CN103041976B - Method for preparing argentiferous antibacterial coating on surface of CoCr alloy material for oral use - Google Patents
Method for preparing argentiferous antibacterial coating on surface of CoCr alloy material for oral use Download PDFInfo
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- CN103041976B CN103041976B CN201210568067.6A CN201210568067A CN103041976B CN 103041976 B CN103041976 B CN 103041976B CN 201210568067 A CN201210568067 A CN 201210568067A CN 103041976 B CN103041976 B CN 103041976B
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Abstract
The invention discloses a method for preparing an argentiferous antibacterial coating on a surface of CoCr alloy material for oral use. The method is characterized by including the steps of (1) cleaning the surface of the CoCr alloy material; (2) preparing the argentiferous antibacterial coating on the surface of the CoCr alloy material; (3) cleaning the obtained the CoCr alloy material with the argentiferous antibacterial coating, drying and storing. The method for preparing the argentiferous antibacterial coating on the surface of CoCr alloy material for oral use has the advantages of industrialization, low cost and the like, and antibacterial material prepared by the method is high in biocompatibility, good in stability and has good antibacterial action to common oral bacteria like streptococcus mutans and white candida.
Description
Technical field
The invention belongs to oral medical consumptive material technical field, be specifically related to a kind of method of preparing silver-containing antibacterial coating at oral cavity CoCr alloy material surface.
Background technology
Cochrome has good physics, chemical property, and suitable mechanical property and good processing performance, to mucous membrane nonirritant.At the clinical base that is widely used in preparing oral artificial tooth.Base is called tooth base, is one of chief component of removable denture, and it covers on the alveolar ridge of anodontia, each portion of artificial tooth can be linked to be to an entirety, is arrangemant of artificial tooth's basis.Cochrome base complete denture has the following advantages compared with conventional resins base complete denture: one, wear light and handy, comfortable, foreign body sensation is little.Two, be difficult for jackknifing.Three, tasteless, do not absorb water, fineness is good.Four, there is good biocompatibility.
Oral cavity is the body cavity of an opening, is exposed in a large amount of biologies, chemistry and mechanical stimulus.Intraoral microorganism comprises bacterium, fungi, virus etc., and only bacterium just reaches kind more than 400, and major part exists with symbiotic form.Removable partial denture can increase bacterial plaque adhering on facing, thereby has increased the incidence of oulitis, periodontitis and dental caries disease.After artificial tooth reparation, by oral cavity pathogen, caused, secondary caries gingivitis, denture stomatitis and periodontosis be clinical oral problem in the urgent need to address always.Streptococcus oralis is the dominant microflora in oral cavity, is the main cariogenic bacteria in bacterial plaque, be also artificial tooth mainly adhere to one of flora.Streptococcus mutans is not only the Main Pathogenic Bacteria of bizet dental caries disease, is also the Main Pathogenic Bacteria of root Caries.Therefore, artificial tooth is antibacterial to keeping oral cavity to have safely vital meaning.
Nano silver antimicrobials because its has a broad antifungal spectrum, antibacterial efficacy are lasting, Heat stability is good, be difficult for producing bacterial drug resistance and the advantage such as biological safety is good, become the focus of studying in lithotroph anti-biotic material.Nano Silver can interact with the cell membrane of microorganism, changes the electronics transmission of biomembranous permeability and film respiratory chain.Undersized Nano Silver has relatively large specific area, is conducive to contact and enter with bacterium surface in bacterium, disturbs the permeability of bacterium and the respiratory function of film.The toxicity research that at present Nano Silver is acted on to cell has had a lot of reports.Most of documents are all thought, Nano Silver exists certain cytotoxicity to cell, and the Nano Silver of different size variable concentrations is also different to the toxic action of dissimilar cell, it is generally acknowledged, the size of Nano Silver and surface chemical property are the principal elements that determines Nano Silver toxicity.Therefore, reduce the Nano Silver toxicity that may exist, and unique anti-microbial property of performance Nano Silver becomes it and provides good approach in clinical use.
