CN104671828A - Preparation method of nano-silicon-coated microhard abrasive particles for tribochemical method silicon coating system for dental zirconia ceramic - Google Patents
Preparation method of nano-silicon-coated microhard abrasive particles for tribochemical method silicon coating system for dental zirconia ceramic Download PDFInfo
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- CN104671828A CN104671828A CN201510038357.3A CN201510038357A CN104671828A CN 104671828 A CN104671828 A CN 104671828A CN 201510038357 A CN201510038357 A CN 201510038357A CN 104671828 A CN104671828 A CN 104671828A
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Abstract
The invention relates to a preparation method of nano-silicon-coated microhard abrasive particles for a dental zirconia ceramic tribochemical silicon coating. The preparation method comprises the following steps: vaporizing silicon serving as a raw material by virtue of pulse discharging to form nano-silicon spheres; preparing nano-silicon slurry with good dispersity and certain viscosity from the prepared nano-silicon spheres, adding hard abrasive particles into the nano-silicon slurry, and adequately and uniformly stirring to uniformly adhere the nano-silicon spheres to the surfaces of the hard abrasive particles; finally heating and drying in a high temperature furnace, oxidizing the surfaces of the nano-silicon spheres to form a silica covering layer; simultaneously melting the silica covering layer to generate a certain binding force with the abrasive particles. By virtue of a tribochemical method, after the surface of the dental zirconia ceramic is processed by virtue of the microhard abrasive particles, the binding strength between the ceramic and resin can be remarkably improved, and the effect of the microhard abrasive particles is similar to the effects of mainstream products in the current market. The preparation method is simple and stable in process, low in cost and applicable to large-scale batch production.
Description
Technical field
The present invention relates to the preparation method of the coated micro-hard abrasive of a kind of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon, belong to field of material preparation.
Background technology
All-ceramic Dental Material can be divided into the kinds such as alumina-based ceramic, zirconia-based ceramics and glass-based pottery according to main component difference.Wherein, zirconia-based ceramics relies on outstanding mechanical property and good aesthetic properties to be shown one's talent in All-ceramic Dental Material, especially for when making the dummies such as many units fixed bridge, planting body, telescope crown with All-ceramic material, zirconia-based ceramics replaces the pottery of other kind and becomes first-selected or even unique selection.
In All-ceramic restoration process, resin cement is used by routine because the performance in bonding strength, color matching, marginal seal, water solubility etc. is all better than other caking agent kind.Research finds, well bonding not only can increase reparation retention, and dummy and abutment can be tightly linked and become overall, the effect of effective dispersion cushion effect, on the other hand, resin adhesive can also make up all-ceramic prosthesis and add the microfissure formed man-hour before dimerization, reduces the hidden danger that stress concentration caused thus brings.People more and more recognize, combination good between resin/pottery is the important factor affecting All-ceramic restoration success ratio.Generally believe at present, the mechanism that is combined with interlaminar resin of pottery mainly comprise alligatoring ceramic surface and infiltrate resin solidify dash forward between the mechanical interlock effect that produces and the chemical adhesive effect passed through between the two, the latter is the bonding key of acquisition firm stable.Silane coupling agent is as a kind of binding agent extensively used in stomatology field, and it take Siliciumatom as core, and usual one end is-CH=CH
2or-NH
2, polyaddition reaction can be there is with the ethylene linkage (C=C) in resinous substrates; The other end comprises alkoxyl group (as-OCH
3or-OCH
2cH
3), can be hydrolyzed in acid condition and become silanol groups (Si-OH), can and ceramic surface Si-OH between there is polycondensation.And the stable chemical nature of zirconia ceramics, its apolar surfaces is difficult to by hydroxylation, therefore also directly cannot realize silanization.In order to change the character on zirconia ceramics surface, tribo-chemistry method (Tribochemical method) generally acknowledges that the most effective its principle of method at zirconium surface formation silica coating is the alumina grit using a kind of special surface coverage silicon oxide layer, high velocity air during sandblasting drives gravel bombardment ceramic surface, local produces High Temperature High Pressure instantaneously, and after gravel comes off, the silicon oxide layer on its surface is just coated on ceramic surface due to the effect of friction.Classical tribo-chemistry method silicon coating system comprises Rocatec and CoJet and uses the zirconia ceramics of this method process to be recognized after silanization, significantly can to improve adhesiveproperties, also become the reference standard weighing other zirconium white bonding plane treatment process.But although confirm that effectively existing tribo-chemistry method coat system is expensive, application is few at home.The core of this technology is the preparation of the alumina particle being surrounded by silicon-dioxide, and current its preparation method mainly contains sol-gel method, chemical deposition etc., but its complex process, high in cost of production.
