CN109161938B - Antibacterial and corrosion-resistant capsaicin composite ZnO/Zn coating and preparation and application thereof - Google Patents
Antibacterial and corrosion-resistant capsaicin composite ZnO/Zn coating and preparation and application thereof Download PDFInfo
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- CN109161938B CN109161938B CN201811146047.3A CN201811146047A CN109161938B CN 109161938 B CN109161938 B CN 109161938B CN 201811146047 A CN201811146047 A CN 201811146047A CN 109161938 B CN109161938 B CN 109161938B
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/22—Electroplating: Baths therefor from solutions of zinc
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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Abstract
The invention belongs to the field of composite metal coatings, and particularly relates to preparation and application of an antibacterial and corrosion-resistant capsaicin composite ZnO/Zn coating. The antibacterial and corrosion-resistant capsaicin composite ZnO/Zn coating is prepared by compounding capsaicin in alkaline deposition liquid under the condition of constant current deposition to obtain a zinc array with pores on the surface, and then drying the zinc array in a nitrogen environment to naturally form ZnO nanoneedles on the surface of the zinc array in the air to form the capsaicin composite ZnO/Zn coating. The capsaicin composite ZnO/Zn coating surface can form needle-shaped ZnO, has good antibacterial and corrosion resistant properties, is suitable for steel structure protection in water environment or marine environment damaged by biological activity, and has good fouling protection application value.
Description
Technical Field
The invention belongs to the field of electrochemical coatings, and particularly relates to an antibacterial and corrosion-resistant capsaicin composite ZnO/Zn coating as well as preparation and application thereof.
Background
The marine environment is a complex corrosive environment, not only is seawater itself a strong electrolyte, but also its very high biological activity seriously harms human marine activity. A large number of artificial steel facilities exist in the marine environment, wherein a plurality of key parts such as ship propellers, submarine steel cables and the like are protected by adopting a metal coating due to special service environment, and a zinc-based coating is widely applied due to negative self-corrosion potential and good barrier function. However, while zinc-based coatings provide good protection against chemical and electrochemical corrosion, they are still subject to microbial corrosion and biofouling.
Researches show that antibacterial properties can be obtained by compounding an antibacterial agent into a metal coating material, but the antibacterial agent used by the prior art is mainly an antifouling agent, has a short half-life period, still has certain harm to the environment, and cannot fundamentally obtain an environment-friendly, nontoxic and pollution-free microbial corrosion and fouling protection technology.
Disclosure of Invention
Aiming at the problems of microbial corrosion and biological fouling of the zinc coating in steel protection and the environmental pollution problem of the prior art, the invention aims to provide an antibacterial and corrosion-resistant capsaicin composite ZnO/Zn coating and preparation and application thereof.
In order to realize the purpose, the invention adopts the following technical scheme:
a preparation method of antibacterial and corrosion-resistant capsaicin composite ZnO/Zn coating comprises adding capsaicin into alkaline zinc plating solution, and obtaining zinc array by constant current method; then in N2After drying, needle-like ZnO surface is formed naturally in air.
The alkaline zinc plating liquid system is as follows: dissolving 14-18 g/L NaOH and 1.9-2.2 g/L ZnO in 1L distilled water; the addition amount of the capsaicin is 0.2-1.0 g/L.
The addition amount of the capsaicin is 0.6 g/L.
The cathode of the constant current method is a carbon steel substrate, the anode is a pure zinc sheet, and the current density is 15-25 mAcm-2。
Said N is2The drying time is more than 10min, and the moisture is ensured not to participate in the oxidation reaction of Zn in the air.
An antibacterial and corrosion-resistant capsaicin composite ZnO/Zn coating is prepared by the method.
An application of an antibacterial and corrosion-resistant capsaicin composite ZnO/Zn coating, and an application of the composite coating in antibacterial or corrosion protection in a bioactive environment.
The composite coating is applied to being used as an antibacterial layer or an anti-corrosion layer in a bioactive environment.
