CN106053471A - Method for showing austenite crystal boundary of micro-alloyed steel in vacuum hot-corrosion condition - Google Patents
Method for showing austenite crystal boundary of micro-alloyed steel in vacuum hot-corrosion condition Download PDFInfo
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- CN106053471A CN106053471A CN201610631231.1A CN201610631231A CN106053471A CN 106053471 A CN106053471 A CN 106053471A CN 201610631231 A CN201610631231 A CN 201610631231A CN 106053471 A CN106053471 A CN 106053471A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention relates to a method for showing an austenite crystal boundary of micro-alloyed steel in a vacuum hot-corrosion condition. The method comprises the following steps: cutting, grinding, polishing, cleaning, vacuum heating, rapid cooling in a protective atmosphere, metallographic observation of austenite crystal grains and picture acquisition, and analysis of metallographs and analysis of dimensional measurement of austenite crystal grains. Compared with conventional technology, the method enables two experimental processes including simulation of a heating schedule and hot-corrosion showing of austenite crystal grains to be combined and completed. The experimental process is simplified, the energy consumption and emission are reduced, and the experimental efficiency is increased.
Description
Technical field
A kind of method that the present invention relates to manifest Microalloyed Austenite crystal boundary under Vacuum Heat etching condition, belongs to metallurgical skill
Art field.
Background technology
The austenite actuargrain size of steel is very big to the performance impact of steel, obtains thick after the cooling of thick austenite crystal
Transmutation product, the mechanical property such as the intensity of steel, toughness, fatigue resistance is the most poor.Clearly manifest and accurately measure austenite in fact
Border crystallite dimension, for the development law of material structure in Study on Steel production process, conservative control technological parameter and guarantee product
Performance is significant.Therefore austenite crystal display packing constantly explored by vast material metallurgy personage the most always, improve,
Innovation.The assessment method of the austenite grain size of steel is a lot, can using method: acieration, netted simulation acieration, ferrite
Net method, oxidizing process, directly harden method or the method such as Grain boundary attack method, cementite network method carries out manifesting evaluation, wherein crystal grain
Boundary corrosion method and oxidizing process are two kinds of most common methods.Oxidizing process is that the oxide network utilizing austenite grain boundary is evaluated
The austenite grain size of steel, and Grain boundary attack method is that sample heats under assigned temperature fast quickly cooling after certain time
But, corrode out by original austenite crystal prevention with aggressive agent and show a kind of method of complete austenite crystal.The most extensively should
For micro alloyed steel is the Grain boundary attack method in heat chemistry etch method.
In mentioning the patent manifested about Microalloyed Austenite crystal boundary, the most unanimously have employed the corrosion of heat chemistry etch method
Manifest austenite grain boundary.Micro alloyed steel for different carbon contents and different microalloy element amount uses specific caustic to join
With suitable caustic solution, demonstrate that austenite grain boundary is the major way that current austenite shows.As
200810079326.2 caustic proposed: distilled water+CrO3+ picric acid+oxirane, etching time is 40 ~ 60min,
201110009408.1 caustic proposed: saturated picric acid solution+liquid detergent+ferric chloride, and 201110334961.2
Corrosive liquids with 201310091213.5 propositions: tap water+picric acid+hair cream+dimethylbenzene+hydrochloric acid+Fluohydric acid .+copper chloride.
All with the invention belongs to different directions；The oxidizing process manifesting austenite grain boundary that GBT6394-2002 proposes, is to utilize austenite
The oxide network of crystal boundary manifests austenite crystal, but the method includes quenching process and heated oxide, and operation is longer, energy
Consume higher.
The method of the Microalloyed Austenite Display of Grain Boundary mentioned in above patent and GB, measures micro alloyed steel in reality
The work of austenite crystal is used.But the effect that austenite grain boundary corrosion manifests is unstable, when specimen surface corrodes
Between the consuming time of groping too many, often need to adjust etching time.If it is the most shallow to examine under a microscope grain boundary corrosion, then also
Need to place into caustic and continue corrosion, extend etching time；If specimen surface color is more black and tissue occurs, then corrosion is described
Too deep, handy sand paper fine grinding, polishing, place in caustic and again corrode, go to show for 1 ~ 2 time it is generally required to repeat above corrosion
Show complete crystal boundary, the common Fig. 1 of austenite grain boundary corrosive effect.The metallograph gathered is being carried out austenite grain size
During measurement, Grain boundary attack method causes specimen surface residual not clear up corrosive liquid thoroughly more, the metallograph surface of shooting
Containing a lot of stains, this metallograph is carried out image procossing difficulty bigger, it is difficult to use image processing software to realize high accuracy
, measure austenite grain size efficiently.
