CN114923845A - Nickel-based alloy intercrystalline corrosion sensitivity detection method - Google Patents
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Abstract
The invention provides a method for detecting intergranular corrosion sensitivity of a nickel-based alloy, which is used for detecting the intergranular corrosion sensitivity of the nickel-based alloy by adopting a self-made corrosion test solution and a double-ring electrochemical potentiodynamic reactivation measurement method.
Description
Technical Field
The invention belongs to the technical field of chemical industry, relates to alloy intercrystalline corrosion detection, and particularly relates to a nickel-based alloy intercrystalline corrosion sensitivity detection method.
Background
Intergranular corrosion is the state of localized corrosion damage that occurs and progresses in a particular corrosive environment along or next to the grain boundaries of a material. The intercrystalline corrosion is very harmful, and the intercrystalline bonding force is greatly lost, so that the strength of the material is almost completely lost, and therefore, the intercrystalline corrosion resistance is one of important performance parameter indexes of the nickel-based alloy.
Among the various intercrystalline corrosion performance detection methods, the double-ring electrochemical potentiodynamic reactivation measurement method is a common nondestructive detection method; at present, a common standard method for detecting the double-ring electrochemical potentiodynamic reactivation measurement method of the nickel-based alloy is GB 29088 + 2012 'measurement method for corrosion double-ring electrochemical potentiodynamic reactivation of metals and alloys'. However, in actual testing, many high-grade nickel-based alloys (e.g., 625, 825) fail to detect activation and reactivation peaks under such corrosion conditions, and thus it is difficult to assess the intergranular corrosion susceptibility of nickel-based alloys according to standard methods.
Disclosure of Invention
The invention aims to provide a method for detecting the intergranular corrosion sensitivity of a nickel-based alloy, which can quickly, accurately and reliably detect the intergranular corrosion resistance of the nickel-based alloy.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a nickel-based alloy intercrystalline corrosion sensitivity detection method comprises the following steps:
the method comprises the following steps: sensitizing the nickel-based alloy to be tested, and preparing the nickel-based alloy with the working area of 1cm 2 Cleaning the electrochemical sample for standby;
step two: preparing a corrosion test solution, and preparing test conditions for intercrystalline corrosion sensitivity detection; the corrosion test solution is a mixed aqueous solution of sulfuric acid, hydrochloric acid and magnesium chloride, wherein the concentration of the sulfuric acid is 0.5-2mol/L, the concentration of the hydrochloric acid is 1-3 mol/L and the concentration of the magnesium chloride is 0.3-1 mol/L;
step three: and (3) placing the three-electrode system in a corrosion test solution with a constant temperature of 30 ℃ for soaking for 5-10 min to stabilize the open-circuit potential of the working electrode, then anodizing to a passivation area at a scanning rate of 6V/h, and using an antimony electrode as a reference electrode for detection, wherein the passivation potential range is 300-500 mV. After reaching the passivation potential, the potential is reversely reduced to the initial open-circuit potential at the same scanning speed;
step four: measuring reactivation scan peak currentI r And corresponding activation scan peak currentI p The ratio of the two is obtained.
In the first step, after the nickel-based alloy to be tested is sensitized, epoxy resin is used for feeding a sample of a welding leadPackaging, wet grinding the packaged sample by using water sand paper, removing oil by using ethanol or acetone after grinding, cleaning by using deionized water, drying, sealing a gap between the sample and epoxy resin by using paraffin, and keeping 1cm 2 The working area of (a). At least three replicates of each set of experiments were taken.
In the second step, the corrosion test solution is an aqueous solution prepared from deionized water, analytically pure concentrated sulfuric acid, concentrated hydrochloric acid and magnesium chloride; the configuration method comprises the following steps:
firstly, taking 600mL of deionized water by using a 1L measuring cylinder, and pouring the deionized water into a beaker;
then, 27.2mL-109mL of sulfuric acid with the concentration of 95% -98% is taken by using a 200mL measuring cylinder and a 5mL liquid-transferring gun and slowly poured into a beaker to avoid the solution from boiling due to heat;
then, taking 84.5-253 mL of hydrochloric acid solution by using a 500mL measuring cylinder and a 5mL liquid transfer gun, and pouring the hydrochloric acid solution with the concentration of 36-38% into a beaker;
and finally, adding 61g-203g of magnesium chloride hexahydrate into the sulfuric acid-hydrochloric acid solution, stirring until the magnesium chloride hexahydrate is completely dissolved, pouring the solution into a 1L volumetric flask after the temperature of the solution is reduced to the room temperature, and adding deionized water to the scale of the volumetric flask for later use.
The test condition is that the test container is made of glass and plastic; the temperature keeping system selects a constant temperature water bath and a constant temperature box; a Bio-Logic SP150 electrochemical workstation is selected for the electrochemical testing system, has a potentiodynamic potential detection function and can complete the potentiodynamic potential activation measurement work.
