CN114808095A - Electrolytic etching method for displaying two-phase structure and grain boundary of duplex stainless steel - Google Patents
Electrolytic etching method for displaying two-phase structure and grain boundary of duplex stainless steel Download PDFInfo
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- 238000000866 electrolytic etching Methods 0.000 title claims abstract description 132
- 229910001039 duplex stainless steel Inorganic materials 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 32
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 67
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 58
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 238000005868 electrolysis reaction Methods 0.000 claims description 73
- 229910001220 stainless steel Inorganic materials 0.000 claims description 34
- 239000010935 stainless steel Substances 0.000 claims description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 13
- 238000005530 etching Methods 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 239000011651 chromium Substances 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 10
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 8
- 229910052804 chromium Inorganic materials 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910018648 Mn—N Inorganic materials 0.000 claims description 2
- 229910003296 Ni-Mo Inorganic materials 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical class [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 claims description 2
- 230000009977 dual effect Effects 0.000 claims 2
- 230000001747 exhibiting effect Effects 0.000 claims 1
- 229910001566 austenite Inorganic materials 0.000 abstract description 12
- 239000013078 crystal Substances 0.000 abstract description 7
- 229910045601 alloy Inorganic materials 0.000 abstract description 4
- 239000000956 alloy Substances 0.000 abstract description 4
- 238000005498 polishing Methods 0.000 description 49
- 239000000243 solution Substances 0.000 description 16
- 230000003628 erosive effect Effects 0.000 description 15
- 239000000463 material Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 13
- 239000000843 powder Substances 0.000 description 13
- 238000005520 cutting process Methods 0.000 description 12
- 239000011521 glass Substances 0.000 description 12
- 239000007787 solid Substances 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 229910052748 manganese Inorganic materials 0.000 description 7
- 239000011572 manganese Substances 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 229910003460 diamond Inorganic materials 0.000 description 6
- 239000010432 diamond Substances 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- 239000004744 fabric Substances 0.000 description 6
- 239000007921 spray Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 229910000859 α-Fe Inorganic materials 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 238000003486 chemical etching Methods 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
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- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
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- 230000003287 optical effect Effects 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
- C25F3/06—Etching of iron or steel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/42—Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
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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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- Mechanical Engineering (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses an electrolytic etching method for displaying a two-phase structure and a grain boundary of duplex stainless steel, which comprises the following steps: s1, preparing an electrolytic etching agent I and an electrolytic etching agent II; s2, soaking the duplex stainless steel sample in an electrolytic etching agent I for electrolytic etching; s3, taking the duplex stainless steel sample processed in the step S2 out of the electrolytic etching agent I, cleaning and drying the duplex stainless steel sample, and then soaking the duplex stainless steel sample in an electrolytic etching agent II for electrolytic etching; s4, taking the duplex stainless steel sample processed in the step S3 out of the electrolytic etching agent II, and cleaning and drying to obtain an etched duplex stainless steel sample; wherein the electrolytic etching agent I is potassium hydroxide aqueous solution with the concentration of 10-30%; the electrolytic etching agent II is concentrated nitric acid with volume concentration of 60-70%. The electrolytic etching method can quickly and effectively display the grain boundary of the crystal grains to obtain the relevant information of the shape, the size and the like of the ferrite-austenite two-phase crystal grains in the alloy.
Description
Technical Field
The invention relates to the technical field of metallographic erosion methods, in particular to an electrolytic etching method for displaying a two-phase structure and a grain boundary of a two-phase stainless steel.
Background
Resource-saving duplex stainless steel, the adopted strategy is to partially replace the contents of Ni and Mo by low-cost austenitizing elements N and Mn. Although the resource saving type duplex stainless steel is cost-effective due to the low concentration of Ni and Mo, it is superior in strength and ductility to ferritic SUS 430, austenitic SUS 304, and other high Ni content duplex stainless steels while greatly reducing quality requirements and ensuring good corrosion resistance. Especially, the cost and resources are further strictly controlled in the modern society, so that the economical duplex stainless steel gradually shows a new corner. Meanwhile, the metastable austenite of the resource-saving duplex stainless steel can generate TRIP and/or TWIP effect, so that the mechanical property is broken through, the application in some severe performance fields is expanded, and the application range of the resource-saving duplex stainless steel is continuously expanded.