Summary of the invention
The technical problem to be solved in the present invention is, not enough for prior art, proposes a kind of simple, efficient, low energy consumption
The method manifesting Microalloyed Austenite crystal boundary under Vacuum Heat etching condition.
The present invention solves that the technical scheme that above-mentioned technical problem proposes is: under a kind of Vacuum Heat etching condition, manifest micro-conjunction
The method of gold steel austenite grain boundary, comprises the following steps:
(i) prepared by sample
A. cutting: first carry out cutting on strand and intercept sample；
B. grind away: again the sample that strand intercepts is ground off iron scale on abrasive machine, grind off the sample after iron scale at gold
Refine on phase sand paper；
C. polishing: the sample after fine grinding polishes on buffing machine again；
D. clean: by the sample alcohol washes after polishing, dry up；
(ii) the heat treated of style under vacuum condition
A. heating in vacuum: using the heating furnace with fine vacuum atmosphere to heat after sample is taken out 2-3 vacuum, sample is with stove
It is warming up to each design temperature 1200 DEG C, is then incubated 45min；
B. protective atmosphere rapid cooling: use noble gas quickly to cool down sample under vacuum, will use noble gas under vacuum
The sample extremely fast cooled down is immersed in ethanol, in case metallographic observation uses；
(iii) austenite crystal metallographic observation and picture collection: when carrying out metallographic observation, the ethanol of specimen surface is dried up, be placed on
In metallurgical microscope, use suitable amplification that austenite crystal carries out observational study, and gather relevant metallograph, in case
Crystal grain data analysis；
(iv) metallograph analysis is measured with austenite grain size and is analyzed
A. metallograph pixel dualization processes, austenite crystal differential reinforcement；
B. complete austenite crystal is demarcated；
C. austenite crystal is considered as spheroidal particle, adds up austenite grain size.
The improvement of technique scheme is: in described step B (i), grind off the sample after iron scale successively 180#,
Refine on 400#, 600#, 800#, 1000#, 1200#, 1500#, 1800#, 2000# abrasive paper for metallograph.
The improvement of technique scheme is: in described step C (i), and polishing agent uses fine-grained diamond polishing cream,
Use water as lubricant.
The improvement of technique scheme is: in described step D (i), the sample dried up is immersed in ethanol on pretreatment,
Specimen surface for laboratory observation guarantees, without defects such as any pit, pit, stains, the most not leave cut.
The present invention uses technique scheme to provide the benefit that:
(1) compared with traditional handicraft, the heating cycle of sample is simulated and is manifested two realities with austenite crystal heat erosion by the present invention
Test technique to have combined, simplify experimental procedure, contribute to reducing energy consumption and discharge, improve conventional efficient；
(2) compared with heat chemistry etch method, eliminate numerous and diverse corrosion and manifest operation, solve that corrosive liquid proportioning is unreasonable, invade
The erosion time controls the corrosive liquid of improper, specimen surface residual and does not clears up and completely etc. cause austenite to manifest unsharp problem, letter
Change austenite crystal and manifested technique, saved experimental period, improve conventional efficient, also improve austenite crystal simultaneously
Manifest effect；
(3) compared with oxidizing process method, abandoned quenching sample long-time heating oxidizing process in Muffle furnace, can effectively reduce
Energy consumption in experimentation, has preferable effects of energy saving and emission reduction；
(4) austenite crystal of the micro alloyed steel that the inventive method can be used in different-alloy content range manifests, also simultaneously
Can be the size of second phase particles, distribution, quantity SEM observe lay the first stone；
(5), in step of the present invention A (ii), sample is warming up to each design temperature 1200 DEG C with stove, is then incubated 45min, so pastes
Nearly production scene, the situation of sample is close to the situation of strand when producing；
(6), in step of the present invention B (ii), use noble gas that sample is quickly cooled down under vacuum, it is possible to prevent at sample
Mill, throwing plane produce thick oxide layer, and affect austenite grain boundary manifests effect.
Accompanying drawing explanation
The invention will be further described below in conjunction with the accompanying drawings:
Fig. 1 is common micro alloyed steel crystal grain heat chemistry etchant corrosive effect figure；
Fig. 2 is the sample prepared of embodiment of the present invention Electronic Speculum figure under 5000X；
Fig. 3 is the austenite crystal 100X metallograph of embodiment of the present invention sample.
