CN105369301B - Compound zinc coating of a kind of chitosan and preparation method thereof - Google Patents
Compound zinc coating of a kind of chitosan and preparation method thereof Download PDFInfo
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- CN105369301B CN105369301B CN201510962421.7A CN201510962421A CN105369301B CN 105369301 B CN105369301 B CN 105369301B CN 201510962421 A CN201510962421 A CN 201510962421A CN 105369301 B CN105369301 B CN 105369301B
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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
- 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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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
Abstract
The invention belongs to electrochemical plating fields, and in particular to compound zinc coating of a kind of chitosan and preparation method thereof.The compound zinc coating of chitosan, by electro-deposition, the electro-deposition in the zinc sulfate bath system containing chitosan obtains the compound zinc coating of chitosan, wherein, the chitosan of 0.2~1.0g of addition in every liter of zinc sulfate bath system.Chitosan composite deposite prepared by the present invention has the advantages that green non-pollution, antibacterial surface effect is good, preparation process is simple, and the fields such as the protection of iron structure and marine anti-pollution have good application value under the water environment under microbiological effect.
Description
Technical field
The invention belongs to electrochemical plating fields, and in particular to compound zinc coating of a kind of chitosan and preparation method thereof.
Background technology
Electrochemical plating is to form metal that is uniform, fine and close, being well combined or conjunction in article surface using metal electrodeposition
Golden sedimentary.Electrochemical plating has had the developing history of more than 200 years, and earliest plating is 1803 French
L.Brugnattlli is gold-plated in the success of silver strip surface.Then, electrochemical plating gold, silver, copper, nickel, chromium, zinc technology develop gradually,
So that electroplating industry 19th century mid-term form more rounded system.In numerous steel coating, zinc coating due to its from
Corrosion potential is relatively negative, has the protective action of sacrificial anode to steel, in addition, zinc coating crystal structure is fine and close, barrier action is good,
So as to be widely used in steel protection.
In water body environment, the service life of steel by physical factor, chemical factor and biological factor collective effect,
Traditional steel zinc coating corrodes acceleration problem, but right caused by good can resisting chemical factor and part physical factor
It is ineffective in the influence of biological factor.The influence of biological factor is mainly manifested in caused by the metabolism of microorganism in water environment
Corrode acceleration problem and biodeterioration problem caused by the attachment and growth of biology, and during these, the microorganisms such as bacterium
Attachment be a vital step, therefore, the antibacterial and protective method for studying steel is very necessary.
Common antibacterial anti-fouling method is mostly to add toxic organic matter or heavy metal ion at this stage, the dirt for environment
Extremely serious, green non-poisonous antibiotic method is contaminated as trend of the times.
Invention content
It is on active service in water body environment the problem of encountering for above-mentioned steel, to be answered present invention aims at a kind of chitosan is provided
Zinc coating of conjunction and preparation method thereof.
To achieve the above object, the present invention takes following technical scheme to implement：
A kind of compound zinc coating of chitosan, by electro-deposition, electricity is heavy in the zinc sulfate bath system containing chitosan
Product, obtains the compound zinc coating of chitosan, wherein, the chitosan of 0.2~1.0g of addition in every liter of zinc sulfate bath system.
The chitosan of 0.6g is added in every liter of zinc sulfate bath system.
The bath system is zinc sulfate bath system, and wherein ingredient and its mass fraction is：250~400g/L
ZnSO4·7H2O, 80~250g/L Na2SO4, 25~30g/L H3BO3, 40~45g/L Al2(SO4)3·18H2O。
The preparation method of the compound zinc coating of a kind of chitosan, by electro-deposition, in the zinc sulfate plating solution containing chitosan
To the zinc coating that substrate surface electro-deposition chitosan to be protected is compound in electro-deposition in system.
Specifically, using DC power supply galvanostatic deposition, using steel to be protected as pulse power cathode, using pure zinc metal sheet as arteries and veins
Positive pole is rushed, steel to be protected and pure zinc metal sheet are immersed in the zinc sulfate bath system containing chitosan in 1~20mA cm-2
Under current density, by compound zinc coating electro-deposition in steel surface to be protected.