The invention has the beneficial effects that:
the invention takes the natural antibacterial product capsaicin as an antibacterial additive to be compounded into the zinc-based electroplated layer, and can naturally form a nanometer needle-shaped ZnO film on the surface of the zinc-based electroplated layer, so that the chemical antibacterial action of the capsaicin is combined with the physical antibacterial action of the nanometer ZnO column, and the corrosion resistance and the antibacterial activity of the composite electroplated layer are greatly enhanced. Compared with a conventional zinc coating, the capsaicin composite ZnO/Zn electroplated coating can be compounded with natural antibacterial capsaicin to obtain chemical antibacterial activity, and can independently form nano needle-shaped ZnO on the surface of the coating to further obtain physical antibacterial property, so that the coating has excellent corrosion resistance and sterilization property. The method specifically comprises the following steps:
(1) the invention not only has the advantages of negative self-corrosion potential and good barrier effect of the common zinc coating, but also has the effects of green, non-toxic, environment-friendly, microbial corrosion resistance and biofouling prevention, and has multiple functions.
(2) According to the invention, capsaicin is used as a plating solution additive for controlling the surface structure and appearance of the plating layer, so that the coating is different from other zinc-based plating layers, and the surface can spontaneously form ZnO nanoneedles in an air environment, thereby achieving the physical antibacterial effect.
(3) The capsaicin is successfully adsorbed and compounded in the coating, so that the coating has a chemical antibacterial effect without pollution.
(4) According to the invention, the chemical antibacterial effect of capsaicin and the physical antibacterial effect of ZnO are combined by utilizing the compounding of capsaicin and the influence on zinc deposition, so that the antibacterial property is greatly improved.
(5) The thickness of the capsaicin composite ZnO/Zn coating can be designed according to the application environment and the service life of the substrate, so that the service life of the structure is guaranteed;
(6) the invention provides a method for preventing steel structures from microbial corrosion and fouling in marine environments, wherein the plating layer is firmly combined with a substrate.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) photograph (i), an X-ray crystal diffraction (XRD) pattern (ii) and an electron energy spectrum (EDS) surface distribution diagram (iii) of the pure zinc plating layer AB (a, b), the capsaicin composite ZnO/Zn plating layer AC1(c, d), AC2(e, f) and AC3(g, h) provided by the example of the present invention. Wherein b, d, f and h are respectively enlarged images of a, c, e and g;
is a diffraction peak of Zn; is ZDiffraction peak of nO;
diffraction peaks for the Fe matrix.
Fig. 2 is a Tafel polarization curve diagram of pure zinc coatings BB, capsaicin composite ZnO/Zn coatings BC1, BC2 and BC3 provided by the embodiment of the invention after being exposed for 14 days in Sulfate Reducing Bacteria (SRB).
FIG. 3 shows that the pure zinc plating CB, the capsaicin composite ZnO/Zn plating CC1, the CC2 and the CC3 provided by the embodiment of the invention are 107Fluorescence micrographs of cfu/mL E.coli (E.coli) after 24h of immersion in Phosphate Buffered Saline (PBS) suspension.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to provide a more complete understanding of the invention by one of ordinary skill in the art, and are not intended to be limiting in any way.
Example 1:
preparing a capsaicin composite ZnO/Zn electroplated layer:
1) preparing an alkaline zinc plating solution system: 16g/L NaOH and 2.0g/L ZnO in distilled water, and the mixture is Jblank for standby.
Then 0.2g/L, 0.6g/L and 1.0g/L capsaicin are respectively added into Jblank, stirred for half an hour and then kept stand to respectively obtain JC1, JC2 and JC 3.
2) A20 # standard carbon steel sheet is used as a base material, each surface of a test piece is polished by 80#, 400#, 1000# and 2000# sandpaper aqueous phase sandpaper, the test piece is placed into absolute ethyl alcohol for 10min to remove oil stains on the surface, and then the exposed part of the test piece is immersed into 1mol/L HCl for 5s to activate the surface for later use.