Titanium dioxide (TiO
2) belong to N-shaped semi-conducting material, there is band structure.When being subject to energy higher than the optical excitation of energy gap, light induced electron transits to conduction band from valence band, in valence band, forms photohole.Light induced electron and hole are at TiO
2surface forms redox light-catalyzed reaction position.TiO
2have that chemical stability is good, the advantage such as biocompatibility, nontoxic, pollution-free and production cost are lower.Dichloride in anatase type TiO
2be a kind of antibacterial agent, there is good sterilization effectiveness, good heat resistance, security performance is good, continuation is long, the feature such as easy to use.Therefore, TiO
2at biomedical sector, be widely used.
In artificial tooth preparation research, TiO
2with the anti-biotic material composition of Nano Silver as resin base, result of study shows: nano silver antimicrobials is read coccus, staphylococcus aureus, EHEC to streptococcus mutans, Bacillus acidi lactici, actinomyces viscosus, white all good bactericidal effect.This patent adopts TiO
2as the surface film of CoCr alloy, ensure on the one hand the biocompatibility of artificial tooth, also can serve as on the one hand in addition the effective carrier of nano silver material.This patented method is simple, and cost is low, and Industrialized processing technique maturation effectively avoids Nano Silver to enter the internal circulation system of human body, the nano material toxicity that minimizing may exist.
Summary of the invention
The object of the invention is to provide a kind of oral cavity CoCr alloy material surface to prepare the method for silver-containing antibacterial coating, has solved conventional oral cavity CoCr alloy material in prior art and has carried out usually causing the problems such as secondary caries gingivitis, denture stomatitis and periodontosis after artificial tooth reparation.
In order to solve these problems of the prior art, technical scheme provided by the invention is:
A method for silver-containing antibacterial coating is prepared in oral cavity with CoCr alloy material surface, it is characterized in that said method comprising the steps of:
(1) clean CoCr alloy material surface;
(2) pass through step I) or step I i) at CoCr alloy material surface, prepare silver-containing antibacterial coating:
I) nano-Ag particles is added to titanium dioxide (TiO
2) sol solution, stir, standby; TiO 2 sol solution containing Nano Silver is coated in to step (1) CoCr alloy material surface after treatment, then the CoCr alloy material calcining after applying is formed to silver-containing antibacterial coating;
Ii) TiO 2 sol solution is coated in to step (1) CoCr alloy material surface after treatment, then the CoCr alloy material calcining after applying is formed to titanium dioxide film; Then the solution that makes silver ion by photo-reduction method on titanium dioxide film secure attachment silver particle as silver-containing antibacterial coating;
(3) the CoCr alloy material of the silver-containing antibacterial coating of acquisition is cleaned to dry rear preservation.
Preferably, in described method, CoCr alloy material is for forming according to gear division routine embedding casting in advance before in step (1), and CoCr alloy material surface is by stand-by after polishing, clean, being dried.
Preferably, titanium dioxide (TiO in described method step (2)
2) sol solution directly forms after titanium salt is hydrolyzed or titanium salt coagulates formation through separating.
Preferably, TiO in described method
2the preparation method of film is: with the pretreated matrix of process, be impregnated in colloidal sol, speed with 3-5cm/min upwards at the uniform velocity lifts taking-up, after taking-up at 100 ℃ of dry 10min, according to required film thickness, membrane is repeatedly repeatedly, put into Muffle furnace and be warming up to 500 ℃ with the speed of 2-5 ℃/min, cooling with stove after insulation 90min, make titanium dioxide (or Nano Silver-titanium dioxide) film.
Preferably, the described method step i) preparation method of middle silver-containing antibacterial coating is: with the pretreated matrix of process, be impregnated into containing in the TiO 2 sol solution of Nano Silver, speed with 3-5cm/min upwards at the uniform velocity lifts taking-up, after taking-up at 100 ℃ of dry 10min, according to required film thickness repeatedly membrane repeatedly, put into Muffle furnace and be warming up to 500 ℃ with the speed of 2-5 ℃/min, cooling with stove after insulation 90min, make silver-containing antibacterial coating (being Nano Silver-titanium deoxid film).
Preferably, described in described method, titanium salt is selected from titanium tetrachloride (TiCl
4), butyl titanate (Ti (OCH
2cH
2cH
2cH
3)
4), isopropyl titanate (Ti(OCH (CH
3)
2)
4).
