CN103041976A - 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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- CN103041976A CN103041976A CN2012105680676A CN201210568067A CN103041976A CN 103041976 A CN103041976 A CN 103041976A CN 2012105680676 A CN2012105680676 A CN 2012105680676A CN 201210568067 A CN201210568067 A CN 201210568067A CN 103041976 A CN103041976 A CN 103041976A
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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 for preparing the 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 are to the mucous membrane nonirritant.At the clinical base that is widely used in preparing oral artificial tooth.Base is called the tooth base, is one of chief component of removable denture, and it covers on the alveolar ridge of anodontia, can be linked to be an integral body to each one of artificial tooth, is arrangemant of artificial tooth's basis.Cochrome base complete denture is compared with conventional resins base complete denture and is had the following advantages: 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, has good biocompatibility.
The oral cavity is the body cavity of an opening, is exposed in a large amount of biologies, chemistry and the 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.Caused by oral cavity pathogen after the artificial tooth reparation, 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 the oral cavity, is the main cariogenic bacteria in the bacterial plaque, also be artificial tooth mainly adhere to one of flora.Streptococcus mutans is not only the Main Pathogenic Bacteria of bizet dental caries disease, also is the Main Pathogenic Bacteria of root Caries.Therefore, artificial tooth is antibiotic to keeping the oral cavity that vital meaning is arranged safely.
Nano silver antimicrobials becomes the focus of studying in the lithotroph anti-biotic material because its has a broad antifungal spectrum, antibacterial efficacy are lasting, Heat stability is good, be difficult for producing the advantages such as bacterial drug resistance and biological safety are good.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 in the bacterium with bacterium surface, disturbs the permeability of bacterium and the respiratory function of film.The toxicity research that at present Nano Silver is acted on 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 cells, 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 toxicity that Nano Silver may exist, and unique anti-microbial property of performance Nano Silver becomes it and provides preferably approach in clinical use.
Titanium dioxide (TiO
2) belong to the N-shaped semi-conducting material, have band structure.When being subject to energy and being higher than the optical excitation of energy gap, light induced electron transits to conduction band from valence band, forms photohole in valence band.Light induced electron and hole are at TiO
2The surface 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, have good sterilization effectiveness, good heat resistance, security performance is good, continuation is long, the characteristics such as easy to use.Therefore, TiO
2Be widely used at biomedical sector.
In the 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, in addition on the one hand also can be as the effective carrier of nano silver material.This patented method is simple, and cost is low, and Industrialized processing technique is ripe, 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 to prepare the method for silver-containing antibacterial coating with the CoCr alloy material surface, has solved in the prior art oral cavity commonly used and has carried out usually causing the problems such as secondary caries gingivitis, denture stomatitis and periodontosis after the artificial tooth reparation with the CoCr alloy material.
In order to solve these problems of the prior art, technical scheme provided by the invention is:
A kind of oral cavity prepares the method for silver-containing antibacterial coating with the CoCr alloy material surface, it is characterized in that said method comprising the steps of:
(1) cleaning CoCr alloy material surface;
(2) pass through step I) or step I i) prepare the silver-containing antibacterial coating at the CoCr alloy material surface:
I) nano-Ag particles is added titanium dioxide (TiO
2) sol solution, stir, for subsequent use; The TiO 2 sol solution that will contain Nano Silver is coated in the CoCr alloy material surface after step (1) is processed, and then the CoCr alloy material calcining after applying is formed the silver-containing antibacterial coating;
Ii) TiO 2 sol solution is coated in the CoCr alloy material surface after step (1) is processed, then the CoCr alloy material calcining after applying is formed titanium dioxide film; Then the solution that makes silver ion by the photo-reduction method on titanium dioxide film secure attachment silver particle as the silver-containing antibacterial coating;
(3) the CoCr alloy material with the silver-containing antibacterial coating that obtains cleans, and preserves after dry.
Preferably, the CoCr alloy material is to cast according to the conventional embedding of tooth section in advance before in step (1) to form in the described method, and the CoCr alloy material surface is by polishing, cleaning, dry rear stand-by.
Preferably, titanium dioxide (TiO in the described method step (2)
2) titanium salt is hydrolyzed rear directly formation to sol solution or titanium salt coagulates formation through separating.
Preferably, TiO in the described method
2The thin film technology method is: with the pretreated matrix of process, be impregnated in the colloidal sol, speed with 3-5cm/min upwards at the uniform velocity lifts taking-up, take out rear at 100 ℃ of dry 10min, membrane is repeatedly repeatedly according to required film thickness, put into Muffle furnace and be warming up to 500 ℃ with the speed of 2-5 ℃/min, with the stove cooling, make titanium dioxide (or Nano Silver-titanium dioxide) film behind the insulation 90min.
