CN114481134B - Corrosive liquid for displaying austenitic grain size of T91 steel and method for displaying austenitic grain size of T91 steel - Google Patents
Corrosive liquid for displaying austenitic grain size of T91 steel and method for displaying austenitic grain size of T91 steel Download PDFInfo
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- CN114481134B CN114481134B CN202210127173.4A CN202210127173A CN114481134B CN 114481134 B CN114481134 B CN 114481134B CN 202210127173 A CN202210127173 A CN 202210127173A CN 114481134 B CN114481134 B CN 114481134B
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 56
- 239000010959 steel Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000007788 liquid Substances 0.000 title claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910001566 austenite Inorganic materials 0.000 claims abstract description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 230000000694 effects Effects 0.000 claims abstract description 9
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 8
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 5
- 238000005260 corrosion Methods 0.000 claims abstract description 5
- 230000007797 corrosion Effects 0.000 claims abstract description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000000691 measurement method Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000004381 surface treatment Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 18
- 238000010586 diagram Methods 0.000 description 16
- 235000019441 ethanol Nutrition 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 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 description 7
- 238000005530 etching Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 241000282326 Felis catus Species 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910000734 martensite Inorganic materials 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/28—Acidic compositions for etching iron group metals
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/18—Hardening; Quenching with or without subsequent tempering
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Pathology (AREA)
- Immunology (AREA)
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
The invention discloses a corrosive liquid for displaying the austenite grain size of T91 steel and a method for displaying the austenite grain size of the T91 steel, wherein the corrosive liquid comprises the following substances in proportion: sodium dodecyl benzene sulfonate: ferric chloride: 36% -38% hydrochloric acid: absolute ethanol = 1g:4.5 to 5.5g: 45-55 mL: 90-110 mL; through heat treatment and surface treatment of the T91 steel sample and corrosion treatment by using the corrosive liquid, the austenitic grain boundary of the T91 steel can be clearly displayed, the austenitic grain size of the T91 steel can be measured, the metallographic display effect is improved, and the technical problem of incomplete grain boundary display or display is solved.
Description
Technical Field
The invention belongs to the technical field of metallurgical analysis, and particularly relates to a corrosive liquid for displaying the austenitic grain size of T91 steel and a method for displaying the austenitic grain size of T91 steel.
Background
The grain size of the steel has great influence on mechanical properties, physical properties and chemical properties, so that the evaluation of the actual grain size has great significance for judging the quality of the steel, checking the correctness of a hot working process, researching the influence of the grain size on related properties and the like.
T91 steel is a novel martensitic heat-resistant steel developed by the cooperation of American national treelike laboratory and the metallurgical materials laboratory of the American combustion engineering company. The method reduces the carbon content on the basis of 9Cr1MoV steel, strictly limits the contents of sulfur and phosphorus, and adds a small amount of vanadium and niobium elements for alloying. The matrix structure of the alloy is tempered martensite, and the alloy cannot be well displayed by common reagents such as 4% nitrate alcohol solution or saturated picric acid solution, cannot display grain boundaries or is incomplete, and has low efficiency.
Disclosure of Invention
The invention aims to provide a corrosive liquid for displaying the austenite grain size of T91 steel, which has simple composition and convenient preparation, and can clearly display grain boundaries by corroding the T91 steel, and determine the austenite grain size of the T91 steel.
The invention also aims to provide a method for displaying the austenite grain size of the T91 steel, which can clearly display the austenite grain boundary of the T91 steel by heat treatment, surface treatment and corrosion treatment of the T91 steel sample by using the corrosive liquid in the invention, and determine the austenite grain size of the T91 steel.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
An etching solution showing austenite grain size of T91 steel, which consists of the following substances in proportion: sodium dodecyl benzene sulfonate: ferric chloride: 36% -38% hydrochloric acid: absolute ethanol = 1g:4.5 to 5.5g: 45-55 mL: 90-110 mL.
