CN114457335B - Metallographic etchant for copper-iron-carbon alloy and use method thereof - Google Patents
Metallographic etchant for copper-iron-carbon alloy and use method thereof Download PDFInfo
- Publication number
- CN114457335B CN114457335B CN202210132238.4A CN202210132238A CN114457335B CN 114457335 B CN114457335 B CN 114457335B CN 202210132238 A CN202210132238 A CN 202210132238A CN 114457335 B CN114457335 B CN 114457335B
- Authority
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- China
- Prior art keywords
- etchant
- iron
- copper
- carbon alloy
- metallographic
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 229910001339 C alloy Inorganic materials 0.000 title claims abstract description 17
- QPBIPRLFFSGFRD-UHFFFAOYSA-N [C].[Cu].[Fe] Chemical compound [C].[Cu].[Fe] QPBIPRLFFSGFRD-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000005498 polishing Methods 0.000 claims abstract description 6
- 244000137852 Petrea volubilis Species 0.000 claims abstract description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 239000011780 sodium chloride Substances 0.000 claims abstract description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 5
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 5
- 239000000956 alloy Substances 0.000 claims description 14
- 229910045601 alloy Inorganic materials 0.000 claims description 13
- 238000005530 etching Methods 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 229910017112 Fe—C Inorganic materials 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 4
- 150000003839 salts Chemical class 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 231100000206 health hazard Toxicity 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000007654 immersion Methods 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- IYRDVAUFQZOLSB-UHFFFAOYSA-N copper iron Chemical compound [Fe].[Cu] IYRDVAUFQZOLSB-UHFFFAOYSA-N 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
Classifications
-
- 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
- C23F1/18—Acidic compositions for etching copper or alloys thereof
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
Abstract
The invention relates to a copper-iron-carbon alloy metallographic etchant and a use method thereof, wherein the etchant comprises the following components in percentage by weight: acetic acid: 5-30% of sodium chloride: 1 to 3 percent of sodium sulfate: 0.5-2%, and the balance being water; the application method comprises the following steps: polishing the copper-iron-carbon alloy sample by adopting coarse-grain, medium-grain and fine-grain water sand paper, polishing by adopting grinding paste, cleaning and drying, immersing the copper-iron-carbon alloy sample in the etchant, keeping the temperature of the etchant at 15-35 ℃, immersing the copper-iron-carbon alloy sample in the depth of 1-3 mm, immersing the copper-iron-carbon alloy sample for 20-50 s, taking out the copper-iron-carbon alloy sample, sequentially cleaning and drying by using deionized water and absolute ethyl alcohol, and observing and recording a microstructure by using a metallographic microscope. The invention adopts weak acid and salts to prepare the etchant, the grain boundary and the second phase of the metallographic structure have good display effect and uniform corrosion, and compared with the etchant prepared from strong acid and strong oxidizing ferric salt, the etchant has low oxidizing property and corrosivity and can not cause environmental pollution and health hazard.
Description
Technical Field
The invention relates to a copper-iron-carbon alloy metallographic etching agent and a use method thereof, belonging to the technical field of metallographic etching.
Background
The internal structure of the alloy material directly determines the mechanical properties such as strength and hardness and the physical properties such as electric conduction and heat conduction, and metallographic analysis is one of the most basic, direct and simple methods for researching the microstructure of the metal material, and the basic steps are that a polished alloy sample is immersed in a metallographic etching agent for a plurality of times, and the microstructure is observed by a metallographic microscope after cleaning and blow-drying; since different structures (such as crystal grains and grain boundaries, and a matrix and a second phase) are corroded at different speeds and depths in the etchant, images with different shades are displayed in a microscope. Copper-iron alloy has high strength and low cost, and has been studied widely in recent years, and literature search shows thatThe metallographic etchant generally adopts FeCl 3 The mixed solution of HCl and water has strong oxidizing property and corrosiveness, is extremely easy to cause excessive corrosion, leads to inaccurate metallographic analysis, and is unfavorable for the health of experimental staff and easy to pollute the water body and the atmosphere.
Disclosure of Invention
The invention aims to provide a copper-iron-carbon alloy metallographic etchant which has weaker oxidizing property, can be uniformly corroded and is more environment-friendly, and a use method thereof, wherein the etchant comprises the following components in percentage by weight: acetic acid: 5-30% of sodium chloride: 1 to 3 percent of sodium sulfate: 0.5-2%, and the balance being water; the application method comprises the following steps: polishing copper-iron-carbon alloy samples sequentially by using water sand paper with 180 meshes, 600 meshes, 1500 meshes and 2000 meshes, polishing sequentially by using grinding paste with granularity of 1 mu m and 0.5 mu m, cleaning and drying by using absolute ethyl alcohol, immersing the copper-iron-carbon alloy samples in the metallographic etchant, keeping the temperature of the etchant at 15-35 ℃, immersing depth of 1-3 mm, immersing for 20-50 s, taking out the samples, cleaning and drying sequentially by using deionized water and absolute ethyl alcohol, and observing and recording microscopic structures by using a metallographic microscope.
Compared with the prior art, the method adopts weak acid and salts to prepare the copper-iron-carbon alloy metallographic etchant, the grain boundary and the second phase of the metallographic structure have good display effect, and compared with the existing strong acid and strong oxidizing ferric salt etchant, the method has lower oxidizing property and corrosivity, can more uniformly corrode the alloy to enable metallographic analysis to be more accurate, and has little harm to the health and environment of experimental staff.
