CN104596901B - A kind of method for measuring austenite grain size - Google Patents
A kind of method for measuring austenite grain size Download PDFInfo
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- CN104596901B CN104596901B CN201510011332.4A CN201510011332A CN104596901B CN 104596901 B CN104596901 B CN 104596901B CN 201510011332 A CN201510011332 A CN 201510011332A CN 104596901 B CN104596901 B CN 104596901B
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Abstract
The invention discloses a kind of measuring method of austenite grain size, this method by steel samples by carrying out austenitizing heating, rapid cooling, and carry out sample preparation according to the requirement of electron probe, line analysis is carried out to a certain element using electron probe, by measuring the method for distance between spectral line crest number and crest in active length come the quick austenite grain size for measuring sample.Such a analysis method is simple and easy to apply, do not influenceed by steel sample form factor, without corrosive agent, so as to can reach the effect saved the energy, reduce environmental pollution, and more directly perceived and accurate testing result can be provided, austenite grain size measurement request can be met completely.
Description
Technical field
It is more particularly to a kind of that austenite is measured using electron probe the invention belongs to material microstructure method of inspection field
The method of crystallite dimension.
Background technology
Traditional directly etching method is used to observe the tissues of steel samples, it is impossible to corrodes and austenite grain boundary, generally without
In direct measurement autstenitic grain size.Autstenitic grain size measurement typically has method of directly hardening, oxidizing process, ferrite net method.
Wherein directly the method for hardening is to want heating quenching to obtain martensite, shows crystal boundary with bitter taste acid corrosion, picric acid is poisonous, and
Surfactant is added, how much addition needs repeatedly to attempt, and the parameter such as corrosion temperature and time is also required to grope, and will
Ask steel grade phosphorus content high, repeatedly corrosion is often difficult to obtain satisfied effect, for medium carbon steel, particularly with close to eutectoid composition
Steel grade corrosive effect extreme difference；Oxidizing process, due to needing to tilt sample polishing after oxidation, what grinding and polishing had obtained shallow to obtain is decarburization
Layer, grinding and polishing has obtained deep and can only corrode martensitic structure, can not corrode oxide network, it is difficult to obtain promising result, often
Operation is multiple, and effect is bad will also to be repeated to test；Ferrite net method be in order to 730 DEG C or so austenite grain boundary formation iron
Ferritic network, but during practical operation, medium carbon steel frequently results in granular ferrite, and not shows completely along crystal boundary, effect
It is unsatisfactory, and carbon content be more than it is inapplicable when 0.77%.Existing autstenitic grain size e measurement technology mostly exist not environmentally,
The shortcomings of cumbersome, efficiency is low, effect is undesirable.
The content of the invention
It is an object of the invention to provide a kind of method for measuring autstenitic grain size, without corrosion, no specimen shape will
Ask, without being counted in grain size statistical software, directly can go out austenite grain size by count measurement, measurement accuracy is higher.
To achieve these goals, there is employed herein following technical scheme, it is characterised in that comprises the steps of：
(1) sample preparation：Steel samples are subjected to austenitizing through 860-1300 DEG C of heating, it is then rapid to take out quenching, according to
Requirement of the electron probe detection to steel samples carries out sample preparation, can be without corrosion；
(2) sample is filled：The steel samples prepared are entered into luggage sample by the dress sample requirement of electron probe, set accelerating potential,
Electron beam line；
(3) test：Line analysis test is carried out to the region for needing to detect, steel samples surface is obtained a certain apart from interior element
The quantification spectrogram of line distribution；
(4) analyze：Quantification spectrogram upper ripple peak number amount is distributed according to obtained line, you can obtain this apart from interior austenite crystal
The quantity on boundary, by measuring and calculating the distance between crest, so as to obtain austenite grain size.
Detection elements are easy segregation or the higher alloying element of content in steel samples in step (3).
Electron probe in step (2) uses accelerating potential for 15~25KV, and electronic beam current is 80~120nA, analysis step
Footpath is 0.1~0.5 μm, and beam radius is 0.5~1.0 μm.
Compared with the existing technology, element line analysis quantification collection of illustrative plates is obtained using electron probing analysis, can be with direct measurement
Austenite grain size, reaches without burn into asepsis environment-protecting, simple to operate, efficiently quick, assay be directly perceived, result of calculation
Accurately and reliably effect.
Brief description of the drawings
Fig. 1 measures distribution curve for SCM435 Cr elements；
Fig. 2 measures distribution curve for LX72A Mn elements.
Embodiment
The present invention is described further with reference to embodiment, but embodiment should not be construed as limiting the invention.
