CN104671828B - 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 - Google Patents
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 Download PDFInfo
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- CN104671828B CN104671828B CN201510038357.3A CN201510038357A CN104671828B CN 104671828 B CN104671828 B CN 104671828B CN 201510038357 A CN201510038357 A CN 201510038357A CN 104671828 B CN104671828 B CN 104671828B
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Abstract
The present invention relates to a kind of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon and be coated with the preparation method of micro-hard abrasive.With silicon as raw material, utilize pulsed discharge to make raw material vaporize, form nano silicon spheres.The nano silicon spheres of preparation is formulated as favorable dispersibility, there is the nano-silicon slurry of certain viscosity, in nano-silicon slurry, then add hard abrasive, stir, make nano silicon spheres uniform adhesion on hard abrasive surface.Last heating, drying in high temperature furnace, and make nano silicon spheres surface oxidized, form silica overlayer；Make silicon dioxide layer melt simultaneously, produce certain adhesion with abrasive particle.The hard abrasive that tribochemistry method uses the inventive method to prepare can significantly improve the adhesive strength of pottery and interlaminar resin after processing dental zirconium oxide ceramic surface, its effect is suitable with Vehicles Collected from Market main product.This method technique simple and stable, low cost, be suitable for scale of mass production.
Description
Technical field
The present invention relates to a kind of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon and be coated with micro-hard mill
The preparation method of grain, belongs to field of material preparation.
Background technology
All-ceramic Dental Material can be divided into alumina-based ceramic, zirconia-based ceramics and glass base according to main component difference
The kinds such as pottery.Wherein, zirconia-based ceramics relies on outstanding mechanical performance and good aesthetic properties at All-ceramic Dental Material
In show one's talent, especially for when making the dummy such as many units fixed bridge, implantation body, telescope crown with All-ceramic material, oxidation
Zirconia-based ceramic replaces the pottery of other kind and becomes first-selection and the most uniquely select.
During All-ceramic restoration, resin cement is due in sides such as adhesive strength, color matching, marginal seal, water solubilities
The performance in face is superior to other bonding agent kind and is used by routine.Research finds, good bonding being possible not only to increases reparation
Retention, and dummy can be tightly linked with abutment and be integrally formed, effective dispersion cushion effect effect, on the other hand,
Resin adhesive can also make up the microfissure that all-ceramic prosthesis adds man-hour and formed before dimerization, reduces thus caused stress
Concentrate the hidden danger brought.It is increasingly recognised that, combination good between resin/pottery is to affect All-ceramic restoration success rate
One key factor.At present it is believed that the mechanism that pottery is combined with interlaminar resin mainly includes ceramic surface and the infiltration of roughening
The mechanical interlock effect that produces between the resin of solidification is prominent and by chemical adhesive effect between the two, the latter is to obtain firmly
The key of stable adhesion.Silane coupler is as a kind of binding agent extensively used in stomatology field, and it with silicon atom is
Core, usual one end is-CH=CH2Or-NH2, with the ethylene linkage (C=C) in resinous substrates, polyaddition reaction can occur；The other end
Comprise alkoxyl (such as-OCH3Or-OCH2CH3), can hydrolyze in acid condition and become silanol groups (Si-OH), can be with pottery
Polycondensation reaction is there is between the Si-OH on surface.And the stable chemical nature of zirconia ceramics, its apolar surfaces is difficult to by hydroxyl
Change, the most also cannot be directly realized by silanization.In order to change the character on zirconia ceramics surface, tribochemistry method
(Tribochemical method) is well recognized as maximally effective its principle of method forming silica coating in zirconium surface
Using a kind of special surface to cover the alumina grit of silicon oxide layer, high velocity air during sandblasting drives gravel bombardment ceramic watch
Face, locally moment produce High Temperature High Pressure, gravel come off after its surface silicon oxide layer just due to friction effect and coat pottery
On porcelain surface.Classical tribochemistry method silicon coating system includes that Rocatec and CoJet uses the zirconia ceramics that this method processes
It is recognized and adhesive property can be greatly improved after silanization, the most become and weighed other zirconium oxide bonding plane processing method
Reference standard.But, although confirming effectively, but existing tribochemistry method coat system is expensive, and 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 has sol-gel process,
Chemical deposition etc., but its complex process, high in cost of production.
Summary of the invention
The technical problem to be solved: conventional surface covers the preparation method of the alumina grit of silicon oxide layer
Complex process, high in cost of production problem, propose a kind of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon and be coated with
The preparation method of micro-hard abrasive.
