CN103018141A - Original crystalline grain displaying agent of high-alloy and low-carbon martensite steel and displaying method - Google Patents
Original crystalline grain displaying agent of high-alloy and low-carbon martensite steel and displaying method Download PDFInfo
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- CN103018141A CN103018141A CN2012104977187A CN201210497718A CN103018141A CN 103018141 A CN103018141 A CN 103018141A CN 2012104977187 A CN2012104977187 A CN 2012104977187A CN 201210497718 A CN201210497718 A CN 201210497718A CN 103018141 A CN103018141 A CN 103018141A
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 24
- 239000010959 steel Substances 0.000 title claims abstract description 24
- 229910000734 martensite Inorganic materials 0.000 title claims abstract description 22
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 20
- 239000000956 alloy Substances 0.000 title claims abstract description 20
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 238000005260 corrosion Methods 0.000 claims description 18
- 230000007797 corrosion Effects 0.000 claims description 17
- 229920000742 Cotton Polymers 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 230000003628 erosive effect Effects 0.000 claims description 4
- 238000012856 packing Methods 0.000 claims description 4
- 230000000007 visual effect Effects 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000011156 evaluation Methods 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 abstract 1
- 229910017604 nitric acid Inorganic materials 0.000 abstract 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- 239000003518 caustics Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910001566 austenite Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910000677 High-carbon steel Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910000954 Medium-carbon steel Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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Abstract
The invention relates to an original crystalline grain displaying agent of high-alloy and low-carbon martensite steel and a displaying method. The displaying agent is formed by the following components according to solvent volume (ml) and mass (g): 5-10 ml of concentrated nitric acid, 10-30 ml of concentrated hydrochloric acid, 50-100 ml of alcohol, 0.5-4 g of picric acid and 1.0-6.0 g of sodium dodecyl benzene sulfonate. The displaying method is carried out by the steps of preparing a test sample, configuring the displaying agent, corroding the test sample, organizing and observing, and collecting an image. The original crystalline grain displaying agent of high-alloy and low-carbon martensite steel and the displaying method have the advantages of novel concept, simplicity in operation, complete crystal boundary display effect, capability of clearly recognizing a grain size, and convenience for accurately measuring the original grain size and grain fineness number, and provide good conditions for formulating and optimizing a steel product production process.
Description
Technical field
The invention belongs to ferrous materials microstructure examination reagent technical field, relate in particular to a kind of high alloy mild carbon steel martensite steel and organize micro-detection reagent and method.
Background technology
High alloy low-carbon martensitic steels commercial Application is extensive, the heavy casting and forging of heavy-duty machinery industry especially, the rotor of steam turbine for example, the runner of the hydraulic turbine and blade etc.The original grain of martensite steel is to estimate one of important indicator with the performance of checking martensite steel.For the high alloy martensite steel, contain a large amount of alloying elements, such as chromium, nickel, manganese etc. make it more anti-corrosion, generally the corrosion of its tissue strong acid solution commonly used.But to the corrosion of its original austenite crystal prevention, with the difficult corrosion of common picric acid solution, about the document of this respect also seldom.Patent [201110009408.1] provides a kind of grain size caustic solution of medium and high carbon steel, but to high alloy low-carbon martensitic steels and inapplicable.
Summary of the invention
The object of the present invention is to provide a kind of developer proportioning novel, simple to operate, the Display of Grain Boundary effect is complete, can clear tell grain size, be convenient to Measurement accuracy initial grain size and grain size, for the detection and assessment of this kind steel performance provides Data support, for the formulation of its production technology with optimize high alloy low-carbon martensitic steels original grain developer and the display packing that advantage is provided.
High alloy low-carbon martensitic steels original grain developer of the present invention forms [in solvent volume (ml) and quality (g)] by following component: concentration 65%(massfraction) above red fuming nitric acid (RFNA) 5-10 ml, concentration 36%(massfraction) above concentrated hydrochloric acid 10-30ml, purity 95%(massfraction) above alcohol 50-100ml, picric acid 0.5-4 gram, neopelex 1.0-6.0 gram.
