CN101705468A - Method for preparing slow-release type skeleton-type TiN/Cu-Zu metal layer antibacterial film - Google Patents
Method for preparing slow-release type skeleton-type TiN/Cu-Zu metal layer antibacterial film Download PDFInfo
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- CN101705468A CN101705468A CN200910308258A CN200910308258A CN101705468A CN 101705468 A CN101705468 A CN 101705468A CN 200910308258 A CN200910308258 A CN 200910308258A CN 200910308258 A CN200910308258 A CN 200910308258A CN 101705468 A CN101705468 A CN 101705468A
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Abstract
The invention discloses a method for preparing a slow-release type skeleton-type TiN/Cu-Zu metal layer antibacterial film and relates to a preparation method of an antibacterial film, which solves the problem that an antibacterial film prepared by the conventional method has poor durability of antibacterial effect. The method has the following steps of: 1. putting a matrix on a target platform of a vacuum room; and then heating to 200 DEG C and sputter cleaning for 20 min; 2. rotating the target platform of the vacuum room under the condition that argon flow is 6sccm, nitrogen flow is 2sccm, deposition pressure is 0.56Pa, and the deposition bias of the matrix is compound bias; and alternately depositing TiN layers and metal layers on the surface of the matrix till the total thickness of film layers is 0.1 micrometer-10 micrometers to obtain the slow-release type skeleton-type TiN/Cu-Zu metal layer antibacterial film. After the slow-release type skeleton-type TiN/Cu-Zu metal layer antibacterial film is soaked for three months, the ion dissolving speed is not reduced, and the antibiosis rate against colibacillus can still reach above 97%.
Description
Technical field
The present invention relates to a kind of preparation method of antibacterial film.
Background technology
Human beings'health in the propagation of unwanted bacteria and infection serious threat, the propagation of SARS virus, bird flu etc. especially in recent years and infection, anti-biotic material application is in daily life developed rapidly, publication number is the patent of CN99800249.6 and patent that publication number the is CN101125458A whole Ag of interpolation in stainless steel or plastics, improved the antibacterial effect of material, but Ag etc. has been doped to difficulty and the production cost that has increased the preparation material in the integral material.Publication number be CN1793428A patent disclosure a kind of method of utilizing the high temperature aura to infiltrate Ag or Cu, its technology is that Heating temperature is 800 ℃～1050 ℃, the infiltration time is 2～4 hours, carry out timeliness thermal treatment after the infiltration again, but this method exists antibiotic layer thickness thinner, weares and teares easily and causes the problem of antibacterial effect persistence difference.
Summary of the invention
Technical problem to be solved by this invention is the problem for the antibacterial film antibacterial effect persistence difference that solves existing method preparation, and the preparation method of a kind of slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film is provided.
The preparation method of slow-release type skeleton-type TiN of the present invention/Cu-Zn metal level antibacterial film is as follows: one, matrix being put on the vacuum chamber target platform, is 2 * 10 at vacuum degree in vacuum chamber
-3Under the condition of Pa matrix being heated to 200 ℃, is that 10sccm～20sccm, radio frequency power are that 300W, matrix negative bias are that 800V, pulse-repetition are that 10kHz, pulse width are under the condition of 30 μ s matrix surface to be carried out sputter clean 20min at argon flow amount then; Two, be that 6sccm, nitrogen flow are that 2sccm, deposition pressure are the target platform that 0.56Pa, matrix deposit rotation vacuum chamber under the condition that bias voltage is compound bias voltage at argon flow amount, at matrix surface alternating deposit TiN layer and Cu-Zn metal level, to the rete total thickness be 0.1 μ m～10 μ m, wherein the first layer and outermost layer are the TiN layer in the rete, each amount average out to 1.0 * 10 at matrix surface depositing TiN layer
16～2.0 * 10
17Individual molecule/cm
2, each amount average out to 1.0 * 10 at the matrix surface depositing metal layers
16～1.3 * 10
17Individual atom/cm
2, the atomic percent of Zn is 0%～10% in the metal level, the atomic percent of Cu is 90%～100%, obtains slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film; Wherein volts DS is that 80V, coupling pulsed voltage are that 200V, pulse-repetition are that 10kHz, pulse width are 30 μ s in the described compound bias voltage of step 2; The Ti target adopts the magnetically controlled DC sputtering power supply in the step 2, and sputtering current is 0.6A, and the Cu-Zn target adopts the magnetron sputtering radio-frequency power supply, and radio frequency power is 300W.
