CN102590298A - Method for testing microbiological corrosion resisting performance of antibacterial stainless steel by electrochemical method - Google Patents
Method for testing microbiological corrosion resisting performance of antibacterial stainless steel by electrochemical method Download PDFInfo
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Abstract
The invention relates to two fields of material science and microbial science, belongs to the category of an interdiscipline subject, and particularly discloses a method for testing microbiological corrosion resisting performance of antibacterial stainless steel by an electrochemical method. The electrochemical method is utilized to test the microbiological corrosion resisting situations of the antibacterial stainless steel acted with bacteria for different times, and the situations can be used for evaluating the microbiological corrosion resisting performance of the antibacterial stainless steel. According to the invention, the electrochemical method is utilized to test open circuit potential, electrochemical impedance and polarization curves after the austenite stainless steel is acted with the bacteria for different times so as to evaluate the microbiological corrosion resisting performance of the antibacterial stainless steel. The method disclosed by the invention can solve the problems that the microbiological corrosion resisting performance of the antibacterial stainless steel can not be tested in dry places, deep sea and other environments, and the like, and aims to detect the microbiological corrosion resisting performance of the antibacterial stainless steel more reliably and conveniently.
Description
Technical field
The present invention relates to two fields of material science and microorganism science; Belong to the cross discipline category; Be specially a kind of method of utilizing electrochemical means test anti-bacteria stainless steel microbial corrosion resistance ability; Be the variation that utilizes open circuit potential, electrochemical impedance and polarization curve behind electrochemical means test anti-bacteria stainless steel and the bacterial action different time, and then estimate the method for anti-bacteria stainless steel microbial corrosion resistance ability.
Background technology
Stainless steel is widely used in the various oceanographic engineerings owing to have excellent mechanical property, corrosion resisting property and processing characteristics.When the oxidisability in the environment was enough strong, stainless surface can not only generate passivating film, and any breakage of passivating film can both self be repaired rapidly.Owing to be dissolved with oxygen in the seawater; Set up passive state for stainless steel oxidizing condition is provided; But a large amount of microorganisms that exist in the seawater also are ferocious to the destruction of passivating film, and this has just determined most of stainless steels in seawater, can only set up unsettled passive state.There are some researches show,, can not avoid microbiological corrosion although stainless steel surfaces exists one deck passivating film.Along with the widespread use of stainless steel in industry, its microbiological corrosion more and more receives extensive concern.Particularly the eighties in 20th century, states such as Great Britain and America have set up special microbiological corrosion research institution in succession, and the material of research also expands materials such as stainless steel to except that carbon steel.Stainless steel is usually used in some vitals owing to having good corrosion resisting property and comprehensive mechanical performance, but under the influence of microorganism, corrosion failure takes place for its welded seam and heat-affected zone regular meeting, thereby has influenced its widespread use.
Along with people's has cupric anti-bacteria stainless steel strong, lasting and broad-spectrum bactericidal action and has caused the more and more many concerns of people the enhancing of health and environmental consciousness.Because anti-bacteria stainless steel has the dual characteristics of structured material and antibiotic functional material concurrently, thereby the microbial corrosion resistance of research and discussion anti-bacteria stainless steel can have important use and theoretical value.