The display packing of high alloy low-carbon martensitic steels original grain of the present invention is as follows:
1. the preparation of sample: choose the high alloy low-carbon martensitic steels and make sample, and sample polished, is polished to specimen surface is smooth, no marking, the sample after the polishing with alcohol wash to cleaning surfaces without dirt;
2. the configuration of developer: measure first 5-10ml red fuming nitric acid (RFNA) (more than concentration 65 mass%), pour into more than 50-100ml(purity 95 mass%) shake up in the industrial spirit, shake up putting into 10-30 ml concentrated hydrochloric acid (concentration 36 mass%), pour in the airtight glassware and place; The mentioned solution that taking-up configures before the sample corrosion, adding 0.5-4.0 gram picric acid stirs and shakes up, and adds the stirring of 1.0-6.0 gram neopelex again and shakes up;
3. the corrosion of sample: under 0-40 ℃ room temperature, carry out, the developer solution that configures is poured in the evaporating dish, place skim absorbent cotton in the evaporating dish, absorbent cotton will immerse in the solution fully, and the specimen surface that will corrode down, be placed on the absorbent cotton, avoid sample to contact with the glassware wall, erosion time is controlled at 2-20 min, until the specimen erodes surface discolouration, then take out sample surperficial with alcohol wipe, hot blast drying;
4. metallographic observation and image acquisition: after the sample corrosion finishes, carry out immediately metallographic microstructure and observe and image acquisition, sample is observed and is adopted the metallographic optical microscope, the clear complete crystal boundary of the martensitic original grain of low carbon high alloy that demonstrates, choose the visual field and take pictures, gather metallograph; At last, the analysis to measure crystallite dimension is carried out the grain size evaluation.
Advantage of the present invention is: the developer proportioning is novel, simple to operate, the Display of Grain Boundary effect is complete, can know and tell grain size, be convenient to Measurement accuracy initial grain size and grain size, for formulation and the optimization of this kind steel production technology provides advantage.
Description of drawings
Fig. 1 is the photo of organizing of the rear low carbon high alloy martensite steel of orthonitric acid hydrochloric acid mixed solution corrosion;
Fig. 2 is the original austenite grain photo of the low carbon high alloy martensite steel that corrodes of the present invention.
Embodiment
The preparation of I, sample:
A, sampling
Sample is feeding from the steel of dilivery state directly, must prevent during sampling that temperature from raising and the tissue that causes changes.The selection principle of specimen size is be conducive to grind away, polishing and structure observation easy to operate, and the cylinder sample of φ 10 * 15mm or φ 15 * 18mm for example also can adopt the rectangular parallelepiped sample of 10 * 10 * 15mm or 12 * 15 * 18mm equidimension.
B, grind away
Adopt abrasive paper for metallograph or the waterproof abrasive paper of different meshes that specimen surface is carried out the multi-pass grinding, sand paper order number adopts ascending order, and last one grind away sand paper order number generally gets final product to 1000 or 1200.
C, polishing
Mechanical buffing adopts brilliant polish to polish at buffing machine with woollen, adopts the wetting woollen cloth of water lubrication during polishing, is polished to specimen surface smooth, no marking.Sample alcohol wash after the polishing, cleaning surfaces is without dirt.
The configuration of II, developer
A, developer at room temperature configure, and its one-tenth is grouped into: red fuming nitric acid (RFNA) 5-10 ml, concentrated hydrochloric acid 10-30ml, alcohol 50-100ml, picric acid 0.5-4.0 gram, neopelex 1.0-6.0 gram;
B, measure 5-10ml red fuming nitric acid (RFNA) (more than concentration 65 mass%) first, pour into more than 50-100ml(purity 95 mass%) shake up in the industrial spirit, shake up putting into 10-30 ml concentrated hydrochloric acid (concentration 36 mass%), pour in the airtight glassware and place.
The mentioned solution that taking-up configures before c, the sample corrosion, adding 0.5-4.0 gram picric acid stirs and shakes up, and adds the stirring of 1.0-6.0 gram neopelex again and shakes up.
III, sample corrosion
A, under room temperature (0-40 ℃), get final product;
B, the caustic solution that configures is poured in the evaporating dish in right amount, placed skim absorbent cotton (immersing in the solution) in the evaporating dish, the corrosion sample surface down, be placed on the absorbent cotton, avoid sample to contact with the glassware wall, erosion time is controlled at 2-20 min, until the slightly variable color of specimen erodes surface, the taking-up sample is observed, how see corrosive effect, if corrosion is more shallow, can put into again reagent 1-2 min, then take out sample surperficial with alcohol wipe, hot blast drying.If specimen surface leaves the dirt of unsuitable wiping, can on buffing machine, gently throw, get final product to surface-brightening.