The described matrix of step 1 of the present invention is metal, pottery or plastics; Described metal is stainless steel, aluminium alloy, titanium alloy, copper alloy or soft steel; Described pottery is aluminum oxide, zirconium white or silicon carbide; Described plastics are polyethylene terephthalate, polycarbonate or acrylonitrile-butadiene-styrene copolymer; The mass content of Ti is 99.99% in the target of Ti described in the step 2; The mass content of Cu is 62% in the Cu-Zn target described in the step 2, and the mass content of Zn is 38%, and described Cu is a H62 brass.
It is skeleton that the present invention utilizes copper to be easy to obtain with TiN from the effect of reuniting, copper zinc is the skeleton membrane structure of interior filling, the discontinuous Cu-Zn coacervate that is contained in the slow-release type skeleton-type TiN of gained/Cu-Zn metal level antibacterial film can stop the generation of continuous large-area corrosion dissolution, prevent the quick stripping of a large amount of antibacterial metal ions and run off too fastly that the ion result of extraction is lasting; TiN can play the effect on blocking layer in addition, can the stripping of slowly-releasing ion, the Cu ion of gained slow-release type skeleton-type TiN of the present invention/Cu-Zn metal level antibacterial film and Zn ion dissolution rate are stable, soaking back ion dissolution rate through three months does not descend, and through trimestral immersion slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film still can reach more than 97% to colibacillary antibiotic rate, slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film can the stripping of slowly-releasing ion, has long lasting germ resistance.
Description of drawings
Fig. 1 is the TEM photo of embodiment one gained slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film; Fig. 2 is that slow-release type skeleton-type TiN in the embodiment 13/Cu-Zn metal level antibacterial film is immersed in different time Cu ion and Zn ion dissolution rate graphic representation in 37 ℃ the water,-▲-represents Zn ion dissolution rate curve ,-■-represent Cu ion dissolution rate curve; Fig. 3 soaks different time slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film to colibacillary antibiotic rate graphic representation through 37 ℃ in the embodiment 14.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of slow-release type skeleton-type TiN in the present embodiment/Cu-Zn metal level antibacterial film is as follows: one, matrix being put on the vacuum chamber target platform, is 2 * 10 at vacuum degree in vacuum chamber
-3Under the condition of Pa matrix being heated to 200 ℃, is that 10sccm～20sccm, radio frequency power are that 300W, matrix negative bias are that 800V, pulse-repetition are that 10kHz, pulse width are under the condition of 30 μ s matrix surface to be carried out sputter clean 20min at argon flow amount then; Two, be that 6sccm, nitrogen flow are that 2sccm, deposition pressure are the target platform that 0.56Pa, matrix deposit rotation vacuum chamber under the condition that bias voltage is compound bias voltage at argon flow amount, at matrix surface alternating deposit TiN layer and Cu-Zn metal level, to the rete total thickness be 0.1 μ m～10 μ m, wherein the first layer and outermost layer are the TiN layer in the rete, each amount average out to 1.0 * 10 at matrix surface depositing TiN layer
16～2.0 * 10
17Individual molecule/cm
2, each amount average out to 1.0 * 10 at the matrix surface depositing metal layers
16～1.3 * 10
17Individual atom/cm
2, the atomic percent of Zn is 0%～10% in the metal level, the atomic percent of Cu is 90%～100%, obtains slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film; Wherein volts DS is that 80V, coupling pulsed voltage are that 200V, pulse-repetition are that 10kHz, pulse width are 30 μ s in the described compound bias voltage of step 2; The Ti target adopts the magnetically controlled DC sputtering power supply in the step 2, and sputtering current is 0.6A, and the Cu-Zn target adopts the magnetron sputtering radio-frequency power supply, and radio frequency power is 300W.
Matrix described in the present embodiment step 1 is put into after the oven dry on the vacuum chamber target platform through polishing, acetone ultrasonic cleaning 15min, dehydrated alcohol ultrasonic cleaning 15min.
