CN102756110A - Titanium surface casting modification method for reinforcing titanium-porcelain combination strength - Google Patents
Titanium surface casting modification method for reinforcing titanium-porcelain combination strength Download PDFInfo
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- CN102756110A CN102756110A CN2012102412384A CN201210241238A CN102756110A CN 102756110 A CN102756110 A CN 102756110A CN 2012102412384 A CN2012102412384 A CN 2012102412384A CN 201210241238 A CN201210241238 A CN 201210241238A CN 102756110 A CN102756110 A CN 102756110A
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Abstract
The invention discloses a titanium surface casting modification method for reinforcing titanium-porcelain combination strength and belongs to the technical field of titanium-porcelain metal-porcelain. The method comprises the steps of: selecting one or a plurality of silicon dioxide, aluminum oxide, chromium oxide, low-smelting bonding porcelain powder, high-smelting bonding porcelain powder, screen color porcelain powder and dentin porcelain as basic ingredients of an internal embedding material; regulating the internal embedding material to gel substance through ethyl orthosilicate acidified by hydrochloric acid, or calcium aluminate cement and distilled water and water; wetting a casting wax pattern through amiable fog, coating the internal embedding material on the side to be fused with porcelain, and curing the internal embedding material at room temperature; embedding the internal embedding material through a titanium casting; and commonly casting the internal embedding material. The method disclosed by the invention forms an oxidization shield when the titanium porcelain is formed and the reaction gradient mixed layer and the glass phase in the porcelain powder form chemical combination to improve the titanium-porcelain combination strength.
Description
Technical field
The invention belongs to titanium porcelain metal porcelain technical field; The preparation method who relates to mixed layer in the middle of preparation method and the titanium-porcelain reaction of interior embedded material of titanium surface casting modification; To strengthen the bond strength of titanium-porcelain, promote of the application of titanium-porcelain metal porcelain at clinical oral.
Background technology
Titanium and alloy thereof have light weight, excellent biological compatibility and biological safety and receive much attention far below the price of noble metal, have been widely used in base, joint prosthesis and the body of mouth cavity planting body, fixing, removable denture reparation, complete denture strap etc. at present.Yet the oral cavity titanium prosthesis particularly fixedly the application of titanium porcelain dummy but receive certain restriction; This is because the chemical property of titanium is more active; Oxygen there is high affinity; The titanium surface will generate thick
under the normal temperature oxide-film and titanium substrate are combined closely; Under the molten enclosure temperature of porcelain, that the titanium surface forms easily is loose porous, adhere to relatively poor oxide-film, influences the bond strength of titanium-porcelain.So, improve the bond strength of titanium-porcelain and just must suitably handle the surface of titanium, combine so that improve titanium-porcelain, popularize the titanium-application of porcelain dummy in the clinical oral repair.
The titanium surface treatment method mainly contains surface roughening processing, titanium chemical surface treatment and titanium face coat technology at present.The titanium surface roughening is handled can increase the titanium surface roughness, improves titanium-porcelain bonded area; The titanium chemical surface treatment can be removed the titanium surface contamination, but no matter is that surface roughening is handled or chemical treatment all can not improve in the porcelain process, and the titanium surface formed the problem of thick oxide film.The isolated titanium of titanium face coat (intermediate layer) contacts with oxygen, control titanium surface over oxidation, thus improve titanium-porcelain bond strength.The method for preparing the intermediate layer is different, and ion beam depositing method, differential arc oxidation, ion injection, magnetron sputtering, sol-gel etc. are arranged.The material of coating is also different, just like Au, and the elemental metals of Cr etc.; Just like SiO
2, SnO
2Deng oxide; Also has TiN, nitride such as ZrSiN.Introduce now that the bond strength of titanium-porcelain increases behind the intermediate layer; But can't reach the level of traditional gold-porcelain fully; Reason possibly be that titanium-porcelain interface is a double-decker, promptly is positioned at the titanyl solid solution layer on nearly titanium surface and contains oxygen disilicide layer, these two conversion zones near pottery; Especially the existence of the titanyl solid solution layer of fragility is to cause the main cause that titanium-the porcelain bond strength is low, i.e. the problem that combines of coating and titanium matrix.
The present invention combines the intermediate layer to overcome domestic and international intermediate layer complex manufacturing technology and coating and the relatively poor problem of titanium matrix bond through the titanium-porcelain of casting method preparation.A kind of preparation method who casts titanium and multiple metal and nonmetal reaction and combine is provided, has realized the good combination of titanium and porcelain powder.
