CN101975743A - Method for testing inter-grain corrosion performance of austenitic heat-resistant steel after aging at 650 DEG C - Google Patents

Method for testing inter-grain corrosion performance of austenitic heat-resistant steel after aging at 650 DEG C Download PDF

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CN101975743A
CN101975743A CN 201010557737 CN201010557737A CN101975743A CN 101975743 A CN101975743 A CN 101975743A CN 201010557737 CN201010557737 CN 201010557737 CN 201010557737 A CN201010557737 A CN 201010557737A CN 101975743 A CN101975743 A CN 101975743A
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steel
super304h
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austenitic heat
corrosion performance
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CN101975743B (en
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李新梅
张忠文
杜宝帅
邓化凌
彭宪友
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State Grid Corp of China SGCC
Electric Power Research Institute of State Grid Shandong Electric Power Co Ltd
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Abstract

The invention relates to a method for testing the inter-grain corrosion performance of austenitic heat-resistant steel after aging at 650 DEG C. The method comprises the following steps of: (1) enabling a quantitative relationship between the reactivation rate of austenitic heat-resistant steel Super304H and the relative precipitation amount of M23C6: Ra=0.0493M3-0.0998M2+0.3377M+0.0033, wherein Ra is the reactivation rate, and M is the relative precipitation amount of the M23C6 in the tissue and is calculated according to a ratio of the integrated intensity of the strongest peak of a precipitated phase of the M23C6 to the integrated intensity of the strongest peak of a substrate in X-ray diffraction; and (2) taking Super304H steel samples in different operation times, measuring the relative precipitation amount of the M23C6 in the tissue, substituting in the quantitative relationship formula in the step (1) to calculate the Ra so as to obtain the inter-grain corrosion performance of the Super304H steel. The invention can rapidly and accurately know the change of the inter-grain corrosion performance of the Super304H steel after operation, can avoid damage caused by sampling steel boiler parts, know the inter-grain corrosion degree of the steel in time, acknowledge the change trend of the inter-grain corrosion of the steel and provide a reference for the safety supervision of the boiler parts.

