CN110346274A - A kind of corrosion proof electrochemistry experiment method of test polar region marine steel - Google Patents
A kind of corrosion proof electrochemistry experiment method of test polar region marine steel Download PDFInfo
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- CN110346274A CN110346274A CN201910602816.4A CN201910602816A CN110346274A CN 110346274 A CN110346274 A CN 110346274A CN 201910602816 A CN201910602816 A CN 201910602816A CN 110346274 A CN110346274 A CN 110346274A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
Abstract
The invention discloses a kind of corrosion proof electrochemistry experiment methods of test polar region marine steel, comprising the following steps: (1) prepares sample；(2) prepare testing liquid；(3) electrochemical appliance is assembled；(4) it tests；(5) data processing；(6) data validity determines.The present invention measures the saturation current density intensity of anodic dissolution processes of the polar ocean steel in simulation polar region marine corrosion medium by constant potential, and then evaluates its corrosion resistance, can fast and effeciently detect the corrosion resistance of polar ocean steel；Acceptance criterion is formulated to the availability deciding of parallel test data, the selection for parallel test data provides direct basis.
Description
Technical field
The present invention relates to metallic material corrosions and protection detection field, and in particular to a kind of test polar region marine steel is anti-corrosion
The electrochemistry experiment method of property.
Background technique
The steel material local environment very severe that ship, harbour, drilling platforms in polar ocean environment etc. use, because
To apply in the cold sea area of temperature to -60 DEG C, environment is complicated, undergos ultralow temperature, ice and snow abrasion, and low temperature stormy waves corrodes, freezes
Soil shock etc., and the chloride environment of polar ocean can also promote the corrosion of steel.To guarantee ship, harbour and drilling platforms
Deng the service life of equipment and facility, the corrosion resisting property of effectively evaluating polar ocean steel is particularly important.
Patent CN109187322 describes a kind of pitting corrosion evaluation method of polar ocean steel, by special corruption
Erosion liquid corrode point corrosion pit out, this method is only capable of can be carried out evaluation for the local corrosion of polar region steel, integrate corrosive nature without
Method is evaluated.Electrochemical test method is one of the best approach of quickly and effectively detection metal material corrosion resistance, but
The tolerance interval for providing its parallel sample test result is not known in various national standards.
Summary of the invention
Goal of the invention: the present invention proposes a kind of corrosion proof electrochemistry experiment method of test polar region marine steel.
Technical solution: the technical scheme adopted by the invention is that a kind of marine steel corrosion proof electrochemistry in test polar region is real
Proved recipe method, comprising the following steps: (1) prepare sample: workspace is the region that sample is directly contacted with corrosive media, remaining area
Domain is separated with inert material；(2) prepare testing liquid: sodium chloride and magnesium chloride hexahydrate being taken to be dissolved in deionized water, test temperature
Degree is 21.5~22.5 DEG C；(3) it assembles electrochemical appliance: being filled by electrolytic cell, working electrode, reference electrode, auxiliary electrode, clamping
It sets and is formed with potentiostat；(4) it tests: setting constant potential polarization working electrode potential mode for potentiostat in step (3),
When testing corrosive medium, the time is realized when the sample retention time is greater than stable saturation current value, measures stable saturation current
Value；(5) the saturation current value of step (4) data processing: is obtained into saturation current density divided by workspace areal calculation；(6) data
Availability deciding: the judgement formula of acceptance criterion is as follows:
Wherein, jiFor the saturation current density of each parallel test, jmaxFor the maximum value in parallel test numerical value；jminFor
Minimum value in parallel test numerical value；N is the quantity of parallel test；СR0,95(n) be Р=0.95 when critical coefficient；It is described
The condition of the data fit acceptance criterion of parallel test takes the arithmetic mean of instantaneous value of the saturation current density of parallel test as measurement
As a result；The data of the parallel test do not meet the condition of acceptance criterion, carry out supplement test, repeat step (1) to (6), institute
The condition that data do not meet acceptance criterion still is obtained, then takes the median of the saturation current density of parallel test as measurement result.
Preferably, workspace minimum area is 1cm in the step (1)2。
Preferably, inert material is atoleine or epoxy resin in the step (1).
Preferably, in the step (3) working electrode workspace surface to the distance between reference electrode be 25~
27mm, the distance between working electrode and auxiliary electrode are 3~5mm.
Preferably, the longest duration of test runs of sample is 3600 seconds in the step (4), and sample is satisfied in 1000 seconds
It is less than 0.10mA/cm with current density change2, stop test, measure stable saturation current value.
Preferably, CR in the step (6)0,95(n)=f (n) σr, wherein σrFor periodicity factor, numeric reference
Table 1；F (n) is critical range coefficient, and numerical value depends on the sample size of test, reference table 2.
