time 2 hours.
In the technological process of the present invention, yttrium oxide adds as stablizer.
Compare with existing technology, the present invention has following remarkable advantage:
1. in the zirconium white system, add lanthanum orthophosphate, regulate the intensity size of composite ceramics, solved zirconium white intensity height, hardness and be difficult to the problem of processing greatly, composite ceramics is easily processed, cut down finished cost.
2. owing to form weak interface between lanthanum orthophosphate and the zirconium white, it is toughness reinforcing easily to form tiny crack, makes composite ceramics not only keep higher toughness but also the suitable machinability of tool.
3. by control lanthanum orthophosphate and zirconic proportioning, effectively regulate strong phase and weak relative content mutually in the composite ceramics, realize that intensity and workability are adjustable.
4. because by regulate adding the amount of yttrium oxide, but the content of the tetragonal phase zirconium oxide of phase transformation in the may command composite ceramics, and the toughness of regulating composite ceramics improves the material clinical oral and is applied to power and range of application.
5. make itself and human body dentine color basically identical by adjusting color, obtain splendid aesthetic effect.
The zirconium white that the inventive method makes/lanthanum orthophosphate composite ceramic material bending strength and fracture toughness property are respectively at 165～628MPa and 2.4～9.56MPam
1/2Adjustable in the scope.Be suitable for the clinical oral requirement fully, can be used as the full porcelain bridge hat of dentistry dummy, cut down finished cost, improve the success ratio of clinical experiment.
Embodiment
Now embodiments of the invention are described in the back:
Embodiment 1
30%LaPO
4/ Y-ZrO
2The composite ceramics preparation, concrete processing step is as follows:
A. the preparation of pure phosphoric acid lanthanum powder: by La: P (mol ratio) is 1: 1, with lanthanum trioxide (particle diameter≤0.2um, purity＞99.9%) slowly adds by in the water-reducible phosphate aqueous solution of deionization (20 ℃ of temperature), Deng the reaction finish after, reaction product with deionized water rinsing to the filtered liquid pH value near 7.Dry powder with Rotary Evaporators,, obtain lanthanum phosphate powder 1000 ℃ of calcinings 2 hours;
B. mixed powder preparation: is 30: 70 batch mixings with the lanthanum phosphate powder and the zirconium white of above-mentioned system by mass ratio, wherein Y in the zirconium white
2O
3And ZrO
2Mol ratio be 3: 97, and in the urethane ball grinder of packing into, with batch mixing: agate ball: the mass ratio of ethanol=1: 1.2: 0.8 adds agate ball and ethanol, carries out ball milling with 200 rev/mins rotating speeds, and 20 hours ball milling time, discharging is then dried; Siccative after the oven dry is crossed 60 mesh standard sieves, the gained powder is put into alumina crucible, and place in the globars electric furnace, under air atmosphere, calcine, calcining temperature is 1250 ℃, and be incubated 2 hours, the gained powder reinstalls in the urethane ball grinder, and with batch mixing: agate ball: the mass ratio of ethanol=1: 1.2: 0.8 adds agate ball and ethanol respectively, carries out ball milling with 200 rev/mins rotating speeds, 20 hours ball milling time, discharging is then dried, and lanthanum orthophosphate/Zirconium powder finally is uniformly mixed;
C. composite ceramics preparation: above-mentioned mixed phosphate lanthanum/Zirconium powder is packed in the oil resistant plastics mould, at the inferior static pressure of 200Mpa pressure, then the gained base substrate is put into alumina crucible, and place in the silicon molybdenum rod furnace, under air atmosphere, to calcine, calcining temperature is 1600 ℃, and be incubated 2 hours, obtain zirconium white/lanthanum orthophosphate composite ceramic material.
Test bending strength and fracture toughness property respectively by three-point bending resistance method and monolateral opening beam method, the result shows: present embodiment prepares the bending strength of zirconium white/lanthanum orthophosphate composite ceramic material and fracture toughness property respectively at 337MPa and 4.42MPam
1/2
Embodiment 2
40%LaPO
4/ Y-ZrO
2The composite ceramics preparation, basic identical with the foregoing description, institute's difference is:
A. the preparation of pure phosphoric acid lanthanum powder: by La: P (mol ratio) is 1: 1, with lanthanum trioxide (particle diameter≤0.2um, purity＞99.9%) slowly adds by in the water-reducible phosphoric acid water body lotion of deionization (20 ℃ of temperature), Deng the reaction finish after, reaction product with deionized water rinsing to the filtered liquid pH value near 7.Dry powder with Rotary Evaporators,, obtain lanthanum phosphate powder 1000 ℃ of calcinings 2 hours;
B. mixed powder preparation: is to carry out batch mixing, wherein Y in the zirconium white at 3: 40: 57 with yttrium oxide, the above-mentioned lanthanum phosphate powder that makes and zirconium white by mass ratio
2O
3And ZrO
2Mol ratio be 3: 97, and in the urethane ball grinder of packing into, with batch mixing: agate ball: the mass ratio of ethanol=1: 1.2: 0.8 add agate ball and and ethanol, carry out ball milling with 200 rev/mins rotating speeds, 20 hours ball milling time, discharging is then dried.Siccative after the oven dry is crossed 60 mesh standard sieves, the gained powder is put into alumina crucible, and place in the globars electric furnace, under air atmosphere, calcine, calcining temperature is 1250 ℃, and be incubated 2 hours, the gained powder reinstalls in the urethane ball grinder, with batch mixing: agate ball: the mass ratio of ethanol=1: 1.2: 0.8 adds agate ball and ethanol respectively, carry out ball milling with 200 rev/mins rotating speeds, 20 hours ball milling time, discharging then, dry, lanthanum orthophosphate/Zirconium powder finally is uniformly mixed;
C. composite ceramics preparation: above-mentioned mixed phosphate lanthanum/Zirconium powder is packed in the oil resistant plastics mould, at the inferior static pressure of 200Mpa pressure, then the gained base substrate is put into alumina crucible, and place in the silicon molybdenum rod furnace, under air atmosphere, to calcine, calcining temperature is 1600 ℃, and be incubated 2 hours, obtain zirconium white/lanthanum orthophosphate composite ceramic material.