The duplex stainless steel sample is subjected to mechanical polishing and metallographic erosion, and the tissue is observed by adopting an optical metallographic microscope or a scanning electron microscope. Then the rational performance is achieved by properly adjusting the components and the production process. The methods generally used for metallographic etching of duplex stainless steel mainly include chemical etching and electrolytic etching: the chemical etching comprises the following steps: beraha II ethchant (60mL H) 2 O+30mL HCl+1g K 2 S 2 O 2 ) The Chinese patent CN103123318A discloses a duplex stainless steel metallographic corrosive liquid, the volume of which is as follows: bitter tasteAcid taste: carrying out erosion on the solution of absolute ethyl alcohol in a ratio of 5:1: 100; chinese patent CN106248460A discloses a metallographic corrosion method for duplex stainless steel, which comprises the steps of corroding a sample by using ferric trichloride and hydrochloric acid aqueous solution with the mass concentration of 0.05-0.3% and the pH value of less than or equal to 2; the electrolytic etching comprises the following steps: oxalic acid electrolytic etching, potassium hydroxide/sodium electrolytic etching, ferric chloride electrolytic etching, etc. However, the current etching method usually obtains the metallurgical phase distribution of one phase or multiple phases in the alloy, and only can observe the phase boundary of ferrite and austenite with simple structural distribution, particularly can not display the two-phase grain boundary of the duplex stainless steel, and the observation of the grain size and the shape is carried out. The duplex stainless steel has strict requirements on grain size, so that the display technology of the two-phase grain boundary is particularly important, and the display technology has important significance for technical personnel to judge whether the part has coarse grains, optimize the rolling process and popularize the application of the resource-saving duplex stainless steel.
Disclosure of Invention
The invention aims to provide an electrolytic etching method for displaying a two-phase structure and a grain boundary of a duplex stainless steel, which can effectively and accurately obtain the two-phase structure and the grain boundary of the duplex stainless steel.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides an electrolytic etching method for displaying two-phase structure and grain boundary of duplex stainless steel, which comprises the following steps:
s1, preparing an electrolytic etching agent I and an electrolytic etching agent II;
s2, soaking the duplex stainless steel sample in an electrolytic etching agent I for electrolytic etching;
s3, taking the duplex stainless steel sample processed in the step S2 out of the electrolytic etching agent I, cleaning and drying the duplex stainless steel sample, and then soaking the duplex stainless steel sample in an electrolytic etching agent II for electrolytic etching;
s4, taking the duplex stainless steel sample processed in the step S3 out of the electrolytic etching agent II, and cleaning and drying to obtain an etched duplex stainless steel sample;
wherein the electrolytic etching agent I is a potassium hydroxide aqueous solution with the concentration of 10-30%, and the electrolytic etching agent II is concentrated nitric acid with the volume concentration of 60-70%.
In the invention, a two-step electrolytic etching method is adopted, so that a two-phase structure and a grain boundary of the duplex stainless steel can be clearly displayed. In the first step, a potassium hydroxide aqueous solution is used as an electrolytic etching agent I, and by utilizing the characteristics that the two phases of ferrite and austenite have different corrosion resistance and are not easy to over-corrode in the electrolytic etching agent I, the two-phase boundary can be clearly and visually corroded through etching, and the contrast is bright, so that the comprehensive and clear distribution of the ferrite-austenite two phases is obtained; in the second step, concentrated nitric acid is used as an electrolytic etching agent II, and crystal grain boundaries can be etched, so that the crystal grain boundaries are clearly displayed.
In the invention, the concentration of the potassium hydroxide aqueous solution in the electrolytic etching agent I is controlled to be 10-30%. If the concentration is too high, the phase boundary erosion of ferrite and austenite phases is too deep, and the observation effect is influenced; if the concentration is too low, a good etching effect cannot be achieved.
Further, in step S1, when preparing the electrolytic etchant i, the potassium hydroxide used is pure elemental powder, and the water is deionized water.
Because the electrolytic etchant I has a certain temperature after being prepared, the etchant can be used after being placed for a period of time to cool. Preferably, after preparing the electrolytic etching agent I, standing for 30-60 minutes to cool the electrolytic etching agent I to room temperature.
Further, in step S1, the concentration of the aqueous potassium hydroxide solution is 15%.
Further, in step S2, the duplex stainless steel is a resource saving Mn-N partially or completely substituted Ni-Mo type duplex stainless steel.
Further, in step S2, the components and mass fractions of the duplex stainless steel are as follows: 0.01-0.05% of carbon, 18-25% of chromium, 3.0-12.0% of manganese, 0.1-0.35% of nitrogen, 0.1-2.0% of nickel, 0.1-3.0% of copper, 0.1-0.6% of molybdenum and the balance of iron.
Further, in step S2, the duplex stainless steel sample is polished with sand paper before being etched, and then mechanically polished until the polished surface is bright and has no scratch.
Further, in steps S2 and S3, the stainless steel with Cr content of more than 10% is used as a cathode and the duplex stainless steel sample is used as an anode in the electrolytic etching.
Further, in the step S2, the voltage of electrolytic etching is 2-12V, the electrolytic time is 10-40S, the electrolytic temperature is 15-30 ℃, and the distance between the sample and the cathode is 4-6 cm.
Further, in step S3, the voltage of electrolytic etching is 1-2V, the electrolytic time is 8-12S, the electrolytic temperature is 15-30 ℃, and the distance between the sample and the cathode is 4-6 cm. Since different materials have different corrosion resistances, different etching voltages and electrolysis times need to be selected according to the properties of the materials. If the etching voltage is too high or the electrolysis time is too long, phase boundary and crystal grains are over-corroded, so that the metallographic phase is not clearly displayed and is unknown. On the contrary, if the etching voltage is too low or the electrolysis time is too short, the phase boundary and the grain boundary are not clearly displayed.