Detailed description of the invention
Embodiment
The testing equipment of the method for Microalloyed Austenite crystal boundary is manifested: cutting under the Vacuum Heat etching condition of the present embodiment
(laser high temperature copolymerization is burnt for machine, sample grinding machine, buffing machine, magnifier, metallurgical microscope, scanning electron microscope (Flied emission), vacuum furnace
CLSM).
Test reagent: ethanol, fine-grained diamond polishing cream.
Test comprises the following steps:
(i) prepared by sample
A. cutting: process columned casting blank sample according to burnt (CLSM) crucible size of laser high temperature copolymerization；
B. grind away: again the sample that strand intercepts is ground off iron scale on abrasive machine, grind off the sample after iron scale successively
180#, 400#, 600#, 800#, 1000#, 1200#, 1500#, 1800#, 2000# abrasive paper for metallograph refines；
C. polishing: the sample after fine grinding polishes on buffing machine again, polishing agent uses fine-grained diamond polishing cream, uses water as
Lubricant；
D. clean: by the sample alcohol washes after polishing, dry up；The sample dried up is immersed in ethanol on pretreatment, is used for
The specimen surface of laboratory observation guarantees, without defects such as any pit, pit, stains, the most not leave cut；Prepare sample
The surface observed under 5000X is not as in figure 2 it is shown, obvious cut is observed on surface；
(ii) the heat treated of style under vacuum condition
A. heating in vacuum: put into by sample in CLSM, heats after sample is taken out 2-3 vacuum, and sample is warming up to respectively with stove
Design temperature 1200 DEG C, is then incubated 45min；
B. protective atmosphere rapid cooling: use noble gas quickly to cool down sample under vacuum, will use noble gas under vacuum
The sample extremely fast cooled down is immersed in ethanol, in case metallographic observation uses；
(iii) austenite crystal metallographic observation and picture collection: when carrying out metallographic observation, the ethanol of specimen surface is dried up, be placed on
In metallurgical microscope, use suitable amplification that austenite crystal carries out observational study, and gather relevant metallograph, in case
Crystal grain data analysis；100X austenite crystal metallograph is as shown in Figure 3 under metallurgical microscope for sample；
(iv) metallograph analysis is measured with austenite grain size and is analyzed
A. use IPP(Image-Pro-Plus) software to gather metallograph carry out pixel dualization process, austenite crystal
Differential reinforcement；
B. complete austenite crystal is demarcated；
C. use IPP software statistics to demarcate austenite crystal area, each single austenite crystal is considered as spheroidal particle, enters
OKConversion, counts the size of austenite experience.
The present invention is not limited to above-described embodiment.The technical scheme that all employing equivalents are formed, all falls within the present invention and wants
The protection domain asked.
Claims (4)
1. the method manifesting Microalloyed Austenite crystal boundary under a Vacuum Heat etching condition, it is characterised in that: include following step
Rapid:
(i) prepared by sample
A. cutting: first carry out cutting on strand and intercept sample；
B. grind away: again the sample that strand intercepts is ground off iron scale on abrasive machine, grind off the sample after iron scale at gold
Refine on phase sand paper；
C. polishing: the sample after fine grinding polishes on buffing machine again；
D. clean: by the sample alcohol washes after polishing, dry up；
(ii) the heat treated of style under vacuum condition
A. heating in vacuum: using the heating furnace with fine vacuum atmosphere to heat after sample is taken out 2-3 vacuum, sample is with stove
It is warming up to each design temperature 1200 DEG C, is then incubated 45min；
B. protective atmosphere rapid cooling: use noble gas quickly to cool down sample under vacuum, will use noble gas under vacuum
The sample extremely fast cooled down is immersed in ethanol, in case metallographic observation uses；
(iii) austenite crystal metallographic observation and picture collection: when carrying out metallographic observation, the ethanol of specimen surface is dried up, be placed on
In metallurgical microscope, use suitable amplification that austenite crystal carries out observational study, and gather relevant metallograph, in case
Crystal grain data analysis；
(iv) metallograph analysis is measured with austenite grain size and is analyzed
A. metallograph pixel dualization processes, austenite crystal differential reinforcement；
B. complete austenite crystal is demarcated；
C. austenite crystal is considered as spheroidal particle, adds up austenite grain size.
The method manifesting Microalloyed Austenite crystal boundary under Vacuum Heat etching condition the most according to claim 1, its feature
Be: in described step B (i), grind off the sample after iron scale successively 180#, 400#, 600#, 800#, 1000#,
Refine on 1200#, 1500#, 1800#, 2000# abrasive paper for metallograph.