Described to use DC power supply galvanostatic deposition, depositing current density is 5mA cm-2。
A kind of application of the compound zinc coating of chitosan, the zinc coating antibacterial or it is antifouling in application.
The compound zinc coating of the chitosan, can be applied in the environment under microbiological effect, have good antibiotic property
The surface nature of energy.Compared to conventional antimicrobial, nonpolluting coating, the coating is environmentally protective, nontoxic and pollution-free.
The beneficial effects of the present invention are：
For the present invention by the way that chitosan is made an addition in zinc sulfate bath system, galvanostatic deposition is prepared for chitosan composite zinc
Coating can be applied to the steel material in water environment, green non-poisonous pollution-free, have for the anti-microbial property for improving steel material
Major application meaning；It is characterized in particular in：
(1) present invention not only has barrier propterty of the common coating for steel corrosion, is also equipped with antibacterial, the attachment of resistance to bacterium
Performance；
(2) addition of appropriate chitosan can effectively increase deposition current efficiency in the present invention, reduce protection cost, save
The electric energy energy；
(3) present invention can be protected according to application environment and substrate service life design chitosan thickness of multiple plating and structure
Hinder structure service life；
(4) coating of the present invention is bright fine and close, and silvery white surface is presented, the beauty of substrate is helped to improve in, can be used
In the steel construction for having particular/special requirement；
(5) present invention has the characteristics of green non-poisonous pollution-free, environmental-friendly compared to conventional antimicrobial coating；
(6) coating of the present invention is firmly combined with substrate, provide it is a kind of be on active service in water environment to iron structure it is anti-corrosion
With antibacterial and protective method.
Description of the drawings
Fig. 1 for pure zinc coating (a) provided in an embodiment of the present invention and chitosan plating solution add a concentration of 0.2g/L (b),
0.6g/L (c) and 1.0g/L (d) optical photographs.
Fig. 2 for pure zinc coating (a) provided in an embodiment of the present invention and chitosan plating solution add a concentration of 0.2g/L (b),
0.6g/L (c) and 1.0g/L (d) stereoscan photographs.
Fig. 3 for pure zinc coating (a) provided in an embodiment of the present invention and chitosan plating solution add a concentration of 0.2g/L (b),
0.6g/L (c) and 1.0g/L (d) chitosan composite deposite X ray crystal diffraction spectrograms.
Wherein A is full angle crystal diffraction peak；B is chitosan-zinc complex crystal diffraction peak, and 1 to represent chitosan-zinc multiple
Object characteristic diffraction peak is closed, 2 represent pure zinc characteristic diffraction peak.
Fig. 4 for pure zinc coating (a) provided in an embodiment of the present invention and chitosan plating solution add a concentration of 0.2g/L (b),
0.6g/L (c) and 1.0g/L (d) current efficiency figures.
Fig. 5 for pure zinc coating (a) provided in an embodiment of the present invention and chitosan plating solution add a concentration of 0.2g/L (b),
0.6g/L (c) and 1.0g/L (d) are exposed to 106In cfu/mL Escherichia coli phosphate buffers for 24 hours after fluorescent microscopy images.
Specific embodiment
Below by way of specific embodiment, the invention will be further described, contributes to those of ordinary skill in the art more
It is fully understood by the present invention, but do not limit the invention in any way.
The compound zinc coating of chitosan of the present invention is the concentration according to 0.2~1.0g/L (as mass fraction) by chitosan
It makes an addition in acid zinc sulfate bath system, under the conditions of galvanostatic deposition, by intermolecular interaction, by shell in deposition process
Glycan is compound in inside coating, and forms chitosan-zinc complex adsorption layer in coating surface, has fine and close surface crystal shape
Looks.It is excellent that chitosan composite deposite prepared by the present invention has that green non-pollution, antibacterial surface effect are good, preparation process is simple etc.
Point, the fields such as the protection of iron structure and marine anti-pollution have good application value under the water environment under microbiological effect.