Preferably, in described method step (2), nano-Ag particles is selected from the naked particle of Nano Silver or the surperficial nano-Ag particles containing modified group.
Preferably, in described method, nano-Ag particles directly adds with solid particle existence form or is stored in organic solution and forms the form of mixing nano-Ag particles organic solution and add.Organic solution can be ethanolic solution etc.
Preferably, in described method, the grain diameter of nano-Ag particles is 10 ~ 100 nanometers.
Preferably, in described method, light reaction method comprises the AgNO of preparation containing the 0.02-0.8mol/L of photohole sacrifice agent
3solution, puts into the reaction of photochemical reaction instrument by obtain solution, and ultraviolet lighting reaction 4h, is supported on TiO by silver
2on film.Described hole sacrifice agent is selected from methyl alcohol, ethanol and isopropyl alcohol etc.
In photo-reduction method, in the solution of silver ion, need only containing Ag
+solution just meet the requirement of technical solution of the present invention.The solution of the silver ion preferably, using in described photo-reduction method is AgNO
3solution.
Technical solution of the present invention provides a kind of oral cavity CoCr alloy material surface to prepare the method for silver-containing antibacterial coating, comprises the following steps:
Step 1: clean CoCr alloy material surface, obtains the clean surface with well attached performance;
Step 2: prepare TiO 2 sol solution.TiO 2 sol solution mainly contains titanium tetrachloride (TiCl
4), butyl titanate (Ti (OCH
2cH
2cH
2cH
3)
4), isopropyl titanate (Ti(OCH (CH
3)
2)
4) etc. titanium salt preparation.
By TiO 2 sol solution, obtain containing the method for nanometer silver antimicrobial film and comprise: (1), nano-Ag particles is added to titanium dioxide (TiO
2) sol solution, stir, to be used; Then utilize containing the TiO 2 sol solution of Nano Silver and apply at CoCr alloy material, calcining film forming is containing nanometer silver antimicrobial film.Or (2), utilize TiO 2 sol solution CoCr alloy material apply, calcining film forming be titanium dioxide film (titanium deoxid film).Until titanium dioxide, after carrier surface film forming, utilize photo-reduction technology, on titanium deoxid film, preparation has the silver-colored particle of good adhesion;
Step 3: the CoCr alloy material with silver-containing antibacterial coating obtaining is cleaned, preserve after vacuum drying is spent the night.The CoCr alloy material with silver-containing antibacterial coating obtaining is anti-biotic material, aobvious good biocompatibility, and streptococcus mutans, gold-coloured staphylococci are represented to good antibacterial and bacteriostasis.
The common used material that described CoCr alloy material is used for hospital clinical before use, forms according to gear division routine embedding casting, surperficial by polishing, cleaning, dry rear stand-by.
Described TiO
2the preparation method of film is sol-gal process, through being hydrolyzed direct formation colloidal sol or through separating the solidifying colloidal sol that forms, then making solute polymeric gel, utilizes dip-coating method, spraying process etc. to form modified film (TiO at CoCr material in metal alkoxide or inorganic salts
2film), organic principle is removed in roasting, finally obtains TiO
2dense film.
The nano-Ag particles adding in collosol and gel can be naked particle or the surperficial Nano Silver containing modified group, and Nano Silver existing way can be the organic solutions such as ethanol, or solid particle.The grain diameter of nano-Ag particles is 10 ~ 100 nanometers, and the distribution of particle diameter can change with the requirement of material.Nano-Ag particles must have good dispersion in TiO 2 sol, guarantees the anti-microbial property of film.
Titanium dioxide, after carrier surface film forming, utilizes photo-reduction technology at TiO
2film (TiO after calcining
2dense film) on be fixed and support silver-colored particle; Photo-reduction technology, can be at TiO according to the difference of reaction condition
2the silver-colored particle of preparing nanoscale or micro-meter scale on film, is tightly adhered to TiO
2matrix surface.
The method utilize titanium dioxide high-biocompatibility and and the fixation to nano-Ag particles, can effectively avoid Nano Silver to enter human body on the one hand, the nanometer toxicity that release may exist, simultaneously to streptococcus mutans and effectively antibacterial and bactericidal action of gold-coloured staphylococci.