Embodiment 1
By taking diameter 13mm SCM435 as an example, chemical composition is as shown in table 1.1mm length is intercepted, 860 DEG C of heating is put into
Stove heat 1 hour, is transferred in cold water rapidly, stirring to cooling.According to the sample preparation and dress sample requirement of EPMA-160 type electron probes
Sample preparation and dress sample are carried out, voltage is set, and the parameter such as electronic beam current, selections accelerating potential is 15kV, and electronic beam current is 100nA, selected
A plurality of 300 μm of straight line path is taken, is scanned using the light beam and 0.1 μm of analysis step footpath of 1 μm of diameter, it is measurement to choose Cr
Element, draws line distribution spectrogram of the element on operating path, ordinate is the counting rate of element, can be according to fluctuation characteristic
Judge the relative change of content.Because the Grain Boundary Segregation of Cr elements is acted on, the position being enriched with crystal boundary forms crest, then selects
Multi-strip scanning path is taken, crest quantity, i.e. number of grain boundaries can be measured, average austenite grain size is drawn.
The SCM435 chemical compositions mass percent (%) of table 1
| Steel grade | C | Si | Mn | S | P | Cr | Mo | Ni | Cu | Al |
| SCM435 | 0.36 | 0.19 | 0.72 | 0.004 | 0.008 | 1.02 | 0.22 | 0.03 | 0.06 | 0.015 |
In order to verify the accuracy of this method, compare this method and the obtained result of method corrosion of directly hardening, as a result compared with
It is close, error is within 0.5 grade, and comparable situation is as shown in table 2：
The SCM435 autstenitic grain size measurement results of table 2
Embodiment 2
Exemplified by LX72A using diameter 5.5mm, chemical composition is as shown in table 3.Intercept 1mm length, be put into 860 DEG C plus
Hot stove heat 1 hour, is transferred in cold water rapidly, stirring to cooling.Sample preparation and dress of the sample according to EPMA-160 type electron probes
Sample requirement carries out sample preparation and fills sample, setting voltage, a series of analysis conditions such as electronic beam current, and accelerating potential is 15kV, electron beam
Flow for 100nA, choose a plurality of 500 μm of straight line path, light beam and 0.5 μm of analysis step footpath using 1 μm of diameter can obtain outlet
The precise results of Elemental redistribution, analysis of spectra is element count spectral line, and ordinate is the counting rate of element, can be according to a volt
Property judges the relative change of content.It is measurement element that this steel grade, which chooses Mn elements, is formed because element is enriched in crystal boundary to crystal boundary
Crest, then chooses multi-strip scanning path, can measure crest quantity, i.e. number of grain boundaries, draw average austenite grain size.
The LX72A chemical compositions mass percent (%) of table 3
| Steel grade | C | Si | Mn | S | P | Cr | Ni | Cu | Al |
| LX72A | 0.73 | 0.2 | 0.50 | 0.005 | 0.008 | 0.01 | 0.01 | 0.04 | 0.001 |
Result is compared with the austenite grain size that oxidizing process is obtained, as a result also relatively, error 0.5 grade with
It is interior, as a result as shown in table 4.
The LX72A austenite grain sizes of table 4
Embodiment described above only expresses the embodiment of the present invention, but can not be therefore understands that for the present invention
The limitation of the scope of the claims.Those skilled in the art falls under the enlightenment of present inventive concept to any variation that the present invention is done
Within the scope of the present invention.
Claims (2)
1. a kind of measuring method of austenite grain size, it is characterised in that：Comprise the steps of：
(1) sample preparation：Steel samples are subjected to austenitizing through 860-1300 DEG C of heating, it is then rapid to take out quenching, according to electronics
Requirement of the probe in detecting to sample carries out sample preparation, without corrosion；
(2) sample is filled：The sample prepared is entered into luggage sample by the dress sample requirement of electron probe, accelerating potential, Electron Beam are set
Stream；
(3) test：Line analysis test is carried out to the region for needing to detect, sample surfaces are obtained a certain apart from determining that interior element is distributed
Quantify spectrogram；
(4) analyze：Quantification spectrogram upper ripple peak number amount is distributed according to obtained line, you can obtain this apart from interior austenite grain boundary
Quantity, by measuring and calculating the distance between crest, so that austenite grain size is obtained, D=L/n, wherein：D represents brilliant
Particle size, L represents measurement distance, and n represents crest number.
2. a kind of measuring method of austenite grain size according to claim 1, it is characterised in that：Described electronics is visited
Pin uses accelerating potential for 15~25KV, and electronic beam current is 80~120nA, and analysis step footpath is 0.1~0.5 μm, and beam radius is
0.5~1.0 μm.
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| CN107290199A (en) * | 2017-08-10 | 2017-10-24 | 南京钢铁股份有限公司 | A kind of method that utilization electron probe quickly characterizes bearing steel segregation |
| CN108254297A (en) * | 2018-03-07 | 2018-07-06 | 马鞍山钢铁股份有限公司 | The assay method of high-carbon steel autstenitic grain size |
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