Technical scheme:
A kind of dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon is coated with the preparation side of micro-hard abrasive
Method, comprises the steps: to be configured to nano silicon spheres nano-silicon slurry, is mixed with hard abrasive material by nano-silicon slurry, then
The mixture obtained is heated, generates nano-silicon and be coated with micro-hard abrasive.
Described nano silicon spheres is prepared by pulsed discharge method.
The described silicon material in pulsed discharge method is intrinsic silicon or doped silicon.
The diameter range of described nano silicon spheres is 10nm～100nm, preferably 20nm～60nm.
The mass fraction of the described oxidized portion in nano silicon spheres is 10%～100%, preferably 10%～30%.
Described silicon slurry is nano silicon spheres be dispersed in Polyethylene Glycol or terpineol a kind of or both mixed liquors
And prepare.
Described hard abrasive is selected from aluminium sesquioxide abrasive particle, diamond abrasive grain or boron carbide 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 more than 7.
The weight of described nano silicon spheres is the 1%～10% of hard abrasive weight, preferably 3%～7%.
Described heating steps is to carry out in oxidation furnace.
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 mass fraction scope of nano silicon spheres is 10%～50%, preferably 20%～40%.
The range of viscosities of described nano-silicon slurry is 1 Pa s～500Pa s.
Beneficial effect
(1) a kind of new nano-silicon that the present invention provides is coated with nano silicon spheres used in the preparation method of micro-hard abrasive
For crystalline state, and its oxidation ratio is controlled, when its surface oxidation moiety content is less, with the silicon dioxide that uses in current production
(noncrystal) is compared, and the amplitude reduced due to non-crystalline material hardness in temperature-rise period is much larger than amorphous material, and the present invention carries
The nano-silicon of confession be coated with micro-hard abrasive can higher friction temperature so that the adhesion of nano-silicon and matrix is higher；(2)
It is high that nano silicon ball productivity is prepared in pulsed discharge, is simple physical process, and without the participation of toxic chemical, environmental protection is without dirt
Dye；(3) a kind of new nano-silicon that the present invention provides is coated with the preparation method of micro-hard abrasive, low cost, and technique is simple and steady
Fixed, it is suitable for large-scale industrial production；(4) a kind of new nano-silicon that the present invention provides is coated with the preparation side of micro-hard abrasive
Method, can accurately control silicon dioxide and aluminium sesquioxide ratio, and the suitability is wide；(5) a kind of new nano-silicon that the present invention provides
It is coated with the preparation method of micro-hard abrasive, provides new approaches for preparing similar material.
Accompanying drawing explanation
Fig. 1 is that the silicon ball SEM picture of nanometer is prepared in the pulsed discharge that utilizes that the present invention provides
Fig. 2 is that the silicon ball XRD figure sheet of nanometer is prepared in the pulsed discharge that utilizes that the present invention provides
Fig. 3 is the SEM picture (overall diagram) of nano-silicon cladding aluminium sesquioxide abrasive material prepared by the method that the present invention provides
Fig. 4 is that nano-silicon prepared by the method utilizing the present invention to provide is coated with the SEM picture of aluminium sesquioxide abrasive material (locally
Enlarged drawing)
Fig. 5 is that nano-silicon cladding aluminium sesquioxide abrasive material prepared by the method utilizing the present invention to provide processes rear oxidation zirconium
The SEM picture on surface
Nano-silicon cladding aluminium sesquioxide abrasive material prepared by the method that Fig. 6 utilizes the present invention to provide processes rear oxidation zirconium table
The EDS picture in face
Detailed description of the invention
Below by detailed description of the invention, the present invention is described in further detail.But those skilled in the art will manage
Solving, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Unreceipted concrete skill in embodiment
Art or condition person, according to the technology described by the document in this area or condition or carried out according to product description.Examination used
Agent or instrument unreceipted production firm person, be can by city available from conventional products.
The value expressed using range format should be interpreted as in a flexible way not only including clearly listing as scope
The numerical value of limit value, but also include containing all single numerical value within the range or subinterval, just as each numerical value and Zi Qu
Between be expressly recited out.Such as, the concentration range of " about 0.1% to about 5% " should be understood to not only to include clearly to list
The concentration of about 0.1% to about 5%, also includes the single concentration (e.g., 1%, 2%, 3% and 4%) in the range of indication and subinterval (example
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, utilizes suitable chemical reagent and physical method by the nano-silicon of preparation
Ball is formulated as favorable dispersibility, has the nano-silicon slurry of certain viscosity, by nano-silicon slurry and the micron hard abrasive material of preparation
Mix according to a certain percentage, put in equipment and stir, make nano silicon spheres be evenly distributed on hard abrasive surface；Again mixture is put
Enter in high temperature furnace and heat, make nano silicon spheres surface aoxidize, produce silicon dioxide layer on its surface, and make silicon dioxide layer send out
Raw micro-molten phenomenon so that it is produce certain adhesion with hard abrasive.
