CN117779040A - Alloy steel corrosive agent and preparation method and application method thereof - Google Patents
Alloy steel corrosive agent and preparation method and application method thereof Download PDFInfo
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- 229910000851 Alloy steel Inorganic materials 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 62
- 239000003518 caustics Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 238000005498 polishing Methods 0.000 claims abstract description 76
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 73
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical class OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910000742 Microalloyed steel Inorganic materials 0.000 claims abstract description 44
- 238000000227 grinding Methods 0.000 claims abstract description 42
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000005260 corrosion Methods 0.000 claims abstract description 37
- 230000007797 corrosion Effects 0.000 claims abstract description 37
- 229910001566 austenite Inorganic materials 0.000 claims abstract description 35
- 239000007864 aqueous solution Substances 0.000 claims abstract description 28
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002453 shampoo Substances 0.000 claims abstract description 23
- 208000001840 Dandruff Diseases 0.000 claims abstract description 22
- 229910000734 martensite Inorganic materials 0.000 claims abstract description 19
- 230000003628 erosive effect Effects 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- 244000137852 Petrea volubilis Species 0.000 claims description 21
- 238000004321 preservation Methods 0.000 claims description 15
- 229920000742 Cotton Polymers 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 239000004744 fabric Substances 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000005096 rolling process Methods 0.000 claims description 8
- 239000008096 xylene Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 238000009837 dry grinding Methods 0.000 claims description 7
- 239000003344 environmental pollutant Substances 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 231100000719 pollutant Toxicity 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 6
- 238000007517 polishing process Methods 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 6
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 238000000861 blow drying Methods 0.000 claims description 2
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 238000005530 etching Methods 0.000 abstract description 10
- 239000003795 chemical substances by application Substances 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 7
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 7
- 238000002161 passivation Methods 0.000 abstract description 4
- 238000005406 washing Methods 0.000 description 12
- 229910000831 Steel Inorganic materials 0.000 description 8
- 239000010959 steel Substances 0.000 description 8
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
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- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 2
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- 238000005482 strain hardening Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Abstract
The invention discloses an alloy steel etching agent, a preparation method and a use method thereof, wherein the etching agent is prepared from supersaturated picric acid water solution, seagull-plate anti-dandruff shampoo, hydrofluoric acid and dimethylbenzene according to the proportion of 1000-1700: 30-50: 1:2 volume ratio; the preparation method comprises the following steps: 1. preparing supersaturated picric acid aqueous solution; 2. mixing to obtain an alloy steel corrosive agent; the application method comprises the following steps: 1. heat treatment and deformation of Ti-containing microalloyed steel; 2. rough grinding, fine grinding and mechanical polishing; 3. erosion. According to the alloy steel corrosive agent, the gull-plate chip removing shampoo is added to remove a passivation oxide film formed by picric acid corrosion, so that corrosion is ensured to be smooth, and trace nitric acid is added to quickly deepen grain boundary corrosion, so that the original austenite grain boundary in the alloy steel and a martensite structure in the grain are clearly displayed; the alloy steel corrosive agent has the advantages of simple preparation process, short corrosion time in the using process, strong repeatability, simplified complex corrosion steps and greatly improved corrosion efficiency.
Description
Technical Field
The invention belongs to the technical field of metallographic phase preparation, and particularly relates to an alloy steel corrosive agent, a preparation method and a use method thereof.
Background
The Ti microalloyed steel is subjected to Nb microalloying, and becomes another steel grade widely applied to high-strength structural members such as automobile girders, the size and uniformity of austenite grains have important influence on the mechanical properties of the steel grade, and the small and uniform grains provide more grain boundaries, so that the strength, the toughness and the crack expansion resistance of the steel can be improved simultaneously. Therefore, the method can accurately and conveniently display the morphology of the austenite, and if the morphology of the austenite intragranular martensite phase can be displayed on the basis, great convenience is brought to the research of the strengthening mechanism of the steel. Whether austenite grains can be clearly revealed is mainly influenced by various factors such as chemical composition of the sample, heat treatment state, etchant, etching method, etching time, and the like. Currently, the main methods for displaying austenite grain boundaries are an oxidation method, a net-like ferrite method, a net-like pearlite method, and a grain boundary corrosion method, among which the grain boundary corrosion method is more commonly used.