Summary of the invention
The present invention seeks to the active chemical property of titanium; Oxygen is had high affinity, and under the molten enclosure temperature of porcelain, that the titanium surface forms easily is loose porous, adhere to relatively poor oxide-film; Influence the problem of the combination of titanium porcelain; Provide a kind of and make the titanium reaction of interior embedded material of casting and molten condition form the method for gradient mixed layer through casting method, realization metal oxide and nonmetal oxide combine with titanium, the oxidation barrier when forming the titanium porcelain; And make the glassy phase in reaction gradient mixed layer and the porcelain powder form chemical bond, improve the bond strength of titanium-porcelain.
For realizing above-mentioned purpose, the technical scheme that the present invention adopts is following.
The surperficial method of casting modification of a kind of titanium with enhancing titanium-porcelain bond strength is characterized in that, specifically may further comprise the steps:
(1) at first selects silica, chromium oxide, aluminium oxide, eutectic bonding porcelain powder, high one or more bases that melt in bonding porcelain powder, screening look porcelain powder and the body porcelain for use as interior embedded material;
(2) the interior embedded material of step (1) is mixed with ethyl orthosilicate through hydrochloric acid (35%HCl) acidifying; The furnishing colloid substance; Mass concentration is adopted in the ethyl orthosilicate acidifying be 35% hydrochloric acid with distilled water by volume 1:1 mix the aqueous hydrochloric acid solution that obtains and carry out acidifying, the volume ratio of aqueous hydrochloric acid solution and ethyl orthosilicate is 1:10;
Perhaps the interior embedded material with step (1) mixes the furnishing colloid substance with aluminous cement and distillation water;
Perhaps the interior embedded material with step (1) mixes the furnishing colloid substance with the distillation water.(3) it is wetting to utilize affine mist that the casting wax pattern is carried out, and a side of porcelain to apply the good interior embedded material of one deck step (2) mediation wax pattern, and coating layer thickness is 0.2-1.0mm, the room temperature spontaneous curing;
(4) adopt titanium casting investment material for oral cavity that the casting wax pattern is carried out embedding.
(5) carry out routine casting.
The basis of embedded material was for containing SiO in above-mentioned steps (1) was preferred
2Deng material.
The preferred ethyl orthosilicate furnishing colloid substance that adopts through hydrochloric acid (HCl) acidifying of above-mentioned steps (2).
Titanium specialty embedded material in the preferred application number 201010205467.1 of above-mentioned steps (4) China and foreign countries' embedded material, its raw material weight consists of: ZrO
2Powder 40-90 part, Al
20
3Powder 10-50 part, metal zirconium powder 1-10 part or metallic titanium powder 1-20 part, aluminous cement 10-50 part, Li
2CO
30.01-1 part; The employing mass percent is that the high efficiency water reducing agent aqueous solution of 1%-5% is in harmonious proportion evenly, and the weight ratio of the powder and the high efficiency water reducing agent aqueous solution is 100:15-25.
The technical characteristic of the inventive method mainly is:
(1) utilize the method for casting that modification is carried out on the titanium surface; Hot conditions when utilizing the titanium casting, oxygen-free environment (being the conventional casting method of dentistry here); The titanium reaction of the basis of embedded material and molten condition in when casting, the oxidation when the surface formation of casting titanium not only can be protected titanium at porcelain but also can form chemically combined reaction intermediate layer with porcelain porcelain powder glassy phase.As being that the interior embedded material of basis reacts generation Ti in when casting with titanium with silica
5Si
3And SiO
2, Ti
5Si
3Protected titanium surface, the shielding titanium when porcelain with the contacting of oxygen, and SiO
2With the glassy phase of porcelain powder be close compatible, can form chemical bond.Utilize the titanium chemical activity at high temperature and the oxygen-free environment in when casting in theory, it is feasible that itself and interior embedded material are reacted, and the intermediate layer mixed layer comprises that the material of new formation is or/and the composition in the interior embedded material.
(2) problems such as the intermediate layer of preparation and titanium matrix bond be relatively poor have been overcome now both at home and abroad, problem such as the crisp loose oxide-film of titanium surface formation matter when having solved porcelain.
When (3) preparing the basis of interior embedded material, according to titanium fusing point and reaction principle, each composition is different with the different middle mixed layers that obtain of strong reaction degree of titanium, like SiO
2When content is high, strong reaction, the reaction mixed layer is thicker; ZrO
2Content when high, a little less than the reaction, the reaction mixed layer is thinner.
