CN103018141B - High alloy low-carbon martensitic steels original grain developer and display packing - Google Patents
High alloy low-carbon martensitic steels original grain developer and display packing Download PDFInfo
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- CN103018141B CN103018141B CN201210497718.7A CN201210497718A CN103018141B CN 103018141 B CN103018141 B CN 103018141B CN 201210497718 A CN201210497718 A CN 201210497718A CN 103018141 B CN103018141 B CN 103018141B
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 23
- 239000010959 steel Substances 0.000 title claims abstract description 23
- 229910000734 martensite Inorganic materials 0.000 title claims abstract description 21
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 19
- 239000000956 alloy Substances 0.000 title claims abstract description 19
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 17
- 238000012856 packing Methods 0.000 title claims abstract description 7
- 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 16
- 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
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 238000005260 corrosion Methods 0.000 claims description 15
- 230000007797 corrosion Effects 0.000 claims description 14
- 229920000742 Cotton Polymers 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 230000003628 erosive effect Effects 0.000 claims description 4
- 239000011521 glass Substances 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
- 230000000694 effects Effects 0.000 abstract description 4
- 238000009472 formulation Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005259 measurement Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000005457 optimization Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 5
- 239000003518 caustics Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000005530 etching Methods 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
- 238000005516 engineering process Methods 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
- 238000005242 forging Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007689 inspection 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
- 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
Abstract
The present invention relates to a kind of high alloy low-carbon martensitic steels original grain developer and display packing, described developer is made up of [in solvent volume (ml) and quality (g)] following component: red fuming nitric acid (RFNA) 5-10ml, concentrated hydrochloric acid 10-30ml, alcohol 50-100ml, picric acid 1-3 gram, neopelex 1.5-5.0 gram.Display packing is pressed sample preparation, developer configuration, sample burn into structure observation and image acquisition step and is implemented.Its advantage is that developer proportioning is novel, simple to operate, and 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 the formulation of this kind of steel manufacturing process and optimization provide advantage.
Description
Technical field
The invention belongs to ferrous materials microstructure examination reagent technique field, particularly relate to a kind of high alloy mild carbon steel martensite steel and carry out organizing micro-detection reagent and method.
Background technology
High alloy low-carbon martensitic steels commercial Application is extensive, the especially heavy casting and forging of heavy machinery industry, the rotor of such as steam turbine, the runner of the hydraulic turbine and blade etc.The original grain of martensite steel evaluates and one of important indicator of the performance of inspection martensite steel.For high alloy martensite steel, containing a large amount of alloying elements, as chromium, nickel, manganese etc., make it more anti-corrosion, and generally strong acid solution is commonly used in the corrosion of its tissue.But to the corrosion of its original austenite crystal prevention, with the more difficult corrosion of common picric acid solution, the document about this respect is also little.Patent [201110009408.1] provides a kind of grain size caustic solution of medium and high carbon steel, but inapplicable to high alloy low-carbon martensitic steels.
Summary of the invention
The object of the present invention is to provide a kind of developer proportioning novel, simple to operate, Display of Grain Boundary effect is complete, clear can tell grain size, be convenient to Measurement accuracy initial grain size and grain size, for the detection and assessment of this kind of steel performance provides Data support, formulation and optimization for its production technology provide high alloy low-carbon martensitic steels original grain developer and the display packing of advantage.