The antibacterial treatment copper-bearing ferritic stainless steel microbial corrosion resistance that " the academic proceeding of national corrosion electrochemistry in 2006 and method of testing " mentioned can research (Qin Liyan etc.), adopt multiple Electrochemical Measurement Technology such as stable state anodic polarization curves, the convergent response of constant potential open circuit and micro-biological process to study antibacterial treatment copper-bearing ferritic stainless steel and containing the corrosion resisting property in the oxygen bacterium solution of having a liking for of nutrient culture media.Result of study shows, stainless corrosion potential E
CorrAppear regularly with the metabolism of having a liking for the oxygen bacterium and to change, increase in time and negative moving.The spot corrosion disruptive potential E of anti-bacteria stainless steel in bacterium liquid
bThan the positive 170mV of common stainless steel.The measurement result of stainless steel constant potential open circuit decay shows that also antibacterial treatment improves the stability of stainless steel passivating film in bacterium liquid, and anti-bacteria stainless steel is than more microbial corrosion resistance of common stainless steel.Its weak point is: the test data of this research does not show that bacterium is under optimum condition of culture (35～37 ℃ of cultivation temperature), to carry out electrochemical property test; Do not reflect the optimum growh state of bacterium, can not contrast two kinds of stainless decay resistances objective and accurately.In addition,, just can guarantee not to be damaged in the surface of testing sample, more can reflect bacterial biof iotalm truly with the situation of change of different time on sample surfaces if adopt the method for electrochemical impedance test in the research.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing electrochemical means test anti-bacteria stainless steel microbial corrosion resistance ability; Solution can't problem, the microbial corrosion resistance ability that is intended to detect more reliably and easily anti-bacteria stainless steel such as can test to the anti-bacteria stainless steel microbial corrosion resistance in environment such as drying, deep-sea.
Technical scheme of the present invention is:
A kind of method of utilizing electrochemical means test anti-bacteria stainless steel microbial corrosion resistance ability; Utilize open circuit potential, electrochemical impedance and polarization curve after electrochemical means obtains anti-bacteria stainless steel and bacterial action different time, and then estimate the microbial corrosion resistance ability of anti-bacteria stainless steel material.It is pointed out that in the electro-chemical test process, the numerical value of the open circuit potential of material, corrosion potential and polarization resistance is high more, its microbial corrosion resistance can be strong more.
1, the preparation of experiment material
Prepare anti-bacteria stainless steel and the common stainless steel sample that is of a size of 10 * 10 * 3mm respectively with wire cutting method, clean, degrease are fixed on sample surfaces with copper conductor one end, and with the epoxy resin for cold edge, other end lead exposes then.After treating the epoxy resin drying, sample exposes other end surface after polishing, polishing, use the acetone soln ultrasonic cleaning, is positioned under the uviol lamp and sterilizes 20～40 minutes, and is subsequent use.
2, the preparation of bacteria suspension
With microbe growth to logarithmic growth after date, add the normal saline solution of 8～9wt ‰ of 4～6ml with the test tube that fresh inclined-plane is housed, scrape the lower inclined plane bacterium, adopt turbidimetry that the bacteria suspension stepwise dilution is become 4～6 * 10 with oese
6The bacterium liquid of cfu/ml.
The bacterium of adopting is Escherichia coli or staphylococcus aureus.
3, the effect of anti-bacteria stainless steel and bacterium
The stainless steel sample for preparing is positioned over is equipped with 4～6 * 10
6In the beaker of cfu/ml bacterium liquid, and submergence wherein, and the other end of copper conductor is exposed at outside the beaker, with the beaker good seal, is positioned in 35～37 ℃ the water-bath, cultivated 2～14 days.
4, the open circuit potential after the effect
After connecting with working electrode (stainless steel sample), to electrode (Pt electrode) and contrast electrode (KCl saturated calomel electrode); Open the electrochemical apparatus power supply; Open V3-Studio software, select the testing procedure of open circuit potential, the test duration of open circuit potential is decided to be 0.5～2 hour.
5, the electrochemical impedance after the effect
Select the mode determination of constant potential (potentiostatic), the scope of impedance is made as 0.01～100000Hz, obtains the Nyquist curve of impedance.
6, the polarization curve after the effect
Select the mode determination of electrokinetic potential-polarization curve, the scope of corrosion potential is made as-0.4～0.6mV, and sweep speed is 0.4～0.6mV/ second.
The invention has the beneficial effects as follows:
1, the present invention adopts electrochemical means, the mode that is used in combination through open circuit potential, electrochemical impedance and polarization curve behind test anti-bacteria stainless steel and the bacterial action different time, and then the microbial corrosion resistance ability of evaluation measured material.What need special instruction is; The test of employing electrochemical impedance; Be that mainly it can utilize small size signal and influences under the prerequisite of sample attribute at minimally; Objective and obtain the Changing Pattern of sample surfaces bacterial biof iotalm exactly, for the stainless steel new material of development microbial corrosion resistance provides more reliably and detects easily new method.