By Fig. 1 (the TEM photo of present embodiment gained slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film) as can be seen the Cu-Zn coacervate filled up in the TiN skeleton.
Embodiment two: what present embodiment and embodiment one were different is that the described matrix of step 1 is metal, pottery or plastics.Other is identical with embodiment one.
Embodiment three: what present embodiment was different with embodiment one or two is that described metal is stainless steel, aluminium alloy, titanium alloy, copper alloy or soft steel.Other is identical with embodiment one or two.
Embodiment four: what present embodiment and embodiment one to three were different is that described pottery is aluminum oxide, zirconium white or silicon carbide.Other is identical with embodiment one to three.
Embodiment five: what present embodiment and embodiment one to four were different is that described plastics are polyethylene terephthalate, polycarbonate or acrylonitrile-butadiene-styrene copolymer. other is identical with embodiment one to four
Embodiment six: present embodiment and embodiment one to five are different is that the mass content of Ti in the target of Ti described in the step 2 is 99.99%.Other is identical with embodiment one to five.
Embodiment seven: present embodiment and embodiment one to six are different is that the mass content of Cu in the Cu-Zn target described in the step 2 is 62%, and the mass content of Zn is 38%, and described Cu is a H62 brass.Other is identical with embodiment one to six.
Embodiment eight: what present embodiment and embodiment one to seven were different is that the rete total thickness is 1.59 μ m in the step 2.Other is identical with embodiment one to seven.
Embodiment nine: present embodiment and embodiment one to eight are different is at every turn at the amount average out to 1.7 * 10 of matrix surface depositing TiN layer in the step 2
16Individual molecule/cm
2Other is identical with embodiment one to eight.
Embodiment ten: present embodiment and embodiment one to nine are different is at every turn at the amount average out to 3.3 * 10 of matrix surface depositing metal layers in the step 2
16Individual atom/cm
2Other is identical with embodiment one to nine.
Embodiment 11: what present embodiment and embodiment one to ten were different is that argon flow amount is 12sccm～18sccm in the step 1.Other is identical with embodiment one to ten.
Embodiment 12: what present embodiment and embodiment one to 11 were different is that argon flow amount is 15sccm in the step 1.Other is identical with embodiment one to 11.
Embodiment 13: the slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film with embodiment one gained in the present embodiment carries out the experiment of ion stripping quantity, and experimental technique is as follows:
Slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film is cut into 1.5 * 1.5cm size, is immersed in respectively in the 15ml deionized water, wherein soaking temperature is 37 ℃, and soak time was respectively 15 days, 30 days, 60 days, 90 days.Soak the back and take out sample, Cu ion in the solution, Zn ionic weight are tested, test result such as Fig. 2, find out that by Fig. 2 (slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film is immersed in different time Cu ion and Zn ion dissolution rate graphic representation in 37 ℃ the water) Cu ion and Zn ion dissolution rate are stable, soaked back ion dissolution rate through three months and do not descend.
Embodiment 14: slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film that present embodiment will be soaked through embodiment 13 adopts method with plastic film to carry out the anti-microbial property test with reference to Japanese JISZ 280-2000 " antibiotic fabricated product germ resistance test method and antibacterial effect " standard.Test strain is intestinal bacteria ATCC 25922.Concrete steps are as follows:
(1) intestinal bacteria ATCC 25922 was cultivated 24 hours under 37 ℃ condition, doubling dilution to activity is 10 in sterile test tube then
5CFU/ml.
(2) get the bacterium liquid for preparing according to 0.02mL/cm
2Inoculum size drip through the autoclaved slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film surface and stainless steel sample surfaces that is untreated, and with the covering of aseptic polyethylene film, constant temperature culture 24h under 37 ℃ condition again.
(3) add the abundant wash-out of elutriant, get elutriant and be inoculated in the substratum constant temperature and cultivated 24 hours for 37 ℃.
(4) calculate viable count.The sterilizing rate calculation formula is as follows:
R is an antibiotic rate, and B is the stainless steel sample viable count that is untreated, and C is the viable count of slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film.