In the prior art, the conventional method for corroding austenite grain boundaries, such as supersaturated picric acid solution, sodium dodecyl benzene sulfonate and other activating agents, are not ideal for the appearance of the austenite grain boundaries of Ti microalloyed steel, and particularly the appearance of the austenite grain boundaries is not obvious when the steel is subjected to large deformation. Lv Zhiqing and Fu Motang (CN 103018141A) adopt a formula of concentrated nitric acid, concentrated hydrochloric acid, alcohol, picric acid and sodium dodecyl benzene sulfonate to corrode high-alloy low-carbon martensite, so that austenite grains can be better displayed; xia Zhiwei (CN 104374627A) discloses a corrosive liquid and a corrosion method for corroding the original austenite grain boundary of ultra-low steel by using supersaturated picric acid-detergent-hydrochloric acid, which can obtain a clearer original austenite grain boundary; zeng Hui and vast vast (CN 102590050A) adopt a two-stage erosion method combining supersaturated picric acid-sodium dodecyl benzene sulfonate-hydrogen peroxide thermal erosion and sulfuric acid electrolytic soaking, and better display the prior austenite grain boundaries of P91 and P92 steel by microscopic dark field illumination or bright field illumination after light polishing of a sample. However, the above method is too acidic in the etching solution or complicated in operation steps, and cannot ideally show both the austenitic grain boundary of the Ti microalloy steel and the intra-crystalline martensite phase thereof. Therefore, a method for simultaneously displaying original austenite grain boundaries and intra-grain martensite phases of the Ti microalloyed steel is sought, and great convenience can be brought to the research on the appearance of the austenite grain boundaries and the relationship between the austenite grain size and the martensite of the steel.
Disclosure of Invention
The technical problem to be solved by the invention is to provide an alloy steel corrosive agent aiming at the defects of the prior art. The alloy steel etching agent plays a role of a surfactant by adding the gull plate anti-dandruff shampoo to remove a passivation oxide film formed by picric acid etching, ensures smooth progress of etching, and combines with adding a trace amount of nitric acid to quickly deepen grain boundary etching, so that original austenite grain boundaries and martensite structures in the grains in the alloy steel are clearly displayed at the same time, and the problem that the prior art cannot ideally display the austenite grain boundaries and the martensite phases in the grains of the Ti micro alloy steel at the same time is solved.
In order to solve the technical problems, the invention adopts the following technical scheme: an alloy steel corrosive agent is characterized in that supersaturated bittering acid aqueous solution, seagull-plate anti-dandruff shampoo, hydrofluoric acid and xylene are mixed according to the proportion of 1000-1700: 30-50: 1:2 by volume.
Conventional 4% nitrate alcohol solutions show unclear corrosion of austenite grain boundaries, whereas picric acid aqueous solutions are common etchants for corrosion of austenite grain boundaries. Picric acid is a weak acid, has a smaller ionization degree than nitric acid, and contains a nitro group which is less oxidizing than nitrate, so that it has a weaker corrosion ability than nitric acid. The pearlite, bainite and tempered martensite in the sample can be clearly displayed by using picric acid solution for corrosion. Meanwhile, picric acid is decomposed vigorously in aqueous solution, the corrosion speed is faster than that of picric acid alcohol solution, but when the picric acid corrodes a sample, a layer of indissolvable corrosion product is easily formed on the surface of the sample, so that an oxide film is passivated, and corrosion is difficult to continue. Based on the above, the alloy steel erosion agent is added with the seagull-plate anti-dandruff shampoo in the supersaturated bittering acid aqueous solution, and the ethylene oxide polymer contained in the seagull-plate anti-dandruff shampoo plays a role of a surfactant in the erosion agent and continuously shakes in the erosion process so as to uniformly act on the oxide film to enable the oxide film to fall off, thereby ensuring the smooth progress of the erosion process. Meanwhile, for alloy steel, the oxidizing property of the picric acid is not used for achieving the erosion effect, so the invention adopts hydrofluoric acid to be matched with the picric acid, and the ionization degree of the hydrofluoric acid in water is very small, so that the oxidation effect as severe as nitric acid is not shown to blacken the whole metallographic phase, and meanwhile F - The radius of the product is small, the oxidizing property is strong, so the invention adds trace hydrofluoric acid into the aggressive agent and utilizes trace F - So as to deepen the erosion of the grain boundary rapidly, and the martensite phase is displayed while the original austenite grain boundary of the alloy steel is clearly displayed. In addition, a small amount of dimethylbenzene is added into the erosion agent as an active agent, so that the effective progress of the erosion process is promoted.
The alloy steel aggressive agent is characterized by comprising supersaturated picric acid aqueous solution, gull-plate anti-dandruff shampoo, hydrofluoric acid and dimethylbenzene according to 1200:40:1:2 by volume.
Meanwhile, the invention also discloses a method for preparing the alloy steel corrosive agent, which is characterized by comprising the following steps:
step one, preparing supersaturated picric acid aqueous solution: heating distilled water to 85-95 ℃, adding excessive picric acid, stirring to fully dissolve the picric acid, and taking supernatant to obtain supersaturated picric acid aqueous solution;
step two, mixing: placing the supersaturated picric acid aqueous solution prepared in the first step into a glass container, placing into a water bath device which is preheated to 70-75 ℃ for cooling to the water bath temperature, then adding the seagull plate anti-dandruff shampoo, hydrofluoric acid and dimethylbenzene according to the proportion of the alloy steel corrosive agent, and uniformly stirring to obtain the alloy steel corrosive agent.
The hydrofluoric acid in the alloy steel corrosive agent has stronger volatility, and the main component of the seagull-plate anti-dandruff shampoo as the surfactant is also lower in boiling point of the ethylene oxide polymer, so that the prepared alloy steel corrosive agent is suitable for immediate use.
