CN108004549B - Metallographic etchant and etching method for ferrite/austenite dissimilar steel welded joint - Google Patents
Metallographic etchant and etching method for ferrite/austenite dissimilar steel welded joint Download PDFInfo
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 47
- 239000010959 steel Substances 0.000 title claims abstract description 47
- 229910001566 austenite Inorganic materials 0.000 title claims abstract description 37
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000005530 etching Methods 0.000 title description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000007788 liquid Substances 0.000 claims abstract description 35
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 30
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 230000007797 corrosion Effects 0.000 claims abstract description 25
- 238000005260 corrosion Methods 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000000861 blow drying Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 8
- 230000003628 erosive effect Effects 0.000 claims description 7
- 238000007796 conventional method Methods 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 claims description 2
- 238000003466 welding Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 description 20
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 16
- 238000010586 diagram Methods 0.000 description 11
- 230000004927 fusion Effects 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 238000010248 power generation Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/28—Acidic compositions for etching iron group metals
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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Abstract
The invention provides a metallographic corrosive liquid and a corrosion method for a ferrite/austenite dissimilar steel welding joint, wherein the metallographic corrosive liquid comprises the components of ferric trichloride, nitric acid, glycerol and water, and the dosage ratio of the ferric trichloride, the nitric acid, the glycerol and the water is (10-15g), (20-25m L), (15-20m L) and (25-30m L).
Description
Technical Field
The invention belongs to the technical field of material physical and chemical detection and analysis, and relates to a metallographic corrosive liquid and a corrosion method for a ferrite/austenite dissimilar steel welded joint.
Background
Thermal power generation dominates the electric power industry in China. In order to reduce the environmental problems caused by thermal power generation and improve the power generation efficiency, a plurality of high-parameter and high-capacity units are put into operation in succession, and then the steam temperatures of a boiler superheater and a reheater are required to be continuously increased, but the material cost is controlled, so that the outlet part of the high-temperature section of the heating surface of the boiler of the supercritical (supercritical) unit is made of austenitic heat-resistant steel, and the inlet side of the boiler is made of ferritic steel. Therefore, a large number of dissimilar steel welded joints of austenitic steel and ferritic steel inevitably exist in the heat receiving surfaces of these units. After the operation of a period of time at high temperature and high pressure, the safety problem of dissimilar steel welding joints is increasingly highlighted, a plurality of power plants have leakage accidents, and the leakage parts are all near the side fusion line of the ferritic steel. Therefore, how to effectively evaluate the tissue evolution near the joint fusion line has important significance for ensuring the safe use of the dissimilar steel joint.
In general, a metallographic corrosive agent for ferritic steel adopts a nital solution; the metallographic corrosive agent of the austenitic steel adopts aqua regia. The aqua regia is volatile and highly corrosive, can cause adverse effect to people, and the reaction is violent and difficult to operate, even the aqua regia is dipped by a writing point, the scale is difficult to grasp when the operation is carried out under a body type microscope, the over corrosion of the ferrite steel side of a fusion line or the condition that the austenite steel side cannot be corroded is often caused, and the difficulty is brought to the observation of the tissue evolution near the fusion line.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a metallographic etchant and an etching method for a ferrite/austenite dissimilar steel welded joint, which can make the etching process stable and easy to operate, and have a good display effect on a structure near a corroded joint fusion line.
The purpose of the invention is realized by the following technical scheme:
in one aspect, the invention provides a metallographic etchant for a ferrite/austenite dissimilar steel welded joint, which comprises the components of ferric trichloride, nitric acid, glycerol and water, wherein the dosage ratio of the ferric trichloride, the nitric acid, the glycerol and the water is (10-15 g): 20-25m L): 15-20m L): 25-30m L.
In the above-mentioned metallographic etchant for a welded joint of ferritic/austenitic dissimilar steel, it is preferable that the composition of the metallographic etchant includes 13g of ferric chloride, 22m L of nitric acid, 18m L of glycerol, and 27m L of water.
In the metallographic corrosive liquid for a welded joint of ferritic/austenitic dissimilar steel, preferably, the ferric trichloride, the nitric acid and the glycerol are analytically pure; the water is distilled water.
In the metallographic etchant for a welded joint of ferritic/austenitic dissimilar steel, the nitric acid is preferably contained in an amount of 68% by mass.