When (4) adopting titanium casting investment material for oral cavity that the casting wax pattern is carried out embedding, the embedded material of employing sees that number of patent application is 201010205467.1.
Description of drawings
Fig. 1 is an observed cast body pattern under embodiment 1 SEM;
Fig. 2 is the XRD analysis on embodiment 1 cast titanium top layer;
Fig. 3 is an observed cast body pattern under embodiment 2 SEM;
Fig. 4 is the XRD analysis on embodiment 2 cast titanium top layers;
Fig. 5 is an observed cast body pattern under embodiment 3 SEM;
Fig. 6 is the XRD analysis on embodiment 3 cast titanium top layers.
The practical implementation method
Following examples have further been explained the present invention, but the present invention is not limited to following examples.
Embodiment 1
Get SiO
25g, grinding places porcelain cup subsequent use; Hydrochloric acid with 35% and distilled water inject same beaker with the volume ratio of 1:1; Mixing injects ethyl orthosilicate simultaneously in another beaker, be 1:10 through the hcl acidifying water of mixing and the volume ratio of ethyl orthosilicate; Again hcl acidifying water is slowly splashed in the ethyl orthosilicate beaker, fully stir.Ethyl orthosilicate and acidifying water mixed liquor through stirring constantly add SiO under condition of stirring
2Powder (SiO
2The amount of powder is 3.9-4 a times of ethyl orthosilicate quality), after all adding, continue again to stir 10-15 minute, make SiO
2Powder and mixed liquor are able to abundant mediation.The interior embedded material that be in harmonious proportion to be fit to is coated in the wax pattern handled through affine mist will porcelain one side, and the room temperature spontaneous curing is carried out embedding with titanium specialty embedded material in the application number 201010205467.1 to casting wax pattern, under oxygen free condition, and routine casting.
Fig. 1 is an observed cast body pattern under the SEM; Fig. 2 is the XRD analysis on cast titanium top layer, and the result shows that reaction is mainly Ti in the mixed layer
5Si
3, SiO
2And Ti.
Press porcelain on the ISO9693 porcelain standard through the titanium sample of ultrasonic cleaning, go up bonding porcelain, screening look porcelain, body porcelain respectively, porcelain thickness is layered as 0.2mm, 0.2mm, 0.6mm, sintering in ceramic pressing furnace.On universal testing machine, do three point bending test test titanium-porcelain bond strength by the ISO9693 standard, test result is got mean, sees table 1.
Embodiment 2
Get SiO
2The Al of powder and 2 μ m granularities
2O
3Each 2.5g of powder adds in the ball grinder, grinds 5 minutes to the two kinds abundant mixings of powder; Hydrochloric acid with 35% and distilled water inject same beaker with the volume ratio of 1:1; Mixing injects aluminous cement simultaneously in another beaker, be 1:1 through the hcl acidifying water of mixing and the ratio of aluminous cement; Again hcl acidifying water is slowly splashed in the aluminous cement, fully stir.Aluminous cement and acidifying water mixed liquor through stirring constantly add the SiO of mixing under condition of stirring
2Powder and Al
2O
3The powder mixed powder after all adding, continues to stir 10-15 minute again, makes powder and mixed liquor be able to abundant mediation.The interior embedded material that be in harmonious proportion to be fit to is coated in the wax pattern handled through affine mist will porcelain one side, and the room temperature spontaneous curing is carried out embedding with titanium specialty embedded material in the application number 201010205467.1 to casting wax pattern, under oxygen free condition, and routine casting.
Fig. 3 is an observed cast body pattern under the SEM; Fig. 4 is the XRD analysis of cast titanium, and the result shows that reaction is mainly Al in the mixed layer
2O
3, SiO
2, Ti
5Si
3And Ti.
Press porcelain on the ISO9693 porcelain standard through the titanium sample of ultrasonic cleaning, go up bonding porcelain, screening look porcelain, body porcelain respectively, porcelain thickness is layered as 0.2mm, 0.2mm, 0.6mm, sintering in ceramic pressing furnace.On universal testing machine, do three point bending test test titanium-porcelain bond strength by the ISO9693 standard, test result is got mean, sees table 1.