2, the invention provides a kind of method of utilizing electrochemical means test anti-bacteria stainless steel microbial corrosion resistance ability, this method is measured highly sensitive, can or test with the different strains of same material effect different materials.This method has characteristics such as easy and simple to handle, quick.
Description of drawings
Fig. 1 (a)-(b) is the open circuit potential curve behind anti-bacteria stainless steel and common stainless steel and the Escherichia coli effect different time among the embodiment 1, and wherein, Fig. 1 (a) is 2 days; Fig. 1 (b) is 14 days.
Fig. 2 (a)-(b) is the electrochemical impedance curve behind anti-bacteria stainless steel and common stainless steel and the Escherichia coli effect different time among the embodiment 1, and wherein, Fig. 2 (a) is 2 days; Fig. 2 (b) is 14 days.
Fig. 3 (a)-(b) is the polarization curve behind anti-bacteria stainless steel and common stainless steel and the Escherichia coli effect different time among the embodiment 1, and wherein, Fig. 3 (a) is 2 days; Fig. 3 (b) is 14 days.
Fig. 4 is anti-bacteria stainless steel and common stainless steel and the open circuit potential curve of Escherichia coli effect after 14 days among the embodiment 2.
Fig. 5 is anti-bacteria stainless steel and common stainless steel and the electrochemical impedance curve of Escherichia coli effect after 14 days among the embodiment 2.
Fig. 6 is anti-bacteria stainless steel and common stainless steel and the polarization curve of Escherichia coli effect after 14 days among the embodiment 2.
Embodiment
Embodiment 1:
The present invention selects for use Escherichia coli (ATCC25922) as the bacterial classification representative, the cupric austenite antimicrobial stainless steel and common 304 austenitic stainless steels (contrast stainless steel) of the development of material selection Metal Inst., Chinese Academy of Sciences.Through the stainless steel and the situation of open circuit potential, electrochemical impedance and polarization curve after bacterium contacts different time estimate the anti-bacteria stainless steel microbial corrosion resistance can, anti-bacteria stainless steel is seen table 1 with the stainless chemical analysis composition of contrast.
The chemical analysis composition (w.t.%) of table 1 anti-bacteria stainless steel and common stainless steel
The bacterium that the present invention adopts is Escherichia coli, is provided by Chinese common micro-organisms DSMZ.
1, the preparation of sample
Prepare anti-bacteria stainless steel and the common stainless steel sample that is of a size of 10mm * 10mm * 3mm respectively with wire cutting method, clean, degrease are fixed on sample surfaces with copper conductor one end; With epoxy resin for cold edge, other end lead exposes then, treat the epoxy resin drying after; Sample exposes other end surface after polishing, polishing, use the acetone soln ultrasonic cleaning, is positioned under the uviol lamp and sterilizes 30 minutes; Totally 6 groups of samples are subsequent use.
2, the preparation of bacteria suspension
With microbe growth to logarithmic growth after date, add the normal saline solution of the 8.5wt ‰ of 5ml with the test tube that fresh inclined-plane is housed, scrape the lower inclined plane bacterium, adopt turbidimetry that the bacteria suspension stepwise dilution is become 5 * 10 with oese
6The bacterium liquid of cfu/ml.
3, the effect of anti-bacteria stainless steel and bacterium
The stainless steel sample for preparing is positioned over is equipped with 5 * 10
6In the beaker of cfu/ml bacterium liquid, and submergence wherein, and the other end of copper conductor is exposed at outside the beaker, with the beaker good seal, is positioned in 37 ℃ the water-bath, cultivated 2～14 days.