High alloy low-carbon martensitic steels original grain developer of the present invention is made up of [in solvent volume (ml) and quality (g)] following component: the red fuming nitric acid (RFNA) 5-10ml of concentration 65% (massfraction), the concentrated hydrochloric acid 10-30ml of concentration 36% (massfraction), the alcohol 50-100ml of purity 95% (massfraction), picric acid 1-3 gram, neopelex 1.5-5.0 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 high alloy low-carbon martensitic steels and make sample, and sample is polished, be polished to that specimen surface is smooth, no marking, the sample alcohol washes after polishing to surface cleaning without dirt;
2. the configuration of developer: first measure 5-10ml red fuming nitric acid (RFNA) (concentration 65mass%), pour in 50-100ml (purity 95mass%) industrial spirit and shake up, put into 10-30ml concentrated hydrochloric acid (concentration 36mass%) again to shake up, pour in closed glass vessel and place; Take out the above-mentioned solution that configures before sample corrosion, add 1.0-3.0 gram of picric acid and stir and shake up, then add 1.5-5.0 gram of neopelex and stir and shake up;
3. the corrosion of sample: carry out under the room temperature of 0-40 DEG C, the developer solution configured is poured in evaporating dish, place skim absorbent cotton in evaporating dish, absorbent cotton will immerse in solution completely, and the specimen surface that will corrode down, be placed on absorbent cotton, avoid sample to contact with glassware wall, erosion time controls at 2-20min, until specimen erodes surface discolouration, then sample alcohol wipe surface is taken out, hot blast drying;
4. metallographic observation and image acquisition: after sample corrodes and terminates, carry out metallographic microstructure observation and image acquisition immediately, sample is observed and is adopted metallographic optical microscope, knows and demonstrates the complete crystal boundary of the martensitic original grain of low carbon high alloy, choose visual field to take pictures, gather metallograph; Finally, analysis to measure crystallite dimension, carries out grain size evaluation.
Advantage of the present invention is: developer proportioning is novel, simple to operate, 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 the formulation of this kind of steel manufacturing process and optimization provide advantage.
Accompanying drawing explanation
Fig. 1 is the macrograph of low carbon high alloy martensite steel after the corrosion of orthonitric acid hydrochloric acid mixed solution;
Fig. 2 is the original austenite grain photo of the low carbon high alloy martensite steel that the present invention is corroded.
Embodiment
The preparation of I, sample:
A, sampling
Sample, directly from feeding the steel of dilivery state, must prevent temperature from raising and the tissue change that causes during sampling.The selection principle of specimen size be conducive to grind away, polishing and structure observation easy to operate, the such as cylinder sample of φ 10 × 15mm or φ 15 × 18mm, also can adopt the rectangular parallelepiped sample of 10 × 10 × 15mm or 12 × 15 × 18mm equidimension.
B, grind away
Adopt the abrasive paper for metallograph of different meshes or waterproof abrasive paper to carry out multi-pass grinding to specimen surface, sand paper order number adopts ascending order, and last one grind away sand paper order number is generally to 1000 or 1200.
C, polishing
Mechanical buffing, adopts brilliant polish on buffing machine, to carry out polishing with woollen, adopts water lubrication wetting woollen, be polished to specimen surface smooth, no marking during polishing.Sample alcohol washes after polishing, surface cleaning 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) 5-10ml, concentrated hydrochloric acid 10-30ml, alcohol 50-100ml, picric acid 1.0-3.0 gram, neopelex 1.5-5.0 gram;
B, first measure 5-10ml red fuming nitric acid (RFNA) (concentration 65mass%), pour in 50-100ml (purity 95mass%) industrial spirit and shake up, put into 10-30ml concentrated hydrochloric acid (concentration 36mass%) again to shake up, pour in closed glass vessel and place.
Take out the above-mentioned solution that configures before the corrosion of c, sample, add 1.0-3.0 gram of picric acid and stir and shake up, then add 1.5-5.0 gram of neopelex and stir and shake up.
III, sample corrode
A, to carry out under room temperature (0-40 DEG C);
B, the caustic solution configured to be poured in evaporating dish in right amount, place skim absorbent cotton (immersing in solution) in evaporating dish, corrosion sample surface down, be placed on absorbent cotton, avoid sample to contact with glassware wall, erosion time controls at 2-20min, until the slightly variable color of specimen erodes surface, taking-up sample is observed, how see corrosive effect, if corrosion is more shallow, reagent 1-2min can be put into again, then sample alcohol wipe surface is taken out, hot blast drying.If specimen surface leaves the dirt of unsuitable wiping, gently can throw on buffing machine, to surface-brightening.