Summary of the invention
Technical problem to be solved by this invention: preparation method's complex process, the high in cost of production problem of the alumina grit of conventional surface coverage silicon oxide layer, propose the preparation method of the coated micro-hard abrasive of a kind of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon.
Technical scheme:
The preparation method of the coated micro-hard abrasive of a kind of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon, nano silicon spheres is comprised the steps: to be mixed with nano-silicon slurry, nano-silicon slurry is mixed with hard abrasive material, again the mixture obtained is heated, generate the coated micro-hard abrasive of nano-silicon.
Described nano silicon spheres is prepared by impulsive discharge method.
Silicon material in described impulsive discharge method is intrinsic silicon or doped silicon.
The diameter range of described nano silicon spheres is 10nm ~ 100nm, preferred 20nm ~ 60nm.
The massfraction of the oxidized portion in described nano silicon spheres is 10% ~ 100%, preferably 10% ~ 30%.
Described silicon slurry nano silicon spheres is dispersed in a kind of in polyoxyethylene glycol or Terpineol 350 or both mixed solutions prepare.
Described hard abrasive is selected from aluminium sesquioxide abrasive particle, diamond abrasive grain or norbide abrasive particle.
The particle size range of described hard abrasive is 30 μm ~ 200 μm, preferably 30 μm ~ 100 μm.
The Mohs' hardness of described hard abrasive is greater than 7.
The weight of described nano silicon spheres is 1% ~ 10% of hard abrasive weight, preferably 3% ~ 7%.
Described heating steps carries out in oxidized still.
The temperature range of described heating steps is 100 DEG C ~ 1100 DEG C, preferably 500 DEG C ~ 800 DEG C.
In described nano-silicon slurry, the massfraction scope of nano silicon spheres is 10% ~ 50%, preferably 20% ~ 40%.
The range of viscosities of described nano-silicon slurry is 1 Pas ~ 500Pas.
beneficial effect
(1) in the preparation method of the coated micro-hard abrasive of a kind of new nano-silicon provided by the invention, nano silicon spheres used is crystalline state, and its oxidation ratio is controlled, when its surface oxidation moiety content is less, compared with the silicon-dioxide used in present product (noncrystal), because the amplitude of the hardness reduction of non-crystalline material in temperature-rise period is much larger than amorphous material, the coated micro-hard abrasive of nano-silicon provided by the invention can be higher friction temperature, thus make the bonding force of nano-silicon and matrix stronger; (2) to prepare nano silicon ball productive rate high in impulsive discharge, is simple physical process, without the participation of toxic chemical, environment friendly and pollution-free; (3) preparation method of the coated micro-hard abrasive of a kind of new nano-silicon provided by the invention, cost is low, and technique is simple and stable, is applicable to large-scale industrial production; (4) preparation method of the coated micro-hard abrasive of a kind of new nano-silicon provided by the invention, accurately can control silicon-dioxide and aluminium sesquioxide ratio, suitability is wide; (5) preparation method of the coated micro-hard abrasive of a kind of new nano-silicon provided by the invention, provides new approaches for preparing analogous material.
Accompanying drawing explanation
Fig. 1 is the silicon ball SEM picture utilizing impulsive discharge to prepare nanometer provided by the invention
Fig. 2 is the silicon ball XRD figure sheet utilizing impulsive discharge to prepare nanometer provided by the invention
Fig. 3 is the SEM picture (overall diagram) of the coated aluminium sesquioxide abrasive material of nano-silicon prepared by method provided by the invention
Fig. 4 is the SEM picture (partial enlarged drawing) of the coated aluminium sesquioxide abrasive material of nano-silicon utilizing method provided by the invention to prepare
Fig. 5 is the SEM picture on the nano-silicon coated aluminium sesquioxide abrasive material process rear oxidation zirconium surface utilizing method provided by the invention to prepare
The EDS picture on the nano-silicon that Fig. 6 utilizes method provided by the invention to prepare coated aluminium sesquioxide abrasive material process rear oxidation zirconium surface
Embodiment
Below by embodiment, the present invention is described in further detail.But it will be understood to those of skill in the art that the following example only for illustration of the present invention, and should not be considered as limiting scope of the present invention.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by the conventional products of commercial acquisition.
