CN102719824A - Dopamine-nanosilver composite coating and preparation method thereof - Google Patents
Dopamine-nanosilver composite coating and preparation method thereof Download PDFInfo
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- CN102719824A CN102719824A CN2012101921743A CN201210192174A CN102719824A CN 102719824 A CN102719824 A CN 102719824A CN 2012101921743 A CN2012101921743 A CN 2012101921743A CN 201210192174 A CN201210192174 A CN 201210192174A CN 102719824 A CN102719824 A CN 102719824A
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Abstract
The invention discloses a dopamine-nanosilver composite coating and a preparation method thereof. Firstly, pure titanium or a titanium alloy with titanium dioxide nanotube arrays grown on the surface of the titanium alloy is put in a dopamine buffer solution, then the pure titanium loaded with the dopamine or the titanium alloy with the titanium dioxide nanotube arrays grown on the surface of the titanium alloy is put in a silver nitrate solution, and nanosilver particles are obtained by photoreduction. According to the dopamine-nanosilver composite coating and the preparation method thereof, the chelating property of the dopamine and metal ions and the reducibility in an auto polymerization process are utilized, and the antibacterial performance of material is improved by preparing the nanosilver coating on the surface of the titanium alloy, which has important application value and guiding significance for developing novel functional metal implant material.
Description
Technical field
The present invention relates to the metal surface properties modification field, more particularly, relate to the compound and preparation method thereof of metal titanium (Ti) and titanium alloy surface and argent.
Background technology
As everyone knows, silver (Ag) extensively is used on the anti-biotic material since ancient times, and nanometer silver has excellent anti-microbial property, and the nano silver particles specific surface area is big, its anti-microbial effect and silver ions (Ag
+) relevant.Titanium (Ti) and titanium alloy are with its excellent physics, chemical property and excellent biological compatibility; Become present most widely used tissue repair and equivalent material; But because therefore itself biologically active not need carry out surface treatment to it, as at alloy surface growth titanium oxide (TiO
2) nano-tube film improves its biological activity.Simultaneously, in implant surgery, infectation of bacteria also is another major reason that causes embedded material to lose efficacy.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art; Proposition utilizes the chelating properties of Dopamine HCL and metals ion and the reductibility in the auto-polymerization process; Prepare the anti-microbial property that the nanometer silver coating improves material at titanium alloy surface, this has important use for the functional metal implant material of development of new and is worth and directive significance.
The object of the invention is achieved through following technical proposals:
Dopamine HCL-nanometer silver compound coating and preparation method thereof, carry out according to following step:
At first, i.e. step 1 is put into buffered soln (the being Tris solution) dipping of Dopamine HCL with the titanium alloy of pure titanium of metal base material or surface growth Nano tube array of titanium dioxide, to obtain load the metal base material of Dopamine HCL is arranged
The concentration of wherein said Dopamine HCL is 0.1-0.3mg/ml;
Said metal base material is the titanium alloy of pure titanium, titanium alloy, surface growth Nano tube array of titanium dioxide or the pure titanium of surface growth Nano tube array of titanium dioxide; Wherein the preparation of the selection of titanium alloy and surface growth titania nanotube can be implemented according to the record that utilizes the prior art method of doping nano-Ag particles " a kind of in titania nanotube " (application number is 201010278615.2, the applying date be that on September 11st, 2010, open day are on December 22nd, 2010); (atomic molar of Ti and Zr is than being (7-9): (3-1) to select the Ti-Zr alloy; The atomic molar ratio of preferred Ti and Zr is 7: 3,8: 2 or 9: 1), (atomic molar of Ti, Zr and Nb is than being (73-74): (2-4): (22-25) for the Ti-Zr-Nb alloy; The atomic molar ratio of preferred Ti, Zr and Nb is 74: 4: 22 or 73: 2: 25) or the Ti-Zr-Nb-Sn alloy (the atomic molar ratio of Ti, Zr, Nb and Sn is 72: 4: 22: 2), utilize anonizing to prepare the surface titanium dioxide nanotube;
Said dipping temperature is 20-25 ℃;
Said time of immersion is 20-24 hour;
The pH of said buffered soln is 8-8.5;
Then, promptly step 2 has the metal base material of Dopamine HCL to place silver nitrate solution to flood load, and photoreduction obtains nano-Ag particles simultaneously, wherein:
Said silver nitrate solution is the aqueous solution of Silver Nitrate, and concentration is 0.01-0.05mol/L
Said dipping temperature is 20-25 ℃;
Said time of immersion is 10-15min;
The processing parameter of said illumination is that light source employing xenon source, light intensity are 150mw/cm
2
Technical scheme of the present invention is a matrix with the titanium alloy, utilizes the chelating of Dopamine HCL and the method that reduction characteristic prepares the nanometer silver antimicrobial coating, and purpose is that nano-Ag particles is evenly distributed on titanium alloy surface, and with Dopamine HCL form compound, shown in accompanying drawing 2.Through the energy spectrum analysis and the Raman spectrum analysis (accompanying drawing 3 and 4) of surperficial composition, the final nanometer silver that forms in the surface of metal base.The antimicrobial coating and the titanium alloy substrate caking power that are obtained by above method are strong, and the nano-Ag particles controlled amount, are evenly distributed.Low, easy and simple to handle, the consuming time weak point of implementation cost of the present invention can be widely used in the preparation of the antibacterial surface coating of metal medical appliance.