The meter characteristic value of 1 data of table
2 critical range coefficient f (n) of table
| n | f(n) | n | f(n) |
| 3 | 3.3 | 7 | 4.2 |
| 4 | 3.6 | 8 | 4.3 |
| 5 | 3.9 | 9 | 4.4 |
| 6 | 4.0 | 10 | 4.5 |
Preferably, n is at least with a batch of 3 samples in the step (6).
Preferably, the result that supplement is tested in the step (6) does not meet the condition of acceptance criterion still, then takes all parallel
The median of the saturation current density of test is as measurement result.
The present invention passes through the anodic dissolution processes in constant potential measurement polar ocean with punching block lopar marine corrosion medium
Saturation current density intensity, and then evaluate its corrosion resistance.Specifically, sample stable state saturation current density depends in electrolyte
In the activity intensity of its surface-active corrosion area, constant potential E=-300mV (saturation Ag/AgCl electricity is applied to working electrode
Pole), the electric current rapid growth in electrode system, that is, the anodic dissolution processes of sample surfaces, reach stable after a period of time,
Electric current stops increasing over time or slightly increase, and current steady state value is named as " saturation current ", reflects test
Sample anodes dissolution maximum intensity state, the saturation current value of unit area is known as saturation current density, and as test is surveyed
Amount is as a result, be used for the evaluation parameter of sample etches stability.
The utility model has the advantages that the present invention can the corrosion resistance quickly and effectively to polar ocean steel can be carried out detection；To flat
The availability deciding of row test data has formulated acceptance criterion, and the selection for parallel test data provides direct basis.
Detailed description of the invention
Fig. 1 is test data figure of the invention.
Specific embodiment
Further description of the technical solution of the present invention with reference to the accompanying drawings and examples.
Embodiment 1
Test the electrochemical corrosion performance of polar region ship steel E36 (smelting process 1), comprising the following steps:
(1) it prepares sample: selecting sample workspace area for 1.0cm2, remaining surface epoxy resin plastic packaging, sample
Quantity is 3；
(2) it prepares testing liquid: analyzing the sodium chloride of pure rank using the electronic balance weighing 9.926g of 0.001g precision
(NaCl) and 3.416g analyzes the magnesium chloride hexahydrate (MgCl of pure rank2·6H2O it) is dissolved in 1000ml deionized water；By solution
It pours into electrolytic cell, is put into thermostat water bath, adjust the temperature to 21.5~22.5 DEG C；
(3) assemble electrochemical appliance: auxiliary electrode is platinum plate electrode, reference electrode is saturation Ag/AgCl electrode, work electricity
Pole workspace surface is 27mm to the distance between reference electrode, and the distance between working electrode and auxiliary electrode are 5mm, by three
Electrode accesses VSP electrochemical workstation；
(4) test: the test pattern of setting VSP electrochemical workstation is constant potential polarization working electrode potential mode, if
Setting constant potential is E=-300mV (saturation Ag/AgCl electrode), and the longest duration of test runs of sample is 3600 seconds；If saturation
The stabilization time of electric current is shorter, then can shorten duration of test runs；If current density change is less than 0.10mA/ in 1000 seconds
cm2, then can be considered stabling current density and stop measuring, successively 3 Duplicate Samples tests are completed, measure stable saturation current
Value；
(5) it is close that saturation current value that step (4) measures divided by workspace areal calculation data processing: is obtained into saturation current
Degree, obtains the final saturation current density numerical value of 3 Duplicate Samples are as follows: 5.70mA/cm2、5.99mA/cm2、5.85mA/cm2,
Data graphs are shown in Fig. 1.