Further, in steps S3 and S4, washing of the duplex stainless steel sample was performed using absolute ethanol.
Compared with the prior art, the invention has the beneficial effects that:
1. in the resource-saving duplex stainless steel, ferrite and austenite phases have different corrosion resistance, and the invention takes common chemical reagents in a laboratory, namely potassium hydroxide and concentrated nitric acid, as an electrolytic etching agent and successfully etches out the phase boundary and the grain boundary of the two phases by a two-step etching method. Wherein, potassium hydroxide aqueous solution (electrolytic etching agent I) is used as the ferrite-austenite two-phase boundary etching agent, and the two-phase boundary can be clearly and visually eroded through the first step of electrolytic etching, so that the contrast is distinct, and the comprehensive and clear distribution of ferrite-austenite two phases is obtained. And then, concentrated nitric acid (electrolytic etching agent II) is used for carrying out second-step electrolytic etching, so that grain boundaries can be quickly and effectively shown on the basis of clear two-phase boundaries, and relevant information such as the shape, the size and the like of ferrite-austenite two-phase grains in the alloy can be obtained, which cannot be achieved by a common erosion method.
2. The invention provides an important basis for researching the two-phase distribution and the grain detail information of the duplex stainless steel, and simultaneously provides a new method for etching the duplex stainless steel, thereby having important practical application value. The method provides reliable basis for the parameters of the subsequent processing treatment process and provides accurate and reliable data parameters for practical application.
Drawings
FIG. 1 is a 500-fold metallographic structure picture of a specimen of example 1 of the present invention;
FIG. 2 is a 200-fold metallographic structure picture of a specimen of example 2 of the present invention;
FIG. 3 is a 500-fold metallographic structure picture of a specimen of example 3 of the invention;
FIG. 4 is a 1000 SEM micrograph of a specimen of example 3 of the present invention;
FIG. 5 is a 500-fold metallographic structure picture of a specimen of example 4 of the present invention;
FIG. 6 is a 500-fold metallographic structure picture of a sample of comparative example 1 of the present invention;
fig. 7 is a 500-fold metallographic structure picture of a sample of comparative example 2 of the present invention.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Example 1
The selected material is a resource-saving duplex stainless steel hot rolled plate of 20Cr3Mn1Ni, and the material comprises the following components in percentage by mass: c: 0.02%, Cr: 20%, Mn: 3%, Ni: 1%, Si: 0.35, N: 0.2 percent, and the balance being Fe; the metallographic microscope was Leica DM 13000H.
The specific operation steps of this embodiment are as follows:
the first step is as follows: and preparing a metallographic specimen.
(1) Cutting a gold phase sample from the hot rolled plate by using a molybdenum wire cutting machine;
(2) polishing the observation surface of the metallographic specimen by using 80#, 180#, 240#, 400#, 800# and 1000# sandpaper from thick to thin;
(3) and mechanically polishing the observation surface of the metallographic sample by using a metallographic polishing machine provided with velvet polishing cloth until the polishing surface is bright and has no scratch, wherein the polishing agent used for mechanical polishing is a diamond spray polishing agent with the particle size of 1.5 mu m.
The second step is that: preparing an electrolytic etching agent.
Preparing an electrolytic etching agent I: measuring 85ml of deionized water by using a measuring cylinder and pouring into a beaker; weighing 15g of potassium hydroxide solid powder by using a balance, and slowly pouring the weighed potassium hydroxide solid powder into the same beaker while continuously stirring by using a glass rod; the solution was stirred with a glass rod until completely mixed. At the moment, the etchant has a certain temperature, and the etchant is required to be placed in a room-temperature environment for standing for 30-60 minutes until the solution is cooled to 10-30 ℃, and then the etchant can be used.
Preparing an electrolytic etching agent II: 50ml of concentrated nitric acid with the concentration of 65-68% is measured by a measuring cylinder.
The third step: and (3) carrying out first-step electrolytic etching on the metallographic specimen by using a direct-current voltage-stabilizing power supply.
(1) Immersing a stainless steel bar in the electrolytic etching agent I, and connecting the stainless steel bar with the negative electrode of a direct-current stabilized power supply through a lead to be used as the cathode of an electrolytic cell;
(2) immersing the polished surface of the metallographic specimen in the electrolytic etching agent I, and connecting the polished surface of the metallographic specimen with the positive electrode of a direct-current stabilized power supply through a lead to be used as the anode of an electrolytic cell;
(3) starting electrolysis, wherein the electrolysis voltage is 8V, the electrolysis time is 25s, and the electrolysis temperature is 25 ℃. The distance between the sample and the cathode was 5cm during electrolysis. The sample was rinsed with absolute ethanol and blown dry.
The fourth step: and (3) carrying out second-step electrolytic etching on the metallographic specimen by using a direct-current voltage-stabilizing power supply.
