CN104215489A - Preparation method of retained austenite standard sample of high-carbon chromium bearing steel - Google Patents
Preparation method of retained austenite standard sample of high-carbon chromium bearing steel Download PDFInfo
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- CN104215489A CN104215489A CN201410482566.2A CN201410482566A CN104215489A CN 104215489 A CN104215489 A CN 104215489A CN 201410482566 A CN201410482566 A CN 201410482566A CN 104215489 A CN104215489 A CN 104215489A
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Abstract
The invention relates to a preparation method of a retained austenite standard sample of high-carbon chromium bearing steel. The preparation method comprises the following steps: performing thermal treatment on high-carbon chromium bearing steel at 820 DEG C to 930 DEG C, then performing cold treatment respectively at -40 DEG C to -196 DEG C and performing tempering treatment at 150 DEG C to 200 DEG C, thereby obtaining a retained austenite sample containing austenite and carbide; separating by an electrochemical extraction method and determining the content of carbide in the sample; determining the content of austenite in the sample by an X-ray scattering method; and plotting a curve relating to the content of retained austenite and the thermal treatment technology according to the prepared retained austenite standard sample of the high-carbon chromium bearing steel. Compared with the prior art, errors cannot be introduced during the preparation process, the accurate testing on the content of retained austenite in the high-carbon chromium bearing steel containing carbide can be carried out, and thus a guarantee for accurately controlling the content of retained austenite in the high-carbon chromium bearing steel in industrial production can be provided.
Description
Technical field
The present invention relates to detection technique and standard specimen preparing technical field, especially relate to a kind of high-carbon-chromium bearing steel retained austenite standard specimen preparation method.
Background technology
At present, conventional retained austenite standard specimen is that employing 316 powder of stainless steel and the reduced iron powder analyzing pure grade mix in proportion, makes the standard specimen of different austenite content (1%, 2.5%, 5%, 10%, 20%) respectively.This standard specimen does not have practical significance for the mensuration of the content of retained austenite in high-carbon-chromium bearing steel.Reason mainly contains: (1) standard specimen is different with industrial products state.Containing a large amount of carbonide in high-carbon-chromium bearing steel, when adopting X-ray diffraction method to measure residual austenite content, first need deduction carbide content could obtain retained austenite measurement result accurately.And not carbide-containing in existing standard specimen, namely do not consider the impact of carbonide.(2) standard specimen purity has error, because atomization 316 powder of stainless steel austenite phase content cannot reach more than 98%, total also have a certain amount of ferrite.(3) granularity of the two kinds of powder used in the mixed quadrat method of existing standard specimen is not quite similar, and two kinds of powder are mixed as far as possible fully just notional result, in fact standard specimen itself has brought error into.(4) standard specimen can only be used for Authentication devices whether normal operation, cannot realize the correction to carbide-containing sample retained austenite measurement result.
Summary of the invention
Object of the present invention be exactly in order to overcome above-mentioned prior art exist defect and a kind of high-carbon-chromium bearing steel retained austenite standard specimen preparation method is provided, the preparation process of standard specimen itself can not introduce error, the accurate test of residual austenite content in the high-carbon-chromium bearing steel to carbide-containing can be realized, for the residual austenite content that in commercial production, precisely control controls in high-carbon-chromium bearing steel is given security.
Object of the present invention can be achieved through the following technical solutions:
A kind of high-carbon-chromium bearing steel retained austenite standard specimen preparation method, adopts following steps:
(1) high-carbon-chromium bearing steel is heat-treated at 820 DEG C ~ 930 DEG C, then respectively in-40 ~-196 DEG C of cold treatments, temper at 150 DEG C ~ 200 DEG C, obtain the retained austenite sample containing austenite, carbonide;
(2) employing galvanochemistry extraction is separated the carbide content in above-mentioned sample;
(3) employing X-ray diffraction method measures the residual austenite content in above-mentioned sample;
(4) according to the high-carbon-chromium bearing steel retained austenite standard specimen prepared, the curve participating in austenite content and Technology for Heating Processing is drawn.
Described high-carbon-chromium bearing steel, before heat-treating, is incubated more than 1 hour, progressively cools to 700 ~ 740 DEG C and be incubated more than 2 hours at 800 ~ 820 DEG C of temperature, then naturally cools in atmosphere.