Preferably, described method step i) preparation method of silver-containing antibacterial coating is in: with the pretreated matrix of process, be impregnated in the TiO 2 sol solution that contains Nano Silver, speed with 3-5cm/min upwards at the uniform velocity lifts taking-up, after taking out 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, with the stove cooling, make silver-containing antibacterial coating (being Nano Silver-titanium deoxid film) behind the insulation 90min.
Preferably, titanium salt is selected from titanium tetrachloride (TiCl described in the described method
4), butyl titanate (Ti (OCH
2CH
2CH
2CH
3)
4), isopropyl titanate (Ti(OCH (CH
3)
2)
4).
Preferably, nano-Ag particles is selected from the naked particle of Nano Silver or the surperficial nano-Ag particles that contains modified group in the described method step (2).
Preferably, nano-Ag particles directly adds with the solid particle existence form or is stored in the organic solution and forms the form of mixing nano-Ag particles organic solution and add in the described method.Organic solution can be ethanolic solution etc.
Preferably, the grain diameter of nano-Ag particles is 10 ~ 100 nanometers in the described method.
Preferably, the light reaction method comprises that preparation contains the AgNO of the 0.02-0.8mol/L of photohole sacrifice agent in the described method
3Solution is put into the reaction of photochemical reaction instrument with obtain solution, and ultraviolet lighting reaction 4h is supported on TiO with silver
2On the film.Described hole sacrifice agent is selected from methyl alcohol, ethanol and isopropyl alcohol etc.
As long as contain Ag in the solution of silver ion in the photo-reduction method
+Solution just satisfy the requirement of technical solution of the present invention.The solution of the silver ion that preferably, uses in the described photo-reduction method is AgNO
3Solution.
Technical solution of the present invention provides a kind of oral cavity to prepare the method for silver-containing antibacterial coating with the CoCr alloy material surface, may further comprise the steps:
Step 1: cleaning CoCr alloy material surface obtains the clean surface with well attached performance;
Step 2: preparation 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.
Obtaining the method that contains the nanometer silver antimicrobial film by TiO 2 sol solution comprises: (1), nano-Ag particles is added titanium dioxide (TiO
2) sol solution, stir, to be used; Then utilize the TiO 2 sol solution that contains Nano Silver to apply at the CoCr alloy material, the calcining film forming namely contains the nanometer silver antimicrobial film.Perhaps (2), utilize TiO 2 sol solution to apply at the CoCr alloy material, the calcining film forming is titanium dioxide film (titanium deoxid film).After the carrier surface film forming, utilize the photo-reduction technology until titanium dioxide, prepare the silver-colored particle with good adhesion at titanium deoxid film;
Step 3: the CoCr alloy material with silver-containing antibacterial coating that will obtain cleans, and preserves after vacuum drying is spent the night.The CoCr alloy material with silver-containing antibacterial coating that obtains is anti-biotic material, shows good biocompatibility, and streptococcus mutans, gold-coloured staphylococci are represented good antibiotic and bacteriostasis.
The common used material that described CoCr alloy material uses for hospital clinical before use namely forms according to the routine embedding casting of tooth section, and is surperficial by polishing, cleaning, dry rear stand-by.
Described TiO
2The thin film technology method is sol-gal process, through being hydrolyzed direct formation colloidal sol or through separating the solidifying colloidal sol that forms, then making the solute polymeric gel, utilizes dip-coating method, spraying process etc. to form modified film (TiO at the CoCr material in metal alkoxide or inorganic salts
2Film), organic principle is removed in roasting, obtains at last TiO
2Dense film.
The nano-Ag particles that adds in collosol and gel can be naked particle or the surperficial Nano Silver that contains modified group, and the 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, guarantee the anti-microbial property of film.
Titanium dioxide utilizes the photo-reduction technology at TiO after the carrier surface film forming
2Film (TiO after the calcining
2Dense film) is fixed on and supports silver-colored particle; The photo-reduction technology can be at TiO according to the difference of reaction condition
2The silver-colored particle of preparation nanoscale or micro-meter scale is tightly adhered to TiO on the film
2Matrix surface.
The method utilize titanium dioxide high-biocompatibility and and to the fixation of nano-Ag particles, can effectively avoid Nano Silver to enter human body on the one hand, the nanometer toxicity that release may exist is simultaneously to streptococcus mutans and effectively antibiotic and bactericidal action of gold-coloured staphylococci.