The method manifesting Microalloyed Austenite crystal boundary under Vacuum Heat etching condition the most according to claim 2, its feature
Being: in described step C (i), polishing agent uses fine-grained diamond polishing cream, uses water as lubricant.
The method manifesting Microalloyed Austenite crystal boundary under Vacuum Heat etching condition the most according to claim 3, its feature
It is: in described step D (i), the sample dried up is immersed in ethanol on pretreatment, true for the specimen surface of laboratory observation
Protect without defects such as any pit, pit, stains, the most do not leave cut.
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Cited By (9)
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|---|---|---|---|---|
| CN106404484A (en) * | 2016-09-19 | 2017-02-15 | 太原理工大学 | Method for displaying grain structure of invar alloy through high-temperature oxidation |
| CN109297781A (en) * | 2018-10-25 | 2019-02-01 | 西北稀有金属材料研究院宁夏有限公司 | A kind of beryllium oxide ceramics metallographic thermal etching and the display methods of metallographic structure |
| CN110174402A (en) * | 2019-05-14 | 2019-08-27 | 南京钢铁股份有限公司 | A method of distinguishing hot-rolled steel red oxidization skin and red corrosion product |
| CN110487985A (en) * | 2019-08-15 | 2019-11-22 | 钢铁研究总院 | A kind of measurement method of low-alloy steel heat treatment process austenite grain size |
| CN110926913A (en) * | 2019-12-31 | 2020-03-27 | 北京科技大学 | Display method of spring steel austenite grains |
| CN112378823A (en) * | 2020-11-11 | 2021-02-19 | 成都先进金属材料产业技术研究院有限公司 | Method for displaying twin-crystal-free structure grain size of austenitic stainless steel after solid solution |
| CN113176181A (en) * | 2021-04-28 | 2021-07-27 | 钢铁研究总院 | Grain size testing method |
| CN113640183A (en) * | 2021-08-05 | 2021-11-12 | 常州天山重工机械有限公司 | Method for detecting austenite grains of carburized steel by oxidation method |
| CN115954065A (en) * | 2022-12-07 | 2023-04-11 | 重庆大学 | Prediction method for austenite grain size of TSCR (thyristor switched reactor) process of microalloyed steel |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106404484A (en) * | 2016-09-19 | 2017-02-15 | 太原理工大学 | Method for displaying grain structure of invar alloy through high-temperature oxidation |
| CN109297781A (en) * | 2018-10-25 | 2019-02-01 | 西北稀有金属材料研究院宁夏有限公司 | A kind of beryllium oxide ceramics metallographic thermal etching and the display methods of metallographic structure |
| CN110174402A (en) * | 2019-05-14 | 2019-08-27 | 南京钢铁股份有限公司 | A method of distinguishing hot-rolled steel red oxidization skin and red corrosion product |
| CN110174402B (en) * | 2019-05-14 | 2021-07-13 | 南京钢铁股份有限公司 | Method for distinguishing red oxide skin and red corrosion product of hot rolled steel |
| CN110487985A (en) * | 2019-08-15 | 2019-11-22 | 钢铁研究总院 | A kind of measurement method of low-alloy steel heat treatment process austenite grain size |
| CN110926913A (en) * | 2019-12-31 | 2020-03-27 | 北京科技大学 | Display method of spring steel austenite grains |
| CN112378823A (en) * | 2020-11-11 | 2021-02-19 | 成都先进金属材料产业技术研究院有限公司 | Method for displaying twin-crystal-free structure grain size of austenitic stainless steel after solid solution |
| CN113176181A (en) * | 2021-04-28 | 2021-07-27 | 钢铁研究总院 | Grain size testing method |
| CN113640183A (en) * | 2021-08-05 | 2021-11-12 | 常州天山重工机械有限公司 | Method for detecting austenite grains of carburized steel by oxidation method |
| CN113640183B (en) * | 2021-08-05 | 2024-01-12 | 常州天山重工机械有限公司 | Method for inspecting carburizing steel austenite grains by oxidation method |
| CN115954065A (en) * | 2022-12-07 | 2023-04-11 | 重庆大学 | Prediction method for austenite grain size of TSCR (thyristor switched reactor) process of microalloyed steel |
| CN115954065B (en) * | 2022-12-07 | 2024-05-07 | 重庆大学 | Austenite grain size prediction method for micro-alloyed steel TSCR process |
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