CN108535309A - Fe in a kind of in situ measurement low-carbon alloy steel3The method of C amount of precipitations - Google Patents

Fe in a kind of in situ measurement low-carbon alloy steel3The method of C amount of precipitations Download PDF

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CN108535309A
CN108535309A CN201810338057.0A CN201810338057A CN108535309A CN 108535309 A CN108535309 A CN 108535309A CN 201810338057 A CN201810338057 A CN 201810338057A CN 108535309 A CN108535309 A CN 108535309A
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skk
fighting
precipitations
amount
temperature
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CN108535309B (en
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周红伟
唐明星
李家琪
叶昕
周佩剑
司聪
郭忠亮
何宜柱
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Changzhou Dongfang Special Steel Co ltd
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Anhui University of Technology AHUT
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    • G01N25/00—Investigating or analyzing materials by the use of thermal means

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Abstract

Fe in a kind of in situ measurement low-carbon alloy steel of present invention offer3The method of C amount of precipitations belongs to metal material technical field of measurement and test.Low-carbon alloy steel curved beam to be measured through solution treatment is processed into steel in-fighting test sample by this method first, then an in-fighting test sample is mounted in in-fighting test equipment, it is rapidly heated by room temperature to cooling down immediately after 350 DEG C, measures the peaks SKK for being cooled to room temperature process；SKK peak of the steel in-fighting test sample after Overheating Treatment after third pacing amount solution treatment, the in-fighting test sample after Overheating Treatment for then obtaining step 3 are rapidly heated after being cooled to room temperature to target temperature T0Afterwards, soaking time t2, 350 DEG C of peaks SKK for being cooled to room temperature process are measured, by repeating the process of step 4, the in-fighting curve of sample is handled under the different soaking times obtained to measurement, and Fe is determined according to SKK peak intensities3C amount of precipitations obtain carbide Fe3The kinetic characteristics that C is precipitated.The present invention is easy to operate, and sample is easy to prepare, and high certainty of measurement, speed are fast.

Description

Fe in a kind of in situ measurement low-carbon alloy steel3The method of C amount of precipitations
Technical field：
The invention belongs to metal material technical field of measurement and test, and in particular to Fe in a kind of in situ measurement low-carbon alloy steel3C is analysed The method of output.
Background technology：
Carbon (C) element is one of alloying element mostly important in steel.C atoms are easy to form cementite Fe in steel3C, The carbide is one of most important composition phase in structure of steel, and quantity, form and distribution have directly the performance of steel material It influences.Therefore, it is also to need to consider the problems of first that can steel material C atoms when formulating tempering process, which fully be precipitated, accurate Really measure Fe in steel3C amount of precipitations are to formulate the theoretical foundation of rational heat treatment process.
Now in the art, Fe in steel3The method that the detection methods of C amount of precipitations uses generally has metallographic method, hardness method and interior Consumption method.The Internal Friction Peak patent being disclosed " measures Fe in low-carbon microalloy Steel material3The method of C meltages and amount of precipitation " is (public The number of opening：CN104007244A).But this Internal Friction Measurements measure Fe3The method of C amount of precipitations surveys the heat treatment of steel curved beam and in-fighting Examination individually carries out, and multiple samples is first carried out to the heat treatment test of different temperatures and different tempering times, then to heat- treated steel sample Sample in being processed into, the heavy workload of in-fighting test, the efficiency of test are low.
In-fighting is a kind of physical property of material, different defect type in metal material, such as solute atoms, dislocation, crystalline substance The defects of boundary, will present out the Internal Friction Peak of different characteristic.Internal Friction Peak can be used for test in analysis of metallic materials defect it is related Information is obtained about relevant informations such as defect kind, configuration, distribution, solubility and thermodynamic processes.Steel material heating and It will appear two kinds of main Internal Friction Peaks in temperature-fall period, be distributed as the peaks Snoek and the peak Snoek-Koster-Ke (SKK).Wherein, The peaks Snoek are located at 20~60 DEG C or so, are the in-fightings caused by the micro- diffusion of C or N atoms in body-centered cubic.Another peak SKK 180~250 DEG C of ranges are normally at, producing cause is that there are stress fields, C atoms to be answered in dislocation around dislocation due to deformation Field of force range forms Cottrell air mass, which can generate pinning effect to the sliding of dislocation, hinder its movement, and work as dislocation When overcoming pinning effect and moving, and the C atoms in Cottrell air mass can be made to generate redistribution, this dislocation motion and gas The reciprocation of group repeatedly, will produce in-fighting, and the intensity of Internal Friction Peak is directly proportional to the content of solid solution condition C atoms；For same In a kind of steel sample, Fe3C amount of precipitations are more, and the content of solid solution condition C atoms is fewer, and the intensity at the peaks SKK is lower.The peaks SKK are to relax Henan type Internal Friction Peak is heating up in temperature-fall period, and the intensity of Internal Friction Peak is kept approximately constant.