On the other hand, the invention also provides a preparation method of the metallographic corrosive liquid of the ferrite/austenite dissimilar steel welded joint, which comprises the following steps:
adding water into ferric trichloride, stirring to dissolve the ferric trichloride, then adding glycerol, fully and uniformly stirring, finally adding nitric acid, fully and uniformly stirring, and standing to obtain a metallographic corrosive liquid.
In the above preparation method, the standing time is preferably 20-25 min.
In another aspect, the present invention further provides a method for corroding a ferrite/austenite dissimilar steel welded joint by using the metallographic corrosive liquid for the ferrite/austenite dissimilar steel welded joint, comprising the steps of:
preprocessing a welded joint sample; fully immersing the pretreated welded joint sample into a metallographic corrosive liquid, placing the metallographic corrosive surface on the side, and vibrating the sample or stirring the metallographic corrosive liquid to enable bubbles to fully and quickly leave the surface of the welded joint sample, so that the corrosion effect cannot be influenced by the attachment of the bubbles to the surface of the sample until the metallographic corrosive surface is corroded and is silver gray; and taking out the corroded welded joint sample, washing with water, washing with alcohol, and blow-drying to finish the metallographic corrosion process.
In the above method of corroding a welded joint of ferritic/austenitic dissimilar steel, preferably, the method of pretreating a welded joint specimen is: cutting, coarse grinding, fine grinding, mechanical polishing, ultrasonic cleaning, alcohol washing and blow-drying are carried out on the welded joint sample according to a conventional method.
In the method for corroding the ferrite/austenite dissimilar steel welded joint, the corrosion time of the welded joint sample in the metallographic corrosive liquid is preferably 10-20 min.
Aqua regia is a mixture of 1:3 concentrated nitric acid and concentrated hydrochloric acid, is volatile and has strong corrosivity. The invention avoids concentrated hydrochloric acid, adopts ferric trichloride, provides chloride ions with coordination capacity (the existence of nitric acid and chloride ions indirectly realizes the corrosion effect of aqua regia, but the corrosivity is greatly weakened due to low concentration and weak acidity), and also provides high-valence iron ions with oxidation capacity. In addition, the glycerol is used as an active agent, so that the corrosion effect of the surface of the sample is improved; the water is added as a solvent, so that the strength of the acid is diluted, the corrosion process is stable and slow, the operation is easy, and the corrosive has a very good effect on corrosion of ferrite and austenite dissimilar steel joints due to the synergistic effect of the components and the specific proportion.
By adopting the metallographic corrosive liquid and the corrosion method of the ferrite/austenite dissimilar steel welded joint, metallographic structures near a fusion line can be obviously displayed, and the corrosion process is slow and stable and is easy to operate and control; the method can be carried out at normal temperature and under conventional conditions without heating and external current.
Drawings
FIG. 1 is a metallographic structure diagram showing the effect of erosion of a ferrite side near a weld line by dipping aqua regia with a writing tip in example 4 of the present invention;
FIG. 2 is a metallographic structure diagram showing the erosion effect of the austenite side near the weld line when the nib of a writing brush dipped with aqua regia does not contact the weld line in example 4 of the present invention;
FIG. 3 is a metallographic structure diagram showing an erosion effect of a welded joint sample corroded by being immersed in a nital solution in example 4 of the present invention;
FIG. 4 is a metallographic structure diagram showing an erosion effect of a welded joint sample corroded by immersion in aqua regia in example 4 of the present invention;
FIG. 5 is a metallographic structure diagram showing an erosion effect of a metallographic etchant with which a welded joint sample in example 4 of the present invention was immersed.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1
The implementation provides a metallographic corrosive liquid for a ferrite/austenite dissimilar steel welded joint, which comprises 13g of ferric trichloride, 22m L of nitric acid with the mass fraction of 68%, 18m L of glycerol and 27m L of distilled water, wherein the ferric trichloride, the nitric acid and the glycerol are all analytically pure.
The implementation also provides a preparation method of the metallographic corrosive liquid of the ferrite/austenite dissimilar steel welded joint, which comprises the following steps:
taking 13g of ferric trichloride, pouring into a beaker, adding 27m L of distilled water, stirring with a glass rod to dissolve the ferric trichloride, adding 18m L of glycerol, stirring, finally pouring 22m L of nitric acid with the mass fraction of 68%, fully stirring, and standing for 20 minutes to obtain the metallographic etchant.