A method of displaying austenite grain size of T91 steel, the method comprising the steps of:
(1) Heat treatment of the sample;
(2) Carrying out rough grinding, fine grinding and polishing treatment on the heat-treated sample until the mirror surface effect is achieved, and observing the surface under a microscope to avoid scratches, water marks and dirt;
(3) Immersing the polished sample in the corrosive liquid for 10s, cleaning, drying, observing grain boundaries under a microscope, and determining the austenite grain size of the T91 steel.
In the step (1), the heat treatment method comprises the following steps: the sample was heated to 1050.+ -. 10 ℃ and incubated for 60.+ -. 5 minutes, then the heated sample was rapidly quenched into water.
In the step (3), the steps of cleaning and drying are as follows: washing with distilled water, washing with ethanol, and drying with hot air.
In the step (3), the austenite grain size of the T91 steel is evaluated according to the GB/T6394-2017 metal average grain size measurement method.
The evaluation method is a picture comparison method, a cut-off method or an area method.
Compared with the prior art, in the method for displaying the austenite grain size of the T91 steel, the used corrosive components are common chemical reagents, the preparation method is simple and easy to realize, the method is suitable for displaying the austenite grain size of the T91 steel, improves the metallographic display effect, and solves the technical problem of crystal boundary display or incomplete display.
Drawings
FIG. 1 is a grain size diagram of T91 steel treated by the method of example 1;
FIG. 2 is a grain size diagram of T91 steel treated by the method of comparative example 1;
FIG. 3 is a grain size diagram of T91 steel treated by the method of comparative example 2;
FIG. 4 is a grain size diagram of T91 steel treated by the method of comparative example 3;
FIG. 5 is a grain size diagram of T91 steel treated by the method of comparative example 4;
FIG. 6 is a grain size diagram of T91 steel treated by the method of comparative example 5;
FIG. 7 is a grain size diagram of T91 steel treated by the method of comparative example 6.
Detailed Description
The present invention will be described in detail with reference to examples.
In the examples and comparative examples, hydrochloric acid was used in an amount of 36 to 38 mass%.
Example 1
A method of displaying austenite grain size of T91 steel comprising the steps of:
(1) Sample heat treatment: heating the sample to 1050 ℃ and preserving heat for 60 minutes, and then rapidly quenching the heated sample into water;
(2) Carrying out rough grinding, fine grinding and polishing treatment on the heat-treated sample until the mirror surface effect is achieved, and observing the surface under a microscope to avoid scratches, water marks and dirt;
(3) Preparing a corrosive liquid: fully mixing 1g of sodium dodecyl benzene sulfonate, 5g of FeCl 3·6H2 O, 50mL of hydrochloric acid and 100mL of absolute ethyl alcohol to prepare a corrosive liquid;
(4) Immersing the polished sample in corrosive liquid for 10s, washing with distilled water, washing with ethanol, drying with hot air, observing grain boundary under a microscope, displaying a photo according to austenite grain size, and evaluating the austenite grain size of the T91 steel according to a GB/T6394-2017 metal average grain size measurement method.
The grain size diagram of the T91 steel in this example is shown in FIG. 1, from which it can be seen clearly that the grain boundaries are intact, with a grain size grade of 8.5.
Comparative example 1
A method of displaying austenite grain size of T91 steel comprising the steps of:
a. sample preparation: the sample is subjected to rough grinding, fine grinding and polishing, so that the observation surface of the sample achieves a mirror effect, and no scratch, water trace and dirt are generated on the observation surface under a microscope;
b. The method comprises the steps of preparing an etching solution, wherein the etching solution comprises 60mL of saturated picric acid aqueous solution, two drops of white cat detergent and 0.3g of ferric chloride (FeCl 3·6H2 O), and the preparation method of the etching solution comprises the following steps:
1) Adding picric acid into distilled water, stirring until picric acid is not dissolved, filtering undissolved picric acid by a filter screen to obtain saturated picric acid solution;
2) Adding two drops of white cat detergent and 0.3g of ferric chloride (FeCl 3·6H2 O) into 60mL of saturated picric acid aqueous solution, and continuously stirring to uniformly mix the solutions, thus obtaining the corrosive liquid;
c. And (3) corrosion: immersing the polished sample into the prepared corrosive liquid, continuously wiping the test surface with absorbent cotton dipped with the corrosive liquid at normal temperature, taking out after 2 minutes, washing with water, washing with ethanol, drying with hot air, and observing the grain boundary under a microscope, wherein the result is shown in figure 2, and the method cannot show clear grain boundary.