(1) Immersing a stainless steel bar in an electrolytic etching agent II, and connecting the stainless steel bar with the negative electrode of a direct-current stabilized power supply through a lead to be used as the cathode of an electrolytic cell;
(2) immersing the polished surface of the metallographic specimen in an electrolytic etching agent II, and connecting the polished surface of the metallographic specimen with the anode of a direct-current stabilized power supply through a lead to be used as the anode of an electrolytic cell;
(3) starting electrolysis, wherein the electrolysis voltage is 1.2V, the electrolysis time is 10s, and the electrolysis temperature is 25 ℃. The distance between the sample and the cathode was 5cm during electrolysis.
The fifth step: the samples were washed and observed. And after the electrolysis is finished, taking out the metallographic sample from the electrolytic etching agent, washing the metallographic sample by absolute ethyl alcohol, and drying by a hot air blower. And (4) placing the metallographic specimen into a metallographic microscope for observation.
The erosion effect is shown in figure 1. The results show that the two-phase stainless steel electrolytically etched by the method has distinct relative ratios, clear and visible grain boundaries and good erosion effect.
Example 2
The selected material is 20Cr3Mn1Ni resource-saving duplex stainless steel plate after solution treatment, and the material comprises the following components in percentage by mass: c: 0.02%, Cr: 20%, Mn: 3%, Ni: 1%, Si: 0.35, N: 0.2 percent, and the balance being Fe; the metallographic microscope was Leica DM 13000H.
The specific operation steps of this embodiment are as follows:
the first step is as follows: and preparing a metallographic specimen.
(1) Cutting a metallographic sample from the plate by using a molybdenum wire cutting machine;
(2) polishing the observation surface of the metallographic specimen by using 80#, 180#, 240#, 400#, 800# and 1000# sandpaper from thick to thin;
(3) and mechanically polishing the observation surface of the metallographic specimen by using a metallographic polishing machine provided with velvet polishing cloth until the polishing surface is bright and has no scratches. The polishing agent used for mechanical polishing was 1.5 μm diamond spray polishing agent.
The second step is that: preparing electrolytic etching agent
Preparing an electrolytic etching agent I: measuring 85ml of deionized water by using a measuring cylinder and pouring into a beaker; weighing 15g of potassium hydroxide solid powder by using a balance, and slowly pouring the weighed potassium hydroxide solid powder into the same beaker while continuously stirring by using a glass rod; the solution was stirred with a glass rod until completely mixed. At the moment, the etchant has a certain temperature, and the etchant needs to be placed in a room-temperature environment for standing for 30-60 minutes until the solution is cooled to 10-30 ℃, and then the etchant can be used.
Preparing an electrolytic etching agent II: 50ml of concentrated nitric acid with the concentration of 65-68% is measured by a measuring cylinder.
The third step: and (3) carrying out first-step electrolytic etching on the metallographic specimen by using a direct-current voltage-stabilizing power supply.
(1) Immersing a stainless steel bar in the electrolytic etching agent I, and connecting the stainless steel bar with the negative electrode of a direct-current stabilized power supply through a lead to be used as the cathode of an electrolytic cell;
(2) immersing the polished surface of the metallographic specimen in an electrolytic etching agent I, and connecting the polished surface of the metallographic specimen with the anode of a direct-current stabilized power supply through a lead to be used as the anode of an electrolytic cell;
(3) starting electrolysis, wherein the electrolysis voltage is 8V, the electrolysis time is 30s, and the electrolysis temperature is 25 ℃. The distance between the sample and the cathode was 5cm during electrolysis. The sample was rinsed with absolute ethanol and blown dry.
The fourth step: and (3) carrying out second-step electrolytic etching on the metallographic specimen by using a direct-current voltage-stabilizing power supply.
(1) Immersing a stainless steel bar in an electrolytic etching agent II, and connecting the stainless steel bar with the negative electrode of a direct-current stabilized power supply through a lead to be used as the cathode of an electrolytic cell;
(2) immersing the polished surface of the metallographic specimen in an electrolytic etching agent II, and connecting the polished surface of the metallographic specimen with the anode of a direct-current stabilized power supply through a lead to be used as the anode of an electrolytic cell;
(3) starting electrolysis, wherein the electrolysis voltage is 1.3V, the electrolysis time is 10s, and the electrolysis temperature is 25 ℃. The distance between the sample and the cathode was 5cm during electrolysis.
The fifth step: the samples were washed and observed. After the electrolysis is finished, taking out the metallographic sample from the electrolytic etching agent, washing the metallographic sample by absolute ethyl alcohol, and drying by a hot air blower; and (4) placing the metallographic specimen into a metallographic microscope for observation.
The erosion effect is shown in figure 2. The results show that the two-phase stainless steel electrolytically etched by the method has distinct relative ratios, clear and visible grain boundaries and good erosion effect.
Example 3
The selected material is 20Cr3Mn1Ni2Cu resource-saving duplex stainless steel plate after solution treatment, and the material comprises the following components in percentage by mass: c: 0.02%, Cr: 20%, Mn: 3%, Ni: 1%, Cu: 2%, Si: 0.35, N: 0.2 percent, and the balance being Fe; the metallographic microscope was model Leica DM 13000H.