The implementation also provides a method for corroding the ferrite/austenite dissimilar steel welded joint, which adopts the metallographic corrosive liquid of the ferrite/austenite dissimilar steel welded joint and comprises the following steps:
cutting, coarse grinding, fine grinding, mechanical polishing, ultrasonic cleaning, alcohol washing and blow-drying a ferrite/austenite dissimilar steel welding joint sample according to a conventional method; fully immersing the pretreated welded joint sample into a metallographic corrosive liquid, placing the metallographic corrosive surface on the side, and vibrating the sample or stirring the metallographic corrosive liquid to enable bubbles to fully and quickly leave the surface of the welded joint sample, so that the corrosion effect cannot be influenced by the attachment of the bubbles to the surface of the sample, and corroding for about 15min until the metallographic corrosive surface is corroded to be silver gray; and taking out the corroded welded joint sample, washing with water, washing with alcohol, and blow-drying to complete the metallographic corrosion process to obtain the metallographic sample to be observed.
Example 2
The implementation provides a metallographic corrosive liquid for a ferrite/austenite dissimilar steel welded joint, which comprises 10g of ferric trichloride, 25m L of nitric acid with the mass fraction of 68%, 15m L of glycerol and 25m L of distilled water, wherein the ferric trichloride, the nitric acid and the glycerol are all analytically pure.
The implementation also provides a preparation method of the metallographic corrosive liquid of the ferrite/austenite dissimilar steel welded joint, which comprises the following steps:
pouring 10g of ferric trichloride into a beaker, adding 25m L of distilled water, stirring with a glass rod to dissolve the ferric trichloride, adding 15m L of glycerol, stirring, finally pouring 25m L of nitric acid with the mass fraction of 68%, fully stirring, and standing for 20 minutes to obtain the metallographic etchant.
The implementation also provides a method for corroding the ferrite/austenite dissimilar steel welded joint, which adopts the metallographic corrosive liquid of the ferrite/austenite dissimilar steel welded joint and comprises the following steps:
cutting, coarse grinding, fine grinding, mechanical polishing, ultrasonic cleaning, alcohol washing and blow-drying a ferrite/austenite dissimilar steel welding joint sample according to a conventional method; fully immersing the pretreated welded joint sample into a metallographic corrosive liquid, placing the metallographic corrosive surface on the side, and vibrating the sample or stirring the metallographic corrosive liquid to enable bubbles to fully and quickly leave the surface of the welded joint sample, so that the corrosion effect cannot be influenced by the attachment of the bubbles to the surface of the sample, and corroding for about 10min until the metallographic corrosive surface is corroded to be silver gray; and taking out the corroded welded joint sample, washing with water, washing with alcohol, and blow-drying to finish the metallographic corrosion process.
Example 3
The implementation provides a metallographic corrosive liquid for a ferrite/austenite dissimilar steel welded joint, which comprises 15g of ferric trichloride, 20m L of nitric acid with the mass fraction of 68%, 15m L of glycerol and 25m L of distilled water, wherein the ferric trichloride, the nitric acid and the glycerol are all analytically pure.
The implementation also provides a preparation method of the metallographic corrosive liquid of the ferrite/austenite dissimilar steel welded joint, which comprises the following steps:
taking 15g of ferric trichloride, pouring the ferric trichloride into a beaker, adding 25m L of distilled water, stirring by using a glass rod to dissolve the ferric trichloride, adding 15m L of glycerol, stirring, finally pouring 20m L of nitric acid with the mass fraction of 68%, fully stirring, and standing for 20 minutes to obtain the metallographic etchant.
The implementation also provides a method for corroding the ferrite/austenite dissimilar steel welded joint, which adopts the metallographic corrosive liquid of the ferrite/austenite dissimilar steel welded joint and comprises the following steps:
cutting, coarse grinding, fine grinding, mechanical polishing, ultrasonic cleaning, alcohol washing and blow-drying a ferrite/austenite dissimilar steel welding joint sample according to a conventional method; fully immersing the pretreated welded joint sample into a metallographic corrosive liquid, placing the metallographic corrosive surface on the side, and vibrating the sample or stirring the metallographic corrosive liquid to enable bubbles to fully and quickly leave the surface of the welded joint sample, so that the corrosion effect cannot be influenced by the attachment of the bubbles to the surface of the sample, and corroding for about 20min until the metallographic corrosive surface is corroded to be silver gray; and taking out the corroded welded joint sample, washing with water, washing with alcohol, and blow-drying to finish the metallographic corrosion process.