Denture base material-CoCr the alloy that another object of the present invention is to provide a kind of clinical use, the method for silver-containing antibacterial material is prepared on surface.In technical solution of the present invention, sol-gal process particularly, through being hydrolyzed direct formation colloidal sol or through separating the solidifying colloidal sol that forms by metal alkoxide or inorganic salts, then make solute polymeric gel, utilize dip-coating method, spraying process etc. to form modified film, roasting removal organic principle at CoCr material, finally obtain TiO
2dense film.The feature such as the method has can industrialization, cost is low, the anti-biotic material of preparation has high-hydrophilic, high-biocompatibility, good stability, and streptococcus mutans, white are read to the oral cavity common bacterias such as coccus there is good antibacterial action.
With respect to scheme of the prior art, advantage of the present invention is:
Denture base material-CoCr alloy material material strip silver-containing antibacterial coating that the present invention obtains, in conjunction with TiO
2with the antibacterial activity of Ag, aobvious strong wetability again, existing good biocompatibility, the mechanical property of maintenance artificial tooth material.Through test, confirm, this CoCr alloy material with silver-containing antibacterial coating is anti-biotic material, and streptococcus mutans, gold-coloured staphylococci are represented to good antibacterial and bacteriostasis.
Anti-biotic material prepared by the inventive method, introduces when nano silver antimicrobials, can effectively avoid Nano Silver to enter the internal circulation system of human body, the nano material toxicity that minimizing may exist.Preparation method of the present invention adopts the techniques that are produced on a large scale such as sol-gal process, simple, not high to equipment requirement, can realize suitability for industrialized production, can be for the preparation of the antibacterial surface film of various metal medical materials or medicine equipment.
In sum, the denture base material-CoCr alloy surface that the invention discloses a kind of clinical use is prepared the method for silver-containing antibacterial material.Step 1: clean CoCr alloy material surface, obtains the clean surface with well attached performance; Step 2: prepare TiO 2 sol solution.Obtain containing the method for nanometer silver antimicrobial film and comprise: (1) adds TiO 2 sol solution by nano-Ag particles, stirs, to be used; Or (2) until titanium dioxide after carrier surface film forming, utilize photo-reduction technology, preparation has the silver-colored particle of good adhesion; Step 3: utilize TiO 2 sol solution to apply at CoCr material, calcining film forming.The silver-containing antibacterial coating CoCr material of acquisition is cleaned, after vacuum drying is spent the night, preserved.The feature such as the method has can industrialization, cost is low, the anti-biotic material high-biocompatibility of preparation, good stability, and streptococcus mutans, white are read to the oral cavity common bacterias such as coccus there is good antibacterial action.
The specific embodiment
Below in conjunction with specific embodiment, such scheme is described further.Should be understood that these embodiment are not limited to limit the scope of the invention for the present invention is described.The implementation condition adopting in embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in normal experiment.
Embodiment 1
Get CoCr alloy material surface, surface finish is clean, dried for standby after supersound washing.TiO
2colloidal sol is according to butyl titanate (Ti(OC
4h
9)
4) as sol precursor.Required reagent is butyl titanate, ethanol, deionized water, red fuming nitric acid (RFNA) and acetylacetone,2,4-pentanedione, and its mol ratio is 1:35:2:0.15:0.3.Colloidal sol room temperature ageing 7 days after configuration.At TiO
2the mol ratio that is 1000:2 according to the mol ratio of Ag and Ti in colloidal sol adds the nano-Ag particles of 50nm, stirs.
Adopt dip-coating method, prepare film.The film of preparation is put into Muffle furnace and is warming up to 500 ℃ with the speed of 3 ℃/min, cooling with stove after insulation 90min, system containing Ag and TiO
2the CoCr alloy material of sol pellicle.
Prepare containing Ag and TiO
2antibacterial film (silver-containing antibacterial coating) surface smoothing of the CoCr alloy material of sol pellicle, antibacterial experiment research shows to have good antibacterial activity.