Description of drawings
The synoptic diagram of Fig. 1 technical scheme of the present invention
Fig. 2 ESEM characterizes the pattern photo before and after the loading nano silvery, the wherein pattern behind (a) load Dopamine HCL; (b) pattern behind the direct depositing nano silver; The pattern of the nano-Ag particles that (c) generates through Dopamine HCL reduction
The EDAX results synoptic diagram of Fig. 3 surface composition
Fig. 4 is through the Raman spectrum of the nanometer silver coating of Dopamine HCL reduction generation
Embodiment
Further specify technical scheme of the present invention below in conjunction with specific embodiment.Wherein silver nitrate solution is selected its aqueous solution; Temperature is chosen as under 25 degrees centigrade floods; It is 150mw/cm that said light source adopts xenon source, light intensity
2The pH value of said Tris solution is 8.5.ESEM is S4800; Hitachi, Japan.Raman spectrum is selected the inVia reflex of Britain Reinshaw company, RENISHAW laser Raman spectrometer for use; Power spectrum is selected the Apollo XV type power spectrum probe of U.S. EDAX company for use.
Embodiment 1
With pure titanium is matrix, and preparation nanometer silver antimicrobial coating utilizes the chelating of Dopamine HCL and reduction characteristic to prepare nano-Ag particles.Said is matrix with pure titanium, is the pure titanium plate that is of a size of 10*10*6mm, and the Ti sheet is cleaned up with deionized water, and ultrasonic 5 minutes after drying of absolute ethyl alcohol are subsequent use.
Said nano-Ag particles is to utilize the Dopamine HCL reduction method to prepare, and the Ti sheet is placed Dopamine HCL Tris solution reaction 24 hours, is placed on Silver Nitrate (AgNO again
3) make through illumination reaction in the solution, sample is taken out, use the absolute ethyl alcohol ultrasonic cleaning, promptly obtain equally distributed nano-Ag particles on the Ti surface.
The processing parameter of preparation nanometer silver is:
Tris concentration: 0.3mg/ml
Dopamine concentration: 0.1mg/ml
Silver nitrate solution concentration: 0.01mol/L
Light application time: 10min
Embodiment 2
With pure titanium is matrix, and preparation nanometer silver antimicrobial coating utilizes the chelating of Dopamine HCL and reduction characteristic to prepare nano-Ag particles.Said is matrix with pure titanium, is the pure titanium plate that is of a size of 10*10*6mm, and the Ti sheet is cleaned up with deionized water, and ultrasonic 5 minutes after drying of absolute ethyl alcohol are subsequent use.
Said nano-Ag particles is to utilize the Dopamine HCL reduction method to prepare, and the Ti sheet is placed Dopamine HCL Tris solution reaction 24 hours, is placed on Silver Nitrate (AgNO again
3) make through illumination reaction in the solution, sample is taken out, use the absolute ethyl alcohol ultrasonic cleaning, promptly obtain equally distributed nano-Ag particles on the Ti surface.
The processing parameter of preparation nanometer silver is:
Tris concentration: 0.3mg/ml
Dopamine concentration: 0.2mg/ml
Silver nitrate solution concentration: 0.01mol/L
Light application time: 10min
Embodiment 3
With pure titanium is matrix, and preparation nanometer silver antimicrobial coating utilizes the chelating of Dopamine HCL and reduction characteristic to prepare nano-Ag particles.Said is matrix with pure titanium, is the pure titanium plate that is of a size of 10*10*6mm, and the Ti sheet is cleaned up with deionized water, and ultrasonic 5 minutes after drying of absolute ethyl alcohol are subsequent use.
Said nano-Ag particles is to utilize the Dopamine HCL reduction method to prepare, and the Ti sheet is placed Dopamine HCL Tris solution reaction 24 hours, is placed on Silver Nitrate (AgNO again
3) make through illumination reaction in the solution, sample is taken out, use the absolute ethyl alcohol ultrasonic cleaning, promptly obtain equally distributed nano-Ag particles on the Ti surface.