Galvanochemistry extraction adopts following steps:
A, adopt Linear cut that the sample after thermal treatment is processed into thin slice, after surface treatment, sample dries 3 hours, weighs, spot welding iron wire, smears electrolysis silica gel, post-drying and weigh;
B, adopt suitable electrolytic solution, cathode material, electrolytic potential electrolysis sample, electrolysis temperature controls at 0 DEG C ~ 5 DEG C;
C, the carbonide selected in suitable filtering membrane filtration electrolytic solution;
Carbide content in d, gravimetric determination standard specimen.
Described electrolytic solution is 50g/L potassium chloride+10g/L citric acid+aqueous solution, and cathode material is austenitic stainless steel, the PVDF filtering membrane of filtering membrane to be aperture be 0.1um.
X-ray diffraction method adopts following steps:
Sample after thermal treatment is processed into rectangular block, sample surfaces polishing by a, employing Linear cut;
B, austenite more than gate time 2s, martensite more than gate time 1s, and select maximum collimator diameter, suitable X-ray tube pressure/pipe stream, chromium target, 4 Ψ angles, suitable martensite, austenite 2 θ sweep limit and Scanning steps;
C, each sample replication more than 3 times, measurement point stochastic distribution, retained austenite measurement result is the mean value of repeatedly replication result.
Following formula is adopted to revise residual austenite content measurement result in sample:
V
γ＝V
γ′(1-V
c)
V
γ-retained austenite volume fraction, V
γthe retained austenite volume fraction that '-X-ray diffraction method measures, V
cthe carbide volume fraction that-galvanochemistry extraction measures.
The high-carbon-chromium bearing steel retained austenite standard specimen obtained can also adopt method of analysis of variance to check the homogeneity of retained austenite, carbonide.
Compared with prior art, the present invention has the following advantages:
(1) have selected multiple Technology for Heating Processing, therefore a series of different heat treatment state, the carbide content standard specimen different with residual austenite content can be prepared.
(2) standard specimen preparation itself adopts actual high-carbon-chromium bearing steel product, therefore standard specimen itself can not bring error into.
(3) can realize under carbide content unknown condition with the accurate test of X-ray diffraction method to residual austenite content in high-carbon-chromium bearing steel.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention;
Fig. 2 is the curve map between residual austenite content and Technology for Heating Processing.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment
GCr15 bearing steel retained austenite X ray test preparation of standard sample method.
High-carbon-chromium bearing steel retained austenite X ray test standard specimen preparation method, as shown in Figure 1, high-carbon-chromium bearing steel sample after heat treatment obtains the different sample of a series of residual austenite content, carbide content to its technique; Carbide content measures and adopts galvanochemistry extraction to realize in conjunction with gravimetric method; Residual austenite content measures and adopts X-ray diffraction method to realize; Adopt equation to calculate the exact level of retained austenite, adopt homogeneity, the stability of retained austenite and carbonide in method of analysis of variance, t check analysis method check sample, last definite value, prepares a series of retained austenite standard specimen; Relation curve between drafting residual austenite content and Technology for Heating Processing as shown in Figure 2.Its concrete steps are as follows:
1 thermal treatment
(1) GCr15 bearing steel sample is processed into the rectangular block of multiple 10mm × 15mm × 20mm, part is heat-treated, and all the other are retained (at least 45, for the uniformity testing of standard specimen characteristic magnitude, stability test and definite value).Need heat treated standard specimen to be incubated more than 1 hour at 800 ~ 820 DEG C of temperature, progressively cool to 700 ~ 740 DEG C and be incubated more than 2 hours, then naturally cool in atmosphere.
(2) sample oil quenching process at 820 ~ 930 DEG C of temperature, grouping temper at cold treatment+150 DEG C of temper, 150 ~ 200 DEG C of temperature at-70 ~-196 DEG C of temperature respectively.
In 2 samples, carbide content measures
(1) adopt wire cutting method that the sample after thermal treatment is processed into thin slice, after surface treatment, sample is dried about 3 hours, weighs, spot welding iron wire, smears quantitative electrolysis silica gel, post-drying and weigh.
(2) adopt suitable electrolytic solution, cathode material, electrolytic potential electrolysis standard specimen, and control electrolysis temperature at 0 DEG C ~ 5 DEG C.
(3) carbonide in suitable filtering membrane, filtration devices electrolytic solution is selected.
(4) carbide content in gravimetric determination standard specimen.