3) And (3) adjusting to a constant current mode by using a DJS-292E constant potential rectifier, connecting the steel to be protected treated in the step 2) with the negative electrode of the direct current power supply, and connecting the pure zinc sheets with the same size with the positive electrode of the direct current power supply. Immersing the zinc-containing alkaline zinc plating solution in the alkaline zinc plating solution systems Jblank, JC1, JC2 and JC3 prepared in the step 1). At 20mA cm-2Depositing for 20min under constant current density to obtain composite zinc coatings AB, AC1, AC2 and AC 3;
4) and after the electrodeposition is finished, taking out the plated steel sheet, washing the surface of the plated steel sheet with secondary distilled water for 2-3 times, drying the steel sheet with high-purity nitrogen for 10min, and standing the steel sheet in the air for 30 min. Obtaining the capsaicin composite ZnO/Zn electroplated layer.
The morphology, structure and element distribution of all electroplated layer materials are shown in figure 1. As shown in fig. 1(i), the addition and recombination of capsaicin significantly changes the morphology of the zinc array, thereby affecting the morphology of the ZnO film formed on the surface. With the increase of the addition amount of the capsaicin, the surface of the electroplated layer is changed from a dense hexagonal platelet arrangement to a porous appearance, and ZnO formed on the surface of the electroplated layer is also changed from a conventional platelet to a nano needle structure. Further XRD results (fig. 1(ii)) show that, on the surface of carbon steel, not only the zinc array is deposited to obtain a zinc array, but also a nano needle structure of ZnO can be naturally formed in the air by the technical means of the present invention. Finally, the EDS surface distribution of AC2 (fig. 1(iii)) results show that zinc, as a main element of the plating layer, is uniformly distributed inside the plating layer; c is used as a main element of capsaicin and is mainly distributed in the gully-shaped appearance of the electroplated layer, which indicates that the capsaicin is mainly compounded by adsorption; and the O element as a characteristic element of the co-existence of capsaicin and ZnO nanoparticles is matched with the shapes of gully shapes and nano needle-shaped structures in the SEM, so that the co-existence of capsaicin, ZnO nanoparticles and zinc in the composite electroplated layer is proved, namely, the capsaicin composite ZnO/Zn electroplated layer is successfully obtained by the technical means of the invention.
Example 2:
and (3) evaluating the microbial corrosion resistance of the capsaicin composite ZnO/Zn electroplated layer:
the sulphate plating bath systems Jblank and JC1, JC2 and JC3 were prepared according to the procedure of example 1 at 15mA cm-2Constant current deposition is carried out for 20min under current density, composite zinc coatings BB, BC1, BC2 and BC3 are obtained, and the electroplated coatings are subsequently treated according to the step (4) in the example 1. Subsequently, the prepared BB, BC1, BC2 and BC3 plating layers were immersed in typical marine corrosive microorganism Sulfate Reducing Bacteria (SRB) for 14 days, and the corrosion resistance of the BB, BC1, BC2 and BC3 plating layers was evaluated using a Tafel curve (as shown in fig. 2). According to the polarization curve, the hot pepper is observedThe increase of the concentration of the additive elements and the positive shift of the self-corrosion potential of the plating layer indicate that the corrosion sensitivity is reduced; however, the self-corrosion current density of the coating tends to decrease and then increase, which indicates that the corrosion rate of the coating decreases and then increases. Therefore, in conclusion, compared with a pure zinc plating layer, the corrosion resistance of the capsaicin composite ZnO/Zn plating layer is improved, but the microbial corrosion resistance of BC1 and BC2 plating layers with the capsaicin addition concentration of 0.2-0.6 g/L is optimal.