Embodiment 1：
The compound zinc coating preparation method of chitosan
1) zinc sulfate bath system is prepared, by 250g ZnSO4·7H2O、80g Na2SO4、25g H3BO3、40g Al2
(SO4)3·18H2O is dissolved in 1L distilled water, is that blank sulfate bath S1 is spare；By 400g ZnSO4·7H2O、250g
Na2SO4、30g H3BO3、45g Al2(SO4)3·18H2O is dissolved in 1L distilled water, is that blank sulfate bath S2 is spare；
0.2g/L, 0.6g/L and 1.0g/L are added respectively into blank sulfate bath S1, S2 of above-mentioned zinc sulfate plating solution
Chitosan sulfate composite zinc plating solution SE1 (comprising 3 kinds of chitosan concentrations) is prepared with SE2 (comprising 3 kinds of chitosans in chitosan
Concentration) it is spare.
2) 20# carbon steel coupons working surface is polished step by step to 2000# with SiC water phases sand paper, in the ultrasonic wave in absolute ethyl alcohol
10min is cleaned, it is spare as steel matrix to be protected thoroughly to remove steel disc surface and oil contaminant and impurity；
3) it using DJS-292E type potentiostats, is adjusted under constant current mode, the steel to be protected with treated in step 2)
DC power cathode is connected, DC power anode is connected with the pure zinc metal sheet of identical size.It is immersed in the shell of step 1) preparation
In glycan zinc sulfate bath system S1 and SE1, in 5mA cm-2Under current density, galvanostatic deposition is carried out, obtains about 30 μ m-thicks
Zinc coating is AC1 and AE1；It is immersed in the chitosan sulfate zinc bath system S1 and SE1 of step 1) preparation, in 10mA
cm-2Under current density, galvanostatic deposition is carried out, the zinc coating for obtaining about 30 μ m-thicks is AC2 and AE2；It is immersed in step 1)
In the chitosan sulfate zinc bath system S2 and SE2 of preparation, in 20mA cm-2Under current density, galvanostatic deposition is carried out, is obtained
The zinc coating of about 30 μ m-thicks is AC3 and AE3.
4) after the completion of electro-deposition, the steel disc plated is taken out, surface is rinsed residual electroplate liquid 2~3 times with redistilled water, done
It is dry.Tri- kinds of coating optical photographs of the pure zinc coatings of wherein AC1 and AE1 are as shown in Figure 1.
It can be observed by figure, compound zinc coating (Fig. 1 b, c, d) the purer zinc coating (Fig. 1 a) for being added to chitosan is apparent more
Add light smooth, and the addition (0.2g/L, 0.6g/L) of appropriate chitosan makes coating apparent finer and close.
Meanwhile pure zinc coating is scanned electron microscope observation and X ray crystal diffraction with tri- kinds of coating of AE1 to AC1
Analysis, the coating surface morphology photo observed under scanning electron microscope is shown by Fig. 2.Pure zinc coating (Fig. 2 a) surface is shown
Go out the irregular close hexagon platelet pattern of zinc deposit classics；The compound zinc coating of 0.2g/L chitosans is added in plating solution
(Fig. 2 b) surface equally shows hexagon platelet pattern, but chitosan-zinc complexes of some sheets occurs in surface；In plating solution
Significant change has occurred in compound zinc coating (Fig. 2 c) surface for adding in 0.6g/L chitosans, shows fine and close chitosan-zinc
The densest crystal surface texture that compound be combined with each other with zinc-base bottom；The compound zinc coating of 1.0g/L chitosans is added in plating solution
There is more loose surface in (Fig. 2 d) surface, is mainly shown as some big sheet chitosan-zinc complexes and is covered in six
The surface at side shape platelet zinc-base bottom.
By the X ray crystal diffraction collection of illustrative plates of Fig. 3 A coating it is found that all zinc coatings are all shown (101) (102) (112)
(002) the crystal diffraction peak at the zinc-base bottom of (100) (103), the addition of chitosan clearly enhance (100) crystal orientation, but drop
Low (002) and (102) crystal orientation, illustrates influence showed increased of a certain phase due to chitosan.By further studying, scheme
3B shows the composite deposite being prepared in the bath system for being added to chitosan and shows apparent chitosan-zinc
The characteristic absorption peak of compound further demonstrates the co-deposition of chitosan-zinc complexes.