Example 4 comparative experiment
Adopting aqua regia to corrode a ferrite/austenite dissimilar steel welded joint sample to obtain a metallographic sample to be tested, wherein the metallographic structure diagram of the corrosion effect is shown in figures 1, 2 and 4; adopting a nitric acid alcohol solution with the volume fraction of 10% to corrode a ferrite/austenite dissimilar steel welded joint sample to obtain a metallographic sample to be tested, wherein the metallographic structure diagram of the corrosion effect is shown in figure 3; the metallographic structure diagram of the corrosion effect of the metallographic specimen to be measured obtained by corroding with the metallographic corrosive liquid in the embodiment 1 of the invention is shown in fig. 5.
In FIG. 1, a writing point is used for dipping aqua regia, and the aqua regia is operated under a body type microscope, and the aqua regia contacts with the ferrite side near a fusion line, so that the metallographic structure of the ferrite side near the fusion line is over-corroded; in FIG. 2, the nib of a writing brush is dipped in aqua regia, and the writing brush is operated under a body microscope, and the aqua regia does not contact the side of the austenite near the fusion line, so that the side of the austenite near the fusion line is not corroded to form a metallographic structure; as can be seen from FIGS. 1 and 2, the scale of the etching using aqua regia is difficult to control and difficult to operate.
In fig. 4, the welded joint sample is immersed in aqua regia for corrosion, and as can be seen from the metallographic structure diagram of the corrosion effect in fig. 4, the metallographic structure is corroded on the austenite side, but the ferrite side is corroded.
In fig. 3, the welded joint sample is immersed in a nital solution with a volume fraction of 10% to corrode, and as can be seen from the metallographic structure diagram of the corrosion effect in fig. 3, the metallographic structure is corroded on the ferrite side, but the metallographic structure is not corroded on the austenite side.
Fig. 5 is a metallographic structure diagram showing an erosion effect of a metallographic sample obtained by the metallographic corrosive liquid according to example 1 of the present invention, and it can be seen from fig. 5 that both a ferrite side and an austenite side near a weld line show a perfect metallographic structure.
Claims (8)
1. A metallographic etchant aiming at a metallographic structure near a weld joint weld line of ferrite/austenite dissimilar steel is characterized by comprising the components of ferric trichloride, nitric acid, glycerol and water, wherein the dosage ratio of the ferric trichloride, the nitric acid, the glycerol and the water is (10-15 g): 20-25m L): 15-20m L): 25-30m L;
the mass fraction of the nitric acid is 68 percent;
the metallographic corrosive liquid is prepared by the following method:
adding water into ferric trichloride, stirring to dissolve the ferric trichloride, then adding glycerol, fully and uniformly stirring, finally adding nitric acid, fully and uniformly stirring, and standing to obtain a metallographic corrosive liquid.
2. The metallographic etchant according to claim 1, which comprises 13g of ferric chloride, 22m of nitric acid L, 18m of glycerol L and 27m of water L.
3. A metallographic etchant according to claim 1 or 2, characterized in that: the ferric trichloride, the nitric acid and the glycerol are analytically pure; the water is distilled water.
4. A method of preparing a metallographic etchant according to any one of claims 1 to 3, comprising the steps of:
adding water into ferric trichloride, stirring to dissolve the ferric trichloride, then adding glycerol, fully and uniformly stirring, finally adding nitric acid, fully and uniformly stirring, and standing to obtain a metallographic corrosive liquid.
5. The method of claim 4, wherein: standing for 20-25 min.
6. A method for corroding a metallographic structure near a weld line of a ferritic/austenitic dissimilar steel weld joint by using the metallographic corrosive liquid described in any one of claims 1 to 3, comprising the steps of:
preprocessing a welded joint sample; fully immersing the pretreated welded joint sample into a metallographic corrosive liquid, placing the metallographic corrosive surface on the side, and fully and quickly separating bubbles from the surface of the welded joint sample by adopting a vibration sample or stirring the metallographic corrosive liquid until the metallographic corrosive surface is corroded and is silvery; and taking out the corroded welded joint sample, washing with water, washing with alcohol, and blow-drying to finish the metallographic corrosion process.
7. The method of claim 6, wherein: the method for pretreating the welded joint sample comprises the following steps: cutting, coarse grinding, fine grinding, mechanical polishing, ultrasonic cleaning, alcohol washing and blow-drying are carried out on the welded joint sample according to a conventional method.
8. The method of claim 6, wherein: and the erosion time of the welded joint sample in the metallographic corrosive liquid is 10-20 min.
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CN109706456A (en) * | 2019-03-07 | 2019-05-03 | 济南大学 | A kind of metallographic etchant of ferritic stainless steel and its prepare corrosion method |
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