Example 3:
and (3) evaluating the antibacterial performance of the capsaicin composite ZnO/Zn electroplated layer:
the sulphate plating bath systems Jblank and JC1, JC2 and JC3 were prepared according to the procedure of example 1 at 25mA cm-2Constant current deposition is carried out for 20min under the current density, composite zinc coatings of CB, CC1, CC2 and CC3 are obtained, and the electroplated coating is subsequently treated according to the step (4) in the example 1. Subsequently, the prepared plating layers of CB, CC1, CC2, and CC3 were immersed in 107And (5) soaking the E.coliPBS suspension for 24 hours in cfu/mL. Taking out, adding mixed staining agent (mixture of 4mg/L ethidium bromide and 4mg/L acridine orange), staining at 30 deg.C in dark for 30min, and observing under 200 times of Olimbas fluorescence microscope. The bright spots in the figure are bacteria attached to the surface of the coating, and it is known from the figure that a large number of living bacteria are attached to the surface of the pure zinc coating CB, and many of the bacteria are clustered, have already formed colonies, and tend to be connected into a dense biofilm. And the bacterial adhesion rate of surfaces of capsaicin composite ZnO/Zn electroplated layers CC1, CC2 and CC3 is greatly reduced, wherein almost no bacteria are found on the surface of the CC2 composite electroplated layer, and the surfaces show particularly excellent antibacterial adhesion performance.
Claims (7)
1. A preparation method of an antibacterial and corrosion-resistant capsaicin composite ZnO/Zn coating is characterized by comprising the following steps: adding capsaicin into the alkaline zinc plating solution, and obtaining a zinc array by a constant current method; then in N2After drying, the needle-shaped ZnO surface is naturally formed in the air;
the alkaline zinc plating liquid system is as follows: dissolving 14-18 g/L NaOH and 1.9-2.2 g/L ZnO in 1L distilled water; the addition amount of the capsaicin is 0.2-1.0 g/L.
2. The process according to claim 1, wherein: the addition amount of the capsaicin is 0.6 g/L.
3. The process according to claim 1, wherein: the cathode of the constant current method is a carbon steel substrate, the anode is a pure zinc sheet, and the current density is 15-25 mA cm-2。
4. The process according to claim 1, wherein: said N is2The drying time is more than 10min, and the moisture is ensured not to participate in the oxidation reaction of Zn in the air.
5. An antibacterial and corrosion-resistant capsaicin composite ZnO/Zn coating prepared by the method of claim 1, wherein: a capsaicin composite ZnO/Zn coating prepared by the method as defined in claim 1.
6. The use of the antibacterial and corrosion-resistant capsaicin composite ZnO/Zn coating as claimed in claim 5, wherein: the composite coating is applied to antibacterial or corrosion protection in a bioactive environment.
7. The use of the antimicrobial corrosion resistant capsaicin composite ZnO/Zn coating according to claim 6, wherein: the composite coating is applied to being used as an antibacterial layer or an anti-corrosion layer in a bioactive environment.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1096071A (en) * | 1996-09-20 | 1998-04-14 | Nisshin Steel Co Ltd | Corrosion resistant metallic material having antibacterial property |
| CN102758227A (en) * | 2012-06-08 | 2012-10-31 | 中国科学院海洋研究所 | Bactericidal and corrosion-resistant zinc plating layer suitable for marine environment steelwork material |
| CN104725980A (en) * | 2015-03-10 | 2015-06-24 | 铜陵市陵阳化工有限责任公司 | Cathode electrophoretic coating having antibacterial and moth-preventing functions and preparation method of cathode electrophoretic coating |
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- 2018-09-29 CN CN201811146047.3A patent/CN109161938B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1096071A (en) * | 1996-09-20 | 1998-04-14 | Nisshin Steel Co Ltd | Corrosion resistant metallic material having antibacterial property |
| CN102758227A (en) * | 2012-06-08 | 2012-10-31 | 中国科学院海洋研究所 | Bactericidal and corrosion-resistant zinc plating layer suitable for marine environment steelwork material |
| CN104725980A (en) * | 2015-03-10 | 2015-06-24 | 铜陵市陵阳化工有限责任公司 | Cathode electrophoretic coating having antibacterial and moth-preventing functions and preparation method of cathode electrophoretic coating |
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