In conclusion the addition of chitosan changed dramatically coating surface morphology and crystal structure in plating solution, further test
The success for having demonstrate,proved chitosan is compound.
Embodiment 2：
The compound zinc coating current efficiency comparison of chitosan
Prepare pure zinc coating AC2 and three kinds of chitosan composite deposite AE2 according to step in embodiment 1, and before deposition after
Quality of coating is weighed, the cathode efficiency in deposition process is calculated according to formula (1).
Wherein, ηcFor cathode efficiency；m1For sample mass before deposition, g；m2For sample mass after deposition, g；E is electricity
The electrically charged amount of sub- institute, C；J is current density, mA cm-2；S is exposure deposition reaction area in the plating solution, cm2；When t is deposition
Between, s；MZnFor the molal weight of Zn, g/mol；NAFor Avgadro constant.
As shown in figure 4, the appropriate addition (0.2g/L, 0.6g/L) of chitosan in the plating solution makes the compound zinc coating electricity of chitosan
The purer zinc coating increase of efficiency is flowed, helps to save electric energy, it is cost-effective.Excessively high chitosan concentration (1.0g/L) not only makes to sink
Product cost increase, and waste of energy.Therefore, the optimal a concentration of 0.6g/L of addition of chitosan, effectively increases cathode efficiency.
Embodiment 3
The compound zinc coating anti-microbial property of chitosan
Escherichia coli used in experiment (E.coli), using the pure zinc coating AC3 prepared according to step in embodiment 1 and three kinds
Chitosan composite deposite AE3 carries out antibacterial experiment.Antibiotic property test experiments method is：
1) the E.coli single bacterium colonies of picking solid medium conservation are in Luria-Bertani fluid nutrient mediums (LB, 10g/L
NaCl, 10g/L peptone and 5g/L yeast extracts, distilled water are prepared, and pH is incubated overnight in being adjusted to 7) at 37 DEG C, uses bacterium colony meter
Number method (CFU) calculates bacterial concentration in bacterium solution.At room temperature, bacterium solution under 4000rpm is centrifuged into 5min using centrifuge, isolated
Thalline uses phosphate buffer (PBS, 8.0g/L NaCl, 0.2g/L KCl, 1.44g/L Na2HPO4, 0.44g/L- 1KH2PO4, distilled water preparation) and oscillation cleaning, it is configured to 106The E.coli bacterium solutions of cfu/mL.
2) at 37 DEG C, zinc coating test piece AC3 and AE3 are respectively exposed to 106In cfu/mL E.coli PBS bacterium solutions
It takes out afterwards for 24 hours, after gently being rinsed using sterilizing PBS, 30min is fixed with sterilizing PBS 5% glutaraldehydes prepared, dark after flushing
Dyeing 30min in 1g/mL 4', 6- diamidino -2-phenylindones (DAPI) is immersed in room, using Olympus fluorescence microscopy
Mirror amplifies observation of taking pictures under excitation wavelength using 400 times.Data are analyzed using 6.0 softwares of Image-pro Plus.
As shown in figure 5, bright dot blue in figure be attached to coating surface microorganism combined with coloring agent after
The image generated under fluorescence excitation.Fig. 5 a are the fluorogram of pure Zinc Deposit, and surface bacteria has begun largely to adhere to,
And show bacterial accumulation, it is the preneoplastic state to form complete bio film.The compound zinc coating of chitosan (Fig. 5 b, c, d) surface has
A small amount of bacterium attachment, but the state of single attachment is presented, without clustering phenomena, it is good to illustrate that the compound zinc coating of chitosan has
Anti-microbial property, effectively inhibit the attachment of bacterium.
To sum up, the zinc coating that the addition of chitosan makes anti-microbial property bad has good antibacterial properties, and in shell
The attachment of bacterium is effectively inhibited under the optimal addition concentration of glycan.
