A kind of method of zirconium surface processingTechnical field
The invention discloses a kind of methods of zirconium surface processing, specially dental prosthetic technical field.
Background technique
Dental prosthetic refer to repair one or more because dieback rot, saprodontia or external force injury damage tooth structureProcess.Dental prosthetic material has the form and feature of standard, can make and be applied on the tooth of damage and reaches reparationPurpose.Dental prosthetic material includes the tooth structure that filling or founding materials can substitute damage, and traditional repair materials useMetal or resin all lack enough intensity and aesthetics, and easily lead to colour fading or fracture, in addition, these metals and resin are repairedIt is multiple unsuitable as premanillary teeth in aesthetic.Noble metal, such as billon are widely used as dentistry veneer, inlay, edgeFace, tooth stake and corona, precious metal alloys price is higher, and with the rise in price of noble metal, makes the cost of dummyIt can rise sharply.Furthermore the color of noble metal and the creamy white difference of dermal tooth are larger, so aesthetically nor one fineSelection.Non-noble metal alloy is also recommended and uses, but the dispute in terms of health is continuous always, with mentioning for living standardHeight, people also increase the expectation of dental prosthetic aesthetics aspect.For example, for the entire visible part such as tooth of dummyHat, what ceramics were repaired needs the demand much larger than metallic prosthetic to make oxygen since ceramics have good intensity and lasting robustnessThe application for changing this repair materials of zirconium greatly increases, and a kind of dental material of prevalence is recently become, because it has high intensity, anti-foldingIt is disconnected, the opaque capable basic tooth structure for covering discoloration.Its bending strength be 900 to 1100 megapascal, fracture toughness be 8 to10 megapascal (MPa)s become a kind of suitable material, both can directly make complete crown, but due to the oxidation after sintering crystallizationThe compact structure of zirconium, hardness are very big, it is difficult to be surface-treated to surface treatment, cause aesthetic effect bad, because of zirconia materialIn there is no glass ion, so existing etching agent can not do acid etching to zirconium surface, so bonding effect at a specified future dateFruit is undesirable, and zirconium oxide inlay and zirconium oxide veneer restorations body not can guarantee bonding force, but at present on the market, without any oneZirconium oxide tooth table of the money product without the either chemical still physics of any technology, after energy acid etching sintering crystallizationFace can be processed into for a great problem zirconium surface.For this purpose, we have proposed a kind of sides of zirconium surface processingMethod comes into operation, to solve the above problems.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of zirconium surface processing, to solve to propose in above-mentioned background techniqueThe problem of.
To achieve the above object, the invention provides the following technical scheme: a kind of method of zirconium surface processing, this methodSpecific step is as follows: being processed to dental zirconium oxide zirconium block, is polished into zirconium oxide corona；Then zirconium oxide is usedDyeing liquor dyes corona, and dries dyeing liquor, is sintered using zirconium oxide crystal growing furnace to zirconium oxide；Prepare tableZirconium oxide corona is immersed in surface processing solution by surface treatment solution, it is ensured that the surfaces externally and internally of corona all touches solution, toothThe inner surface of hat is used for upper porcelain or glazing for being bonded in abutment, outer surface；The zirconium oxide corona after surface treatment fromIt takes out and cleans in solution, upper porcelain or glazing are carried out to corona, are then sintered again, final dental prosthesis is obtained.
Preferably, the zirconium oxide corona obtains model data by 3D scanner, is ground with CAD/CAM in processingGrind shape close to teeth patterning zirconium block.
Preferably, the surface processing solution includes chloroacetic chloride, and wherein the weight content of chloroacetic chloride is in 0.001-10%Between.
Preferably, the surface processing solution further includes ethanedioly chloride, and wherein the weight content of ethanedioly chloride existsBetween 0.001-10%.
Preferably, the surface processing solution further includes nitric acid and hydrofluoric acid, and the volume ratio range of the two is 1:Between 0.1-4.
Preferably, the surface processing solution further includes the hydrogen peroxide of 0.1-20% by weight.
Preferably, the surface treatment is handled using ultrasonic impact, and ultrasonic frequency exists in 20-40KHz, intensity1-200w/cm2, the time of surface treatment continues 10-90min.
Preferably, specific step is as follows for the method for the surface treatment:
S81: surface processing solution is placed in first container；
S82: zirconium oxide corona is placed in the interior container for having net to hold in the palm, wherein the size of the container compares first containerIt is small, and its bottom and surrounding are evenly distributed with through-hole；
S83: being put into the container equipped with the zirconium oxide corona after sintering crystallization in first container, guarantees in net supportZirconium oxide corona is all immersed in the surface processing solution in first container by mesh；
S84: after the completion of surface treatment, net support container is taken out out of first container, and be put into clear water and clean, held in the palm from netThe zirconium oxide corona after cleaning is taken out in container.