In steel material, the main of C is exactly with Fe3C is main existence form, Fe3Release is come from decomposable process in C By the C atoms spread, it will influence SKK peak intensities.Therefore, the intensity at the peaks SKK is with Fe3The increase of C amount of precipitations and reduce.
Invention content：
The object of the present invention is to provide Fe in a kind of in situ measurement low-carbon alloy steel3The method of C amount of precipitations, this method pass through Test the Internal Friction Peak of temperature-fall period after the heat treatment of in-fighting sample, measurement efficiently and accurately after heat treatment Fe in steel3C is precipitated Amount.
Fe in a kind of in situ measurement low-carbon alloy steel provided by the present invention3The method of C amount of precipitations is as follows：
(1) solution treatment of low-carbon alloy steel curved beam to be measured：
The low-carbon alloy steel curved beam to be measured is taken into a temperature more than austenite transformation finishing temperature, when keeping the temperature one section Between after water quenching obtain the steel in-fighting test sample after solution treatment, the C atoms in steel in-fighting sample exist in the form of being dissolved, nothing Fe3C is precipitated.
(2) peaks SKK of the steel in-fighting test sample after solution treatment are measured：
Steel in-fighting test sample after step (1) described solution treatment is mounted in in-fighting test equipment, it is fast by room temperature Speed cools down immediately after being warming up to 350 DEG C, and it is in-fighting test phase that room temperature is cooled to from 350 DEG C, measures 350 DEG C and is cooled to room temperature mistake The peaks SKK of journey, the peaks SKK are most strong, as no Fe3The intensity at the peaks SKK when C is precipitated, the reference value as follow-up test.
(3) SKK peak of the steel in-fighting test sample after solution treatment after Overheating Treatment is measured：
Step (2) treated steel in-fighting test sample is rapidly heated to target temperature T0After kept the temperature, when heat preservation Between be t1, then fast cooling is to 350 DEG C, and 350 DEG C of peaks SKK for being cooled to room temperature process of measurement, being cooled to room temperature from 350 DEG C is In-fighting test phase, t1Soaking time has Fe3C is precipitated, and the peak intensity at the peaks SKK declines.
(4) the in-fighting test sample after Overheating Treatment for obtaining step (3), is rapidly heated after being cooled to room temperature to mesh Mark temperature T0After kept the temperature, soaking time t2, 350 DEG C of peaks SKK for being cooled to room temperature process are measured, room is cooled to from 350 DEG C Temperature is in-fighting test phase, due to soaking time (t1+t2) increase, Fe3C amount of precipitations increase, and the intensity at the peaks SKK is compared with step (3) Middle result further declines.
(5) by repeating the process of step (4), the in-fighting curve of sample carries out under the different soaking times obtained to measurement Processing, Fe is determined according to SKK peak intensities3C amount of precipitations obtain carbide Fe3The kinetic characteristics that C is precipitated.
Heating rate in step (2)-(4) and rate of temperature fall >=30 DEG C/min, the cooling speed of the in-fighting test phase Rate is 2 DEG C/min；Soaking time in the step (1) is 120min；Steel in-fighting examination after solution treatment described in step (1) Sample removes surface scale, is processed into in-fighting sample.
In-fighting test equipment described in step (2) is MFP-1000 Internal Friction Meters, and heat treatment pipe type is equipped in the Internal Friction Meter Stove, thermometric error are ± 3 DEG C, and highest measurement temperature is up to 1000 DEG C.
The shape of low-carbon alloy steel curved beam to be measured described in step (1) is the cuboid of 80 × 10 × 5mm, is passed through after water quenching The oxide skin on processing removal surface.
The specification of steel in-fighting test sample after solution treatment described in step (2) is 1.5 × 2.5 × 65mm, and by institute The surface for stating the steel in-fighting test sample after solution treatment is carried out with 100# -200# -400# -600# -800# sand paper successively Polishing, is then polished so that surface is smooth.