Comparative example 2
A method of displaying austenite grain size of T91 steel comprising the steps of:
(1) The sample is subjected to rough grinding, fine grinding and polishing treatment until the mirror surface effect is achieved, and no scratch, water trace and dirt are generated on the surface of the sample under observation of a microscope;
(2) Preparing a corrosive liquid: fully mixing 1g of sodium dodecyl benzene sulfonate, 5g of FeCl 3·6H2 O, 50mL of hydrochloric acid and 100mL of ethanol to prepare a corrosive liquid;
(3) Immersing the polished sample in the corrosive liquid for 20s, washing with distilled water, washing with ethanol, drying with hot air, and observing the microstructure image under a microscope.
The grain size diagram of the T91 steel in this comparative example is shown in fig. 3, from which it can be seen that no grain boundaries can be observed.
Comparative example 3
A method of displaying austenite grain size of T91 steel comprising the steps of:
(1) Sample heat treatment: heating the sample to 1050 ℃ and preserving heat for 60 minutes, and then rapidly quenching the heated sample into water;
(2) Carrying out rough grinding, fine grinding and polishing treatment on the heat-treated sample until the mirror surface effect is achieved, and observing the surface under a microscope to avoid scratches, water marks and dirt;
(3) Preparing a corrosive liquid: fully mixing 1g of sodium dodecyl benzene sulfonate, 3·6H2 O3 g of FeCl, 40mL of hydrochloric acid and 100mL of ethanol to prepare a corrosive liquid;
(4) Immersing the polished sample in the corrosive liquid for 15s, washing with distilled water, washing with ethanol, drying with hot air, and observing the microstructure image under a microscope.
The grain size diagram of the T91 steel in this comparative example is shown in fig. 4, and it can be seen from the diagram that although grain boundaries can be displayed, the grain boundaries are incomplete and unclear, and the corrosion time is longer than that required in example 1, and the matrix is blackened, which affects the observation.
Comparative example 4
A method for displaying the austenite grain size of T91 steel was the same as in example 1 except that the composition of the etching solution was replaced with 1g of sodium dodecylbenzenesulfonate, 5g of FeCl 3·6H2 O, 50mL of hydrochloric acid, and 100mL of distilled water.
The grain size diagram of the T91 steel in this comparative example is shown in fig. 5, and it can be seen from the diagram that the method cannot clearly show a complete grain boundary, and water marks and black spots easily appear on the test surface of the sample.
Comparative example 5
A method for exhibiting austenite grain size of T91 steel was the same as in example 1 except that the heating temperature in step (1) was lowered to 950 ℃.
The grain size diagram of the T91 steel in the comparative example is shown in FIG. 6, and it can be seen from the diagram that the grain boundary obtained by the method is finer, and the structure floats up at the same time, which is not beneficial to observation.
Comparative example 6
A method of displaying austenite grain size of T91 steel comprising the steps of:
(1) The sample is subjected to rough grinding, fine grinding and polishing treatment until the mirror surface effect is achieved, and no scratch, water trace and dirt are generated on the surface of the sample under observation of a microscope;
(2) Preparing a corrosive liquid: fully mixing 1g of sodium dodecyl benzene sulfonate, 5g of FeCl 3·6H2 O, 50mL of hydrochloric acid and 100mL of ethanol to prepare a corrosive liquid;
(3) Immersing the polished sample in the corrosive liquid for 8s, washing with distilled water, washing with ethanol, drying with hot air, and observing the microstructure image under a microscope.