In a preferred embodiment, above-mentioned nano silicon spheres is with silicon as raw material, utilizes pulsed discharge to produce
High Temperature High Pressure energy makes raw material vaporize, and forms nano silicon spheres.More specifically pulsed discharge processing method can refer to document CN
103252542A、CN 102744477A.In this discharge-treating method, the silicon raw material of employing can be intrinsic silicon or doping
Silicon.Nano-particle prepared by pulse discharge method is pure physical process, without the addition of chemical substance in preparation process, is using
In journey safer.The diameter range of above-mentioned nano silicon spheres is 10nm～100nm, preferably 20nm～60nm；Oxygen in nano silicon spheres
The mass fraction of change part is 10%～100%, preferably 10%～30%.
In one embodiment, nano silicon spheres is dispersed in Polyethylene Glycol and prepares by silicon slurry, nano-silicon
In slurry, the mass fraction scope of nano silicon spheres is 10%～50%, preferably 20%～40%, and the range of viscosities of nano-silicon slurry is 1
Pa s～500Pa s.Being mixed with hard abrasive by silicon slurry, hard abrasive is selected from aluminium sesquioxide abrasive particle, Buddha's warrior attendant stone grinder again
Grain, boron carbide abrasive particle；The particle size range of hard abrasive is 30 μm～200 μm, preferably 30 μm～100 μm；The Mohs of hard abrasive
Hardness is more than 7；The weight of nano silicon spheres is the 1%～10% of hard abrasive weight, preferably 3%～7%.
In one embodiment, heating steps is to carry out in oxidation furnace；The temperature range of heating steps be 100 DEG C～
1100 DEG C, preferably 500 DEG C～800 DEG C.
Embodiment 1
To mix P monocrystal silicon (0.01 Ω cm) as raw material, pulse discharge method is utilized to prepare nano-silicon in deionized water
Ball, mean diameter 10nm of silicon ball, utilize Polyethylene Glycol to become nano silicon spheres mass fraction 15% with the Compound mixed solution of terpineol
Slurry, its viscosity is 105 Pa s, is then 100 μm aluminium sesquioxide by weight the ratios of 1:3 by nano-silicon slurry and particle diameter
Example mixes, and stirs, makes nano silicon spheres uniform adhesion at alchlor abrasive surface.Finally it is heated in high temperature furnace
600 DEG C, keep 1 hour, make nano silicon spheres surface aoxidize, form silicon dioxide layer, and make it produce with aluminium sesquioxide
Certain adhesion.
Embodiment 2
To mix P monocrystal silicon (0.01 Ω cm) as raw material, pulse discharge method is utilized to prepare nano-silicon in deionized water
Ball, mean diameter 20nm of silicon ball, utilize Polyethylene Glycol to become nano silicon spheres mass fraction 10% with the Compound mixed solution of terpineol
Slurry, its viscosity is 156 Pa s, is then 30 μm aluminium sesquioxide by weight the ratios of 1:4 by nano-silicon slurry and particle diameter
Mixing, stirs, makes nano silicon spheres uniform adhesion at alchlor abrasive surface.Finally it is heated in high temperature furnace
600 DEG C, keep 2 hours, make nano silicon spheres surface aoxidize, form silicon dioxide layer, and make it produce with aluminium sesquioxide
Certain adhesion.
Embodiment 3
To mix P monocrystal silicon (0.01 Ω cm) as raw material, pulse discharge method is utilized to prepare nano-silicon in deionized water
Ball, mean diameter 50nm of silicon ball, utilize Polyethylene Glycol and terpineol to be configured to the slurry of nano silicon spheres mass fraction 15%, its
Viscosity is 178 Pa s, then by the ratio mixing that nano-silicon slurry and particle diameter are 30 μm diamond abrasive grains 1:4 by weight, fills
Divide and stir, make nano silicon spheres uniform adhesion on diamond abrasive surface.Finally in high temperature furnace, it is heated to 600 DEG C, keeps
1.5 hours, make nano silicon spheres surface aoxidize, form silicon dioxide layer, and make it produce certain adhesion with diamond.
Performance test:
It is coated with micro-hard abrasive by the nano-silicon that dental zirconium oxide pottery uses the inventive method prepare and carries out surface
After tribochemistry method silicon coating processes.