Claims (6)
1. a kind of compound zinc coating of chitosan, it is characterised in that：By electro-deposition, in the zinc sulfate plating liquid containing chitosan
Electro-deposition in system obtains the compound zinc coating of chitosan, wherein, the shell of 0.2~1.0g of addition in every liter of zinc sulfate bath system
Glycan；
The bath system is zinc sulfate bath system, and wherein ingredient and its mass fraction is：250~400g/L ZnSO4·
7H2O, 80~250g/L Na2SO4, 25~30g/L H3BO3, 40~45g/L Al2(SO4)3·18H2O；
Using DC power supply galvanostatic deposition, using steel to be protected as pulse power cathode, using pure zinc metal sheet as the pulse power just
Steel to be protected and pure zinc metal sheet are immersed in the zinc sulfate bath system containing chitosan in 1~20mA cm by pole-2Current density
Under, by compound zinc coating electro-deposition in steel surface to be protected.
2. according to the compound zinc coating of the chitosan described in claim 1, it is characterised in that：Every liter of zinc sulfate plating liquid
The chitosan of 0.6g is added in system.
3. a kind of preparation method of the compound zinc coating of chitosan described in claim 1, it is characterised in that：It is heavy by electricity
Product, to the zinc that substrate surface electro-deposition chitosan to be protected is compound in electro-deposition in the zinc sulfate bath system containing chitosan
Coating.
4. according to the preparation method of the compound zinc coating of the chitosan described in claim 3, it is characterised in that：Using direct current
Source galvanostatic deposition, using steel to be protected as pulse power cathode, using pure zinc metal sheet as pulse power anode, by steel to be protected with
Pure zinc metal sheet is immersed in the zinc sulfate bath system containing chitosan in 1~20mA cm-2Under current density, by compound zinc coating
Electro-deposition is in steel surface to be protected.
5. according to the preparation method of the compound zinc coating of the chitosan described in claim 4, it is characterised in that：It is described to use directly
Galvanic electricity source galvanostatic deposition, depositing current density are 5mA cm-2。
6. a kind of application of the compound zinc coating of chitosan described in claim 1, it is characterised in that：The zinc coating is anti-
Bacterium or it is antifouling in application.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106337194A (en) * | 2016-09-26 | 2017-01-18 | 山东金宝电子股份有限公司 | Surface treatment composite additive capable of improving corrosion resistance of copper foil |
| CN106917131B (en) * | 2017-02-28 | 2018-09-25 | 湖北大学 | A kind of preparation method of chitosan/molybdenum disulfide photocatalysis antibacterial coating |
| CN110462111B (en) * | 2017-03-29 | 2022-01-07 | 古河电气工业株式会社 | Integrated body, composite material having the same, terminal for electrical contact, and printed wiring board |
| CN107858720B (en) * | 2017-11-22 | 2019-03-19 | 中国科学院海洋研究所 | The wear-resistant alkaline-resisting ferrocene-zinc composite plating solution of one kind and its application |
| CN112126876B (en) * | 2020-09-03 | 2022-08-23 | 余姚市永林机械科技有限公司 | Plating assistant liquid and hot galvanizing process using same |
| CN115537887B (en) * | 2022-09-29 | 2024-01-19 | 新东北电气集团高压开关有限公司 | Preparation method of metal surface coating applied to marine environment |
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| 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 |
| CN102899692A (en) * | 2012-10-25 | 2013-01-30 | 中国科学院海洋研究所 | Method for preparing marine antifouling zinc coating solution |
| CN105079878A (en) * | 2015-09-14 | 2015-11-25 | 江南大学 | Preparation method of nano antibacterial coating based on chitosan complex micelle |
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2015
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102899692A (en) * | 2012-10-25 | 2013-01-30 | 中国科学院海洋研究所 | Method for preparing marine antifouling zinc coating solution |
| CN105079878A (en) * | 2015-09-14 | 2015-11-25 | 江南大学 | Preparation method of nano antibacterial coating based on chitosan complex micelle |
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