As shown in fig. 7, the grain size diagram of the T91 steel in this comparative example shows that the texture surface is blackened, and the grain boundaries are covered, which is not easy to observe.
The above detailed description of a corrosive liquid showing the austenite grain size of T91 steel and a method showing the austenite grain size of T91 steel with reference to the examples is illustrative and not restrictive, and several examples can be listed according to the defined scope, and therefore, variations and modifications without departing from the general inventive concept should be considered as falling within the scope of the present invention.
Claims (4)
1. A method of displaying austenite grain size of T91 steel, the method comprising the steps of:
(1) Heat treatment of the sample;
(2) Carrying out rough grinding, fine grinding and polishing treatment on the sample after the heat treatment until the mirror surface effect is achieved;
(3) Immersing the polished sample in corrosive liquid for 10s, cleaning, drying, observing grain boundaries under a microscope, and determining the austenite grain size of the T91 steel;
The corrosive liquid consists of the following substances: sodium dodecyl benzene sulfonate: ferric chloride: 36% -38% hydrochloric acid: absolute ethanol = 1g:4.5 to 5.5g: 45-55 mL: 90-110 mL; the corrosion liquid can clearly display grain boundaries, and the austenite grain size of the T91 steel is measured;
in the step (1), the heat treatment method comprises the following steps: the sample was heated to 1050.+ -. 10 ℃ and incubated for 60.+ -. 5 minutes, then the heated sample was rapidly quenched into water.
2. The method according to claim 1, wherein in step (3), the washing and drying are: washing with distilled water, washing with alcohol, and drying with hot air.
3. The method according to claim 1, wherein in step (3), the austenite grain size of the T91 steel is assessed according to the GB/T6394-2017 metal average grain size measurement method.
4. A method according to claim 3, wherein the method of assessment is a picture contrast method, a cut-off method or an area method.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210127173.4A CN114481134B (en) | 2022-02-10 | 2022-02-10 | Corrosive liquid for displaying austenitic grain size of T91 steel and method for displaying austenitic grain size of T91 steel |
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| CN202210127173.4A CN114481134B (en) | 2022-02-10 | 2022-02-10 | Corrosive liquid for displaying austenitic grain size of T91 steel and method for displaying austenitic grain size of T91 steel |
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| CN114481134B true CN114481134B (en) | 2024-04-30 |
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| CN111103183A (en) * | 2020-01-03 | 2020-05-05 | 中国石油天然气集团有限公司 | Method for displaying macroscopic morphology of high-steel-grade pipeline circumferential weld in multiple ways |
| CN113403621A (en) * | 2021-06-07 | 2021-09-17 | 武钢集团昆明钢铁股份有限公司 | Metallographic corrosive agent for austenitic Fe-Mn-Al-C series low-density high-strength steel and preparation method and application thereof |
-
2022
- 2022-02-10 CN CN202210127173.4A patent/CN114481134B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0943230A (en) * | 1995-07-31 | 1997-02-14 | Kawasaki Steel Corp | Corrosion liquid for old austenite grain boundary appearance of steel and exhibition method with the use of it |
| CN102401759A (en) * | 2010-09-07 | 2012-04-04 | 鞍钢股份有限公司 | Freeze-etching agent of ultra-low-carbon steel casting billet macrograph grain structure, and preparation method thereof |
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| CN104634640A (en) * | 2015-02-05 | 2015-05-20 | 东北大学 | Nickel based corrosion-resisting alloy dendritic crystal etching agent and preparation method and using method thereof |
| CN110068492A (en) * | 2018-01-24 | 2019-07-30 | 宝山钢铁股份有限公司 | A kind of metallographic etching agent and its application method for the dyeing of advanced high-strength steel retained austenite |
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