Drawings
FIG. 1 is a microstructure of a Cu-10Fe-0.1C alloy of example 1 after etching with an etchant of the present invention;
FIG. 2 is a schematic diagram of a Cu-10Fe-0.1C alloy of example 1 using a strong oxidizing etchant (FeCl) 3 +HCl+H 2 O) etched microstructure;
FIG. 3 is a microstructure of example 2 Cu-16Fe-0.02C alloy etched using the etchant of the present invention.
Detailed Description
Example 1:
the embodiment provides a method for preparing a metallographic specimen of a heat-treated Cu-10Fe-0.1C alloy by using the etchant, which comprises the following components in percentage by weight: acetic acid: 15%, sodium chloride: 1%, sodium sulfate: 0.5 percent of water and the balance of water, and the specific steps are as follows:
the Cu-10Fe-0.1C alloy subjected to solution treatment is sampled, sequentially polished by using water sand paper with 180 meshes, 600 meshes, 1500 meshes and 2000 meshes, sequentially polished by using grinding paste with granularity of 1 mu m and 0.5 mu m, washed by using absolute ethyl alcohol and dried, then immersed in the etchant, the temperature of the etchant is kept at 20 ℃, the immersion depth is 2mm, the immersion time is 30s, the sample is taken out, sequentially washed by using deionized water and absolute ethyl alcohol and dried, then observed by using a metallographic microscope, the appearance is observed, the crystal boundary is clear and discernable, the light gray part is a copper-rich matrix, the dark gray dendritic iron-rich phase and the black spherical iron-rich phase are also quite clear, and the etching effect is good.
To facilitate comparative observation of the effect of the etchant of the present invention, the solution-treated Cu-10Fe-0.1C alloy was sampled in the same manner, and was polished, washed, and blow-dried by the same procedure as in example 1, and then immersed in a strongly oxidizing etchant (5 g FeCl 3 +10mL HCl+100mL H 2 O mixture) using the same etching parameters as in example 1, the samples were taken out, washed and dried, and then observed with a metallographic microscope, and fig. 2 is an observed etching profile, and it was found that the etching was very uneven, that some local grain boundaries had been excessively etched to appear thicker, and that some local grain boundaries had not been completely etched out, which could affect the accurate analysis of metallographic phase. The metallographic etching effect of the strong oxidizing etchant is inferior to that of the etchant of the invention.
Example 2:
the embodiment provides a method for preparing an as-cast Cu-16Fe-0.02C alloy metallographic specimen by using the etchant, which comprises the following components in percentage by weight: acetic acid: 25%, sodium chloride: 1.5%, sodium sulfate: 1 percent, the balance is water, and the specific steps are as follows:
the cast Cu-16Fe-0.02C alloy is sampled, polished by water sand paper with 180 meshes, 600 meshes, 1500 meshes and 2000 meshes in sequence, polished by grinding paste with granularity of 1 mu m and 0.5 mu m in sequence, washed by absolute ethyl alcohol and dried, immersed in the etchant, the temperature of the etchant is kept at 30 ℃, the immersion depth is 1.5mm, the immersion time is 20s, the sample is taken out, washed by deionized water and absolute ethyl alcohol in sequence and dried, then observed by a metallographic microscope, the observed etched appearance is shown in FIG. 3, the light gray part is a copper-rich matrix, the gray-black dendrite is an iron-rich second phase, the boundary between the two phases is clear, the structure appearance is clear, and the metallographic etched effect is good.
Claims (1)
1. The metallographic etchant for the copper-iron-carbon alloy is characterized by comprising the following components in percentage by weight: acetic acid: 5-30% of sodium chloride: 1 to 3 percent of sodium sulfate: 0.5-2%, and the balance being water;
the using method of the copper-iron-carbon alloy metallographic etching agent comprises the following steps: polishing copper-iron-carbon alloy samples sequentially by using water sand paper with 180 meshes, 600 meshes, 1500 meshes and 2000 meshes, polishing sequentially by using grinding paste with granularity of 1 mu m and 0.5 mu m, cleaning and drying by using absolute ethyl alcohol, immersing the copper-iron-carbon alloy samples in the metallographic etchant, keeping the temperature of the etchant at 15-35 ℃, immersing depth of 1-3 mm, immersing for 20-50 s, and sequentially cleaning and drying the samples by using deionized water and absolute ethyl alcohol after the samples are taken out;
the Cu-Fe-C alloy is Cu-10Fe-0.1C alloy or Cu-16Fe-0.02C alloy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210132238.4A CN114457335B (en) | 2022-02-15 | 2022-02-15 | Metallographic etchant for copper-iron-carbon alloy and use method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210132238.4A CN114457335B (en) | 2022-02-15 | 2022-02-15 | Metallographic etchant for copper-iron-carbon alloy and use method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114457335A CN114457335A (en) | 2022-05-10 |
| CN114457335B true CN114457335B (en) | 2023-10-27 |
Family
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Family Applications (1)
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| CN202210132238.4A Active CN114457335B (en) | 2022-02-15 | 2022-02-15 | Metallographic etchant for copper-iron-carbon alloy and use method thereof |
Country Status (1)
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