The processing parameter of preparation nanometer silver is:
Tris concentration: 0.3mg/ml
Dopamine concentration: 0.3mg/ml
Silver nitrate solution concentration: 0.01mol/L
Light application time: 10min
Embodiment 4
Titanium alloy or metal titanium with the surface growth Nano tube array of titanium dioxide are matrix, and preparation nanometer silver antimicrobial coating utilizes the chelating of Dopamine HCL and reduction characteristic to prepare nano-Ag particles.
The titanium alloy of said surface growth Nano tube array of titanium dioxide is that the record that utilizes the prior art method of doping nano-Ag particles " a kind of in titania nanotube " (application number is 201010278615.2, the applying date be that on September 11st, 2010, open day are on December 22nd, 2010) prepares; Utilize anonizing; With Ti-Zr alloy (the atomic molar ratio of Ti and Zr is 7: 3) is substrate; Use 800,1000 and 2000 order sand paperings to smooth respectively on the surface; The back cleans up with deionized water, and ultrasonic 5 minutes after drying of absolute ethyl alcohol are subsequent use.Adopt two electrode systems at NH
4React in the F-glycerin/water mixing solutions and make.Sample is taken out, for use with absolute ethyl alcohol ultrasonic cleaning after drying.
The processing parameter that adopts during anodic oxidation constitutes is:
Anodic oxidation voltage: 30V
Anodizing time: 3h
Concentration of electrolyte: glycerine: the volume ratio of water is 1: 1, adds 0.3MNH
4F
Said nano-Ag particles is to utilize the Dopamine HCL reduction method to prepare, and the titanium alloy of surface growth Nano tube array of titanium dioxide is placed Dopamine HCL Tris solution reaction 24 hours, is placed on Silver Nitrate (AgNO again
3) make through illumination reaction in the solution, sample is taken out, use the absolute ethyl alcohol ultrasonic cleaning, promptly at TiO
2Nanotube surface obtains equally distributed nano-Ag particles.
The processing parameter of preparation nanometer silver is:
Tris concentration: 0.3mg/ml
Dopamine concentration: 0.1mg/ml
Silver nitrate solution concentration: 0.01mol/L
Light application time: 10min
Embodiment 5
Titanium alloy or metal titanium with the surface growth Nano tube array of titanium dioxide are matrix, and preparation nanometer silver antimicrobial coating utilizes the chelating of Dopamine HCL and reduction characteristic to prepare nano-Ag particles.
The titanium alloy of said surface growth Nano tube array of titanium dioxide is that the record that utilizes the prior art method of doping nano-Ag particles " a kind of in titania nanotube " (application number is 201010278615.2, the applying date be that on September 11st, 2010, open day are on December 22nd, 2010) prepares; Utilize anonizing; With Ti-Zr alloy (the atomic molar ratio of Ti and Zr is 7: 3) is substrate; Use 800,1000 and 2000 order sand paperings to smooth respectively on the surface; The back cleans up with deionized water, and ultrasonic 5 minutes after drying of absolute ethyl alcohol are subsequent use.Adopt two electrode systems at NH
4React in the F-glycerin/water mixing solutions and make.Sample is taken out, for use with absolute ethyl alcohol ultrasonic cleaning after drying.Adopt two electrode systems at NH
4React in the F-glycerin/water mixing solutions and make.
The processing parameter that adopts during anodic oxidation constitutes is:
Anodic oxidation voltage: 30V
Anodizing time: 3h
Concentration of electrolyte: glycerine: the volume ratio of water is 1: 1, adds 0.3MNH
4F
Said nano-Ag particles is to utilize the Dopamine HCL reduction method to prepare, and the titanium alloy of surface growth Nano tube array of titanium dioxide is placed Dopamine HCL Tris solution reaction 24 hours, is placed on Silver Nitrate (AgNO again
3) make through illumination reaction in the solution, sample is taken out, use the absolute ethyl alcohol ultrasonic cleaning, promptly at TiO
2Nanotube surface obtains equally distributed nano-Ag particles.The processing parameter of preparation nanometer silver is:
Tris concentration: 0.3mg/ml
Dopamine concentration: 0.2mg/ml
Silver nitrate solution concentration: 0.01mol/L
Light application time: 10min
Embodiment 6
Titanium alloy or metal titanium with the surface growth Nano tube array of titanium dioxide are matrix, and preparation nanometer silver antimicrobial coating utilizes the chelating of Dopamine HCL and reduction characteristic to prepare nano-Ag particles.