IV, metallographic observation and image acquisition
After the sample corrosion finishes, should carry out immediately metallographic microstructure and observe and image acquisition;
A, sample are observed and are adopted the metallographic optical microscope, according to the grain size of sample, regulate microscopical object lens multiple, regulate the microscope depth of field, until the visual field is clear; The clear complete crystal boundary of the martensitic original grain of low carbon high alloy that shows.
B, choose the visual field and take pictures, gather metallograph.
C, analysis to measure crystallite dimension are carried out the grain size evaluation.
Embodiment 1
Under 25 ℃ of room temperatures, measure first 5ml red fuming nitric acid (RFNA) (concentration 65 mass%), pour 50ml(purity 95 mass% into) shake up in the industrial spirit, shake up putting into 15ml concentrated hydrochloric acid (36 mass%), pour in the airtight glassware and place.The mentioned solution that taking-up configures before the sample corrosion, adding 1 gram picric acid stirs and shakes up, and adds 1.5 gram neopelexes stirrings again and shakes up.Pour in right amount the caustic solution that configures in the evaporating dish, place skim absorbent cotton (immersing in the solution) in the evaporating dish, want corrosion sample 1Cr12Ni1Mo steel surface down, be placed on the absorbent cotton, avoid sample to contact with the glassware wall, erosion time is controlled at 8 min, then takes out sample surperficial with alcohol wipe, then hot blast drying carries out microstructure observation and electronic image capture.Calculating the sample mean crystallite dimension is 0.105mm, and grain size is 3.6 grades.
Embodiment 2 implements with embodiment 1 method, and its set of dispense when etching condition is listed in the table 1.
Embodiment 3 implements with embodiment 1 method, and its set of dispense when etching condition is listed in the table 1.
Embodiment 4 implements with embodiment 1 method, and its set of dispense when etching condition is listed in the table 1.
Claims (2)
1. high alloy low-carbon martensitic steels original grain developer, it is characterized in that: developer forms [in solvent volume (ml) and quality (g)] by following component: concentration 65%(massfraction) above red fuming nitric acid (RFNA) 5-10 ml, concentration 36%(massfraction) above concentrated hydrochloric acid 10-30ml, purity 95%(massfraction) above alcohol 50-100ml, picric acid 0.5-4 gram, neopelex 1.0-6.0 gram.
2. one kind is utilized developer claimed in claim 1 to the display packing that high alloy low-carbon martensitic steels original grain shows, it is characterized in that: carry out according to the following steps:
1. the preparation of sample: choose the high alloy low-carbon martensitic steels and make sample, and sample polished, is polished to specimen surface is smooth, no marking, the sample after the polishing with alcohol wash to cleaning surfaces without dirt;
2. the configuration of developer: measure first 5-10ml red fuming nitric acid (RFNA) (more than the concentration 65mass%), pour into more than 50-100ml(purity 95 mass%) shake up in the industrial spirit, shake up putting into 10-30 ml concentrated hydrochloric acid (concentration 36 mass%), pour in the airtight glassware and place; The mentioned solution that taking-up configures before the sample corrosion, adding 0.5-4.0 gram picric acid stirs and shakes up, and adds the stirring of 1.0-6.0 gram neopelex again and shakes up;
3. the corrosion of sample: under 0-40 ℃ room temperature, carry out, the developer solution that configures is poured in the evaporating dish, place skim absorbent cotton in the evaporating dish, absorbent cotton will immerse in the solution fully, and the specimen surface that will corrode down, be placed on the absorbent cotton, avoid sample to contact with the glassware wall, erosion time is controlled at 2-20 min, until the specimen erodes surface discolouration, then take out sample surperficial with alcohol wipe, hot blast drying;