The specific operation steps of this embodiment are as follows:
the first step is as follows: and preparing a metallographic specimen.
(1) Cutting a metallographic sample from the plate by using a molybdenum wire cutting machine;
(2) polishing the observation surface of the metallographic specimen by using 80#, 180#, 240#, 400#, 800# and 1000# sandpaper from thick to thin;
(3) and mechanically polishing the observation surface of the metallographic specimen by using a metallographic polishing machine provided with velvet polishing cloth until the polishing surface is bright and has no scratches. The polishing agent used for mechanical polishing was 1.5 μm diamond spray polishing agent.
The second step is that: preparing electrolytic etching agent
Preparing an electrolytic etching agent I: measuring 85ml of deionized water by using a measuring cylinder and pouring into a beaker; weighing 15g of potassium hydroxide solid powder by using a balance, and slowly pouring the weighed potassium hydroxide solid powder into the same beaker while continuously stirring by using a glass rod; the solution was stirred with a glass rod until completely mixed. At the moment, the etchant has a certain temperature, and the etchant needs to be placed in a room-temperature environment for standing for 30-60 minutes until the solution is cooled to 10-30 ℃, and then the etchant can be used.
Preparing an electrolytic etching agent II: 50ml of concentrated nitric acid with the concentration of 65-68% is measured by a measuring cylinder.
The third step: and (3) carrying out first-step electrolytic etching on the metallographic specimen by using a direct-current voltage-stabilizing power supply.
(1) Immersing a stainless steel bar in the electrolytic etching agent I, and connecting the stainless steel bar with the negative electrode of a direct-current stabilized power supply through a lead to be used as the cathode of an electrolytic cell;
(2) immersing the polished surface of the metallographic specimen in an electrolytic etching agent I, and connecting the polished surface of the metallographic specimen with the anode of a direct-current stabilized power supply through a lead to be used as the anode of an electrolytic cell;
(3) starting electrolysis, wherein the electrolysis voltage is 10V, the electrolysis time is 25s, and the electrolysis temperature is 25 ℃. The distance between the sample and the cathode was 5cm during electrolysis. The sample was rinsed with absolute ethanol and blown dry.
The fourth step: and (3) carrying out second-step electrolytic etching on the metallographic specimen by using a direct-current voltage-stabilizing power supply.
(1) Immersing a stainless steel bar in an electrolytic etching agent II, and connecting the stainless steel bar with the negative electrode of a direct-current stabilized power supply through a lead to be used as the cathode of an electrolytic cell;
(2) immersing the polished surface of the metallographic specimen in an electrolytic etching agent II, and connecting the polished surface of the metallographic specimen with the anode of a direct-current stabilized power supply through a lead to be used as the anode of an electrolytic cell;
(3) starting electrolysis, wherein the electrolysis voltage is 1.3V, the electrolysis time is 12s, and the electrolysis temperature is 25 ℃. The distance between the sample and the cathode was 5cm during electrolysis.
The fifth step: the samples were washed and observed. After the electrolysis is finished, taking out the metallographic sample from the electrolytic etching agent, washing the metallographic sample by absolute ethyl alcohol, and drying by a hot air blower; and (4) placing the metallographic specimen into a metallographic microscope for observation.
The erosion effect is shown in fig. 3 and 4. The results show that the two-phase stainless steel etched by the method has distinct relative ratios, clear crystal grain boundaries and good erosion effect.
Example 4
The selected material is a resource-saving duplex stainless steel hot rolled plate of 20Cr6Mn1Ni, and the material comprises the following components in percentage by mass: c: 0.02%, Cr: 20%, Mn: 6%, Ni: 1%, Si: 0.35, N: 0.2 percent, and the balance being Fe; the metallographic microscope was Leica DM 13000H.
The specific operation steps of this embodiment are as follows:
the first step is as follows: and preparing a metallographic specimen.
(1) Cutting a gold phase sample from the hot rolled plate by using a molybdenum wire cutting machine;
(2) polishing the observation surface of the metallographic specimen by using 80#, 180#, 240#, 400#, 800# and 1000# sandpaper from thick to thin;
(3) and mechanically polishing the observation surface of the metallographic specimen by using a metallographic polishing machine provided with velvet polishing cloth until the polishing surface is bright and has no scratches. The polishing agent used for mechanical polishing was 1.5 μm diamond spray polishing agent.
The second step is that: preparing electrolytic etching agent
Preparing an electrolytic etching agent I: measuring 85ml of deionized water by using a measuring cylinder and pouring into a beaker; weighing 15g of potassium hydroxide solid powder by using a balance, and slowly pouring the weighed potassium hydroxide solid powder into the same beaker while continuously stirring by using a glass rod; the solution was stirred with a glass rod until completely mixed. At the moment, the etchant has a certain temperature, and the etchant needs to be placed in a room-temperature environment for standing for 30-60 minutes until the solution is cooled to 10-30 ℃, and then the etchant can be used.