Present embodiment prepares the bending strength of zirconium white/lanthanum orthophosphate composite ceramic material and fracture toughness property respectively at 239MPa and 2.56MPam
1/2
Claims (2)
1. machinable zirconium white/lanthanum phosphoric acid full porcelain mouth mending material preparation methods is characterized in that the content of weak phase lanthanum orthophosphate in the control material and can undergo phase transition the content of toughness reinforcing tetragonal phase zirconium oxide; And lanthanum orthophosphate is uniformly distributed in the zirconium white, this method includes following processing step:
A. the preparation of pure phosphoric acid lanthanum powder: the mol ratio by La: P is 1: 1, the lanthanum trioxide of particle diameter≤0.2um, purity＞99.9% is slowly added by in the water-reducible phosphoric acid water body lotion of deionization, after reaction is finished with reaction product with deionized water rinsing to the filtered liquid pH value near 7.Dry powder with Rotary Evaporators,, obtain lanthanum phosphate powder 900-1100 ℃ of calcining 2 hours;
B. mixed powder preparation: is 0: 10 with yttrium oxide, the above-mentioned lanthanum phosphate powder that makes and zirconium white by mass ratio: 90-5: carry out batch mixing, wherein Y in the zirconium white at 45: 50
2O
3And ZrO
2Mol ratio be 3: 97; With batch mixing: agate ball: the mass ratio of ethanol=1: 1.2: 0.8 is packed in the urethane ball grinder, carries out ball milling with 150-250 rev/min rotating speed, and the ball milling time is 16-24 hour, discharging then, oven dry; Siccative after the oven dry is crossed 60 mesh standard sieves, the gained powder is put into alumina crucible, and place in the globars electric furnace, under air atmosphere, calcine, calcining temperature is 1200-1300 ℃, and is incubated 1-3 hour; The gained powder is again with batch mixing: agate ball: the mass ratio of ethanol=1: 1.2: 0.8 is packed in the urethane ball grinder, carry out ball milling with 150-250 rev/min rotating speed, the ball milling time is 16-24 hour, discharging then, oven dry, and lanthanum orthophosphate/Zirconium powder finally is uniformly mixed;
C. composite ceramics preparation: above-mentioned mixed phosphate lanthanum/Zirconium powder is packed in the oil resistant plastics mould, at the inferior static pressure of 150-250Mpa pressure, then the gained base substrate is put into alumina crucible, and place in the silicon molybdenum rod furnace, calcine under air atmosphere, calcining temperature is 1500-1650 ℃, and is incubated 1-3 hour, obtain zirconium white/lanthanum orthophosphate composite ceramic material, be machinable zirconium white/lanthanum phosphoric acid full porcelain mouth mending material material.
2. a kind of machinable zirconium white according to claim 1/lanthanum phosphoric acid full porcelain mouth mending material preparation methods, it is characterized in that the sintering condition that described composite ceramics prepares: calcining temperature is 1600 ℃, soaking time 2 hours.
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|---|---|---|---|
| CNA2008100324166A CN101219894A (en) | 2008-01-08 | 2008-01-08 | Process for manufacturing zirconium oxide/lanthanum phosphoric acid full porcelain oral cavity body material which can be cut |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102631291A (en) * | 2011-09-27 | 2012-08-15 | 廖书辉 | Medical high-performance composite material |
| CN108395240A (en) * | 2018-04-25 | 2018-08-14 | 东南大学 | The preparation method of lanthanum orthophosphate, lanthanum orthophosphate porous ceramics and its preparation method and application |
| JP2021091633A (en) * | 2019-12-10 | 2021-06-17 | 株式会社トクヤマデンタル | Method for producing mill blank for dental process, and method for producing dental prosthesis |
-
2008
- 2008-01-08 CN CNA2008100324166A patent/CN101219894A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102631291A (en) * | 2011-09-27 | 2012-08-15 | 廖书辉 | Medical high-performance composite material |
| CN108395240A (en) * | 2018-04-25 | 2018-08-14 | 东南大学 | The preparation method of lanthanum orthophosphate, lanthanum orthophosphate porous ceramics and its preparation method and application |
| CN108395240B (en) * | 2018-04-25 | 2020-05-05 | 东南大学 | Preparation method of lanthanum phosphate, lanthanum phosphate porous ceramic and preparation method and application thereof |
| JP2021091633A (en) * | 2019-12-10 | 2021-06-17 | 株式会社トクヤマデンタル | Method for producing mill blank for dental process, and method for producing dental prosthesis |
| JP7422995B2 (en) | 2019-12-10 | 2024-01-29 | 株式会社トクヤマデンタル | Method for manufacturing a mill blank for dental processing and method for manufacturing a dental prosthesis |
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Open date: 20080716 |