Another object of the present invention is to provide a kind of denture base material of clinical use-CoCr alloy, the surface prepares the method for silver-containing antibacterial material.Sol-gal process particularly in the technical solution of the present invention, through being hydrolyzed direct formation colloidal sol or through separating the solidifying colloidal sol that forms with metal alkoxide or inorganic salts, then make the solute polymeric gel, utilize dip-coating method, spraying process etc. to form modified film, roasting removal organic principle at the CoCr material, obtain at last TiO
2Dense film.But the method has the characteristics such as industrialization, cost be low, and the anti-biotic material of preparation has high-hydrophilic, high-biocompatibility, good stability, and streptococcus mutans, white are read the oral cavity common bacterias such as coccus have good antibacterial action.
With respect to scheme of the prior art, advantage of the present invention is:
The denture base material that the present invention obtains-CoCr alloy material strip silver-containing antibacterial coating is in conjunction with TiO
2With the antibacterial activity of Ag, show again strong wetability, existing good biocompatibility, the mechanical property of maintenance artificial tooth material.Confirm that through test this CoCr alloy material with the silver-containing antibacterial coating is anti-biotic material, and streptococcus mutans, gold-coloured staphylococci are represented good antibiotic and bacteriostasis.
The anti-biotic material of the inventive method preparation when introducing 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, and is simple, not high to equipment requirement, can realize suitability for industrialized production, can be used for the antibacterial surface thin film technology of various metal medical materials or medicine equipment.
In sum, the invention discloses a kind of denture base material of clinical use-CoCr alloy surface and prepare the method for silver-containing antibacterial material.Step 1: cleaning CoCr alloy material surface obtains the clean surface with well attached performance; Step 2: preparation TiO 2 sol solution.Obtaining the method that contains the nanometer silver antimicrobial film comprises: (1) adds TiO 2 sol solution with nano-Ag particles, stirs, and is to be used; Perhaps (2) after the carrier surface film forming, utilize the photo-reduction technology until titanium dioxide, the silver-colored particle that preparation has good adhesion; Step 3: utilize TiO 2 sol solution to apply at the CoCr material, the calcining film forming.The silver-containing antibacterial coating CoCr material that obtains is cleaned, preserves after vacuum drying is spent the night.But the method has the characteristics such as industrialization, cost be low, the anti-biotic material high-biocompatibility of preparation, good stability, and streptococcus mutans, white are read the oral cavity common bacterias such as coccus have 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 explanation the present invention.The implementation condition that adopts among the embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in the normal experiment.
Embodiment 1
Get the CoCr alloy material surface, surface finish cleaning, dried for standby after the 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.The ageing of colloidal sol room temperature is 7 days after the configuration.At TiO
2Mol ratio according to Ag and Ti in the colloidal sol is the nano-Ag particles of the mol ratio adding 50nm of 1000:2, stirs.
Adopt dip-coating method, the preparation film.The film of preparation is put into Muffle furnace and is warming up to 500 ℃ with the speed of 3 ℃/min, behind the insulation 90min with the stove cooling, system contain Ag and TiO
2The CoCr alloy material of sol pellicle.
What prepare contains Ag and TiO
2The antibacterial film of the CoCr alloy material of sol pellicle (silver-containing antibacterial coating) surface smoothing, antibacterial experiment studies show that to have good antibacterial activity.
Embodiment 2
Get the CoCr alloy material surface, surface finish cleaning, dried for standby after the 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.The ageing of colloidal sol room temperature is 2 days after the configuration.At TiO
2Be that the mol ratio of 1000:5 adds the nano-Ag particles that particle diameter is about 80nm according to the mol ratio of Ag and Ti in the colloidal sol, stir.
Adopt dip-coating method, the preparation film.The film of preparation is put into Muffle furnace and is warming up to 500 ℃ with the speed of 3 ℃/min, with the stove cooling, prepares and contains Ag and TiO behind the insulation 90min
2The CoCr alloy material of sol pellicle.
What prepare contains Ag and TiO
2The antibacterial film of the CoCr alloy material of sol pellicle (silver-containing antibacterial coating) surface smoothing, antibacterial experiment studies show that to have good antibacterial activity.
Embodiment 3
Get the CoCr alloy material surface, surface finish cleaning, dried for standby after the 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.The ageing of colloidal sol room temperature is 5 days after the 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, with the stove cooling, obtains containing TiO behind the insulation 90min
2The CoCr alloy material of film.
