CN101349621A - Method for clearly displaying low carbon low alloy steel austenite crystal - Google Patents
Method for clearly displaying low carbon low alloy steel austenite crystal Download PDFInfo
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- CN101349621A CN101349621A CNA2008100793262A CN200810079326A CN101349621A CN 101349621 A CN101349621 A CN 101349621A CN A2008100793262 A CNA2008100793262 A CN A2008100793262A CN 200810079326 A CN200810079326 A CN 200810079326A CN 101349621 A CN101349621 A CN 101349621A
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Abstract
The invention relates to a method for clearly displaying lower carbon and low alloy steel austenite crystal, which belongs to the technical field of physical detection. The method is used to solve the problem that lower carbon and low alloy steel can not clearly display the austenite crystal thereof. The method comprises a quenching process and a corrosion process, which is characterized in that the proportion of corrosive agent in the process of corroding is that CrO3 8g-10g, NaOH 40g-50g, picric acid 1.6g-2g, epoxyethane 2ml-4ml and distilled water 80ml-100ml. The method adopts specific corrosive agent and is matched with a correct corrosion method, which can clearly display austenite grain boundary. The method fills a gap of low carbon alloy steel austenite grain boundary display technology, which provides an important theoretical basis for a manufacturing enterprise to research the influence of technological parameters to microstructure evolution when the steel is deforming, and plays an important function for producing low carbon alloy steel, reasonably controlling technological parameters and guaranteeing the property of products.
Description
Technical field
Type of the present invention relates to a kind of metallographic structure explicit representation, and method that particularly can clear demonstration mild carbon steel low alloy steel austenite crystal grain belongs to the physical detection technical field.
Technical background
The autstenitic grain size of steel has a significant impact intensity, toughness and the fatigue behaviour etc. of steel, for the development law of material structure in the research steel production run, reasonable CONTROL PROCESS parameter and guarantee that properties of product have vital role, therefore the detection of austenite grain size has very important meaning, and raising is constantly inquired into, innovated to its display packing by numerous insiders.Can austenite crystal clearly be shown multiple factors such as the chemical constitution depend on sample, condition of heat treatment, etch time, etching method, etchant, display packing commonly used has oxidizing process, ferrite net method, netted pearlite method, heating slow cooling method, grain boundary corrosion method, network cementite method etc., and wherein effect is preferably the grain boundary corrosion method.At present, it is saturated picric acid aqueous solution and saturated picral that the grain boundary corrosion method is used maximum mordant, in addition, can add some surfactants such as washing powder, washing agent etc. and strengthen corrosive effect.This etchant centering, high-carbon steel are very effective, but for the low-carbon and low-alloy high purity steel, the problem that austenite grain boundary is difficult to show not can solve always.With regard to prior art, Wieder-man etc. adopt boiling CrO
3-NaOH corrodes low, medium alloy steel, and effect is better; Dong Yuhua, CrO is adopted in high your presence etc.
3-NaOH-picric acid corroded pipeline steel, the austenite grain boundary of display pipeline steel preferably; Wang Jing, it is apparent in view that the mordant of employing neopelex+picric acid such as Xiao Furen+distilled water ten bromogeramines has corroded X70 pipe line steel austenite grain boundary.But above-mentioned caustic solution is only limited to the corrosion of special component steel, but also can not fully clearly show original austenite crystal prevention, and the austenite grain boundary of the high purity steel especially extremely low to carbon content, that impurity content is very low can show basically.Therefore looking for the etching method of the clear demonstration low carbon low alloy steel austenite of a kind of energy crystal boundary, is considerable to microstructure evolution rule in this type of steel research deformation process.
Summary of the invention
The method that the purpose of this invention is to provide a kind of clearly displaying low carbon low alloy steel austenite crystal, thus the important theory foundation provided for studying technological parameter in such steel deformation process to the influence of microstructure evolution.
The alleged problem of the present invention is that following technical scheme solves:
A kind of method of clearly displaying low carbon low alloy steel austenite crystal, be used for C content≤and contain the low-carbon low-alloy steel of microalloy elements such as small amount of N b, V, Ti, Mo in 0.10%, it comprises quenching process and corrosion process, and its special feature is: the mordant proportioning is as follows in the described corrosion process: CrO
38g~10g, NaOH 40g~50g, picric acid 1.6g~2g, oxirane 2ml~4ml, distilled water 80ml~100ml.