Preparing an electrolytic etching agent II: 50ml of concentrated nitric acid with the concentration of 65-68% is measured by a measuring cylinder.
The third step: and (3) carrying out first-step electrolytic etching on the metallographic specimen by using a direct-current voltage-stabilizing power supply.
(1) Immersing a stainless steel bar in the electrolytic etching agent I, and connecting the stainless steel bar with the negative electrode of a direct-current stabilized power supply through a lead to be used as the cathode of an electrolytic cell;
(2) immersing the polished surface of the metallographic specimen in an electrolytic etching agent I, and connecting the polished surface of the metallographic specimen with the anode of a direct-current stabilized power supply through a lead to be used as the anode of an electrolytic cell;
(3) starting electrolysis, wherein the electrolysis voltage is 10V, the electrolysis time is 30s, and the electrolysis temperature is 25 ℃. The distance between the sample and the cathode was 5cm during electrolysis. The sample was rinsed with absolute ethanol and blown dry.
The fourth step: and (3) carrying out second-step electrolytic etching on the metallographic specimen by using a direct-current voltage-stabilizing power supply.
(1) Immersing a stainless steel bar in an electrolytic etching agent II, and connecting the stainless steel bar with the negative electrode of a direct-current stabilized power supply through a lead to be used as the cathode of an electrolytic cell;
(2) immersing the polished surface of the metallographic specimen in an electrolytic etching agent II, and connecting the polished surface of the metallographic specimen with the anode of a direct-current stabilized power supply through a lead to be used as the anode of an electrolytic cell;
(3) starting electrolysis, wherein the electrolysis voltage is 1.5V, the electrolysis time is 12s, and the electrolysis temperature is 25 ℃. The distance between the sample and the cathode was 5cm during electrolysis.
The fifth step: the samples were washed and observed. After the electrolysis is finished, taking out the metallographic sample from the electrolytic etching agent, washing the metallographic sample by absolute ethyl alcohol, and drying by a hot air blower; and (4) placing the metallographic specimen into a metallographic microscope for observation.
The erosion effect is shown in figure 5. The results show that the two-phase stainless steel electrolytically etched by the method has distinct relative ratios, clear and visible grain boundaries and good erosion effect.
Comparative example 1
The selected material is 20Cr6Mn1Ni resource-saving duplex stainless steel plate after solution treatment, and comprises the following components in percentage by mass: c: 0.02%, Cr: 20%, Mn: 6%, Ni: 1%, Si: 0.35, N: 0.2 percent, and the balance being Fe; the metallographic microscope was Leica DM 13000H.
The specific operation steps of this embodiment are as follows:
the first step is as follows: and preparing a metallographic specimen.
(1) Cutting a gold phase sample from the hot rolled plate by using a molybdenum wire cutting machine;
(2) polishing the observation surface of the metallographic specimen by using 80#, 180#, 240#, 400#, 800# and 1000# sandpaper from thick to thin;
(3) and mechanically polishing the observation surface of the metallographic sample by using a metallographic polishing machine provided with velvet polishing cloth until the polishing surface is bright and has no scratch. The polishing agent used for mechanical polishing was 1.5 μm diamond spray polishing agent.
The second step is that: preparing electrolytic etching agent
Preparing an electrolytic etching agent I: measuring 85ml of deionized water by using a measuring cylinder and pouring into a beaker; weighing 15g of potassium hydroxide solid powder by using a balance, and slowly pouring the weighed potassium hydroxide solid powder into the same beaker while continuously stirring by using a glass rod; the solution was stirred with a glass rod until completely mixed. At the moment, the etchant has a certain temperature, and the etchant needs to be placed in a room-temperature environment for standing for 30-60 minutes until the solution is cooled to 10-30 ℃, and then the etchant can be used.
Preparing an electrolytic etching agent II: 50ml of concentrated nitric acid with the concentration of 65-68% is measured by a measuring cylinder.
The third step: and (3) carrying out first-step electrolytic etching on the metallographic specimen by using a direct-current voltage-stabilizing power supply.
(1) Immersing a stainless steel bar in the electrolytic etching agent I, and connecting the stainless steel bar with the negative electrode of a direct-current stabilized power supply through a lead to be used as the cathode of an electrolytic cell;
(2) immersing the polished surface of the metallographic specimen in an electrolytic etching agent I, and connecting the polished surface of the metallographic specimen with the anode of a direct-current stabilized power supply through a lead to be used as the anode of an electrolytic cell;
(3) starting electrolysis, wherein the electrolysis voltage is 10V, the electrolysis time is 30s, and the electrolysis temperature is 25 ℃. The distance between the sample and the cathode was 5cm during electrolysis. The sample was rinsed with absolute ethanol and blown dry.
The fourth step: and (3) carrying out second-step electrolytic etching on the metallographic specimen by using a direct-current voltage-stabilizing power supply.