The method is characterized in that distilled water is poured into a beaker and then placed on a resistance furnace to be heated to 85-95 ℃; in the second step, the glass container is a beaker, and the water bath device is a water bath furnace.
In addition, the invention also discloses a use method of the alloy steel corrosive agent, which is characterized by comprising the following steps:
step one, heat treatment and deformation of Ti-containing microalloyed steel: the Ti-containing microalloy steel is subjected to heat preservation at 1100-1250 ℃ for 3-6 h, then is rolled, and is immediately quenched to room temperature to obtain a hot rolled plate; the rolling temperature is 900-1100 ℃, and the rolling reduction is 35-65%;
step two, rough grinding, fine grinding and mechanical polishing: cutting the hot rolled plate obtained in the first step into a metallographic specimen, embedding the metallographic specimen, and then carrying out rough grinding, fine grinding and mechanical polishing to obtain the metallographic specimen to be corroded;
step three, erosion: placing the corrosive agent in a water bath furnace with the temperature of 70-75 ℃, then clamping the metallographic specimen to be corroded in the second step by using tweezers, immersing the metallographic specimen in the thermal-insulation corrosive agent, enabling the polished surface to face upwards and continuously shaking for corrosion, taking out the metallographic specimen after the surface starts darkening and blackening for 8-9 s, flushing off dark substances on the surface by using clear water, dipping in ethanol by using cotton, wiping and drying for metallographic structure observation.
The invention carries out hot rolling deformation on Ti-containing microalloy steel after heat preservation, and in the deformation process, a large amount of dislocation accumulation is generated at the austenitic grain boundary of the Ti-containing microalloy steel, so that the dislocation density at the grain boundary is increased, and meanwhile, in the process of austenite nucleation and growth, the distortion exists at the grain boundary; based on the principle of lowest energy, solute atoms are easy to be biased and aggregated at the grain boundary, so that distortion is eliminated, and the grain boundary energy is reduced. And therefore the grain boundary is more prone to corrosion relative to the intra-grain structure. The invention ensures that the Ti-containing microalloy steel can present clear austenite grain boundaries after being acted by the corrosive agent by carrying out heat treatment and deformation on the Ti-containing microalloy steel.
According to the invention, the metallographic sample to be corroded is continuously rocked in the corrosion process of the step three, so that the passivation oxide film formed in the corrosion process is promoted to fall off, and other pollutants can be prevented from forming on the corrosion surface.
Typically, the erosion process is timed using a stopwatch.
The method is characterized in that the Ti-containing microalloyed steel in the first step comprises the following components in percentage by mass: 0.05 to 0.25 percent of C, 0.01 to 0.1 percent of Ti, 0.15 to 0.3 percent of Si, 0.8 to 2.0 percent of Mn, 0.01 to 0.04 percent of Als, less than or equal to 0.03 percent of P, less than or equal to 0.025 percent of S, less than or equal to 0.007 percent of N, the balance of Fe and unavoidable impurities, the thickness of the Ti-containing microalloy steel is 6 to 12mm, and the thickness of the hot rolled plate is 4.2 to 4.8mm.
The method is characterized in that the method for coarse grinding-fine grinding in the coarse grinding-fine grinding-mechanical polishing in the second step comprises the following steps: adopting 400 to sample the metallographic specimen after the sample is inlaid # Silicon carbide metallographic sand paper is polished to remove surface inserts and pollutants, and then 600 is adopted in sequence # →800 # →1000 # →1200 # →1500 # The abrasive paper is polished, and the scratch directions of the surface of the metallographic specimen are ensured to be tidy and arranged along the same direction when the next-stage abrasive paper is replaced every timeThe metallographic specimen is rotated by 90 degrees and polished, and the lower surface of the metallographic specimen is kept horizontal by uniform force in the polishing process, wherein 600 percent of the lower surface is a metal # 、800 # 、1000 # 、1200 # The sand paper is polished by dry grinding 1500 # The sand paper is polished by water mill. According to the invention, the dry grinding and the water grinding are combined, so that adverse phenomena such as pits and the like on the surface of a metallographic specimen are avoided.
The method is characterized in that the mechanical polishing method in the coarse grinding-fine grinding-mechanical polishing in the second step comprises the following steps: the surface of the metallographic specimen after rough grinding and fine grinding is washed clean by water, then polishing paste with the grain diameter of 2.5 mu m is uniformly smeared, scratches on the surface of the metallographic specimen are polished perpendicular to the linear speed direction of a polishing machine, water is sprayed on the surface of polishing cloth to keep moist during polishing, water polishing is continuously carried out on the polishing cloth after the scratches on the surface of the metallographic specimen are polished clean, and cotton is adopted to dip ethanol for wiping and blow-drying after the metallographic specimen is washed with water. After coarse grinding and fine grinding, the metal particles on the surface of the metallographic sample are washed clean by water; the surface of the polishing cloth is sprayed with water to keep moist during polishing, so that surface work hardening of the metallographic specimen is avoided, scratches on the surface of the metallographic specimen are polished cleanly, water polishing is continuously carried out on the polishing cloth to remove impurities on the surface of the metallographic specimen, and finally the polished metallographic specimen is washed, wiped and dried, so that the surface of the metallographic specimen to be corroded is kept clean and dry.