Embodiment 2
Get CoCr alloy material surface, surface finish is clean, dried for standby after supersound washing.TiO
2colloidal sol is according to isopropyl titanate (Ti (OCH (CH
3)
2)
4) as sol precursor.Required reagent is isopropyl titanate, ethanol, deionized water, red fuming nitric acid (RFNA) and acetylacetone,2,4-pentanedione, and its mol ratio is 1:28:6:0.15:0.3.Colloidal sol room temperature ageing 2 days after configuration.At TiO
2the mol ratio that is 1000:5 according to the mol ratio of Ag and Ti in colloidal sol adds particle diameter to be about the nano-Ag particles of 80nm, stirs.
Adopt dip-coating method, prepare film.The film of preparation is put into Muffle furnace and is warming up to 500 ℃ with the speed of 3 ℃/min, cooling with stove after insulation 90min, prepares containing Ag and TiO
2the CoCr alloy material of sol pellicle.
Prepare containing Ag and TiO
2antibacterial film (silver-containing antibacterial coating) surface smoothing of the CoCr alloy material of sol pellicle, antibacterial experiment research shows to have good antibacterial activity.
Embodiment 3
Get CoCr alloy material surface, surface finish is clean, dried for standby after supersound washing.TiO
2colloidal sol is according to butyl titanate (Ti(OC
4h
9)
4) as sol precursor.Required reagent is butyl titanate, ethanol, deionized water, red fuming nitric acid (RFNA) and acetylacetone,2,4-pentanedione, and its mol ratio is 1:30:5:0.2:0.2.Colloidal sol room temperature ageing 5 days after configuration.
Adopt dip-coating method, the film on preparation CoCr surface.The film of preparation is put into Muffle furnace and is warming up to 500 ℃ with the speed of 3 ℃/min, cooling with stove after insulation 90min, obtains containing TiO
2the CoCr alloy material of film.
By 1.275g AgNO
3be dissolved in the water of 150ml, add 8g absolute ethyl alcohol, be mixed with the AgNO of 0.1mol/L
3solution, puts into reaction in photochemical reaction instrument (uviol lamp 300W, apart from 8cm) by obtain solution and silver was supported on to TiO in 4 hours
2on film, cleaning-drying obtains containing Ag and TiO
2the CoCr alloy material of sol pellicle.。
The CoCr film surface preparing is level and smooth, and antibacterial experiment research shows to have good antibacterial activity.
Embodiment 4
Get CoCr alloy material surface, surface finish is clean, dried for standby after supersound washing.TiO
2colloidal sol is according to butyl titanate (Ti(OC
4h
9)
4) as sol precursor.Required reagent is butyl titanate, ethanol, deionized water, red fuming nitric acid (RFNA) and acetylacetone,2,4-pentanedione, and its mol ratio is 1:30:5:0.2:0.2.Colloidal sol room temperature ageing 5 days after configuration.
Adopt dip-coating method, the film on preparation CoCr surface.The film of preparation is put into Muffle furnace and is warming up to 500 ℃ with the speed of 3 ℃/min, cooling with stove after insulation 90min, obtains containing TiO
2the CoCr alloy material of film.
By 0.63g AgNO
3be dissolved in the water of 150ml, add 4g anhydrous isopropyl alcohol, preparation is into about the AgNO of 0.05mol/L
3solution, puts into reaction in photochemical reaction instrument (uviol lamp 500W, apart from 8cm) by obtain solution and silver was supported on to TiO in 2 hours
2on film, cleaning-drying obtains containing Ag and TiO
2the CoCr alloy material (anti-biotic material) of sol pellicle.
Prepare containing Ag and TiO
2antibacterial film (antimicrobial coating) surface smoothing of the CoCr alloy material of sol pellicle, antibacterial experiment research shows to have good antibacterial activity.
Above-mentioned example is only explanation technical conceive of the present invention and feature, and its object is to allow person skilled in the art can understand content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalent transformations that Spirit Essence does according to the present invention or modification, within all should being encompassed in protection scope of the present invention.