Description

Test the method for austenitic heat-resistance steel intercrystalline corrosion performance after 650 ℃ of timeliness
Technical field
The present invention relates to a kind of method of tested steel intercrystalline corrosion performance, the method for austenitic heat-resistance steel intercrystalline corrosion performance belongs to the metal material technical field after 650 ℃ of timeliness of especially a kind of test.
Background technology
Austenitic stainless steel often is selected in the corrosion environment and uses at present, so corrosion resistance is the important performance index of one item.The characteristics of intercrystalline corrosion are to begin corrosion along crystal boundary, make intercrystalline forfeiture adhesion.According to " carbonide is separated out and caused the poor chromium of intergranular " theory, in conjunction with M 23C 6Time-temperature-separate out figure and time-temperature-corrosion diagram as can be known, 450 ℃ of-850 ℃ of temperature ranges because M 23C 6Sening as an envoy to along partial crystallization produces poor Cr phenomenon around the crystal boundary, causes that intercrystalline corrosion takes place less than the lowest limit 11.5% of its corrosion resistance the content of Cr around the crystal boundary.Intercrystalline corrosion also can be accelerated general corrosion, and therefore, the research of Intergranular Corrosion of Austenitic Stainless Steel is one of Recent study emphasis.The evaluation method of intercrystalline corrosion has a variety of, as oxalic acid etch method, iron sulfate-sulfuric acid etch method, natal etch method, copper-copper sulphate-sulfuric acid process and copper-copper sulphate-50% sulfuric acid process etc., but the quantitative evaluation intercrystalline corrosion sensitivity level that these methods have, but it is consuming time long and be destructive, quick, the nondestructive characteristics of having of having, but be a kind of quilitative method.Galvanochemistry potentiokinetic reactivation technology has accurately quantitative characteristics, utilizes the reactivation rate can characterize the intercrystalline corrosion performance quickly and easily.
In ultra-supercritical boiler, superheater and the reheater tube environmental baseline of living in that is in operation is the most abominable, its side of waring oneself in front of a fire causes heavy corrosion because of sodium potassium sulfate exists, and the temperature range of operation of Super304H steel just is in the strongest temperature range of sodium potassium sulfate corrosion (600 ℃-750 ℃), so the intercrystalline corrosion performance of research Super304H steel under the high-temperature aging condition has important practical significance.Therefore under running temperature, need to propose a kind of method of testing Super304H steel intercrystalline corrosion performance, grasps the situation of change of Super304H steel intercrystalline corrosion susceptibility after 650 ℃ of timeliness, thus the realization effective supervision.
Summary of the invention
The objective of the invention is for overcoming above-mentioned the deficiencies in the prior art, provide a kind of after 650 ℃ of timeliness of a kind of quantitative test are provided under the prerequisite of not destroying test specimen the method for austenitic heat-resistance steel intercrystalline corrosion performance, by measuring M in the tissue 23C 6Quantity realize the method for austenitic heat-resistance steel intercrystalline corrosion performance after 650 ℃ of timeliness.
For achieving the above object, the present invention adopts following technical proposals:
The method of austenitic heat-resistance steel intercrystalline corrosion performance after 650 ℃ of timeliness of a kind of test may further comprise the steps:
1) austenitic heat-resistance steel Super304H reactivation rate and M 23C 6Have quantitative relationship: Ra=0.0493M relatively between the amount of separating out 3-0.0998M 2+ 0.3377M+0.0033, Ra are the reactivation rate, and M is M in the tissue 23C 6The amount of separating out relatively, M is according to M in the X-ray diffraction 23C 6The ratio calculation of the integrated intensity of the integrated intensity of precipitated phase highest peak and matrix highest peak is come out;
2) get the difference Super304H steel of working times, measure M in the tissue 23C 6The M of the amount of separating out relatively, the quantitative relation formula in the substitution step 1) is calculated Ra, can learn the degree of Super304H steel intercrystalline corrosion.
Super304H steel supply of material state is solution treatment, the M during solution treatment in the tissue 23C 6Do not produce poor Cr phenomenon because of all dissolving in the matrix crystal boundary, shown good anti intercrystalline corrosion performance.Under 650 ℃ of temperature, behind the timeliness 100h because M 23C 6Separate out fast, make austenite grain boundary that M be arranged 23C 6Separate out, and intracrystalline also has some graininess M 23C 6Separate out, make M 23C 6The amount of separating out increases fast, reactivation rate R aValue also increases fast; Along with the prolongation of aging time, M on the crystal boundary 23C 6The quantity of separating out constantly increase, its size constantly increases, and makes the poor Cr degree of crystal boundary increase, and causes the continuous broadening of corrosion width of crystal boundary, and intracrystalline graininess M 23C 6Constantly separate out and grow up, obvious poor Cr also occurs around the particle, intracrystalline etch pit quantity and size enlarge markedly, and make R aValue constantly increases; Behind the certain hour, M on the crystal boundary 23C 6Begin to be isolated graininess distribution because of the Ostwald slaking takes place, its amount of separating out speedup slows down, and crystal boundary makes its poor Cr degree alleviate R because of the diffusion of Cr aIt is slow that the speedup of value is tending towards.
Compare with conventional intercrystalline corrosion method of testing, the present invention can learn the variation of the postrun intercrystalline corrosion susceptibility of Super304H steel quickly and accurately, and is convenient and swift.Can avoid boiler component sampling to cause damage, reduce maintenance cost, and can in time grasp the intercrystalline corrosion degree of steel, understand the variation tendency of steel intercrystalline corrosion, provide foundation the safety supervision of boiler component.
Description of drawings
Fig. 1 is the XRD figure spectrum behind 650 ℃ of Ageing Treatment 500h of Super304H steel;
Fig. 2 is the XRD figure spectrum behind 650 ℃ of Ageing Treatment 300h of Super304H steel;
Fig. 3 is the XRD figure spectrum behind 650 ℃ of Ageing Treatment 200h of Super304H steel;
Fig. 4 is the XRD figure spectrum behind 650 ℃ of Ageing Treatment 100h of Super304H steel;
Fig. 5 is the XRD figure spectrum behind 650 ℃ of operations of Super304H steel 168h;
Fig. 6 is the XRD figure spectrum behind 650 ℃ of Ageing Treatment 0h of Super304H steel;
Fig. 7 is the polarization curve behind 650 ℃ of Ageing Treatment 500h of Super304H steel;
Fig. 8 is the polarization curve behind 650 ℃ of Ageing Treatment 300h of Super304H steel;
Fig. 9 is the polarization curve behind 650 ℃ of Ageing Treatment 200h of Super304H steel;
Figure 10 is the polarization curve behind 650 ℃ of Ageing Treatment 100h of Super304H steel;
Figure 11 is the polarization curve behind 650 ℃ of operations of Super304H steel 168h;
Figure 12 is the polarization curve behind 650 ℃ of Ageing Treatment 0h of Super304H steel.
Embodiment
The present invention is further described below in conjunction with drawings and Examples.
Be depicted as the XRD figure spectrum and the polarization curve of 650 ℃ of Ageing Treatment different times of Super304H steel as Fig. 1-12.
Also can test out Super304H steel reactivation rate Ra by other method of testings that can cause that the boiler component sampling damages, for example: the Super304H steel is carried out 650 ℃ of Ageing Treatment, be 0h to the processing time respectively, 100h, 168h, 200h, the Super304H steel of 300h and 500h carries out the test of galvanochemistry potentiokinetic reactivation method, Ra uses the dicyclo method to measure electrochemical emf activation (based on the Cihal method) (Corrosion of metals and alloys-Electrochemical potentiokinetic reactivation measurement using the double loop method (based on Cihal ' s method)) test gained according to the corrosion of DIN EN ISO12732-2006 metal and alloy, and the reactivation rate Ra that obtains steel is respectively 0.0032,0.2978,0.4729,0.6162 and 0.6521.
Test under the above-mentioned different aging time M in the Super304H structure of steel respectively 23C 6The M of the amount of separating out relatively, be respectively 0,1.0212%, 1.4591%, 1.5680%, 1.8645% and 1.9695%.M is according to M in the X-ray diffraction 23C 6The ratio calculation of the integrated intensity of the integrated intensity of precipitated phase highest peak and matrix highest peak is come out;
Be that (M of all the other Ageing Treatment times calculates similarly for the calculating principle of example brief description M with the sample of Ageing Treatment 500h below, repeat no more): preparation 500h Ageing Treatment sample, (concrete parameter is: target is the Cu target to carry out X-ray diffraction, 20 °-100 ° of sweep limits, accelerating potential 45kV, electric current 100mA, sweep velocity is 2 °/min, 0.020 ° of continuous sweep of stepping), its collection of illustrative plates as shown in Figure 1.The integrated intensity of measuring austenitic matrix (γ) highest peak is 52601, M 23C 6The integrated intensity of highest peak is 1036, and the intensity of the strongest phase in the X-ray diffraction curve (γ phase) is defined as 1, then in this curve:
Figure BDA0000034074320000031
Be relative intensity, can represent M 23C 6Relative content.
Quantitative relationship according to Ra and M: Ra=0.0493M 3-0.0998M 2+ 0.3377M+0.0033 calculates the value of Ra respectively, and as shown in table 1, in the formula: Ra is the reactivation rate, and M is M in the tissue 23C 6The amount of separating out relatively.According to M in the tissue 23C 6The M of the amount of separating out relatively can learn the degree of Super304H steel intercrystalline corrosion.
The measured value of Ra and more as shown in table 1 according to the quantitative relation formula calculated value under the different condition, as seen, according to quantitative relation formula Ra=0.0493M 3-0.0998M 2Super304H steel reactivation rate that+0.3377M+0.0033 can learn and the deviation control between the measured value illustrate that the Super304H steel reactivation rate and the measured value that calculate according to this quantitative relation formula are more approaching in 4%, can practical application.
The measured value of table 1 austenite heat-resistance structure of steel reactivation rate and calculated value are relatively
Figure BDA0000034074320000032
Figure BDA0000034074320000041