The method of above-mentioned clearly displaying low carbon low alloy steel austenite crystal, described corrosion process comprises the steps:
A. prepare sample: with quenching buck, polishing;
B. dispose mordant: take by weighing the mordant constituent according to proportioning, get distilled water and be put in the vessel, in distilled water, add CrO then
3, treat CrO
3Slowly add NaOH again after the dissolving fully, add picric acid solution after NaOH adds again, add oxirane at last and stir, the solution after preparing is heated to 110 ℃~130 ℃ insulations;
C. sample corrodes: the sample that polishes is put in the mordant corrodes, the sample etch faces up, and etch time 40min~60min treats to take out when the sample polished surface becomes iron cyan, cleans, dries up, and can examine under a microscope austenite crystal.
The present invention is directed to the problem that present low-carbon low-alloy steel still can't clear its austenite crystal of demonstration, but a kind of method of clearly displaying low carbon low alloy steel austenite crystal is provided.It adopts specific mordant to be equipped with suitable caustic solution, can clearly demonstrate austenite grain boundary, this method has been filled up the blank of carbon low alloy steel austenite grain boundary display technique, for technological parameter in such steel deformation process of production business research provides the important theory foundation to the influence of microstructure evolution, to producing the reasonable CONTROL PROCESS parameter of low-carbon low-alloy steel and guaranteeing that product all can play an important role.
Description of drawings
Fig. 1 is the austenite grain boundary of the embodiment of the invention 1;
Fig. 2 is the austenite grain boundary of the embodiment of the invention 2;
Fig. 3 is the austenite grain boundary of the embodiment of the invention 3.
Embodiment
The inventive method is applicable to C content smaller or equal to 0.10%, and contains the high purity steel low-carbon low-alloy steel of microalloy elements such as Nb, V, Ti, Mo.Its characteristics adopt specific mordant and caustic solution at the steel grade chemical constitution.The proportional quantity of the mordant among the present invention is groped out by experimental study repeatedly.CrO in the described mordant
3, NaOH, picric acid decompose strong when being put in the distilled water heating, etch rates is very fast, but easily produce the corrosion product of one deck indissoluble during its corrosion sample, cause passivation, cause crystal boundary unintelligible, add the epoxy hexane in mordant, the increase surfactivity also suppresses intergranular structure and separates out, and can make austenite grain boundary more clear.The inventive method comprises quenching and corrodes two processes.Wherein, quenching process is heated to 1050~1200 ℃ of austenitizing temperatures with sample, and the insulation certain hour allows the whole solid solutions of carbonide in matrix, then sample is put into temperature and is lower than 20 ℃ quenching-in water.Corrosion process with the quenching buck, the polishing after join mordant, mordant after preparing is heated to 110~130 ℃ and be incubated on thermostatic oven, then the sample of polishing is put in the solution and corrodes, the sample etch etch that faces up, the etch time is subjected to all multifactor impacts such as the material, condition of heat treatment, reagent character, temperature of sample, become iron cyan with the sample polished surface and exceed, the etch time is 40min~60min usually.When the iron cyan film occurring on the sample polished surface, take out, clean, dry up, can examine under a microscope austenite crystal clearly.
Below provide several specific embodiments
Embodiment 1: the chemical constitution of sample 1 is C:0.08%, Si:0.24%, Mn:1.36%, V:0.035%, Ti:0.023%, Nb:0.030%, Als:0.032%, P:0.012%, S:0.003%.Sample quenches: sample is heated to 1050 ℃, and the insulation certain hour allows the whole solid solutions of carbonide in matrix, then sample is put into temperature and is lower than 20 ℃ quenching-in water; With quenching buck, polishing; According to following proportioning configuration mordant: CrO
39g, NaOH 40g, picric acid 1.6g, oxirane 2ml, distilled water 80ml.Measure 80ml distilled water during preparation earlier and be put in the vessel, in distilled water, add CrO then
3, treat CrO
3Add NaOH again after the dissolving fully.Because the NaOH amount is many, and can produce strong themopositive reaction, so should slowly add in order to avoid splash, adds picric acid solution and oxirane after NaOH adds again.The caustic solution for preparing is heated to 110 ℃ and be incubated on thermostatic oven, the sample of polishing is put in the solution corrodes then, and the sample etch faces up, etch time 40min.When becoming iron cyan on the sample polished surface, take out, clean, dry up, can examine under a microscope austenite crystal.As seen from Figure 1, austenite grain boundary clearly shows, and tissue does not occur.