The method is characterized in that the original austenite grain boundary and the intra-grain martensite structure of the Ti microalloy steel can be observed at the same time during the metallographic structure observation in the second step.
Compared with the prior art, the invention has the following advantages:
1. according to the alloy steel corrosive agent, the supersaturated picric acid solution is added to ensure the corrosion effect on austenite grain boundaries in alloy steel, the seagull plate anti-dandruff shampoo is added to play the role of a surfactant to remove passivation oxide films formed by picric acid corrosion, smooth corrosion is ensured, and trace nitric acid is added to quickly deepen the grain boundary corrosion, so that the original austenite grain boundaries and martensite structures in the austenite grain boundaries in the alloy steel are clearly displayed, and great convenience is brought to analysis of the appearance of austenite grains and the relationship between the austenite grains and martensite.
2. The alloy steel corrosive agent has the advantages of less composition components, low cost, simple and convenient preparation process and easy realization.
3. The alloy steel corrosive agent has the advantages of simple use method, short corrosion time, strong repeatability, simplified fussy corrosion steps and greatly improved corrosion efficiency.
4. The etchant and the etching method have wide application range and are effective for the appearance of Ti-containing microalloy low-carbon steel austenite grains with different components and martensite thereof.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
Fig. 1 shows commercial marks of the gull-plate anti-dandruff shampoo used in examples 1 to 3 of the present invention.
FIG. 2 is a chart (500X) of the metallographic structure of a Ti-containing microalloyed steel eroded by the alloy steel etchant of example 1 of the invention.
FIG. 3 is a chart (500X) of the metallographic structure of a Ti-containing microalloyed steel eroded by the alloy steel etchant of example 2 of the invention.
FIG. 4 is a metallographic structure (500X) of a Ti-containing microalloyed steel eroded by the alloy steel etchant of example 3 of the invention.
FIG. 5 is a metallographic structure (500X) of a Ti-containing microalloyed steel eroded by the alloy steel etchant of example 4 of the invention.
Detailed Description
The gull-plate anti-dandruff shampoo adopted in the embodiments 1 to 4 is a commercial product, the manufacturer is Shanghai household united stock limited company, and the commodity mark is shown in figure 1; the mass content of Hf in hydrofluoric acid is above 40.0%, and C in xylene 8 H 10 The mass content is more than 99.0%.
In the invention, the microstructure of the corroded alloy steel is observed by adopting a metallographic microscope Zeiss HAL 100 in the embodiments 1-4.
Example 1
The alloy steel corrosive agent of the embodiment is prepared from supersaturated bittering acid aqueous solution, seagull-plate anti-dandruff shampoo, hydrofluoric acid and xylene according to a ratio of 1200:40:1:2 by volume.
The preparation method of the alloy steel corrosive agent comprises the following steps:
step one, preparing supersaturated picric acid aqueous solution: pouring distilled water into a beaker, heating to 90 ℃ in a resistance furnace, adding excessive picric acid, stirring to fully dissolve the picric acid, and taking supernatant fluid of the picric acid to obtain supersaturated picric acid aqueous solution;
step two, mixing: and (3) placing the supersaturated picric acid aqueous solution prepared in the step (I) in a beaker, placing in a water bath furnace which is preheated to 70 ℃ for cooling to the water bath temperature, then adding the gull-plate anti-dandruff shampoo, hydrofluoric acid and dimethylbenzene according to the proportion of the alloy steel corrosive agent, and uniformly stirring to obtain the alloy steel corrosive agent.