Following formula is adopted to revise residual austenite content measurement result in sample:
V
γ＝V
γ′(1-V
c)
V
γ-retained austenite volume fraction, V
γthe retained austenite volume fraction that '-X-ray diffraction method measures, V
cthe carbide volume fraction that-galvanochemistry extraction measures.
In 3 samples, residual austenite content measures
(1) suitably processing sample is surperficial.
(2) residual austenite content measurement result is accurately obtained according to after the impact of aforementioned formula (1) deduction carbonide.Test parameter selects austenite more than gate time 2s, martensite more than gate time 1s, and selects maximum collimator diameter, suitable X-ray tube pressure/pipe stream, chromium target, 4 Ψ angles, suitable martensite, austenite 2 θ sweep limit and Scanning steps.Each standard specimen replication more than 3 times, measurement point stochastic distribution, retained austenite measurement result is the mean value of repeatedly replication result.
4 standard specimen inspection and definite values
(1) uniformity testing of retained austenite and carbonide
Randomly draw at least 15 standard specimens in the sample retained in step 1, after heat treatment adopt X-ray diffraction method to measure paralympic content, each sample is chosen unduplicated 3 positions and is marked, each position replication three times; Adopt galvanochemistry extraction in conjunction with the carbide content of institute's mark position on gravimetric determination 15 standard specimens, 3 samples are got along depth direction in each position.The inspection of raw data Grubbs test method also adopts method of analysis of variance to check the homogeneity of retained austenite, carbonide after rejecting abnormalities value.
(2) retained austenite and carbide stability inspection
In sample, its Technology for Heating Processing of temperature stability Main Basis of retained austenite, is placed in selected suitable temperature lower a few hours by the standard specimen of 15 in 4 (1), adopts X-ray diffraction method to measure residual austenite content afterwards; Under the prerequisite ensureing same test conditions, first close rear thin mode is adopted to check retained austenite to the stability of time, accumulated time more than 6 months; All adopt the stability of t check analysis method inspection retained austenite.Carbonide stability checking is identical with retained austenite mode.
(3) definite value analysis
Sample after qualified to homogeneity, stability test carries out definite value analysis (comprising outlier inspection, test of normality, the assessment of uncertainty and the determination of standard value).
According to above step, the standard specimen of a series of known residual austenite content, carbide content can be prepared, and draw the graph of relation between residual austenite content and Technology for Heating Processing, see Fig. 2.The accurate quantitative analysis to retained austenite in actual sample can be realized with reference to this curve and Technology for Heating Processing.
Claims (7)
1. a high-carbon-chromium bearing steel retained austenite standard specimen preparation method, is characterized in that, the method adopts following steps:
(1) high-carbon-chromium bearing steel is heat-treated at 820 DEG C ~ 930 DEG C, then respectively in-40 DEG C ~-196 DEG C cold treatments, temper at 150 DEG C ~ 200 DEG C, obtain the retained austenite sample containing austenite, carbonide;
(2) galvanochemistry extraction is adopted to be separated and to measure the carbide content in above-mentioned sample;
(3) employing X-ray diffraction method measures the residual austenite content in above-mentioned sample;
(4) according to the high-carbon-chromium bearing steel retained austenite standard specimen prepared, the curve of residual austenite content and Technology for Heating Processing is drawn.
2. a kind of high-carbon-chromium bearing steel retained austenite standard specimen preparation method according to claim 1, it is characterized in that, described high-carbon-chromium bearing steel is before heat-treating, more than 1 hour is incubated at 800 DEG C ~ 820 DEG C temperature, progressively cool to 700 DEG C ~ 740 DEG C and be incubated more than 2 hours, then naturally cooling in atmosphere.
3. a kind of high-carbon-chromium bearing steel retained austenite standard specimen preparation method according to claim 1, is characterized in that, galvanochemistry extraction adopts following steps:
A, adopt Linear cut that the sample after thermal treatment is processed into thin slice, after surface treatment, sample dries 3 hours, weighs, spot welding iron wire, smears electrolysis silica gel, post-drying and weigh;
B, adopt suitable electrolytic solution, cathode material, electrolytic potential electrolysis sample, electrolysis temperature controls at 0 DEG C ~ 5 DEG C;
C, the carbonide selected in suitable filtering membrane filtration electrolytic solution;
Carbide content in d, gravimetric determination sample.