With 1.275g AgNO
3Be dissolved in the water of 150ml, add the 8g absolute ethyl alcohol, be mixed with the AgNO of 0.1mol/L
3Solution is put into the middle reaction of photochemical reaction instrument (uviol lamp 300W is apart from 8cm) with obtain solution and silver was supported on TiO in 4 hours
2On the film, cleaning-drying obtains to contain Ag and TiO
2The CoCr alloy material of sol pellicle.。
The CoCr film surface for preparing is level and smooth, and antibacterial experiment studies show that to have good antibacterial activity.
Embodiment 4
Get the CoCr alloy material surface, surface finish cleaning, dried for standby after the 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.The ageing of colloidal sol room temperature is 5 days after the 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, with the stove cooling, obtains containing TiO behind the insulation 90min
2The CoCr alloy material of film.
With 0.63g AgNO
3Be dissolved in the water of 150ml, add the 4g anhydrous isopropyl alcohol, preparation is into about the AgNO of 0.05mol/L
3Solution is put into the middle reaction of photochemical reaction instrument (uviol lamp 500W is apart from 8cm) with obtain solution and silver was supported on TiO in 2 hours
2On the film, cleaning-drying obtains to contain Ag and TiO
2The CoCr alloy material (anti-biotic material) of sol pellicle.
What prepare contains Ag and TiO
2Antibacterial film (antimicrobial coating) surface smoothing of the CoCr alloy material of sol pellicle, antibacterial experiment studies show that to have good antibacterial activity.
Above-mentioned example only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the people who is familiar with technique can understand content of the present invention and according to this enforcement, can not limit protection scope of the present invention with this.All equivalent transformations that Spirit Essence is done according to the present invention or modification all should be encompassed within protection scope of the present invention.
Claims (8)
1. an oral cavity prepares the method for silver-containing antibacterial coating with the CoCr alloy material surface, it is characterized in that said method comprising the steps of:
(1) cleaning CoCr alloy material surface;
(2) pass through step I) or step I i) prepare the silver-containing antibacterial coating at the CoCr alloy material surface:
I) nano-Ag particles is added titanium dioxide (TiO
2) sol solution, stir, for subsequent use; The TiO 2 sol solution that will contain Nano Silver is coated in the CoCr alloy material surface after step (1) is processed, and then the CoCr alloy material calcining after applying is formed the silver-containing antibacterial coating;
Ii) TiO 2 sol solution is coated in the CoCr alloy material surface after step (1) is processed, then the CoCr alloy material calcining after applying is formed titanium dioxide film; Then the solution that makes silver ion by the photo-reduction method on titanium dioxide film secure attachment silver particle as the silver-containing antibacterial coating;
(3) the CoCr alloy material with the silver-containing antibacterial coating that obtains cleans, and preserves after dry.
2. method according to claim 1 is characterized in that the CoCr alloy material is to cast according to the conventional embedding of tooth section in advance before in step (1) to form in the described method, and the CoCr alloy material surface is by polishing, cleaning, dry rear stand-by.
3. method according to claim 1 is characterized in that titanium dioxide (TiO in the described method step (2)
2) sol solution with directly form after the titanium salt hydrolysis or the titanium salt solution is solidifying after formation.
4. method according to claim 3 is characterized in that titanium salt is selected from titanium tetrachloride (TiCl described in the described method
4), butyl titanate (Ti (OCH
2CH
2CH
2CH
3)
4), isopropyl titanate (Ti(OCH (CH
3)
2)
4).
5. method according to claim 1 is characterized in that nano-Ag particles is selected from the naked particle of Nano Silver or the surperficial nano-Ag particles that contains modified group in the described method step (2).
6. method according to claim 5 is characterized in that in the described method that nano-Ag particles directly adds with the solid particle existence form or is stored in to form the form of mixing nano-Ag particles organic solution in the organic solution and add.
7. method according to claim 5, the grain diameter that it is characterized in that nano-Ag particles in the described method is 10 ~ 100 nanometers.
8. method according to claim 5 is characterized in that the solution of the silver ion that uses in the described photo-reduction method is AgNO
3Solution.
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Cited By (1)
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| CN108064881A (en) * | 2016-11-14 | 2018-05-25 | 佛山市顺德区美的电热电器制造有限公司 | A kind of argentiferous titanium dioxide composite antibacterial agent and preparation method thereof and antibiotic paint and preparation method thereof |
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| CN108064881B (en) * | 2016-11-14 | 2024-02-13 | 佛山市顺德区美的电热电器制造有限公司 | Silver-containing titanium dioxide composite antibacterial agent and preparation method thereof, and antibacterial coating and preparation method thereof |
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|---|---|
| CN103041976B (en) | 2014-04-30 |
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