The using method of the alloy steel corrosive agent of the embodiment comprises the following steps:
step one, heat treatment and deformation of Ti-containing microalloyed steel: the Ti-containing microalloyed steel with the thickness of 12mm is subjected to heat preservation for 5 hours at 1200 ℃, then is rolled at 900 ℃, the rolling reduction rate is 65 percent, and then is immediately quenched to room temperature, so as to obtain a hot rolled plate with the thickness of 4.8 mm; the Ti-containing microalloyed steel comprises the following components in percentage by mass: 0.080% of C, 0.050% of Ti, 0.24% of Si, 1.15% of Mn, 0.010% of Als, 0.0040% of P, 0.0030% of S, 0.0050% of N, and the balance of Fe and unavoidable impurities;
step two, rough grinding, fine grinding and mechanical polishing: cutting the hot rolled plate obtained in the first step into a metallographic specimen, embedding the metallographic specimen, and then carrying out rough grinding, fine grinding and mechanical polishing to obtain the metallographic specimen to be corroded;
the method for coarse grinding-fine grinding-mechanical polishing comprises the following steps: adopting 400 to sample the metallographic specimen after the sample is inlaid # Silicon carbide metallographic sand paper is polished to remove surface inserts and pollutants, and then 600 is adopted in sequence # →800 # →1000 # →1200 # →1500 # The sand paper is polished and replaced each timeThe scratch directions of the surfaces of the metallographic samples are ensured to be tidy and arranged along the same direction when the grade sand paper is used, the metallographic samples are rotated by 90 degrees and polished when the next grade sand paper is replaced, the lower surfaces of the metallographic samples are kept horizontal due to uniform force in the polishing process, the 600 percent # 、800 # 、1000 # 、1200 # The sand paper is polished by dry grinding 1500 # The sand paper is polished by water mill;
the mechanical polishing method in the rough grinding-fine grinding-mechanical polishing comprises the following steps: washing the surface of the metallographic sample after rough grinding and fine grinding by water, then uniformly smearing polishing paste with the particle size of 2.5 mu m, polishing scratches on the surface of the metallographic sample in the direction perpendicular to the linear speed direction of a polishing machine, sprinkling water on the surface of polishing cloth to keep moist during polishing, continuously polishing the scratches on the surface of the metallographic sample by water after the scratches on the surface of the metallographic sample are polished, and wiping and drying the metallographic sample by adopting cotton dipped with ethanol after washing by water after polishing;
step three, erosion: and (3) placing the corrosive agent in a water bath furnace at 70 ℃ for heat preservation, then clamping the metallographic specimen to be corroded in the second step by using forceps, immersing the metallographic specimen in the heat preservation corrosive agent, enabling the polished surface to face upwards and continuously shaking for corrosion, timing for corrosion by using a stopwatch for 45s, taking out the metallographic specimen after the surface starts darkening and blackening for 8-9 s, taking out the metallographic specimen, washing off the surface dark substances by using clear water, dipping the metallographic specimen in ethanol by using cotton, wiping and drying for metallographic tissue observation.
Fig. 2 is a metallographic structure diagram (500×) of a Ti-containing microalloyed steel eroded by the alloy steel etchant of the present example, and it can be seen from fig. 2 that the original austenite grain boundaries and the intra-grain martensite structure of the Ti-containing microalloyed steel are clearly shown at the same time.
Example 2
The alloy steel etchant of this example was prepared from supersaturated aqueous picric acid, gull-plate anti-dandruff shampoo, hydrofluoric acid and xylene at a rate of 1650:46:1:2 by volume.
The preparation method of the alloy steel corrosive agent comprises the following steps:
step one, preparing supersaturated picric acid aqueous solution: pouring distilled water into a beaker, heating to 94 ℃ in a resistance furnace, adding excessive picric acid, stirring to fully dissolve the picric acid, and taking supernatant fluid of the picric acid to obtain supersaturated picric acid aqueous solution;
step two, mixing: and (3) placing the supersaturated picric acid aqueous solution prepared in the step (I) in a beaker, placing in a water bath furnace which is preheated to 75 ℃ for cooling to the water bath temperature, then adding the gull-plate anti-dandruff shampoo, hydrofluoric acid and dimethylbenzene according to the proportion of the alloy steel corrosive agent, and uniformly stirring to obtain the alloy steel corrosive agent.
The using method of the alloy steel corrosive agent of the embodiment comprises the following steps:
step one, heat treatment and deformation of Ti-containing microalloyed steel: the Ti-containing microalloyed steel with the thickness of 8mm is subjected to heat preservation for 4 hours at 1200 ℃, then is rolled at 904 ℃, the rolling reduction rate is 43.75 percent, and then is immediately quenched to room temperature, so as to obtain a hot rolled plate with the thickness of 4.2 mm; the Ti-containing microalloyed steel comprises the following components in percentage by mass: 0.080% of C, 0.050% of Ti, 0.24% of Si, 1.15% of Mn, 0.010% of Als, 0.0040% of P, 0.0030% of S, 0.0050% of N, and the balance of Fe and unavoidable impurities;
step two, rough grinding, fine grinding and mechanical polishing: cutting the hot rolled plate obtained in the first step into a metallographic specimen, embedding the metallographic specimen, and then carrying out rough grinding, fine grinding and mechanical polishing to obtain the metallographic specimen to be corroded;
the method for coarse grinding-fine grinding-mechanical polishing comprises the following steps: adopting 400 to sample the metallographic specimen after the sample is inlaid # Silicon carbide metallographic sand paper is polished to remove surface inserts and pollutants, and then 600 is adopted in sequence # →800 # →1000 # →1200 # →1500 # The abrasive paper is polished, the scratch directions of the surface of the metallographic specimen are ensured to be tidy and arranged along the same direction when the next-stage abrasive paper is replaced every time, the metallographic specimen is rotated by 90 degrees and polished again when the next-stage abrasive paper is replaced, the lower surface of the metallographic specimen is kept horizontal due to uniform force in the polishing process, the method comprises the following steps of 600 # 、800 # 、1000 # 、1200 # The sand paper is polished by dry grinding 1500 # The sand paper is polished by water mill;
the mechanical polishing method in the rough grinding-fine grinding-mechanical polishing comprises the following steps: washing the surface of the metallographic sample after rough grinding and fine grinding by water, then uniformly smearing polishing paste with the particle size of 2.5 mu m, polishing scratches on the surface of the metallographic sample in the direction perpendicular to the linear speed direction of a polishing machine, sprinkling water on the surface of polishing cloth to keep moist during polishing, continuously polishing the scratches on the surface of the metallographic sample by water after the scratches on the surface of the metallographic sample are polished, and wiping and drying the metallographic sample by adopting cotton dipped with ethanol after washing by water after polishing;
step three, erosion: and (3) placing the corrosive agent in a 75 ℃ water bath furnace for heat preservation, then clamping the metallographic specimen to be corroded in the second step by using forceps, immersing the metallographic specimen in the heat preservation corrosive agent, enabling the polished surface to face upwards and continuously shaking for corrosion, timing corrosion by using a stopwatch for 40s, taking out the metallographic specimen after the surface starts darkening and blackening for 8 s-9 s, taking out the metallographic specimen, washing off the surface dark matter by using clear water, dipping in ethanol by using cotton, wiping and drying for metallographic tissue observation.