Claims (6)
1. a method for silver-containing antibacterial coating is prepared in oral cavity with CoCr alloy material surface, it is characterized in that said method comprising the steps of:
(1) clean CoCr alloy material surface;
(2) pass through step I) or step I i) at CoCr alloy material surface, prepare silver-containing antibacterial coating:
I) nano-Ag particles is added to titanium dioxide (TiO
2) sol solution, stir, standby; TiO 2 sol solution containing Nano Silver is coated in to step (1) CoCr alloy material surface after treatment, then the CoCr alloy material calcining after applying is formed to silver-containing antibacterial coating;
Ii) TiO 2 sol solution is coated in to step (1) CoCr alloy material surface after treatment, then the CoCr alloy material calcining after applying is formed to titanium dioxide film; Then the solution that makes silver ion by photo-reduction method on titanium dioxide film secure attachment silver particle as silver-containing antibacterial coating;
Wherein titanium dioxide (TiO
2) sol solution is by rear titanium salt hydrolysis directly formation or titanium salt solution is coagulated to rear formation; Described titanium salt is selected from titanium tetrachloride (TiCl
4), butyl titanate (Ti (OCH
2cH
2cH
2cH
3)
4), isopropyl titanate (Ti(OCH (CH
3)
2)
4);
(3) the CoCr alloy material of the silver-containing antibacterial coating of acquisition is cleaned to dry rear preservation.
2. method according to claim 1, is characterized in that in described method, CoCr alloy material is for forming according to gear division routine embedding casting in advance before in step (1), and CoCr alloy material surface is by stand-by after polishing, clean, being dried.
3. method according to claim 1, is characterized in that in described method step (2), nano-Ag particles is selected from the naked particle of Nano Silver or the surperficial nano-Ag particles containing modified group.
4. method according to claim 3, is characterized in that nano-Ag particles in described method directly adds with solid particle existence form or is stored in organic solution, to form the form of mixing nano-Ag particles organic solution and add.
5. method according to claim 3, the grain diameter that it is characterized in that nano-Ag particles in described method is 10～100 nanometers.
6. method according to claim 3, the solution that it is characterized in that the silver ion using in described photo-reduction method is AgNO
3solution.
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|---|---|---|---|
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| CN201210568067.6A CN103041976B (en) | 2012-12-25 | 2012-12-25 | Method for preparing argentiferous antibacterial coating on surface of CoCr alloy material for oral use |
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| CN103041976B true CN103041976B (en) | 2014-04-30 |
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Citations (5)
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|---|---|---|---|---|
| CN101161295A (en) * | 2007-11-08 | 2008-04-16 | 浙江大学 | Method for modifying medical metallic grafting body surface collagen by galvano-chemistry method |
| CN101379216A (en) * | 2006-02-03 | 2009-03-04 | 卡罗比亚意大利（共同）股份公司 | A process for functionalizing titanium metal surfaces with nanometric particles of titanium and products thus functionalized |
| CN101491693A (en) * | 2008-09-23 | 2009-07-29 | 西北有色金属研究院 | Preparation method of hydroxylapatite/titanic oxide composite biological coatings |
| US20090269487A1 (en) * | 2006-06-21 | 2009-10-29 | Mohammed Es-Souni | Process for producing a sol-gel-based absorber coating for solar heating |
| CN102525827A (en) * | 2012-01-18 | 2012-07-04 | 重庆大学 | Method for preparing medical titanium material with long-acting antibacterial property and good biocompatibility |
-
2012
- 2012-12-25 CN CN201210568067.6A patent/CN103041976B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101379216A (en) * | 2006-02-03 | 2009-03-04 | 卡罗比亚意大利（共同）股份公司 | A process for functionalizing titanium metal surfaces with nanometric particles of titanium and products thus functionalized |
| US20090269487A1 (en) * | 2006-06-21 | 2009-10-29 | Mohammed Es-Souni | Process for producing a sol-gel-based absorber coating for solar heating |
| CN101161295A (en) * | 2007-11-08 | 2008-04-16 | 浙江大学 | Method for modifying medical metallic grafting body surface collagen by galvano-chemistry method |
| CN101491693A (en) * | 2008-09-23 | 2009-07-29 | 西北有色金属研究院 | Preparation method of hydroxylapatite/titanic oxide composite biological coatings |
| CN102525827A (en) * | 2012-01-18 | 2012-07-04 | 重庆大学 | Method for preparing medical titanium material with long-acting antibacterial property and good biocompatibility |
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