4. a kind of high-carbon-chromium bearing steel retained austenite standard specimen preparation method according to claim 3, it is characterized in that, described electrolytic solution is 50g/L potassium chloride+10g/L citric acid+aqueous solution, and cathode material is austenitic stainless steel, the PVDF filtering membrane of filtering membrane to be aperture be 0.1um.
5. a kind of high-carbon-chromium bearing steel retained austenite standard specimen preparation method according to claim 1, is characterized in that, X-ray diffraction method adopts following steps:
Sample after thermal treatment is processed into rectangular block, sample surfaces polishing by a, employing Linear cut;
B, austenite more than gate time 2s, martensite more than gate time 1s, and select maximum collimator diameter, X-ray tube pressure/pipe stream, chromium target, 4 Ψ angles, martensite, austenite 2 θ sweep limit and Scanning steps;
C, each sample replication more than 3 times, measurement point stochastic distribution, retained austenite measurement result is the mean value of repeatedly replication result.
6. a kind of high-carbon-chromium bearing steel retained austenite standard specimen preparation method according to claim 1, is characterized in that, adopt following formula to revise residual austenite content measurement result in sample:
V
γ＝V
γ′(1-V
c)
V
γ-retained austenite volume fraction, V
γthe retained austenite volume fraction that '-X-ray diffraction method measures, V
cthe carbide volume fraction that-galvanochemistry extraction measures.
7. a kind of high-carbon-chromium bearing steel retained austenite standard specimen preparation method according to claim 1, is characterized in that, the high-carbon-chromium bearing steel retained austenite standard specimen obtained can also adopt method of analysis of variance to check the homogeneity of retained austenite, carbonide.
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| CN105937890A (en) * | 2015-03-03 | 2016-09-14 | 帕纳科公司 | Quantitative x-ray analysis-matrix thickness correction |
| CN106896124A (en) * | 2017-04-24 | 2017-06-27 | 上海应用技术大学 | The assay method of corresponding residual austenite content in a kind of bearing steel material heat treatment process |
| CN107490519A (en) * | 2017-08-07 | 2017-12-19 | 天津重型装备工程研究有限公司 | The method of testing and stress relaxation method for numerical simulation of the mechanical property of alloy forged piece |
| CN109164119A (en) * | 2018-10-30 | 2019-01-08 | 中国航发哈尔滨轴承有限公司 | Aircraft bearing steel residual austenite content detection method |
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Cited By (10)
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| CN105937890A (en) * | 2015-03-03 | 2016-09-14 | 帕纳科公司 | Quantitative x-ray analysis-matrix thickness correction |
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| CN105203426A (en) * | 2015-10-26 | 2015-12-30 | 中航工业哈尔滨轴承有限公司 | Method for measuring content of carbide phase in 8Cr4Mo4V high temperature bearing steel |
| CN105807025A (en) * | 2016-05-18 | 2016-07-27 | 洛阳Lyc轴承有限公司 | Method for distinguishing type of high-carbon-chromium bearing steel metallographic structure |
| CN106896124A (en) * | 2017-04-24 | 2017-06-27 | 上海应用技术大学 | The assay method of corresponding residual austenite content in a kind of bearing steel material heat treatment process |
| CN107490519A (en) * | 2017-08-07 | 2017-12-19 | 天津重型装备工程研究有限公司 | The method of testing and stress relaxation method for numerical simulation of the mechanical property of alloy forged piece |
| CN107490519B (en) * | 2017-08-07 | 2019-08-13 | 天津重型装备工程研究有限公司 | The test method and stress relaxation method for numerical simulation of the mechanical property of alloy forged piece |
| CN109164119A (en) * | 2018-10-30 | 2019-01-08 | 中国航发哈尔滨轴承有限公司 | Aircraft bearing steel residual austenite content detection method |
| CN111650017A (en) * | 2020-05-31 | 2020-09-11 | 河冶科技股份有限公司 | Method for detecting content of residual austenite in high-alloy tool steel |
| CN111650017B (en) * | 2020-05-31 | 2023-04-25 | 河冶科技股份有限公司 | Method for detecting residual austenite content in high alloy tool steel |
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Address after: 200437 No. 99, Handan Road, Shanghai, Hongkou District Patentee after: Shanghai Material Research Institute Co.,Ltd. Address before: 200437 No. 99, Handan Road, Shanghai, Hongkou District Patentee before: SHANGHAI Research Institute OF MATERIALS |