Preferably, the upper porcelain process uses porcelain powder, at paste or paste, uniformly to be smeared with brush with water hybrid modulationIn the outer surface of zirconium oxide corona.
Preferably, the porcelain powder is the feldspar porcelain powder of feldspar content 40-85% and clay content 5-30%.
Preferably, the paste that the glazing process uses powdered frit glaze liquid to be mixed into, oxidation is uniformly applied to brushThe outer surface of zirconium corona.
Compared with prior art, the beneficial effects of the present invention are: the present invention is attached to by the inner surface of zirconium oxide coronaOn abutment, outer surface upper porcelain or glazing, the bonding that can improve between abutment and zirconium oxide corona after the acid etching of surface are strongDegree and the adhesive strength between corona and enamel coating, glaze layer, to improve the durable wear-resistant of dental prosthetic；Surface treatment can be withIncrease the inside and outside surface bond area of zirconium oxide corona, acid etching makes zirconium oxide crown surfaces with more frictional property and coarseProperty, dental prosthesis can will not be moved or be fallen off compared to being attached on abutment with the stronger stable of not acid etching；This hairThe surface treatment time in bright is short, and production efficiency can be improved, and furthermore surface treatment can carry out special control box at room temperature,And it is simple using two containers surface processing solutions and zirconium oxide corona, operating process.
Detailed description of the invention
Fig. 1 is the comparison diagram before acid etching of the present invention and after acid etching；
Fig. 2 is zirconium surface variation diagram after acid etching of the present invention；
Fig. 3 is operation of the present invention case pictorial diagram；
Fig. 4 is production flow diagram of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, completeSite preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based onEmbodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every otherEmbodiment shall fall within the protection scope of the present invention.
Fig. 1-4 is please referred to, the present invention provides a kind of technical solution: a kind of method of zirconium surface processing, this methodSpecific step is as follows: dental zirconium oxide zirconium block is processed, zirconium oxide corona is polished into,；Then zirconium oxide is usedDyeing liquor dyes corona, and dries dyeing liquor, is sintered using zirconium oxide crystal growing furnace to zirconium oxide.Prepare tableZirconium oxide corona is immersed in surface processing solution by surface treatment solution, it is ensured that the surfaces externally and internally of corona all touches solution, toothThe inner surface of hat is used for upper porcelain or glazing for being bonded in abutment, outer surface；The zirconium oxide corona after surface treatment fromIt takes out and cleans in solution, upper porcelain or glazing are carried out to corona, are then sintered again, final dental prosthesis is obtained.
Wherein, in processing, the zirconium oxide corona is obtained in processing by 3D scanner the zirconium oxide coronaModel data is taken, shape is ground close to the zirconium block of teeth patterning with CAD/CAM, the surface processing solution includes acetylChlorine, wherein for the weight content of chloroacetic chloride between 0.001-10%, the surface processing solution further includes ethanedioly chloride, whereinFor the weight content of ethanedioly chloride between 0.001-10%, the surface processing solution further includes nitric acid and hydrofluoric acid, the twoVolume ratio range between 1:0.1-4, the surface processing solution further includes the peroxidating of 0.1-20% by weightHydrogen, the surface treatment are handled using ultrasonic impact, and ultrasonic frequency is in 20-40KHz, and intensity is in 1-200w/cm2,The time of surface treatment continues 10-90min, and specific step is as follows for the method for the surface treatment: S81: will be surface-treated moltenLiquid is placed in first container；S82: zirconium oxide corona is placed in the interior container for having net to hold in the palm, wherein the size of the containerIt is smaller than first container, and its bottom and surrounding are evenly distributed with through-hole；S83: the container equipped with zirconium oxide corona is put into first appearanceIn device, guarantee that the zirconium oxide corona in net support is all immersed in the surface processing solution in first container by mesh；S84: after the completion of surface treatment, net support container is taken out out of first container, and be put into clear water and clean, taken out of net support containerZirconium oxide corona after cleaning out, the upper porcelain process uses porcelain powder with water hybrid modulation at paste or paste, equal with brushThe even outer surface for being applied to zirconium oxide corona, or the paste being mixed into using powdered frit glaze liquid, are uniformly applied to oxygen with brushChange the outer surface of zirconium corona, the porcelain powder is the feldspar porcelain powder of feldspar content 40-85% and clay content 5-30%.