Fig. 3 is a metallographic structure diagram (500×) of a Ti-containing microalloyed steel eroded by the alloy steel etchant of the present example, and it can be seen from fig. 3 that the original austenite grain boundaries and the intra-grain martensite structure of the Ti-containing microalloyed steel are clearly shown at the same time.
Example 3
The alloy steel corrosive agent of the embodiment is prepared from supersaturated bittering acid aqueous solution, seagull-plate anti-dandruff shampoo, hydrofluoric acid and xylene according to the proportion of 1000:32:1:2 by volume.
The preparation method of the alloy steel corrosive agent comprises the following steps:
step one, preparing supersaturated picric acid aqueous solution: pouring distilled water into a beaker, heating to 85 ℃ in a resistance furnace, adding excessive picric acid, stirring to fully dissolve the picric acid, and taking supernatant fluid of the picric acid to obtain supersaturated picric acid aqueous solution;
step two, mixing: and (3) placing the supersaturated picric acid aqueous solution prepared in the step (I) in a beaker, placing in a water bath furnace which is preheated to 70 ℃ for cooling to the water bath temperature, then adding the gull-plate anti-dandruff shampoo, hydrofluoric acid and dimethylbenzene according to the proportion of the alloy steel corrosive agent, and uniformly stirring to obtain the alloy steel corrosive agent.
The using method of the alloy steel corrosive agent of the embodiment comprises the following steps:
step one, heat treatment and deformation of Ti-containing microalloyed steel: the Ti-containing microalloyed steel with the thickness of 10mm is subjected to heat preservation for 6 hours at 1100 ℃, then rolled at 1080 ℃, the rolling reduction is 55%, and then immediately water quenched to room temperature, so as to obtain a hot rolled plate with the thickness of 4.5 mm; the Ti-containing microalloyed steel comprises the following components in percentage by mass: 0.099% of C, 0.031% of Ti, 0.24% of Si, 1.18% of Mn, 0.025% of Als, 0.0025% of P, 0.0045% of S, 0.0043% of N, and the balance of Fe and unavoidable impurities;
step two, rough grinding, fine grinding and mechanical polishing: cutting the hot rolled plate obtained in the first step into a metallographic specimen, embedding the metallographic specimen, and then carrying out rough grinding, fine grinding and mechanical polishing to obtain the metallographic specimen to be corroded;
the method for coarse grinding-fine grinding-mechanical polishing comprises the following steps: adopting 400 to sample the metallographic specimen after the sample is inlaid # Silicon carbide metallographic sand paper is polished to remove surface inserts and pollutants, and then 600 is adopted in sequence # →800 # →1000 # →1200 # →1500 # The abrasive paper is polished, the scratch directions of the surface of the metallographic specimen are ensured to be tidy and arranged along the same direction when the next-stage abrasive paper is replaced every time, the metallographic specimen is rotated by 90 degrees and polished again when the next-stage abrasive paper is replaced, the lower surface of the metallographic specimen is kept horizontal due to uniform force in the polishing process, the method comprises the following steps of 600 # 、800 # 、1000 # 、1200 # The sand paper is polished by dry grinding 1500 # The sand paper is polished by water mill;
the mechanical polishing method in the rough grinding-fine grinding-mechanical polishing comprises the following steps: washing the surface of the metallographic sample after rough grinding and fine grinding by water, then uniformly smearing polishing paste with the particle size of 2.5 mu m, polishing scratches on the surface of the metallographic sample in the direction perpendicular to the linear speed direction of a polishing machine, sprinkling water on the surface of polishing cloth to keep moist during polishing, continuously polishing the scratches on the surface of the metallographic sample by water after the scratches on the surface of the metallographic sample are polished, and wiping and drying the metallographic sample by adopting cotton dipped with ethanol after washing by water after polishing;
step three, erosion: and (3) placing the corrosive agent in a water bath furnace at 72 ℃ for heat preservation, then clamping the metallographic specimen to be corroded in the second step by using forceps, immersing the metallographic specimen in the heat preservation corrosive agent, enabling the polished surface to face upwards and continuously shaking for corrosion, timing for corrosion by using a stopwatch for 47s, taking out the metallographic specimen after the surface starts darkening and blackening for 8-9 s, taking out the metallographic specimen, washing off the surface dark substances by using clear water, dipping the metallographic specimen in ethanol by using cotton, wiping and drying for metallographic tissue observation.