The machinable dental zirconium oxide pottery porcelain block of presintering is cut into 10 × 10 × 2 mm under lasting water cooling3's
Ceramics 60 pieces, fully sintered after be classified as 6 groups and impose respectively following surface process:
Group A, aluminum oxide blast；
Group B, tribochemistry method silicon coating (Cojet system, 3M ESPE, the U.S.)；
Group C, tribochemistry method silicon coating (nano-silicon cladding aluminium sesquioxide abrasive material, embodiment 1)；
Group D, tribochemistry method silicon coating (nano-silicon cladding aluminium sesquioxide abrasive material, embodiment 2)；
Group E, tribochemistry 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.), volatilization 15s naturally
After with oil-free air featheriness do.
With 60 pieces of light-cured composite posts of nylon Mold Making of internal diameter 6mm, high 3mm (Valux Plus, 3M ESPE,
The U.S.), resin column is adhered to each group of pretreatment with resin cement (Choice, Bisco Inc., Schaumburg, the U.S.)
Ceramics on, probe remove unnecessary cement, illumination curing 20s.Often group bonding sample is soaked in 24h in distilled water at room temperature
After embed with self-curing resin, carry out shear bond strength test, test speed is 1.0mm/min, when record resin separates
Big load, and calculate shear bond strength value according to above-mentioned formula.Use one factor analysis of variance to each experimental group bond strength
Value carries out statistical analysis (test level is 0.01).
The shear bonding strength value of each group 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, there is not significant difference (P ＞ 0.05), but be above aluminium oxide between group B-E4 group
Sandblasting group (P < 0.01).Illustrate that several abrasive materials that tribochemistry method uses the present invention to prepare all can improve dental zirconium oxide pottery
With the adhesive strength of resin, and improve effect and Vehicles Collected from Market and commonly use products C ojet system application effect without significant difference.
Claims (10)
1. dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon is coated with a preparation method for micro-hard abrasive,
It is characterized in that, comprise the steps: to be configured to nano silicon spheres nano-silicon slurry, nano-silicon slurry is carried out with hard abrasive
Mixing, then the mixture obtained is heated, generate nano-silicon and be coated with micro-hard abrasive；The weight of described nano silicon spheres is
The 1%～10% of hard abrasive weight；The temperature range of described heating steps is 100 DEG C～1100 DEG C.
Dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon the most according to claim 1 is coated with micro-hard
The preparation method of abrasive particle, it is characterised in that: described nano silicon spheres is prepared by pulsed discharge method.
Dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon the most according to claim 2 is coated with micro-hard
The preparation method of abrasive particle, it is characterised in that: the described silicon material in pulsed discharge method is intrinsic silicon or doped silicon.
Dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon the most according to claim 1 is coated with micro-hard
The preparation method of abrasive particle, it is characterised in that: the diameter range of described nano silicon spheres is 10nm～100nm.
Dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon the most according to claim 1 is coated with micro-hard
The preparation method of abrasive particle, it is characterised in that: the mass fraction of the described oxidized portion in nano silicon spheres is 10%～100%.
Dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon the most according to claim 1 is coated with micro-hard
The preparation method of abrasive particle, it is characterised in that: nano silicon spheres is dispersed in Polyethylene Glycol or terpineol by described silicon slurry
A kind of or both mixed liquor and prepare；In described nano-silicon slurry, the mass fraction scope of nano silicon spheres is 10%
～50%；The range of viscosities of described nano-silicon slurry is 1 Pa s～500Pa s.
Dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon the most according to claim 1 is coated with micro-hard
The preparation method of abrasive particle, it is characterised in that: described hard abrasive is selected from aluminium sesquioxide abrasive particle, diamond abrasive grain or carbonization
Boron abrasive particle.
Dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon the most according to claim 1 is coated with micro-hard
The preparation method of abrasive particle, it is characterised in that: the particle size range of described hard abrasive is 30 μm～200 μm.
Dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon the most according to claim 1 is coated with micro-hard
The preparation method of abrasive particle, it is characterised in that: the Mohs' hardness of described hard abrasive is more than 7；The weight of described nano silicon spheres
It is the 3%～7% of hard abrasive weight.
Dental zirconium oxide ceramic friction chemical method silicon coating system nano-silicon the most according to claim 1 cladding is micro-firmly
The preparation method of matter abrasive particle, it is characterised in that: described heating steps is to carry out in oxidation furnace；The temperature of described heating steps
Degree scope is 500 DEG C～800 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| CN104671828A CN104671828A (en) | 2015-06-03 |
| CN104671828B true CN104671828B (en) | 2016-08-24 |
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| CN112869897B (en) * | 2021-01-14 | 2022-01-25 | 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 |
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 |
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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 |
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