4, the open circuit potential after the effect
After connecting with working electrode (stainless steel sample), to electrode (Pt electrode) and contrast electrode (KCl saturated calomel electrode); Open the electrochemical apparatus power supply; Open V3-Studio software, select the testing procedure of open circuit potential, the test duration of open circuit potential is decided to be 1 hour.Fig. 1 (a)-(b) is the open circuit potential behind anti-bacteria stainless steel and common stainless steel and the Escherichia coli effect different time.Can find out from Fig. 1 (a)-(b); Anti-bacteria stainless steel and the bacterial action open circuit potential mobility scale after 2～14 days is-0.17～-0.15V; Apparently higher than the open circuit potential mobility scale-0.24 of common stainless steel～-0.47V, the passivating film that shows the common stainless steel surface is more easily by bacterial corrosion.
5, the electrochemical impedance after the effect
Select the mode determination of potentiostatic, the test specification of electrochemical impedance is made as 0.01～100000Hz.Fig. 2 (a)-(b) is the Nyquist curve behind anti-bacteria stainless steel and common stainless steel and the Escherichia coli effect different time.Can find out from Fig. 2 (a)-(b); Anti-bacteria stainless steel and the bacterial action polarization resistance mobility scale after 2～14 days is 43～152k Ω; And the mobility scale of common stainless steel polarization resistance is 14～60k Ω, shows that point corrosion takes place the passivating film on common stainless steel surface more easily.
6, the polarization curve after the effect
Select the mode determination of electrokinetic potential-polarization curve, the scope of corrosion potential is made as-0.4～0.6mV, and corrosion rate is 0.5mV/ second.Fig. 3 (a)-(b) is the polarization curve behind anti-bacteria stainless steel and common stainless steel and the Escherichia coli effect different time.Can find out from Fig. 3 (a)-(b); Anti-bacteria stainless steel and the bacterial action corrosion potential mobility scale after 2～14 days is-0.32～-0.23V; And the corrosion potential mobility scale of common stainless steel is-0.51～-0.29V, show that anti-bacteria stainless steel has excellent more anti-bacterial corrosion performance than common stainless steel.
Above Electrochemical results shows; The effect of anti-bacteria stainless steel and Escherichia coli is after 2～14 days, and the open circuit potential mobility scale is-0.17～-0.15V, the mobility scale of polarization resistance is 43～152k Ω; The mobility scale of corrosion potential is-0.32-0.23V; All apparently higher than common stainless steel, microbial corrosion resistance can significantly strengthen by the force rate common stainless steel, shows that anti-bacteria stainless steel has excellent microbial corrosion resistance ability.
In addition, the inventive method is applicable to the anti-bacteria stainless steel of mentioning in the Chinese invention patent application (application number: 201010238697.8, denomination of invention: a kind of anti-bacteria stainless steel and heat treatment method thereof and application).
Embodiment 2:
Be with embodiment 1 difference:
In the present embodiment, the principal ingredient of anti-bacteria stainless steel is (wt) %:
C:0.04, Cr:15.30, Ni:1.18, Mn:10.78, Si:0.59, N:0.21, Cu:2.77, all the other are Fe.
Above-mentioned anti-bacteria stainless steel prepares as follows by conventional method:
(1) in vacuum smelting furnace, carry out anti-bacteria stainless steel and smelt, 1480 ℃ of refinings were carried out being cast into ingot casting after the magnetic agitation after 20 minutes;
Behind 2 hours homogenizing annealings of (2) 1150 ℃ of insulations, ingot casting is forged into bar-shaped or block sample.
The Technology for Heating Processing of above-mentioned anti-bacteria stainless steel is:
At 1040 ℃ of insulation 0.5h, fully solid solution is in matrix to make copper in the steel, and air cooling makes the copper in the steel be in hypersaturated state to room temperature.At 700 ℃ of insulation 6h, make oversaturated copper from steel, separate out the copper-rich phase of q.s then, last air cooling is to room temperature.
The bacterium that the present invention adopts is Escherichia coli, is provided by Chinese common micro-organisms DSMZ.