SKK peak intensity of the present invention by comparing solid solution sample and the SKK peak intensities through sample under different soaking times, obtain Go out Fe3Relation curve between C amount of precipitations and soaking time.Equipment for Heating Processing connects two-stage vacuum pump on MFP-1000 Internal Friction Meters (mechanical pump and diffusion pump) and protective gas device are in high vacuum state or argon keeping the temperature with in-fighting sample in test process Under gas shielded atmosphere, prevent sample from aoxidizing the influence to measuring accuracy.
The present invention passes through retest step：Room temperature->Be rapidly heated->Target temperature->Soaking time->Fast prompt drop Temperature to 350 DEG C->Test the peaks SKK-of temperature-fall period>Room temperature realizes an in-fighting sample in situ measurement different heat treatment time Lower SKK peak intensities, are calculated Fe3C amount of precipitations obtain carbide Fe3The kinetic characteristics that C is precipitated.This method is to steel material In-fighting sample after Overheating Treatment, SKK in-fighting peak intensities caused by C atom contents of the real time measure by solid solution condition in sample Variation, determine Fe3The amount of precipitation of C.
The method of the present invention compared with metallographic method mensuration, can measure Fe in tapping with existing hardness method3C amount of precipitations are surveyed Amount method is quick and easy, measuring accuracy is high.Compared with general friction test method needs large batch of heat treatment and in-fighting sample Only need a small amount of sample compared with, method of the invention, testing efficiency is high, and to the low-carbon alloy steel material compatibility of heterogeneity compared with By force, it is with a wide range of applications.
Description of the drawings：
Fig. 1 is an in-fighting test sample initial heating in the embodiment of the present invention 1, heat preservation, the test of the peaks temperature-fall period SKK Process schematic.
Fig. 2 is that an in-fighting test sample in the embodiment of the present invention 1 retest step under different soaking times is shown It is intended to.
Fig. 3 is the graph of relation of SKK the peak intensities variation and soaking time in the embodiment of the present invention 1.
Fig. 4 is the Fe in the embodiment of the present invention 13C amount of precipitations and soaking time graph of relation.
Specific implementation mode：
By taking low-carbon alloy steel Q500 as an example, chemical composition is shown in Table 1, measures Q500 by the method for the invention and is kept the temperature at 700 DEG C Fe under different time3C amount of precipitations.
Table 1：Q500 steel chemical compositions (wt.%)
C Mn Si P S N
≦0.18 ≦1.80 ≦0.60 ≦0.045 ≦0.045 ≦0.015
Embodiment 1：It is as follows：
(1) low-carbon alloy steel curved beam to be measured is processed into the cuboid that specification is 80 × 10 × 5mm, into 910 DEG C of high temperature excessively Solution treatment, keep the temperature 120min after water quenching, the steel sample after higher temperature solid solution be processed into 2-3 root specifications be 1.5 × 2.5 × The in-fighting test sample of 65mm, 100# -200# -400# -600# -800# sand paper is polished successively on surface, is then carried out Polishing so that surface is smooth.
(2) an above-mentioned in-fighting test sample is mounted on MFP-1000 Internal Friction Meters, it is quick by room temperature after pumping high vacuum 350 DEG C are warming up to, heating rate is 30 DEG C/min, is cooled down immediately after reaching 350 DEG C, and the peaks SKK of temperature-fall period, cooling speed are tested Rate is 2 DEG C/min, it is believed that C atoms are completely in the SKK peak intensities under solid solution condition, as subsequent step SKK under the conditions of this The reference value of peak intensity test.
(3) by step (2), treated that steel in-fighting test sample is rapidly heated to after 700 DEG C of target temperature, soaking time 30min, subsequent fast cooling is to 350 DEG C, SKK peak of 350 DEG C of the test to room temperature process；There is Fe after heat preservation 20min3C is precipitated, The intensity at the peaks SKK declines compared with the Internal Friction Peak of step (2).
(4) the in-fighting test sample that step (3) obtains is cooled to after room temperature and is rapidly heated to 700 DEG C, soaking time 30min repeats step test temperature-fall period SKK peaks, and the total soaking time of in-fighting sample is about 60min, obtained SKK peak intensities into One step declines.
(5) by repeat step (4) process, can in situ measurement at 700 DEG C, total soaking time is respectively The intensity at the peaks SKK under the conditions of 30min, 60min, 90min, 180min and 210min；To in sample under different soaking times Consumption spectrum carries out analyzing processing, and Fe is determined according to the intensity at the peaks SKK3C amount of precipitations.