Claims (1)

1. the method for austenitic heat-resistance steel intercrystalline corrosion performance after 650 ℃ of timeliness of a test is characterized in that, may further comprise the steps:
1) austenitic heat-resistance steel Super304H reactivation rate and M 23C 6Have quantitative relationship: Ra=0.0493M relatively between the amount of separating out 3-0.0998M 2+ 0.3377M+0.0033, Ra are the reactivation rate, and M is M in the tissue 23C 6The amount of separating out relatively, M is according to M in the X-ray diffraction 23C 6The ratio calculation of the integrated intensity of the integrated intensity of precipitated phase highest peak and matrix highest peak is come out;
2), measure M in the tissue to postrun Super304H steel 23C 6The M of the amount of separating out relatively, the quantitative relation formula in the substitution step 1) is calculated Ra, can learn the intercrystalline corrosion degree of Super304H steel.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2553412C1 (en) * 2013-11-06 2015-06-10 Открытое акционерное общество "Чепецкий механический завод" (ОАО ЧМЗ) Assessment method of resistance against intergranular corrosion of steels and alloys
CN106290140A (en) * 2016-09-29 2017-01-04 珠海格力电器股份有限公司 A kind of method checking Intergranular Corrosion of Austenitic Stainless Steel sensitivity

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JPS61108967A (en) * 1984-11-01 1986-05-27 Mitsubishi Heavy Ind Ltd Detection of degree of quality deterioration of high-temperature and pressure-resistant material
CN101762454A (en) * 2010-02-03 2010-06-30 海洋王照明科技股份有限公司 Dual-ring electrochemical dynamic potential reactivating evaluating method for diphase stainless steel intercrystalline corrosion sensitivity

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JPS61108967A (en) * 1984-11-01 1986-05-27 Mitsubishi Heavy Ind Ltd Detection of degree of quality deterioration of high-temperature and pressure-resistant material
CN101762454A (en) * 2010-02-03 2010-06-30 海洋王照明科技股份有限公司 Dual-ring electrochemical dynamic potential reactivating evaluating method for diphase stainless steel intercrystalline corrosion sensitivity

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Publication number Priority date Publication date Assignee Title
RU2553412C1 (en) * 2013-11-06 2015-06-10 Открытое акционерное общество "Чепецкий механический завод" (ОАО ЧМЗ) Assessment method of resistance against intergranular corrosion of steels and alloys
CN106290140A (en) * 2016-09-29 2017-01-04 珠海格力电器股份有限公司 A kind of method checking Intergranular Corrosion of Austenitic Stainless Steel sensitivity
CN106290140B (en) * 2016-09-29 2019-10-08 珠海格力电器股份有限公司 A method of examining Intergranular Corrosion of Austenitic Stainless Steel sensibility

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