In the third step, the corrosion test solution is preheated at constant temperature by adopting a constant temperature box or a constant temperature water bath kettle; the working electrode of the three-electrode system is a nickel-based alloy sample, the auxiliary electrode is a platinum electrode, and the reference electrode is an antimony electrode; the passivation potential is determined by a potentiodynamic polarization curve of the nickel-based alloy in a corrosion test solution.
In the fourth step, two peak currents can be obtained on a curve obtained by detection, and then the activation ratio is calculated to judge the intergranular corrosion sensitivity of the nickel-based alloy.
The beneficial effects of the invention are: the method for evaluating the intergranular corrosion sensitivity of the nickel-based alloy has the advantages of simple operation, quick result display, easy popularization and application in a laboratory and accurate and reliable detection result.
Drawings
FIG. 1 shows 825 samples of the plate material at 1.5mol/L H 2 SO 4 + 2mol/L HCl + 0.5mol/L MgCl 2 Dual ring electrochemical potentiodynamic reactivation curves in solution.
FIG. 2 shows 800 plate samples at 2mol/L H 2 SO 4 + 2mol/L HCl + 1mol/L MgCl 2 Bi-cyclic electrochemical potentiodynamic reactivation curves in solution.
Detailed Description
In order to facilitate the understanding of the invention by the skilled person, the invention is further illustrated by the following examples:
example 1
The method of the invention is adopted to carry out intercrystalline corrosion sensitivity detection on 825 plate samples:
the method comprises the following steps: sensitizing a 825 plate sample at the sensitization temperature of 650 +/-10 ℃ for 2 hours, welding a lead on the sensitized sample, then packaging the sample with epoxy resin, polishing the sample, removing oil with absolute ethyl alcohol after polishing, then cleaning the sample with deionized water and drying the sample; then sealing the gap between the sample and the epoxy resin by using paraffin so as to avoid the occurrence of gap corrosion and keep 1cm 2 The working area of (a);
step two: 1.5mol/L H is prepared by deionized water, analytically pure concentrated sulfuric acid, concentrated hydrochloric acid and magnesium chloride 2 SO 4 + 2mol/L HCl + 0.5mol/L MgCl 2 The test solution of (1). Heating the test solution to 30 ℃ by adopting a constant-temperature water bath kettle;
step three: connecting a sample, a platinum electrode and an antimony electrode to an electrochemical workstation, soaking the electrochemical workstation in a solution for 5-10 min until the system is stable, then starting measurement, scanning the sample to 500mV (vs. antimony electrode) from an open circuit potential, wherein the code scanning rate is 6V/s, and scanning to the initial open circuit potential at the same rate in a reverse direction after the sample reaches 500 mV;
step four: obtaining reactivation scan peak current from measured dual potentiodynamic reactivation curvesI r And corresponding activation scan peaksValue currentI p The ratio of the two is 0.37, and the intercrystalline corrosion sensitivity of the alloy can be determined; the double-loop electrochemical potentiodynamic reactivation curve is shown in FIG. 1.
Then, deionized water, analytically pure concentrated sulfuric acid and potassium thiocyanate are utilized to prepare 0.5mol/L H 2 SO 4 + 0.01mol/L of KSCN in the test solution; carrying out corrosion sensitivity detection on the 825 plate sample in the same process again by using the test solution; the detection result shows that 825 alloy has no activation peak and reactivation peak in the corrosion environment, and whether the alloy has intercrystalline corrosion sensitivity cannot be judged.
Example 2
The method of the invention is adopted to carry out intercrystalline corrosion sensitivity detection on 800 plate samples:
the method comprises the following steps: a800 plate sample is selected as a research object, and before the test, 825 sensitization treatment is carried out, wherein the sensitization system is 700 +/-10 ℃, and the temperature is kept for 10 min. Welding a lead on the sensitized sample, then packaging the sample with epoxy resin, polishing, removing oil with absolute ethyl alcohol after polishing, then cleaning with deionized water and drying. Then sealing the gap between the sample and the epoxy resin by using paraffin so as to avoid the occurrence of gap corrosion and keep 1cm 2 The working area of (a);
step two: preparing 2mol/L H by using deionized water, analytically pure concentrated sulfuric acid, concentrated hydrochloric acid and magnesium chloride 2 SO 4 + 2mol/L HCl + 1mol/L MgCl 2 The test solution of (1). Heating the test solution to 30 ℃ by adopting a constant-temperature water bath kettle;
step three: and connecting the sample, the platinum electrode and the antimony electrode to an electrochemical workstation, soaking the sample, the platinum electrode and the antimony electrode in the solution for 5-10 min until the system is stable, and then starting to measure. Scanning a sample to 300mV (vs. antimony electrode) from an open circuit potential, wherein the code scanning rate is 6V/s, and after the sample reaches 300mV, reversely scanning to the initial open circuit potential at the same rate;
step four: obtaining reactivation scan peak current from measured dual potentiodynamic reactivation curvesI r And corresponding activation sweep peak currentI p The ratio of the two is 0.08, and the alloy can be determined to have intergranular corrosionSusceptibility to corrosion; the double loop electrochemical potentiodynamic reactivation curve is shown in FIG. 2.