The numerical value as range limit not only comprising and clearly listing should be interpreted as in a flexible way using the value that range format is expressed, but also comprise and be encompassed in all single numerical value within the scope of this or sub-range, be expressly recited out just as each numerical value and sub-range.Such as, the concentration range of " about 0.1% to about 5% " should be understood to the concentration not only comprising about 0.1% to about 5% clearly listed, also include single concentration in institute's how (as, 1%, 2%, 3% and 4%) and sub-range (such as, 0.1% to 0.5%, 1% to 2.2%, 3.3% to 4.4%).
The present invention utilizes nano silicon spheres as raw material, utilize suitable chemical reagent and physical method that the nano silicon spheres of preparation is formulated as favorable dispersity, there is the nano-silicon slurry of certain viscosity, the nano-silicon slurry of preparation is mixed according to a certain percentage with micron hard abrasive material, the equipment of putting into stirs, and makes nano silicon spheres be evenly distributed on hard abrasive surface; Again mixture is put into High Temperature Furnaces Heating Apparatus to heat, nano silicon spheres surface is oxidized, produces silicon dioxide layer on its surface, and make silicon dioxide layer that micro-molten phenomenon occur, make itself and hard abrasive produce certain bonding force.
In a preferred embodiment, above-mentioned nano silicon spheres is starting material with silicon, and the High Temperature High Pressure energy utilizing impulsive discharge to produce makes starting material vaporize, and forms nano silicon spheres.Impulsive discharge working method more specifically can consult document CN 103252542A, CN 102744477A.In this discharge-treating method, the silicon raw material of employing can be intrinsic silicon or doped silicon.Nano particle prepared by pulse discharge method is pure physical process, adding without chemical substance in preparation process, in use safer.The diameter range of above-mentioned nano silicon spheres is 10nm ~ 100nm, preferred 20nm ~ 60nm; The massfraction of the oxidized portion in nano silicon spheres is 10% ~ 100%, preferably 10% ~ 30%.
In one embodiment, nano silicon spheres is dispersed in polyoxyethylene glycol and prepares by silicon slurry, and in nano-silicon slurry, the massfraction scope of nano silicon spheres is 10% ~ 50%, and preferably 20% ~ 40%, the range of viscosities of nano-silicon slurry is 1 Pas ~ 500Pas.Mixed with hard abrasive by silicon slurry, hard abrasive is selected from aluminium sesquioxide abrasive particle, diamond abrasive grain again, norbide abrasive particle; The particle size range of hard abrasive is 30 μm ~ 200 μm, preferably 30 μm ~ 100 μm; The Mohs' hardness of hard abrasive is greater than 7; The weight of nano silicon spheres is 1% ~ 10% of hard abrasive weight, preferably 3% ~ 7%.
In one embodiment, heating steps carries out in oxidized still; The temperature range of heating steps is 100 DEG C ~ 1100 DEG C, preferably 500 DEG C ~ 800 DEG C.
embodiment 1
To mix P silicon single crystal (0.01 Ω cm) for starting material, pulse discharge method is utilized to prepare nano silicon spheres in deionized water, the median size 10nm of silicon ball, polyoxyethylene glycol is utilized to become the slurry of nano silicon spheres massfraction 15% with the Compound mixed solution of Terpineol 350, its viscosity is 105 Pas, then being 100 μm of aluminium sesquioxides by nano-silicon slurry and particle diameter mixes by weight the ratio of 1:3, stirs, makes nano silicon spheres uniform adhesion at alchlor abrasive surface.Finally in High Temperature Furnaces Heating Apparatus, be heated to 600 DEG C, keep 1 hour, nano silicon spheres surface is oxidized, forms silicon dioxide layer, and make itself and aluminium sesquioxide produce certain bonding force.