The titanium alloy of said surface growth Nano tube array of titanium dioxide is that the record that utilizes the prior art method of doping nano-Ag particles " a kind of in titania nanotube " (application number is 201010278615.2, the applying date be that on September 11st, 2010, open day are on December 22nd, 2010) prepares; Utilize anonizing; With Ti-Zr alloy (the atomic molar ratio of Ti and Zr is 7: 3) is substrate; Use 800,1000 and 2000 order sand paperings to smooth respectively on the surface; The back cleans up with deionized water, and ultrasonic 5 minutes after drying of absolute ethyl alcohol are subsequent use.Adopt two electrode systems at NH
4React in the F-glycerin/water mixing solutions and make.Sample is taken out, for use with absolute ethyl alcohol ultrasonic cleaning after drying.Adopt two electrode systems at NH
4React in the F-glycerin/water mixing solutions and make.
The processing parameter that adopts during anodic oxidation constitutes is:
Anodic oxidation voltage: 30V
Anodizing time: 3h
Concentration of electrolyte: glycerine: the volume ratio of water is 1: 1, adds 0.3MNH
4F
Said nano-Ag particles is to utilize the Dopamine HCL reduction method to prepare, and the titanium alloy of surface growth Nano tube array of titanium dioxide is placed Dopamine HCL Tris solution reaction 24 hours, is placed on Silver Nitrate (AgNO again
3) make through illumination reaction in the solution, sample is taken out, use the absolute ethyl alcohol ultrasonic cleaning, promptly at TiO
2Nanotube surface obtains equally distributed nano-Ag particles.The processing parameter of preparation nanometer silver is:
Tris concentration: 0.3mg/ml
Dopamine concentration: 0.3mg/ml
Silver nitrate solution concentration: 0.01mol/L
Light application time: 10min
More than the present invention has been done exemplary description; Should be noted that; Under the situation that does not break away from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (10)
1. Dopamine HCL-nanometer silver compound coating is characterized in that, carries out according to following step:
At first, i.e. step 1, the buffered soln of the titanium alloy of pure titanium of metal base material or surface growth Nano tube array of titanium dioxide being put into Dopamine HCL floods, and to obtain load the metal base material of Dopamine HCL is arranged;
Then, promptly step 2 has the metal base material of Dopamine HCL to place silver nitrate solution to flood load, and photoreduction obtains nano-Ag particles simultaneously.
2. Dopamine HCL according to claim 1-nanometer silver compound coating is characterized in that, in the said step 1, the concentration of said Dopamine HCL is 0.1-0.3mg/ml; The pH of said buffered soln is 8-8.5.
3. Dopamine HCL according to claim 1-nanometer silver compound coating is characterized in that, in the said step 1, said dipping temperature is 20-25 ℃; Said time of immersion is 20-24 hours.
4. Dopamine HCL according to claim 1-nanometer silver compound coating; It is characterized in that; In the said step 1, said metal base material is the titanium alloy of pure titanium, titanium alloy, surface growth Nano tube array of titanium dioxide or the pure titanium of surface growth Nano tube array of titanium dioxide.
5. Dopamine HCL according to claim 1-nanometer silver compound coating is characterized in that, in the said step 2, said silver nitrate solution is the aqueous solution of Silver Nitrate, and concentration is 0.01-0.05mol/L; Said dipping temperature is 20-25 ℃; Said time of immersion is 10-15min; The processing parameter of said illumination is that light source employing xenon source, light intensity are 150mw/cm
2
6. the preparation method of Dopamine HCL-nanometer silver compound coating is characterized in that, carries out according to following step:
At first, i.e. step 1, the buffered soln of the titanium alloy of pure titanium of metal base material or surface growth Nano tube array of titanium dioxide being put into Dopamine HCL floods, and to obtain load the metal base material of Dopamine HCL is arranged;
Then, promptly step 2 has the metal base material of Dopamine HCL to place silver nitrate solution to flood load, and photoreduction obtains nano-Ag particles simultaneously.
7. the preparation method of Dopamine HCL according to claim 6-nanometer silver compound coating is characterized in that, in the said step 1, the concentration of said Dopamine HCL is 0.1-0.3mg/ml; The pH of said buffered soln is 8-8.5.
8. the preparation method of Dopamine HCL according to claim 6-nanometer silver compound coating is characterized in that, in the said step 1, said dipping temperature is 20-25 ℃; Said time of immersion is 20-24 hours.
9. the preparation method of Dopamine HCL according to claim 6-nanometer silver compound coating; It is characterized in that; In the said step 1, said metal base material is the titanium alloy of pure titanium, titanium alloy, surface growth Nano tube array of titanium dioxide or the pure titanium of surface growth Nano tube array of titanium dioxide.
10. the preparation method of Dopamine HCL according to claim 6-nanometer silver compound coating is characterized in that, in the said step 2, said silver nitrate solution is the aqueous solution of Silver Nitrate, and concentration is 0.01-0.05mol/L; Said dipping temperature is 20-25 ℃; Said time of immersion is 10-15min; The processing parameter of said illumination is that light source employing xenon source, light intensity are 150mw/cm
2
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