Embodiment 2: the chemical constitution of sample 2 is C:0.05%, Si:0.20%, Mn:1.45%, Mo:0.17%, Ti:0.017%, Nb:0.042%, Als:0.030%, P:0.010%, S:0.005%.Sample quenches: sample is heated to 1150 ℃, and the insulation certain hour allows the whole solid solutions of carbonide in matrix, then sample is put into temperature and is lower than 20 ℃ quenching-in water; With quenching buck, polishing; According to following proportioning configuration mordant: CrO
310g, NaOH 50g, picric acid 1.8g, oxirane 3ml, distilled water 90ml.Compound method is with embodiment 1.Caustic solution after preparing is heated to 120 ℃ and be incubated on thermostatic oven, the sample of polishing is put in the solution corrodes then, the sample etch faces up, etch time 50min.When becoming iron cyan on the sample polished surface, take out, clean, dry up, can examine under a microscope austenite crystal.As seen from Figure 2, austenite grain boundary clearly shows, and tissue does not occur.
Embodiment 3: the chemical constitution of sample 3 is C:0.03%, Si:0.20%, Mn:1.72%, Mo:0.25%, Ti:0.015%, Nb:0.040%, V:0.050%, Cu:0.2%, Als:0.025%, P:0.014%, S:0.004%.Sample quenches: sample is heated to 1200 ℃, and the insulation certain hour allows the whole solid solutions of carbonide in matrix, then sample is put into temperature and is lower than 20 ℃ quenching-in water; With quenching buck, polishing; According to following proportioning configuration mordant: CrO
38g, NaOH 45g, picric acid 2g, oxirane 4ml, distilled water 100ml.Compound method is with embodiment 1.Solution after preparing is heated to 130 ℃ and be incubated on thermostatic oven, the sample of polishing is put in the solution corrodes then, the sample etch faces up, about 60min of etch time.When becoming iron cyan on the sample polished surface, take out, clean, dry up, can examine under a microscope austenite crystal.As seen from Figure 3, austenite grain boundary clearly shows, and tissue does not occur.
Claims (2)
1. the method for a clearly displaying low carbon low alloy steel austenite crystal, be used for C content≤and contain the low-carbon low-alloy steel of microalloy elements such as small amount of N b, V, Ti, Mo in 0.10%, it comprises quenching process and corrosion process, it is characterized in that: the mordant proportioning is as follows in the described corrosion process: CrO
38g~10g, NaOH 40g~50g, picric acid 1.6g~2g, oxirane 2ml~4ml, distilled water 80ml~100ml.
2. the method for above-mentioned clearly displaying low carbon low alloy steel austenite crystal, it is characterized in that: described corrosion comprises the steps:
A. prepare sample: with quenching buck, polishing;
B. dispose mordant: take by weighing the mordant constituent according to proportioning, get distilled water and be put in the vessel, in distilled water, add CrO then
3, treat CrO
3Slowly add NaOH again after the dissolving fully, add picric acid solution after NaOH adds again, add oxirane at last and stir, the solution after preparing is heated to 110 ℃~130 ℃ insulations;
C. sample corrodes: the sample that polishes is put in the mordant corrodes, the sample etch faces up, and etch time 40min~60min treats to take out when the sample polished surface becomes iron cyan, cleans, dries up, and can examine under a microscope austenite crystal.