The sample SKK peak intensities of heat preservation 0 minute are 100%, under different soaking times SKK peak intensities under heat preservation 0 minute SKK peak intensities be normalized, keep the temperature 180min and 210min under SKK peak intensities it is almost unchanged, it is believed that Fe3C is complete It is precipitated, reaches equilibrium state.It can be seen from the figure that, with the increase of soaking time, SKK peak intensities decrease, this is because Soaking time is longer, Fe in steel3C amount of precipitations increase, and the C content in solid solution condition is reduced, and the intensity at the peaks SKK is caused to decline. With the increase of soaking time, the SKK peak intensities being completely in C under solid solution condition make ratio, the Fe obtained3C amount of precipitations and guarantor The relation curve of warm time, the Fe in figure after heat preservation 30min, 60min, 90min, 180min and 210min in steel3C amount of precipitations Percentage is 30%, 52%, 74%, 93%, 100%.
Embodiment 2：It is as follows：
(1) low-carbon alloy steel curved beam to be measured is processed into the cuboid that specification is 80 × 10 × 5mm, into 910 DEG C of high temperature excessively Solution treatment keeps the temperature water quenching after 120min, and the C atoms in steel curved beam all exist in the form of being dissolved, no Fe3C is precipitated；Through height Steel sample after warm solution treatment is processed into the in-fighting test sample that 2-3 root specifications are 1.5 × 2.5 × 65mm, and surface is successively 100# -200# -400# -600# -800# sand paper is polished, and is then polished so that surface is smooth.
(2) an above-mentioned in-fighting test sample is mounted on MFP-1000 Internal Friction Meters, it is quick by room temperature after pumping high vacuum 350 DEG C are warming up to, heating rate is 30 DEG C/min, is cooled down immediately after reaching 350 DEG C, and the peaks SKK of temperature-fall period, cooling speed are tested Rate is 2 DEG C/min, it is believed that C atoms are completely in the SKK peak intensities under solid solution condition, as subsequent step SKK under the conditions of this The reference value of peak intensity test.
(3) by step (2), treated that in-fighting test sample is rapidly heated to after 650 DEG C of target temperature, soaking time 45min, subsequent fast cooling is to 350 DEG C, SKK peak of 350 DEG C of the test to room temperature process；There is Fe after heat preservation 45min3C is precipitated, The intensity at the peaks SKK declines compared with the Internal Friction Peak of step (2).
(4) the in-fighting test sample that step (3) obtains is cooled to after room temperature and is rapidly heated to 650 DEG C, soaking time 45min repeats step test temperature-fall period SKK peaks, and the total soaking time of in-fighting sample is about 90min, obtained SKK peak intensities into One step declines；
(5) by repeat step (4) process, can in situ measurement at 650 DEG C, total soaking time is respectively The intensity at the peaks SKK under the conditions of 45min, 90min, 180min, 210min and 300min；To in sample under different soaking times Consumption spectrum carries out analyzing processing, and Fe is determined according to the intensity at the peaks SKK3C amount of precipitations.
Embodiment 3：It is as follows：
(1) low-carbon alloy steel curved beam to be measured is processed into the cuboid that specification is 80 × 10 × 5mm, into 930 DEG C of high temperature excessively Solution treatment keeps the temperature water quenching after 120min, and the C atoms in steel curved beam all exist in the form of being dissolved, no Fe3C is precipitated, through height Steel sample after warm solution treatment is processed into the in-fighting test sample that 2-3 root specifications are 1.5 × 2.5 × 65mm, and surface is successively 100# -200# -400# -600# -800# sand paper is polished, and is then polished so that surface is smooth.
(2) an above-mentioned in-fighting test sample is mounted on MFP-1000 Internal Friction Meters, it is quick by room temperature after pumping high vacuum 350 DEG C are warming up to, heating rate is 30 DEG C/min, is cooled down immediately after reaching 350 DEG C, and the peaks SKK of temperature-fall period, cooling speed are tested Rate is 2 DEG C/min, it is believed that C atoms are completely in the SKK peak intensities under solid solution condition, as subsequent step SKK under the conditions of this The reference value of peak intensity test.
(3) by step (2), treated that in-fighting test sample is rapidly heated to after 750 DEG C of target temperature, soaking time 60min, subsequent fast cooling is to 350 DEG C, SKK peak of 350 DEG C of the test to room temperature process；There is Fe after heat preservation 60min3C is precipitated, The intensity at the peaks SKK declines compared with the Internal Friction Peak of step (2).
(4) the in-fighting test sample that step (3) obtains is cooled to after room temperature and is rapidly heated to 750 DEG C, soaking time 60min repeats the peaks step test temperature-fall period SKK, and the total soaking time of in-fighting sample is about 120min, obtained SKK peak intensities Further decline.