1, the preparation of sample
Prepare anti-bacteria stainless steel and the common stainless steel sample that is of a size of 10mm * 10mm * 3mm respectively with wire cutting method, clean, degrease are fixed on sample surfaces with copper conductor one end, and with the epoxy resin for cold edge, other end lead exposes then.After treating the epoxy resin drying, sample exposes other end surface after polishing, polishing, use the acetone soln ultrasonic cleaning, is positioned under the uviol lamp and sterilizes 30 minutes, and totally 3 groups of samples are subsequent use.
2, the preparation of bacteria suspension
With microbe growth to logarithmic growth after date, add the normal saline solution of the 8.5wt ‰ of 5ml with the test tube that fresh inclined-plane is housed, scrape the lower inclined plane bacterium, adopt turbidimetry that the bacteria suspension stepwise dilution is become 4 * 10 with oese
6The bacterium liquid of cfu/ml.
3, the effect of anti-bacteria stainless steel and bacterium
The stainless steel sample for preparing is positioned over is equipped with 4 * 10
6In the beaker of cfu/ml bacterium liquid, and submergence wherein, and the other end of copper conductor is exposed at outside the beaker, with the beaker good seal, is positioned in 35 ℃ the water-bath, cultivated 14 days.
4, the open circuit potential after the effect
After connecting with working electrode (anti-bacteria stainless steel sample), to electrode (Pt electrode) and contrast electrode (KCl saturated calomel electrode); Open the electrochemical apparatus power supply; Open V3-Studio software; Select the testing procedure of open circuit potential, the test duration of open circuit potential is decided to be 1 hour, measures the open circuit potential after anti-bacteria stainless steel and common stainless steel and Escherichia coli act on different time.Can be found out that by Fig. 4 anti-bacteria stainless steel and the open circuit potential of bacterial action after 14 days be-0.03V, be-0.06V that the passivating film that shows the common stainless steel surface is more easily by bacterial corrosion apparently higher than the open circuit potential of common stainless steel.
5, the electrochemical impedance after the effect
Select the mode determination of potentiostatic, the test specification of electrochemical impedance is made as 0.01～100000Hz, measures the impedance after anti-bacteria stainless steel and common stainless steel and Escherichia coli act on different time.Can find out that by Fig. 5 anti-bacteria stainless steel and the polarization resistance of bacterial action after 14 days are 328k Ω, and the common stainless steel polarization resistance is 118k Ω, shows that point corrosion takes place the passivating film on common stainless steel surface more easily.
6, the polarization curve after the effect
Select the mode determination of electrokinetic potential-polarization curve, the scope of corrosion potential is made as-0.4～0.6mV, and corrosion rate is 0.5mV/ second.Polarization curve according to behind anti-bacteria stainless steel and common stainless steel and the Escherichia coli effect different time can be found out; Anti-bacteria stainless steel and the corrosion potential of bacterial action after 14 days are-0.25V; And the corrosion potential of common stainless steel is-0.31V; Show that anti-bacteria stainless steel has excellent more anti-bacterial corrosion performance than common stainless steel, as shown in Figure 6.
Above Electrochemical results shows that anti-bacteria stainless steel and Escherichia coli effect are after 14 days, and open circuit potential is-0.03V; Polarization resistance is 328k Ω; Corrosion potential is-0.25V that all than the respective value height of common stainless steel, the microbial corrosion resistance ability obviously strengthens than common stainless steel; Bacterium reduces on its surface significantly, shows that anti-bacteria stainless steel has excellent microbial corrosion resistance ability.
Embodiment result shows that the present invention utilizes the microbial corrosion resistance situation behind electrochemical means test austenite antimicrobial stainless steel and the bacterial action different time, and then judges the microbial corrosion resistance ability of anti-bacteria stainless steel material.The present invention utilize open circuit potential, electrochemical impedance and the polarization curve behind electrochemical means test austenite antimicrobial stainless steel and the bacterial action different time estimate anti-bacteria stainless steel microbial corrosion resistance can, be a kind of reliably, anti-bacteria stainless steel microbial corrosion resistance ability detection method easily.