In the present invention, the tooth of zirconium oxide is formed by CADCAM equipment grinding zirconium block.Zirconium block can be suppressed via zirconium powderSintering correction of the flank shape out forms, and also can choose the zirconiums block such as 3Y-PSZ, D-MAX, HASS commercially, and tooth is ground and needs laterUsing high temperature furnace to tooth heat-agglomerating, crystallization conversion is brought it about, the temperature of sintering is 1450-1650 DEG C, the speed of sinteringUsually 3-10 DEG C/min, 3-24h is needed altogether.Zirconium oxide ceramic crown is first to grind hat, thickness in a zirconium oxide to be about0.5-1.2mm, the glazed thickness being sintered after upper porcelain are 0.6-1.2mm.The final form of tooth is determined by the form of upper porcelain.OxidationZirconium complete crown, inlay and veneer are in accordance with 3D data and the final complete dental morphology come, the crystallization conversion of high temperature are groundCarry out the processing simply painted with glazing again later.The thickness of zirconium oxide complete crown and inlay is generally 0.5-2.5mm, outer surfaceUpper a thin layer of glaze can serve as final dummy.The very thin thickness of zirconium oxide veneer is generally in 0.2-1.0mm.
This patent discovery, by experiment, nitric acid or hydrofluoric acid, which is used alone, will lead to acid etching and slows, and use nitreThe mixed solution of acid, hydrofluoric acid and hydrogen peroxide can achieve better effect.Nitric acid, hydrofluoric acid, the mixed liquor of hydrogen peroxideAlso it is proved to effect better than the mixed solution for being only nitric acid and hydrofluoric acid.Ultrasonic impact method and nitric acid, hydrofluoric acid, peroxidatingHydrogen mixed solution, which is used together, can achieve best effect.
Containing nitric acid and hydrofluoric acid, and surface processing solution of the volume ratio of the two between 1:0.1 to 1:4 is preferred(best between 1:0.1 to 1:1.5).If the hydrogen peroxide containing 0.1%-20% is more preferable (best between 5%-15%).Such asFor fruit fluohydric acid content compared to low with nitric acid content, surface treatment process can become very slow, if instead fluohydric acid content compared toNitric acid content is too high, and the hardness of zirconium oxide corona will weaken.If the content of hydrogen peroxide is too low, the surface treatment time willIncrease, content is too high, and the volume ratio of uneven or more the nitric acid of zirconium oxide corona surface treatment meeting and hydrofluoric acid refers in aqueous solutionIn acid volume.
Zirconium oxide corona is immersed in surface processing solution under room temperature China environment and continues to be advisable for 10-90 minutes.IfThe time is surface-treated less than 10 minutes, adhesive strength may be insecure, more than 90 minutes, since zirconium oxide corona is too thin, can leadCorona hardness is caused to reduce
It was verified that even if at room temperature, surface treatment use contains nitric acid, and the solution of hydrofluoric acid and hydrogen peroxide also canReach good result.The method of existing chemical attack zirconium oxide is that in high temperature, (temperature is higher than 400 using calcium sulfate or phosphoric acidDegree Celsius) under carry out, so high temperature, which carries out acid etching, a serious security risk, and it includes nitric acid that we are this, hydrofluoric acid,The solution of hydrogen peroxide, which can at room temperature be handled zirconium surface, can obtain good result
Mentioned above, the surface processing solution that the present invention is shown can additionally contain chloroacetic chloride and ethanedioly chloride.At surfaceManaging the chemical component of solution is dangerous when being processed to surface.
Zirconium oxide corona is soaked in surface processing solution and carries out ultrasonic impact processing.Respectively when observation surface treatmentBetween from 0-120 minutes generate bonding effect, ultrasonic impact frequency is 20KHZ, and intensity is
20W/CM2.Experimental result is shown in Table 1.
The present invention relies on process of surface treatment, and the zirconium oxide corona after acid etching is attached on abutment, the table of zirconium oxide coronaSurface area increases, and has changed and improved adhesion strength after acid etching, due to increasing the mantle friction and roughness of calcium oxide corona,Dummy can be stable be attached on abutment, increase the bonding force of zirconium oxide corona and inlay, greatly reduce dummyActivity or the probability that falls off.
Also, it in the past on the market can be with the product and processing method of acid etching zirconium surface, so that zirconia materialAesthetics mechanicalness can make veneer restorations body, and the bonding on abutment can not achieve.There is such inorganic agent to oxidationZirconium surface carries out acid etching, so that oxidation hat surface is increased evil spirit wiping and roughness, considerably increases bonding rate, make zirconium oxide systemIt is possibly realized as veneer.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be withA variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understandingAnd modification, the scope of the present invention is defined by the appended.