(1) Immersing a stainless steel bar in an electrolytic etching agent II, and connecting the stainless steel bar with the negative electrode of a direct-current stabilized power supply through a lead to be used as the cathode of an electrolytic cell;
(2) immersing the polished surface of the metallographic specimen in an electrolytic etching agent II, and connecting the polished surface of the metallographic specimen with the anode of a direct-current stabilized power supply through a lead to be used as the anode of an electrolytic cell;
(3) starting electrolysis, wherein the electrolysis voltage is 1.2V, the electrolysis time is 12s, and the electrolysis temperature is 25 ℃. The distance between the sample and the cathode was 5cm during electrolysis.
The fifth step: the samples were washed and observed. After the electrolysis is finished, taking out the metallographic sample from the electrolytic etching agent, washing the metallographic sample by absolute ethyl alcohol, and drying by a hot air blower; and (4) placing the metallographic specimen into a metallographic microscope for observation.
The erosion effect is shown in figure 6. The results show that the electrolytic etching voltage in the fourth step is insufficient, so that the grain boundaries are not clearly displayed, and the electrolytic voltage in the fourth step needs to be increased.
Comparative example 2
The selected material is 20Cr3Mn1Ni2Cu resource-saving duplex stainless steel cold-rolled sheet material, and the components of the sheet material by mass percent are as follows: c: 0.02%, Cr: 20%, Mn: 3%, Ni: 1%, Cu: 2%, Si: 0.35, N: 0.2 percent, and the balance being Fe; the metallographic microscope was Leica DM 13000H.
The specific operation steps of this embodiment are as follows:
the first step is as follows: and preparing a metallographic specimen.
(1) Cutting a gold phase sample from the hot rolled plate by using a molybdenum wire cutting machine;
(2) polishing the observation surface of a metallographic sample by using 80#, 180#, 240#, 400#, 800# and 1000# sandpaper from thick to thin;
(3) and mechanically polishing the observation surface of the metallographic specimen by using a metallographic polishing machine provided with velvet polishing cloth until the polishing surface is bright and has no scratches. The polishing agent used for mechanical polishing was 1.5 μm diamond spray polishing agent.
The second step is that: preparing electrolytic etching agent
Preparing an electrolytic etching agent I: measuring 75ml of deionized water by using a measuring cylinder and pouring into a beaker; weighing 25g of potassium hydroxide solid powder by using a balance, and slowly pouring the weighed potassium hydroxide solid powder into the same beaker while continuously stirring by using a glass rod; the solution was stirred with a glass rod until completely mixed. At the moment, the etchant has a certain temperature, and the etchant needs to be placed in a room-temperature environment for standing for 30-60 minutes until the solution is cooled to 10-30 ℃, and then the etchant can be used.
Preparing an electrolytic etching agent II: 50ml of concentrated nitric acid with the concentration of 65-68% is measured by a measuring cylinder.
The third step: and (3) carrying out first-step electrolytic etching on the metallographic specimen by using a direct-current voltage-stabilizing power supply.
(1) Immersing a stainless steel bar in the electrolytic etching agent I, and connecting the stainless steel bar with the negative electrode of a direct-current stabilized power supply through a lead to be used as the cathode of an electrolytic cell;
(2) immersing the polished surface of the metallographic specimen in an electrolytic etching agent I, and connecting the polished surface of the metallographic specimen with the anode of a direct-current stabilized power supply through a lead to be used as the anode of an electrolytic cell;
(3) starting electrolysis, wherein the electrolysis voltage is 10V, the electrolysis time is 25s, and the electrolysis temperature is 25 ℃. The distance between the sample and the cathode was 5cm during electrolysis. The sample was rinsed with absolute ethanol and blown dry.
The fourth step: and (3) carrying out second-step electrolytic etching on the metallographic specimen by using a direct-current voltage-stabilizing power supply.
(1) Immersing a stainless steel bar in an electrolytic etching agent II, and connecting the stainless steel bar with the negative electrode of a direct-current stabilized power supply through a lead to be used as the cathode of an electrolytic cell;
(2) immersing the polished surface of the metallographic specimen in an electrolytic etching agent II, and connecting the polished surface of the metallographic specimen with the anode of a direct-current stabilized power supply through a lead to be used as the anode of an electrolytic cell;
(3) starting electrolysis, wherein the electrolysis voltage is 1.5V, the electrolysis time is 12s, and the electrolysis temperature is 25 ℃. The distance between the sample and the cathode was 5cm during electrolysis.
The fifth step: the samples were washed and observed. After the electrolysis is finished, taking out the metallographic sample from the electrolytic etching agent, washing the metallographic sample by absolute ethyl alcohol, and drying by a hot air blower; and (4) placing the metallographic specimen into a metallographic microscope for observation.
The erosion effect is shown in figure 7. The result shows that the concentration of the potassium hydroxide aqueous solution in the second step of the electrolytic etching agent I is too high, so that the two-phase boundary is etched too deeply during electrolytic etching; and the etching voltage in the fourth step is too high, so that the crystal grains are over-corroded, and the metallographic display is unclear and unclear.