(6) data validity determines: three numerical value of step (5) being brought into the judgement formula left end of acceptance criterion, are calculated
Obtain 4.96；As n=3, the judgement right of formula numerical value of acceptance criterion is 9.9；This time three numerical value of test meet receiving
The condition of criterion, the saturation current density for finally obtaining sample is the arithmetic mean of instantaneous value 5.85mA/cm of three numerical value2。
Embodiment 2
Test the electrochemical corrosion performance of polar region ship steel E36 (smelting process 2), comprising the following steps:
(1)~(4) are same as Example 1；
(5) the saturation current value that step (4) measures is obtained into saturation current density divided by workspace areal calculation, obtains 3
The final saturation current density numerical value of Duplicate Samples are as follows: 7.17mA/cm2、6.98mA/cm2、7.72mA/cm2；
(6) data validity determines: three numerical value of step (5) being brought into the judgement formula left end of acceptance criterion, are calculated
Obtain 10.15；As n=3, the judgement right of formula numerical value of acceptance criterion is 9.9；This time three numerical value of test do not meet receiving
The condition of criterion；
(7) it supplement test: repeats step (1)~(4) and obtains the saturation current density of the 4th test to be 7.54mA/cm2,
By four test results bring into acceptance criterion formula left end calculate 10.06, as n=4, acceptance criterion right end numerical value 10.8,
Four data fit acceptance criterions, the saturation current density for finally obtaining sample is the arithmetic mean of instantaneous value 7.35mA/ of four numerical value
cm2。
Embodiment 3
Test the electrochemical corrosion performance of common ship steel A36, comprising the following steps:
(1)~(4) are same as Example 1；
(5) the saturation current value that step (4) measures is obtained into saturation current density divided by workspace areal calculation, obtains 3
The final saturation current density numerical value of Duplicate Samples are as follows: 9.68mA/cm2、9.19mA/cm2、8.57mA/cm2；
(6) data validity determines: three numerical value of step (5) being brought into the judgement formula left end of acceptance criterion, are calculated
Obtain 12.14；As n=3, the judgement right of formula numerical value of acceptance criterion is 9.9；This time three numerical value of test do not meet receiving
The condition of criterion；
(7) it supplement test: repeats step (1)~(4) and obtains the saturation current density of the 4th test to be 8.95mA/cm2,
By four test results bring into acceptance criterion formula left end calculate 12.20, as n=4, acceptance criterion right end numerical value 10.8,
Four times data do not meet acceptance criterion, therefore take the median 9.07mA/cm of four test bits2As final result.
Embodiment 1 to 3 may determine that the saturation current density value of polar region ship steel E36 (smelting process 1) is minimum, from
And illustrate that its corrosion resistance is best.
Claims (8)
1. a kind of corrosion proof electrochemistry experiment method of test polar region marine steel, it is characterised in that: the following steps are included:
(1) prepare sample: workspace is the region that sample is directly contacted with corrosive media, remaining region inert material point
From；
(2) it prepares testing liquid: sodium chloride and magnesium chloride hexahydrate being taken to be dissolved in deionized water, test temperature is 21.5~22.5
℃；
(3) electrochemical appliance is assembled: by electrolytic cell, working electrode, reference electrode, auxiliary electrode, clamping device and potentiostat
Composition；
(4) it tests: setting constant potential polarization working electrode potential mode for potentiostat in step (3), test corrosive medium
When, the time is realized when the sample retention time is greater than stable saturation current value, measures stable saturation current value；
(5) the saturation current value of step (4) data processing: is obtained into saturation current density divided by workspace areal calculation；
(6) data validity determines: the judgement formula of acceptance criterion is as follows:
Wherein, jiFor the saturation current density of each parallel test, jmaxFor the maximum value in parallel test numerical value；jminIt is parallel
Minimum value in test bit；N is the quantity of parallel test；СR0,95(n) be Р=0.95 when critical coefficient；
The condition of the data fit acceptance criterion of the parallel test, takes the arithmetic mean of instantaneous value of the saturation current density of parallel test
As measurement result；The data of the parallel test do not meet the condition of acceptance criterion, carry out supplement test, repeat step (1)
To (6), the data obtained does not meet the condition of acceptance criterion still, then takes the median of the saturation current density of parallel test as survey
Measure result.
2. a kind of corrosion proof electrochemistry experiment method of test polar region marine steel according to claim 1, feature exist
In: workspace minimum area is 1cm in the step (1)2。
3. a kind of corrosion proof electrochemistry experiment method of test polar region marine steel according to claim 1, feature exist
In: inert material is atoleine or epoxy resin in the step (1).
4. a kind of corrosion proof electrochemistry experiment method of test polar region marine steel according to claim 1, feature exist
In: in the step (3) the workspace surface of working electrode to the distance between reference electrode be 25~27mm, working electrode with
The distance between auxiliary electrode is 3~5mm.
5. a kind of corrosion proof electrochemistry experiment method of test polar region marine steel according to claim 1, feature exist
In: constant potential is set as E=-300mV in the step (4).
6. a kind of corrosion proof electrochemistry experiment method of test polar region marine steel according to claim 1, feature exist
In: the longest duration of test runs of sample is 3600 seconds in the step (4), and sample saturation current density in 1000 seconds becomes
Change and is less than 0.10mA/cm2, stop test, measure stable saturation current value.
7. a kind of corrosion proof electrochemistry experiment method of test polar region marine steel according to claim 1, feature exist
In: CR in the step (6)0,95(n)=f (n) σr,
Wherein, σrFor periodicity factor；F (n) is critical range coefficient, and numerical value depends on the sample size of test.
8. a kind of corrosion proof electrochemistry experiment method of test polar region marine steel according to claim 1, feature exist
In: n is at least with a batch of 3 samples in the step (6).
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