Embodiment 3
Get SiO
2Powder and ZrO
2Each 2.5g of powder adds in the ball grinder and ground 5-10 minute, to grinding evenly; Hydrochloric acid with 35% and distilled water inject same beaker with the volume ratio of 1:1; Mixing injects ethyl orthosilicate simultaneously in another beaker, be 1:10 through the hcl acidifying water of mixing and the volume ratio of ethyl orthosilicate; Hcl acidifying water is slowly being splashed in the ethyl orthosilicate beaker, fully stirring.Ethyl orthosilicate and acidifying water mixed liquor through stirring constantly add the SiO through mixing under condition of stirring
2Powder and ZrO
2Powder after all adding, continues to stir 10-15 minute again, makes powder and mixed liquor be able to abundant mediation.The interior embedded material that be in harmonious proportion to be fit to is coated in the wax pattern handled through affine mist will porcelain one side, and room temperature is dried naturally, carries out embedding with titanium specialty embedded material in the application number 201010205467.1 to casting wax pattern, under oxygen free condition, and routine casting.
Fig. 5 is an observed cast body pattern under the SEM; Fig. 6 is the XRD analysis of cast titanium after ultrasonic cleaning, soak are handled 1 minute, and the result shows that reaction mixed layer product is mainly Ti
5Si
3, SiO
2And Ti.
Press porcelain on the ISO9693 porcelain standard through the titanium sample of ultrasonic cleaning, go up bonding porcelain, screening look porcelain, body porcelain respectively, porcelain thickness is layered as 0.2mm, 0.2mm, 0.6mm, sintering in ceramic pressing furnace.On universal testing machine, do three point bending test test titanium-porcelain bond strength by the ISO9693 standard, test result is got mean, sees table 1.
Titanium and the porcelain powder bond strength parameter of table 1 embodiment 1-3 after the interior embedded material modification of preparation
Claims (3)
1. the surperficial casting of the titanium method of modifying to strengthen titanium-porcelain bond strength is characterized in that, specifically may further comprise the steps:
(1) at first selects silica, aluminium oxide, eutectic bonding porcelain powder, high one or more bases that melt in bonding porcelain powder, screening look porcelain powder and the body porcelain for use as interior embedded material;
(2) the interior embedded material of step (1) is mixed with ethyl orthosilicate through hcl acidifying; The furnishing colloid substance; Mass concentration is adopted in the ethyl orthosilicate acidifying be 35% hydrochloric acid with water by volume 1:1 mix the aqueous hydrochloric acid solution that obtains and carry out acidifying, the volume ratio of aqueous hydrochloric acid solution and ethyl orthosilicate is 1:10;
Perhaps the interior embedded material with step (1) mixes the furnishing colloid substance with aluminous cement and distillation water;
Perhaps the interior embedded material with step (1) mixes the furnishing colloid substance with the distillation water;
(3) it is wetting to utilize affine mist that casting wax pattern inside is carried out, and porcelain one side to apply the good interior embedded material of one deck step (2) mediation wax pattern, and coating layer thickness is 0.2-1.0mm, the room temperature spontaneous curing;
(4) adopt titanium casting investment material for oral cavity that the casting wax pattern is carried out embedding;
(5) carry out routine casting.
2. according to the method for claim 1, it is characterized in that the interior embedded material of step (1) is for containing SiO
2Material.
3. according to the method for claim 1, it is characterized in that embedded material is in the step (4): its raw material weight consists of: ZrO
2Powder 40-90 part, Al
20
3Powder 10-50 part, metal zirconium powder 1-10 part or metallic titanium powder 1-20 part, aluminous cement 10-50 part, Li
2CO
30.01-1 part; The employing mass percent is that the high efficiency water reducing agent aqueous solution of 1%-5% is in harmonious proportion evenly, and the weight ratio of the powder and the high efficiency water reducing agent aqueous solution is 100:15-25.
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Cited By (3)
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| CN103172344A (en) * | 2013-04-09 | 2013-06-26 | 江西恒大高新技术股份有限公司 | Heat-resisting compact inorganic hole sealing agent coating |
| CN108938112A (en) * | 2017-05-17 | 2018-12-07 | 株式会社松风 | The phosphate-based embedded material of dental |
| CN114533318A (en) * | 2022-01-11 | 2022-05-27 | 洛阳北苑新材料技术有限公司 | Porcelain baking method for baking porcelain powder on metal crown |
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| CN108938112A (en) * | 2017-05-17 | 2018-12-07 | 株式会社松风 | The phosphate-based embedded material of dental |
| CN114533318A (en) * | 2022-01-11 | 2022-05-27 | 洛阳北苑新材料技术有限公司 | Porcelain baking method for baking porcelain powder on metal crown |
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