IV, metallographic observation and image acquisition
After sample corrosion terminates, metallographic microstructure observation and image acquisition should be carried out immediately;
A, sample are observed and are adopted metallographic optical microscope, according to the grain size of sample, regulate microscopical object lens multiple, regulate the microscope depth of field, until visual field is clear; The complete crystal boundary of the clear display martensitic original grain of low carbon high alloy.
B, choose visual field and take pictures, gather metallograph.
C, analysis to measure crystallite dimension, carry out grain size evaluation.
Embodiment 1
Under 25 DEG C of room temperatures, first measure 5ml red fuming nitric acid (RFNA) (concentration 65mass%), pour in 50ml (purity 95mass%) industrial spirit and shake up, shake up putting into 15ml concentrated hydrochloric acid (36mass%), pour in closed glass vessel and place.Take out the above-mentioned solution that configures before sample corrosion, add 1 gram of picric acid and stir and shake up, then add 1.5 grams of neopelexes and stir and shake up.The caustic solution configured is poured in evaporating dish in right amount, skim absorbent cotton (immersing in solution) is placed in evaporating dish, want corrosion sample 1Cr12Ni1Mo steel surface down, be placed on absorbent cotton, avoid sample to contact with glassware wall, erosion time controls at 8min, then takes out sample alcohol wipe surface, hot blast drying, then carries out microstructure observation and electronic image capture.Calculating sample mean crystallite dimension is 0.105mm, and grain size is 3.6 grades.
Embodiment 2 is implemented with embodiment 1 method, and its component proportion and etching condition are listed in table 1.
Embodiment 3 is implemented with embodiment 1 method, and its component proportion and etching condition are listed in table 1.
Embodiment 4 is implemented with embodiment 1 method, and its component proportion and etching condition are listed in table 1.
Claims (2)
1. a high alloy low-carbon martensitic steels original grain developer, it is characterized in that: developer is in solvent volume (ml) and quality (g), be made up of following component: mass concentration is the red fuming nitric acid (RFNA) 5-10ml of 65%, mass concentration is the concentrated hydrochloric acid 10-30ml of 36%, mass concentration is the alcohol 50-100ml of 95%, picric acid 1-3 gram, neopelex 1.5-5.0 gram.
2. the display packing utilizing the developer described in claim 1 to show high alloy low-carbon martensitic steels original grain, is characterized in that: carry out according to the following steps:
1. the preparation of sample: choose high alloy low-carbon martensitic steels and make sample, and sample is carried out to sanding and polishing is smooth to specimen surface, no marking, the sample alcohol washes after polishing to surface cleaning without dirt;
2. the configuration of developer: first measure the red fuming nitric acid (RFNA) 5-10ml that mass concentration is 65%, pouring 50-100ml mass concentration into is shake up in the industrial spirit of 95%, then put into mass concentration be 36% concentrated hydrochloric acid 10-30ml shake up, pour in closed glass vessel and place; Take out the above-mentioned solution that configures before sample corrosion, add 1-3.0 gram of picric acid and stir and shake up, then add 1.5-5.0 gram of neopelex and stir and shake up;
3. the corrosion of sample: carry out under the room temperature of 0-40 DEG C, the developer solution configured is poured in evaporating dish, place skim absorbent cotton in evaporating dish, absorbent cotton will immerse in solution completely, and the specimen surface that will corrode down, be placed on absorbent cotton, avoid sample to contact with glassware wall, erosion time controls at 2-20min, until specimen erodes surface discolouration, then sample alcohol wipe surface is taken out, hot blast drying;
4. metallographic observation and image acquisition: after sample corrodes and terminates, carry out metallographic microstructure observation and image acquisition immediately, sample is observed and is adopted metallographic optical microscope, knows and demonstrates the complete crystal boundary of the martensitic original grain of low carbon high alloy, choose visual field to take pictures, gather metallograph; Finally, analysis to measure crystallite dimension, carries out grain size evaluation.
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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 |
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| 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 |
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| 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 |
| 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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| US8945691B2 (en) * | 2009-02-13 | 2015-02-03 | Consolidated Nuclear Security, LLC | Nano-material and method of fabrication |
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