Fig. 4 is a metallographic structure diagram (500×) of a Ti-containing microalloyed steel eroded by the alloy steel etchant of the present example, and it can be seen from fig. 4 that the original austenite grain boundaries and the intra-grain martensite structure of the Ti-containing microalloyed steel are clearly shown at the same time.
Example 4
The alloy steel corrosive agent of the embodiment is prepared from supersaturated bittering acid aqueous solution, seagull-plate anti-dandruff shampoo, hydrofluoric acid and xylene according to 1700:50:1:2 by volume.
The preparation method of the alloy steel corrosive agent comprises the following steps:
step one, preparing supersaturated picric acid aqueous solution: pouring distilled water into a beaker, heating to 90 ℃ in a resistance furnace, adding excessive picric acid, stirring to fully dissolve the picric acid, and taking supernatant fluid of the picric acid to obtain supersaturated picric acid aqueous solution;
step two, mixing: and (3) placing the supersaturated picric acid aqueous solution prepared in the step (I) in a beaker, placing in a water bath furnace which is preheated to 75 ℃ for cooling to the water bath temperature, then adding the gull-plate anti-dandruff shampoo, hydrofluoric acid and dimethylbenzene according to the proportion of the alloy steel corrosive agent, and uniformly stirring to obtain the alloy steel corrosive agent.
The using method of the alloy steel corrosive agent of the embodiment comprises the following steps:
step one, heat treatment and deformation of Ti-containing microalloyed steel: the Ti-containing microalloyed steel with the thickness of 10mm is subjected to heat preservation for 3 hours at 1250 ℃, then is rolled at 1100 ℃, the rolling reduction rate is 35 percent, and then is immediately quenched to room temperature, so as to obtain a hot rolled plate with the thickness of 4.5 mm; the Ti-containing microalloyed steel comprises the following components in percentage by mass: 0.099% of C, 0.031% of Ti, 0.24% of Si, 1.18% of Mn, 0.025% of Als, 0.0025% of P, 0.0045% of S, 0.0043% of N, and the balance of Fe and unavoidable impurities;
step two, rough grinding, fine grinding and mechanical polishing: cutting the hot rolled plate obtained in the first step into a metallographic specimen, embedding the metallographic specimen, and then carrying out rough grinding, fine grinding and mechanical polishing to obtain the metallographic specimen to be corroded;
the method for coarse grinding-fine grinding-mechanical polishing comprises the following steps: adopting 400 to sample the metallographic specimen after the sample is inlaid # Silicon carbide metallographic sand paper is polished to remove surface inserts and pollutants, and then 600 is adopted in sequence # →800 # →1000 # →1200 # →1500 # The abrasive paper is polished, the scratch directions of the surface of the metallographic specimen are ensured to be tidy and arranged along the same direction when the next-stage abrasive paper is replaced every time, the metallographic specimen is rotated by 90 degrees and polished again when the next-stage abrasive paper is replaced, the lower surface of the metallographic specimen is kept horizontal due to uniform force in the polishing process, the method comprises the following steps of 600 # 、800 # 、1000 # 、1200 # The sand paper is polished by dry grinding 1500 # The sand paper is polished by water mill;
the mechanical polishing method in the rough grinding-fine grinding-mechanical polishing comprises the following steps: washing the surface of the metallographic sample after rough grinding and fine grinding by water, then uniformly smearing polishing paste with the particle size of 2.5 mu m, polishing scratches on the surface of the metallographic sample in the direction perpendicular to the linear speed direction of a polishing machine, sprinkling water on the surface of polishing cloth to keep moist during polishing, continuously polishing the scratches on the surface of the metallographic sample by water after the scratches on the surface of the metallographic sample are polished, and wiping and drying the metallographic sample by adopting cotton dipped with ethanol after washing by water after polishing;
step three, erosion: and (3) placing the corrosive agent in a water bath furnace at 73 ℃ for heat preservation, then clamping the metallographic specimen to be corroded in the second step by using forceps, immersing the metallographic specimen in the heat preservation corrosive agent, enabling the polished surface to face upwards and continuously shaking for corrosion, timing for corrosion by using a stopwatch for 47s, taking out the metallographic specimen after the surface starts darkening and blackening for 8-9 s, taking out the metallographic specimen, washing off the surface dark substances by using clear water, dipping the metallographic specimen in ethanol by using cotton, wiping and drying for metallographic tissue observation.