embodiment 2
To mix P silicon single crystal (0.01 Ω cm) for starting material, pulse discharge method is utilized to prepare nano silicon spheres in deionized water, the median size 20nm of silicon ball, polyoxyethylene glycol is utilized to become the slurry of nano silicon spheres massfraction 10% with the Compound mixed solution of Terpineol 350, its viscosity is 156 Pas, then being 30 μm of aluminium sesquioxides by nano-silicon slurry and particle diameter mixes by weight the ratio of 1:4, stirs, makes nano silicon spheres uniform adhesion at alchlor abrasive surface.Finally in High Temperature Furnaces Heating Apparatus, be heated to 600 DEG C, keep 2 hours, nano silicon spheres surface is oxidized, forms silicon dioxide layer, and make itself and aluminium sesquioxide produce certain bonding force.
embodiment 3
To mix P silicon single crystal (0.01 Ω cm) for starting material, pulse discharge method is utilized to prepare nano silicon spheres in deionized water, the median size 50nm of silicon ball, polyoxyethylene glycol and Terpineol 350 is utilized to be mixed with the slurry of nano silicon spheres massfraction 15%, its viscosity is 178 Pas, then being 30 μm of diamond abrasive grains by nano-silicon slurry and particle diameter mixes by weight the ratio of 1:4, stirs, makes nano silicon spheres uniform adhesion on diamond abrasive surface.Finally in High Temperature Furnaces Heating Apparatus, be heated to 600 DEG C, keep 1.5 hours, nano silicon spheres surface is oxidized, forms silicon dioxide layer, and make itself and diamond produce certain bonding force.
performance test:
After carrying out the process of surface friction chemical method silicon coating by the coated micro-hard abrasive of nano-silicon using the inventive method to prepare to dental zirconium oxide pottery.
The machinable dental zirconium oxide of presintering pottery porcelain block is cut into 10 × 10 × 2 mm under lasting water cooling
3ceramics 60 pieces, be divided into 6 groups and impose following surface treatment respectively after fully sintered:
Group A, aluminum oxide blast;
Group B, tribo-chemistry method silicon coating (Cojet system, 3M ESPE, the U.S.);
Group C, tribo-chemistry method silicon coating (the coated aluminium sesquioxide abrasive material of nano-silicon, embodiment 1);
Group D, tribo-chemistry method silicon coating (the coated aluminium sesquioxide abrasive material of nano-silicon, embodiment 2);
Group E, tribo-chemistry method silicon coating (nano-silicon cladding diamond abrasive material, embodiment 3).
By pretreated dental zirconium oxide pottery ceramics silane-coating coupling agent (Bisco, the U.S.), do with oil-free air featheriness after the 15s that naturally volatilizees.
With internal diameter 6mm, nylon Mold Making 60 pieces of light-cured composite post (Valux Plus of high 3mm, 3M ESPE, the U.S.), by resin column with resin cement (Choice, Bisco Inc., Schaumburg, the U.S.) adhere on each group of pretreated ceramics, unnecessary cement removed by probe, illumination curing 20s.Often group bonding sample is soaked in distilled water and embeds with self-curing resin after 24h under room temperature, and carry out shear bond strength test, test speed is 1.0mm/min, ultimate load during record resin isolation, and according to above-mentioned formulae discovery shear bond strength value.One-way analysis of variance is adopted to carry out statistical study (insolation level is 0.01) to each experimental group collected values of bond strength.
The shear bonding strength value of each group of sample is:
Group A, 3.10 ± 1.26MPa;
Group B, 13.45 ± 3.81MPa(Cojet system, 3M ESPE, the U.S.);
Group C, 11.51 ± 2.05MPa(embodiment 1);
Group D, 11.01 ± 3.30MPa(embodiment 2);
Group E, 10.05 ± 1.28MPa(embodiment 3).
Statistic analysis result shows, and there is not significant difference (P > 0.05) between group B-E4 group, but all higher than aluminum oxide blast group (P<0.01).Illustrate that several abrasive materials that tribo-chemistry method uses the present invention to prepare all can improve the bonding strength of dental zirconium oxide pottery and resin, and improve effect and Vehicles Collected from Market commonly uses products C ojet system effect without significant difference.
Claims (10)
1. the preparation method of the coated micro-hard abrasive of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon, it is characterized in that, nano silicon spheres is comprised the steps: to be mixed with nano-silicon slurry, nano-silicon slurry is mixed with hard abrasive material, again the mixture obtained is heated, generate the coated micro-hard abrasive of nano-silicon.