In summary, the invention provides a new etching method for duplex stainless steel, which can respectively etch out the phase boundary and the grain boundary of two phases through two-step electrolytic etching, thereby obtaining the comprehensive and clear distribution of ferrite-austenite two phases and the relevant information of the shape, size and the like of ferrite-austenite two-phase grains in the alloy.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (9)
1. An electrolytic etching method for displaying a two-phase structure and a grain boundary of a duplex stainless steel is characterized by comprising the following steps of:
s1, preparing an electrolytic etching agent I and an electrolytic etching agent II;
s2, soaking the duplex stainless steel sample in an electrolytic etching agent I for electrolytic etching;
s3, taking the duplex stainless steel sample processed in the step S2 out of the electrolytic etching agent I, cleaning and drying the duplex stainless steel sample, and then soaking the duplex stainless steel sample in an electrolytic etching agent II for electrolytic etching;
s4, taking the duplex stainless steel sample processed in the step S3 out of the electrolytic etching agent II, and cleaning and drying to obtain an etched duplex stainless steel sample;
wherein the electrolytic etching agent I is a potassium hydroxide aqueous solution with the concentration of 10-30 percent; the electrolytic etching agent II is concentrated nitric acid with volume concentration of 60-70%.
2. The electrolytic etching method for showing the two-phase structure and grain boundary of duplex stainless steel as claimed in claim 1, wherein step S1 is performed by preparing electrolytic etchant i and then standing for 30-60 minutes.
3. The electrolytic etching method for displaying the two-phase structure and grain boundaries of a duplex stainless steel according to claim 1, wherein in step S2, the duplex stainless steel is a resource-saving Mn-N partially or completely substituted Ni-Mo type duplex stainless steel.
4. The electrolytic etching method for displaying the two-phase structure and the grain boundary of the duplex stainless steel according to claim 3, wherein in the step S2, the components and the mass fractions of the duplex stainless steel are as follows: 0.01-0.05% of carbon, 18-25% of chromium, 3.0-12.0% of manganese, 0.1-0.35% of nitrogen, 0.1-2.0% of nickel, 0.1-3.0% of copper, 0.1-0.6% of molybdenum and the balance of iron.
5. The electrolytic etching method for displaying the two-phase structure and grain boundary of duplex stainless steel according to claim 1, wherein in step S2, the duplex stainless steel sample is sanded and then mechanically polished before etching until the polished surface is bright and has no scratch.
6. The electrolytic etching method for dual phase stainless steel showing two-phase structure and grain boundary of claim 1, wherein in the step of S2 and S3, the stainless steel with Cr content more than 10% is used as cathode and the dual phase stainless steel sample is used as anode.
7. The electrolytic etching method for displaying the two-phase structure and the grain boundary of the duplex stainless steel according to claim 1, wherein in step S2, the voltage of electrolytic etching is 2-12V, the electrolysis time is 10-40S, the electrolysis temperature is 15-30 ℃, and the distance between the sample and the cathode is 4-6 cm.
8. The electrolytic etching method for displaying the two-phase structure and the grain boundary of the duplex stainless steel according to claim 1, wherein in step S3, the voltage of electrolytic etching is 1-2V, the electrolysis time is 8-12S, the electrolysis temperature is 15-30 ℃, and the distance between the sample and the cathode is 4-6 cm.
9. The electrolytic etching method for exhibiting the two-phase structure and grain boundaries of duplex stainless steel according to claim 1, wherein the cleaning of the duplex stainless steel sample is performed using absolute ethanol in steps S3 and S4.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103792128A (en) * | 2014-02-21 | 2014-05-14 | 山西太钢不锈钢股份有限公司 | Method for displaying two-phase grain boundary of duplex stainless steel |
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| CN111077005A (en) * | 2020-01-03 | 2020-04-28 | 昆明理工大学 | Method for displaying thermal deformation recrystallization grain boundary of duplex stainless steel |
| CN113325020A (en) * | 2021-06-24 | 2021-08-31 | 北京科技大学 | Metallographic erosion method for observing duplex stainless steel welded joint under SEM |
| CN217277269U (en) * | 2021-12-31 | 2022-08-23 | 江苏天鼎检测科技有限公司 | Measuring equipment for detecting grain size in duplex stainless steel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103792128A (en) * | 2014-02-21 | 2014-05-14 | 山西太钢不锈钢股份有限公司 | Method for displaying two-phase grain boundary of duplex stainless steel |
| CN108426883A (en) * | 2018-03-22 | 2018-08-21 | 钢铁研究总院 | A kind of aggressive agent and corrosion method of two phase stainless steel |
| CN111077005A (en) * | 2020-01-03 | 2020-04-28 | 昆明理工大学 | Method for displaying thermal deformation recrystallization grain boundary of duplex stainless steel |
| CN113325020A (en) * | 2021-06-24 | 2021-08-31 | 北京科技大学 | Metallographic erosion method for observing duplex stainless steel welded joint under SEM |
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