Claims (6)
1. a method of utilizing electrochemical means test anti-bacteria stainless steel microbial corrosion resistance ability is characterized in that: at first, with microbe growth to logarithmic growth after date, be mixed with 4～6 * 10
6The bacteria suspension of cfu/ml; Then, connect the surface of anti-bacteria stainless steel and common stainless steel one end respectively, and fix with epoxy resin with copper conductor; The other end of copper conductor and sample exposes outside epoxy resin, treat the epoxy resin drying after, the polishing, the polishing sample; Adopt exposed sample one end of acetone ultrasonic cleaning, be positioned over uviol lamp under after the sterilization, be immersed in the bacterium liquid of this concentration of dropping; Cultivation temperature is 35～37 ℃, incubation time 2～14 days; Then, utilize open circuit potential, electrochemical impedance and polarization curve after electrochemical means is tested anti-bacteria stainless steel and common stainless steel and bacterial action different time, and then estimate the microbial corrosion resistance ability of anti-bacteria stainless steel.
2. according to the described method of utilizing electrochemical means test anti-bacteria stainless steel microbial corrosion resistance ability of claim 1, it is characterized in that the bacterium of employing is respectively Escherichia coli and staphylococcus aureus.
According to claim 1 described utilize electrochemical means test anti-bacteria stainless steel microbial corrosion resistance can method, it is characterized in that, describedly be mixed with 4～6 * 10
6The bacteria suspension of cfu/ml adopts the turbidimetry stepwise dilution to obtain.
4. according to the described method of utilizing electrochemical means test anti-bacteria stainless steel microbial corrosion resistance ability of claim 1, it is characterized in that the test duration of open circuit potential is 0.5～2 hour.
5. according to the described method of utilizing electrochemical means test anti-bacteria stainless steel microbial corrosion resistance ability of claim 1, it is characterized in that the test specification of electrochemical impedance is 0.01～100000Hz.
6. according to the described method of utilizing electrochemical means test anti-bacteria stainless steel microbial corrosion resistance ability of claim 1, it is characterized in that the corrosion potential test specification of polarization curve is-0.4～0.6V, sweep speed is 0.4～0.6mV/ second.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103543097A (en) * | 2013-11-05 | 2014-01-29 | 广东电网公司电力科学研究院 | Electrochemical method for determining inter-crystalline corrosion sensibility of austenitic stainless steel |
| CN112725401A (en) * | 2020-12-08 | 2021-04-30 | 上海航天设备制造总厂有限公司 | Method and device for testing microbial corrosion of aerospace metal material in microgravity-resistant environment |
| CN113029930A (en) * | 2021-03-16 | 2021-06-25 | 中国船舶重工集团公司第七二五研究所 | Corrosion test method for marine fouling organisms in real sea environment |
| CN115522204A (en) * | 2022-09-26 | 2022-12-27 | 中国科学院金属研究所 | Anode polarization method for inhibiting microbial corrosion of ocean engineering equipment |
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| CN2741038Y (en) * | 2004-11-13 | 2005-11-16 | 中国海洋大学 | Corrosion tester of fluid media |
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| CN2741038Y (en) * | 2004-11-13 | 2005-11-16 | 中国海洋大学 | Corrosion tester of fluid media |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103543097A (en) * | 2013-11-05 | 2014-01-29 | 广东电网公司电力科学研究院 | Electrochemical method for determining inter-crystalline corrosion sensibility of austenitic stainless steel |
| CN112725401A (en) * | 2020-12-08 | 2021-04-30 | 上海航天设备制造总厂有限公司 | Method and device for testing microbial corrosion of aerospace metal material in microgravity-resistant environment |
| CN112725401B (en) * | 2020-12-08 | 2023-09-01 | 上海航天设备制造总厂有限公司 | Method and device for testing microbial corrosion of aerospace metal material in microgravity resistant environment |
| CN113029930A (en) * | 2021-03-16 | 2021-06-25 | 中国船舶重工集团公司第七二五研究所 | Corrosion test method for marine fouling organisms in real sea environment |
| CN115522204A (en) * | 2022-09-26 | 2022-12-27 | 中国科学院金属研究所 | Anode polarization method for inhibiting microbial corrosion of ocean engineering equipment |
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