Fig. 5 is a metallographic structure diagram (500×) of a Ti-containing microalloyed steel eroded by the alloy steel etchant of the present example, and it can be seen from fig. 5 that the original austenite grain boundaries and the intra-grain martensite structure of the Ti-containing microalloyed steel are clearly shown at the same time.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (9)
1. An alloy steel corrosive agent is characterized in that supersaturated bittering acid aqueous solution, seagull-plate anti-dandruff shampoo, hydrofluoric acid and xylene are mixed according to the proportion of 1000-1700: 30-50: 1:2 by volume.
2. An alloy steel etchant according to claim 1, characterized by a supersaturated aqueous picric acid solution, gull-plate anti-dandruff shampoo, hydrofluoric acid and xylene according to 1200:40:1:2 by volume.
3. A method for preparing the alloy steel etchant according to claim 1 or 2, characterized in that the method comprises the steps of:
step one, preparing supersaturated picric acid aqueous solution: heating distilled water to 85-95 ℃, adding excessive picric acid, stirring to fully dissolve the picric acid, and taking supernatant to obtain supersaturated picric acid aqueous solution;
step two, mixing: placing the supersaturated picric acid aqueous solution prepared in the first step into a glass container, placing into a water bath device which is preheated to 70-75 ℃ for cooling to the water bath temperature, then adding the seagull plate anti-dandruff shampoo, hydrofluoric acid and dimethylbenzene according to the proportion of the alloy steel corrosive agent, and uniformly stirring to obtain the alloy steel corrosive agent.
4. The method according to claim 3, wherein in the first step, distilled water is poured into a beaker and then placed on a resistance furnace to be heated to 85-95 ℃; in the second step, the glass container is a beaker, and the water bath device is a water bath furnace.
5. A method of using the alloy steel etchant according to claim 1 or 2, comprising the steps of:
step one, heat treatment and deformation of Ti-containing microalloyed steel: the Ti-containing microalloy steel is subjected to heat preservation at 1100-1250 ℃ for 3-6 h, then is rolled, and is immediately quenched to room temperature to obtain a hot rolled plate; the rolling temperature is 900-1100 ℃, and the rolling reduction is 35-65%;
step two, rough grinding, fine grinding and mechanical polishing: cutting the hot rolled plate obtained in the first step into a metallographic specimen, embedding the metallographic specimen, and then carrying out rough grinding, fine grinding and mechanical polishing to obtain the metallographic specimen to be corroded;
step three, erosion: placing the corrosive agent in a water bath furnace with the temperature of 70-75 ℃, then clamping the metallographic specimen to be corroded in the second step by using tweezers, immersing the metallographic specimen in the thermal-insulation corrosive agent, enabling the polished surface to face upwards and continuously shaking for corrosion, taking out the metallographic specimen after the surface starts darkening and blackening for 8-9 s, flushing off dark substances on the surface by using clear water, dipping in ethanol by using cotton, wiping and drying for metallographic structure observation.
6. The method according to claim 5, wherein the Ti-containing microalloyed steel in step one consists of the following components in percentage by mass: 0.05 to 0.25 percent of C, 0.01 to 0.1 percent of Ti, 0.15 to 0.3 percent of Si, 0.8 to 2.0 percent of Mn, 0.01 to 0.04 percent of Als, less than or equal to 0.03 percent of P, less than or equal to 0.025 percent of S, less than or equal to 0.007 percent of N, the balance of Fe and unavoidable impurities, the thickness of the Ti-containing microalloy steel is 6 to 12mm, and the thickness of the hot rolled plate is 4.2 to 4.8mm.
7. The method according to claim 5, wherein the coarse grinding-fine grinding-mechanical polishing method in the second step is: adopting 400 to sample the metallographic specimen after the sample is inlaid # Silicon carbide metallographic sand paper is polished to remove surface inserts and pollutants, and then 600 is adopted in sequence # →800 # →1000 # →1200 # →1500 # The abrasive paper is polished, the scratch directions of the surface of the metallographic specimen are ensured to be tidy and arranged along the same direction when the next-stage abrasive paper is replaced every time, the metallographic specimen is rotated by 90 degrees and polished again when the next-stage abrasive paper is replaced, the lower surface of the metallographic specimen is kept horizontal due to uniform force in the polishing process, the method comprises the following steps of 600 # 、800 # 、1000 # 、1200 # The sand paper is polished by dry grinding 1500 # The sand paper is polished by water mill.
8. The method according to claim 5, wherein the mechanical polishing in the rough grinding-fine grinding-mechanical polishing in the second step comprises the steps of: the surface of the metallographic specimen after rough grinding and fine grinding is washed clean by water, then polishing paste with the grain diameter of 2.5 mu m is uniformly smeared, scratches on the surface of the metallographic specimen are polished perpendicular to the linear speed direction of a polishing machine, water is sprayed on the surface of polishing cloth to keep moist during polishing, water polishing is continuously carried out on the polishing cloth after the scratches on the surface of the metallographic specimen are polished clean, and cotton is adopted to dip ethanol for wiping and blow-drying after the metallographic specimen is washed with water.
9. The method according to claim 5, wherein the original austenite grain boundaries and the intra-grain martensite structure of the Ti microalloyed steel are observed simultaneously when the metallographic structure is observed in the second step.
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