Then, deionized water, analytically pure concentrated sulfuric acid and potassium thiocyanate are utilized to prepare 0.5mol/L H 2 SO 4 + 0.01mol/L KSCN test solution; the test solution is adopted to carry out corrosion sensitivity detection on the 800 plate sample again in the same process; the detection result shows that 800 alloy has no activation peak and reactivation peak in the corrosion environment, and whether the alloy has intercrystalline corrosion sensitivity can not be judged.
Claims (4)
1. A nickel-based alloy intercrystalline corrosion sensitivity detection method is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: sensitizing the nickel-based alloy to be tested, and preparing the nickel-based alloy with the working area of 1cm 2 Cleaning the electrochemical sample for standby;
step two: preparing a corrosion test solution, and preparing test conditions for intercrystalline corrosion sensitivity detection; the corrosion test solution is a mixed aqueous solution of sulfuric acid, hydrochloric acid and magnesium chloride, wherein the concentration of the sulfuric acid is 0.5-2mol/L, the concentration of the hydrochloric acid is 1-3 mol/L and the concentration of the magnesium chloride is 0.3-1 mol/L;
step three: placing the three-electrode system in a corrosion test solution with a constant temperature of 30 ℃ for soaking for 5-10 min to stabilize the open-circuit potential of a working electrode, then anodizing the working electrode to a passivation area at a scanning speed of 6V/h, using an antimony electrode as a reference electrode for detection, wherein the passivation potential range is 300-500 mV, and after reaching the passivation potential, reversely reducing the potential to the initial open-circuit potential at the same scanning speed;
step four: measuring reactivation scan peak currentI r And corresponding activation sweep peak currentI p Obtaining the ratio of the two, and judging the intergranular corrosion sensitivity of the nickel-based alloy.
2. The method for detecting the sensitivity of the nickel-based alloy to the intergranular corrosion according to claim 1, wherein the method comprises the following steps: in the first step, after the nickel-based alloy to be tested is sensitized, a sample of the welding wire is encapsulated by epoxy resin, and water is adoptedWet grinding with abrasive paper to polish the packaged sample, removing oil with ethanol or acetone, cleaning with deionized water, drying, sealing the gap between the sample and epoxy resin with paraffin wax, and keeping 1cm 2 At least three parallel samples were taken for each set of tests.
3. The method for detecting sensitivity to intergranular corrosion of a nickel-based alloy according to claim 1, wherein the method comprises the following steps: in the second step, the corrosion test solution is an aqueous solution prepared from deionized water, analytically pure concentrated sulfuric acid, concentrated hydrochloric acid and magnesium chloride, and the preparation method comprises the following steps:
firstly, taking 600mL of deionized water by using a 1L measuring cylinder, and pouring the deionized water into a beaker;
then, 27.2-109 mL of sulfuric acid is taken by using a 200mL measuring cylinder and a 5mL liquid transfer gun, the concentration of the sulfuric acid is 95-98%, and the sulfuric acid is slowly poured into a beaker to avoid the solution from boiling by heat;
then, taking 84.5-253 mL of hydrochloric acid solution by using a 500mL measuring cylinder and a 5mL liquid transfer gun, and pouring the hydrochloric acid solution with the concentration of 36-38% into a beaker;
finally, adding 61g-203g of magnesium chloride hexahydrate into a sulfuric acid-hydrochloric acid solution, stirring until the magnesium chloride hexahydrate is completely dissolved, pouring the solution into a 1L volumetric flask after the temperature of the solution is reduced to room temperature, and adding deionized water to the scale of the volumetric flask for later use;
the test conditions for preparing the intergranular corrosion sensitivity detection include: the test container is made of glass and plastic; the temperature keeping system selects a constant temperature water bath and a constant temperature box; the electrochemical system for testing has the function of electrokinetic potential detection and can complete the electrokinetic potential activation measurement work.
4. The method for detecting the sensitivity of the nickel-based alloy to the intergranular corrosion according to claim 1, wherein the method comprises the following steps: in the third step, the corrosion test solution is preheated at constant temperature by adopting a constant temperature box or a constant temperature water bath kettle; the working electrode of the three-electrode system is a nickel-based alloy sample, the auxiliary electrode is a platinum electrode, and the reference electrode is an antimony electrode; the passivation potential is determined by a potentiodynamic polarization curve of the nickel-based alloy in a corrosion test solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115753579A (en) * | 2022-11-24 | 2023-03-07 | 江苏隆达超合金股份有限公司 | Nickel-based alloy pipe ferric sulfate intergranular corrosion test method |
| CN115808458A (en) * | 2022-11-21 | 2023-03-17 | 华电能源股份有限公司富拉尔基发电厂 | Method for evaluating aging state of heat-resistant steel based on electrochemical technology |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115808458A (en) * | 2022-11-21 | 2023-03-17 | 华电能源股份有限公司富拉尔基发电厂 | Method for evaluating aging state of heat-resistant steel based on electrochemical technology |
| CN115753579A (en) * | 2022-11-24 | 2023-03-07 | 江苏隆达超合金股份有限公司 | Nickel-based alloy pipe ferric sulfate intergranular corrosion test method |
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