4. metallographic observation and image acquisition: after the sample corrosion finishes, carry out immediately metallographic microstructure and observe and image acquisition, sample is observed and is adopted the metallographic optical microscope, the clear complete crystal boundary of the martensitic original grain of low carbon high alloy that demonstrates, choose the visual field and take pictures, gather metallograph; At last, the analysis to measure crystallite dimension is carried out the grain size evaluation.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103454187A (en) * | 2013-08-27 | 2013-12-18 | 宁夏共享集团有限责任公司 | Method for displaying original austenite grain boundary of tempering bainite structure at room temperature |
| CN104374627A (en) * | 2014-11-19 | 2015-02-25 | 苏州华碧微科检测技术有限公司 | Corrosion liquid and corrosion method for ultralow steel original austenite crystal boundary |
| CN104729963A (en) * | 2015-03-31 | 2015-06-24 | 常州天山重工机械有限公司 | Detection and display method of austenite grains of quenched and tempered steel for gears at room temperature |
| CN105136629A (en) * | 2015-08-24 | 2015-12-09 | 首钢总公司 | Display method of zinc crystal grains on the surface of galvanizing plate |
| CN105352779A (en) * | 2015-10-21 | 2016-02-24 | 中国船舶重工集团公司第七二五研究所 | Metallographic erosion method of nickel-aluminum bronze crystal boundary |
| CN105486567A (en) * | 2015-11-24 | 2016-04-13 | 太原理工大学 | Chemical erosion agent for displaying macrostructure of expansion alloy, and erosion method thereof |
| CN105908186A (en) * | 2016-05-06 | 2016-08-31 | 江西昌河航空工业有限公司 | Stainless steel corrosive agent and stainless steel grain size display method |
| CN106086906A (en) * | 2016-06-08 | 2016-11-09 | 中国船舶重工集团公司第七二五研究所 | A kind of cleaning agent for clearing up steel macrostructure hot acid corrosion product |
| CN109001200A (en) * | 2018-06-15 | 2018-12-14 | 济南大学 | A kind of corrosive liquid and caustic solution of medium carbon steel original austenite crystal boundary |
| CN109490302A (en) * | 2018-11-11 | 2019-03-19 | 上海电气上重铸锻有限公司 | A kind of test method of the austenite grain of midium-carbon steel martensitic structure |
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| CN103454187B (en) * | 2013-08-27 | 2016-02-10 | 宁夏共享集团有限责任公司 | A kind of method of room temperature display tempering bainite tissue's original austenite grains border |
| CN104374627A (en) * | 2014-11-19 | 2015-02-25 | 苏州华碧微科检测技术有限公司 | Corrosion liquid and corrosion method for ultralow steel original austenite crystal boundary |
| CN104729963B (en) * | 2015-03-31 | 2017-08-08 | 常州天山重工机械有限公司 | A kind of detection display methods of the austenite crystal of room temperature lower gear quenched and tempered steel |
| CN104729963A (en) * | 2015-03-31 | 2015-06-24 | 常州天山重工机械有限公司 | Detection and display method of austenite grains of quenched and tempered steel for gears at room temperature |
| CN105136629A (en) * | 2015-08-24 | 2015-12-09 | 首钢总公司 | Display method of zinc crystal grains on the surface of galvanizing plate |
| CN105136629B (en) * | 2015-08-24 | 2017-11-17 | 首钢总公司 | A kind of display methods of zinc-plated plate surface zinc crystal grain |
| CN105352779A (en) * | 2015-10-21 | 2016-02-24 | 中国船舶重工集团公司第七二五研究所 | Metallographic erosion method of nickel-aluminum bronze crystal boundary |
| CN105486567A (en) * | 2015-11-24 | 2016-04-13 | 太原理工大学 | Chemical erosion agent for displaying macrostructure of expansion alloy, and erosion method thereof |
| CN105908186A (en) * | 2016-05-06 | 2016-08-31 | 江西昌河航空工业有限公司 | Stainless steel corrosive agent and stainless steel grain size display method |
| CN106086906A (en) * | 2016-06-08 | 2016-11-09 | 中国船舶重工集团公司第七二五研究所 | A kind of cleaning agent for clearing up steel macrostructure hot acid corrosion product |
| CN106086906B (en) * | 2016-06-08 | 2019-02-12 | 中国船舶重工集团公司第七二五研究所 | It is a kind of for clearing up the cleaning agent of steel macrostructure hot acid corrosion product |
| CN109001200A (en) * | 2018-06-15 | 2018-12-14 | 济南大学 | A kind of corrosive liquid and caustic solution of medium carbon steel original austenite crystal boundary |
| CN109490302A (en) * | 2018-11-11 | 2019-03-19 | 上海电气上重铸锻有限公司 | A kind of test method of the austenite grain of midium-carbon steel martensitic structure |
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