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Cited By (16)
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CN102183402A (en) * | 2011-04-01 | 2011-09-14 | 天津万立鑫晟新材料技术研究院有限公司 | Method for preparing grain size test sample of high-chromium cast iron |
CN102313663A (en) * | 2010-06-29 | 2012-01-11 | 鞍钢股份有限公司 | Corrosive agent for dendritic crystal of X70 pipeline steel casting blank and display method |
CN102353566A (en) * | 2011-06-10 | 2012-02-15 | 中国科学院金属研究所 | Method for displaying thermal deformation texture of steel used for nuclear power pressure container |
CN102507292A (en) * | 2011-09-21 | 2012-06-20 | 内蒙古包钢钢联股份有限公司 | Method for displaying austenite grain boundary of low-carbon micro-alloy steel |
CN102539217A (en) * | 2011-12-26 | 2012-07-04 | 昆山全亚冠环保科技有限公司 | Silver-gold alloy metallographic corrosive agent and metallographic display method |
CN102590050A (en) * | 2012-01-19 | 2012-07-18 | 东方电气集团东方锅炉股份有限公司 | Method for displaying P91 and P92 steel original austenite grain boundaries |
CN101995349B (en) * | 2009-08-10 | 2013-01-09 | 鞍钢股份有限公司 | Corrosive agent for metallographic structure of high-steel-grade pipeline steel and display method |
CN103163004A (en) * | 2013-03-21 | 2013-06-19 | 上海大学 | Austenite crystal boundary display method under condition of high-temperature deformation of medium-carbon microalloyed steel |
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 |
CN106053471A (en) * | 2016-08-04 | 2016-10-26 | 南京钢铁股份有限公司 | Method for showing austenite crystal boundary of micro-alloyed steel in vacuum hot-corrosion condition |
CN106596234A (en) * | 2016-12-02 | 2017-04-26 | 昆明理工大学 | Method for displaying original austenite grain boundary of low-carbon microalloyed steel |
CN106756510A (en) * | 2017-01-03 | 2017-05-31 | 华东交通大学理工学院 | A kind of etchant for showing low-alloy wear-resistant steel original austenite crystal prevention and its application |
CN109142010A (en) * | 2018-09-10 | 2019-01-04 | 中国石油天然气集团有限公司 | A kind of method of retained austenite distribution and content in detection low-alloy structural steel |
CN110376047A (en) * | 2019-07-22 | 2019-10-25 | 南京钢铁股份有限公司 | A kind of medium carbon steel autstenitic grain size detection method |
CN112213171A (en) * | 2020-10-22 | 2021-01-12 | 昆明理工大学 | Corrosion display method for original austenite grain boundary of S34MnV steel |
CN113866055A (en) * | 2021-09-01 | 2021-12-31 | 东方电气(广州)重型机器有限公司 | Method for detecting grain size of quenched and tempered steel |
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CN102313663A (en) * | 2010-06-29 | 2012-01-11 | 鞍钢股份有限公司 | Corrosive agent for dendritic crystal of X70 pipeline steel casting blank and display method |
CN102313663B (en) * | 2010-06-29 | 2014-07-30 | 鞍钢股份有限公司 | Corrosive agent for dendritic crystal of X70 pipeline steel casting blank and display method |
CN102183402A (en) * | 2011-04-01 | 2011-09-14 | 天津万立鑫晟新材料技术研究院有限公司 | Method for preparing grain size test sample of high-chromium cast iron |
CN102183402B (en) * | 2011-04-01 | 2013-01-16 | 天津万立鑫晟新材料技术研究院有限公司 | Method for preparing grain size test sample of high-chromium cast iron |
CN102353566A (en) * | 2011-06-10 | 2012-02-15 | 中国科学院金属研究所 | Method for displaying thermal deformation texture of steel used for nuclear power pressure container |
CN102507292A (en) * | 2011-09-21 | 2012-06-20 | 内蒙古包钢钢联股份有限公司 | Method for displaying austenite grain boundary of low-carbon micro-alloy steel |
CN102539217A (en) * | 2011-12-26 | 2012-07-04 | 昆山全亚冠环保科技有限公司 | Silver-gold alloy metallographic corrosive agent and metallographic display method |
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CN103163004A (en) * | 2013-03-21 | 2013-06-19 | 上海大学 | Austenite crystal boundary display method under condition of high-temperature deformation of medium-carbon microalloyed steel |
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 |
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 |
CN106053471A (en) * | 2016-08-04 | 2016-10-26 | 南京钢铁股份有限公司 | Method for showing austenite crystal boundary of micro-alloyed steel in vacuum hot-corrosion condition |
CN106596234A (en) * | 2016-12-02 | 2017-04-26 | 昆明理工大学 | Method for displaying original austenite grain boundary of low-carbon microalloyed steel |
CN106756510A (en) * | 2017-01-03 | 2017-05-31 | 华东交通大学理工学院 | A kind of etchant for showing low-alloy wear-resistant steel original austenite crystal prevention and its application |
CN109142010A (en) * | 2018-09-10 | 2019-01-04 | 中国石油天然气集团有限公司 | A kind of method of retained austenite distribution and content in detection low-alloy structural steel |
CN109142010B (en) * | 2018-09-10 | 2020-12-01 | 中国石油天然气集团有限公司 | Method for detecting distribution and content of residual austenite in low-alloy structural steel |
CN110376047A (en) * | 2019-07-22 | 2019-10-25 | 南京钢铁股份有限公司 | A kind of medium carbon steel autstenitic grain size detection method |
CN112213171A (en) * | 2020-10-22 | 2021-01-12 | 昆明理工大学 | Corrosion display method for original austenite grain boundary of S34MnV steel |
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