Pass through as can be known by Fig. 3 (soaking different time slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial films to colibacillary antibiotic rate graphic representation) that trimestral immersion slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film still can reach more than 97% to colibacillary antibiotic rate through 37 ℃, as seen slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film can the stripping of slowly-releasing ion, has long lasting germ resistance.
Claims (10)
1. the preparation method of slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film, the preparation method who it is characterized in that slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film is as follows: one, matrix is put on the vacuum chamber target platform, being under the condition of 2 * 10-3Pa matrix to be heated to 200 ℃ at vacuum degree in vacuum chamber, is that 10sccm～20sccm, radio frequency power are that 300W, matrix negative bias are that 800V, pulse-repetition are that 10kHz, pulse width are under the condition of 30 μ s matrix surface to be carried out sputter clean 20min at argon flow amount then; Two, at argon flow amount is 6sccm, nitrogen flow is 2sccm, deposition pressure is 0.56Pa, matrix deposits the target platform of rotation vacuum chamber under the condition that bias voltage is compound bias voltage, at matrix surface alternating deposit TiN layer and Cu-Zn metal level, to the rete total thickness be 0.1 μ m～10 μ m, wherein the first layer and outermost layer are the TiN layer in the rete, each 1.0 * 1016～2.0 * 1017 molecule/cm2 of amount average out at matrix surface depositing TiN layer, each 1.0 * 1016～1.3 * 1017 atom/cm2 of amount average out at the matrix surface depositing metal layers, the atomic percent of Zn is 0%～10% in the metal level, the atomic percent of Cu is 90%～100%, obtains slow-release type skeleton-type TiN/Cu-Zn metal level antibacterial film; Wherein volts DS is that 80V, coupling pulsed voltage are that 200V, pulse-repetition are that 10kHz, pulse width are 30 μ s in the described compound bias voltage of step 2; The Ti target adopts the magnetically controlled DC sputtering power supply in the step 2, and sputtering current is 0.6A, and the Cu-Zn target adopts the magnetron sputtering radio-frequency power supply, and radio frequency power is 300W.
2. the preparation method of slow-release type skeleton-type TiN according to claim 1/Cu-Zn metal level antibacterial film is characterized in that the described matrix of step 1 is metal, pottery or plastics.
3. the preparation method of slow-release type skeleton-type TiN according to claim 2/Cu-Zn metal level antibacterial film is characterized in that described metal is stainless steel, aluminium alloy, titanium alloy, copper alloy or soft steel.
4. the preparation method of slow-release type skeleton-type TiN according to claim 2/Cu-Zn metal level antibacterial film is characterized in that described pottery is aluminum oxide, zirconium white or silicon carbide.
5. the preparation method of slow-release type skeleton-type TiN according to claim 2/Cu-Zn metal level antibacterial film is characterized in that described plastics are polyethylene terephthalate, polycarbonate or acrylonitrile-butadiene-styrene copolymer.
6. according to the preparation method of claim 1,2,3,4 or 5 described slow-release type skeleton-type TiNs/Cu-Zn metal level antibacterial film, the mass content that it is characterized in that Ti in the target of Ti described in the step 2 is 99.99%.
7. the preparation method of slow-release type skeleton-type TiN according to claim 6/Cu-Zn metal level antibacterial film, the mass content that it is characterized in that Cu in the Cu-Zn target described in the step 2 is 62%, and the mass content of Zn is 38%, and described Cu is a H62 brass.
8. according to the preparation method of claim 1,2,3,4,5 or 7 described slow-release type skeleton-type TiNs/Cu-Zn metal level antibacterial film, it is characterized in that the rete total thickness is 1.59 μ m in the step 2.
9. the preparation method of slow-release type skeleton-type TiN according to claim 8/Cu-Zn metal level antibacterial film is characterized in that each 1.7 * 1016 molecule/cm2 of amount average out at matrix surface depositing TiN layer in the step 2.
10. according to the preparation method of claim 1,2,3,4,5,7 or 9 described slow-release type skeleton-type TiNs/Cu-Zn metal level antibacterial film, it is characterized in that each 3.3 * 1016 atom/cm2 of amount average out in the step 2 at the matrix surface depositing metal layers.
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