2. the preparation method of the coated micro-hard abrasive of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon according to claim 1, is characterized in that: described nano silicon spheres is prepared by impulsive discharge method.
3. the preparation method of the coated micro-hard abrasive of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon according to claim 2, is characterized in that: the silicon material in described impulsive discharge method is intrinsic silicon or doped silicon.
4. the preparation method of the coated micro-hard abrasive of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon according to claim 1, is characterized in that: the diameter range of described nano silicon spheres is 10nm ~ 100nm, preferred 20nm ~ 60nm.
5. the preparation method of the coated micro-hard abrasive of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon according to claim 1, it is characterized in that: the massfraction of the oxidized portion in described nano silicon spheres is 10% ~ 100%, preferably 10% ~ 30%.
6. the preparation method of the coated micro-hard abrasive of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon according to claim 1, is characterized in that: described silicon slurry nano silicon spheres is dispersed in a kind of in polyoxyethylene glycol or Terpineol 350 or both mixed solutions prepare; In described nano-silicon slurry, the massfraction scope of nano silicon spheres is 10% ~ 50%, preferably 20% ~ 40%; The range of viscosities of described nano-silicon slurry is 1 Pas ~ 500Pas.
7. the preparation method of the coated micro-hard abrasive of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon according to claim 1, is characterized in that: described hard abrasive is selected from aluminium sesquioxide abrasive particle, diamond abrasive grain or norbide abrasive particle.
8. the preparation method of the coated micro-hard abrasive of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon according to claim 1, is characterized in that: the particle size range of described hard abrasive is 30 μm ~ 200 μm, preferably 30 μm ~ 100 μm.
9. the preparation method of the coated micro-hard abrasive of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon according to claim 1, is characterized in that: the Mohs' hardness of described hard abrasive is greater than 7; The weight of described nano silicon spheres is 1% ~ 10% of hard abrasive weight, preferably 3% ~ 7%.
10. the preparation method of the coated micro-hard abrasive of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon according to claim 1, is characterized in that: described heating steps carries out in oxidized still; The temperature range of described heating steps is 100 DEG C ~ 1100 DEG C, preferably 500 DEG C ~ 800 DEG C.
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| CN201510038357.3A CN104671828B (en) | 2015-01-26 | 2015-01-26 | A kind of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon is coated with the preparation method of micro-hard abrasive |
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| CN201510038357.3A CN104671828B (en) | 2015-01-26 | 2015-01-26 | A kind of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon is coated with the preparation method of micro-hard abrasive |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112846192A (en) * | 2021-02-09 | 2021-05-28 | 南通理工学院 | Manufacturing method of metal ceramic composite swinging hammer |
| CN112869897A (en) * | 2021-01-14 | 2021-06-01 | 南京医科大学附属口腔医院 | Zirconia implant surface treatment method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475791A (en) * | 2009-01-20 | 2009-07-08 | 江苏工业学院 | Preparation and use of cerium oxide / silicon oxide compound abrasive |
| CN103223643A (en) * | 2013-05-03 | 2013-07-31 | 鲁启华 | Ultrathin blade |
| CN103500774A (en) * | 2013-09-18 | 2014-01-08 | 南京航空航天大学 | Method for utilizing P-type silicon ball as boron source to prepare local back field |
-
2015
- 2015-01-26 CN CN201510038357.3A patent/CN104671828B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475791A (en) * | 2009-01-20 | 2009-07-08 | 江苏工业学院 | Preparation and use of cerium oxide / silicon oxide compound abrasive |
| CN103223643A (en) * | 2013-05-03 | 2013-07-31 | 鲁启华 | Ultrathin blade |
| CN103500774A (en) * | 2013-09-18 | 2014-01-08 | 南京航空航天大学 | Method for utilizing P-type silicon ball as boron source to prepare local back field |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112869897A (en) * | 2021-01-14 | 2021-06-01 | 南京医科大学附属口腔医院 | Zirconia implant surface treatment method |
| CN112846192A (en) * | 2021-02-09 | 2021-05-28 | 南通理工学院 | Manufacturing method of metal ceramic composite swinging hammer |
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