(5) by repeat step (4) process, can in situ measurement at 700 DEG C, total soaking time is respectively The intensity at the peaks SKK under the conditions of 60min, 120min, 180min and 240min；To the in-fighting of sample under different soaking times compose into Row analyzing processing determines Fe according to the intensity at the peaks SKK3C amount of precipitations.
Specific three examples the above is only the implementation of the present invention not limit the patent use scope of the present invention, all It is to carry out equivalence replacement or equivalent process transformation using content in the present invention, all falls within the scope of the present invention.

Claims (7)

1. Fe in a kind of in situ measurement low-carbon alloy steel3The method of C amount of precipitations, it is characterised in that this method is as follows：
(1) solution treatment of low-carbon alloy steel curved beam to be measured：
The low-carbon alloy steel curved beam to be measured is taken into a temperature more than austenite transformation finishing temperature, after keeping the temperature a period of time Water quenching obtains the steel in-fighting test sample after solution treatment；
(2) peaks SKK of the steel in-fighting test sample after solution treatment are measured：
Steel in-fighting test sample after step (1) described solution treatment is mounted in in-fighting test equipment, is quickly risen by room temperature For temperature to cooling down immediately after 350 DEG C, it is in-fighting test phase that room temperature is cooled to from 350 DEG C, measures 350 DEG C and is cooled to room temperature process The peaks SKK, the peaks SKK are most strong, as no Fe3The intensity at the peaks SKK when C is precipitated, the reference value as follow-up test；
(3) SKK peak of the steel in-fighting test sample after solution treatment after Overheating Treatment is measured：
Step (2) treated steel in-fighting test sample is rapidly heated to target temperature T0After kept the temperature, soaking time is t1, then fast cooling is to 350 DEG C, and 350 DEG C of peaks SKK for being cooled to room temperature process of measurement, it is in-fighting that room temperature is cooled to from 350 DEG C Test phase, in soaking time t1There is Fe3C is precipitated, and the peak intensity at the peaks SKK declines；
(4) the in-fighting test sample after Overheating Treatment for obtaining step (3) is rapidly heated after being cooled to room temperature to target temperature Spend T0After kept the temperature, soaking time t2, 350 DEG C of peaks SKK for being cooled to room temperature process are measured, being cooled to room temperature from 350 DEG C is In-fighting test phase, since soaking time increases, soaking time t1+t2, Fe3C amount of precipitations increase, and the intensity at the peaks SKK is compared with step (3) result further declines in；
(5) by repeating the process of step (4), under the different soaking times obtained to measurement at the in-fighting curve of sample Reason, Fe is determined according to SKK peak intensities3C amount of precipitations obtain carbide Fe3The kinetic characteristics that C is precipitated.
2. Fe in a kind of in situ measurement low-carbon alloy steel according to claim 13The method of C amount of precipitations, it is characterised in that institute The heating rate and rate of temperature fall >=30 DEG C/min in step (2)-(4) are stated, the rate of temperature fall of the in-fighting test phase is 2 ℃/min。
3. Fe in a kind of in situ measurement low-carbon alloy steel according to claim 13The method of C amount of precipitations, it is characterised in that institute It is 120min to state the soaking time in step (1).
4. Fe in a kind of in situ measurement low-carbon alloy steel according to claim 13The method of C amount of precipitations, it is characterised in that step Suddenly the steel in-fighting test sample after solution treatment described in (1) removes surface scale, is processed into in-fighting test sample.
5. Fe in a kind of in situ measurement low-carbon alloy steel according to claim 13The method of C amount of precipitations, it is characterised in that step Suddenly in-fighting test equipment described in (2) is MFP-1000 Internal Friction Meters, and heat treatment pipe type stove is equipped in the Internal Friction Meter, and temperature measures Error is ± 3 DEG C, and highest measurement temperature is up to 1000 DEG C.
6. Fe in a kind of in situ measurement low-carbon alloy steel according to claim 13The method of C amount of precipitations, it is characterised in that step Suddenly the shape of low-carbon alloy steel curved beam to be measured described in (1) is the cuboid of 80 × 10 × 5mm, passes through processing after water quenching and removes table The oxide skin in face.
7. Fe in a kind of in situ measurement low-carbon alloy steel according to claim 13The method of C amount of precipitations, it is characterised in that step Suddenly the specification of the steel in-fighting test sample after solution treatment described in (2) is 1.2 × 1.8 × 65mm, and by the solution treatment The surface of steel in-fighting sample afterwards is polished with 100# -200# -400# -600# -800# sand paper successively, is then thrown Light so that surface is smooth.
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