CN103604821A - Method for measuring austenite content of steel - Google Patents

Method for measuring austenite content of steel Download PDF

Info

Publication number
CN103604821A
CN103604821A CN201310618760.4A CN201310618760A CN103604821A CN 103604821 A CN103604821 A CN 103604821A CN 201310618760 A CN201310618760 A CN 201310618760A CN 103604821 A CN103604821 A CN 103604821A
Authority
CN
China
Prior art keywords
austenite
click
illustrative plates
software
refine
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201310618760.4A
Other languages
Chinese (zh)
Other versions
CN103604821B (en
Inventor
杨英
范益
卞欣
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanjing Iron and Steel Co Ltd
Original Assignee
Nanjing Iron and Steel Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanjing Iron and Steel Co Ltd filed Critical Nanjing Iron and Steel Co Ltd
Priority to CN201310618760.4A priority Critical patent/CN103604821B/en
Publication of CN103604821A publication Critical patent/CN103604821A/en
Application granted granted Critical
Publication of CN103604821B publication Critical patent/CN103604821B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

The invention discloses a method for measuring the austenite content of steel. A Rietveld method is adopted for a steel test sample with a texture, and structure refinement is performed on an XRD (X-ray diffraction) atlas through MAUD refinement software, so that the accuracy of a test result can be improved during measurement of the austenite content of the steel. The Rietveld refinement method has the following advantages that some problems that cannot be solved by a conventional method can be solved; a plurality of phases can be corrected at the same time; furthermore, the austenite content can be still obtained even if the XRD atlas contains a third phase (such as a carbide); the Rietveld refinement method is a structure refinement method; therefore, a quantitative calculation formula does not need to be learned during quantitative analysis.

Description

The measuring method of austenite content in a kind of steel
Technical field
The invention belongs to X-ray diffraction test field, especially relate to the measuring method of austenite content in a kind of steel.
Background technology
Rietveld has proposed to carry out with the matching of full spectrum the method for structure refinement in 1967, started diffraction data to process the new period of carrying out fundamental change.Rietveld method is a kind of method of full spectrum matching, utilize exactly calculated value and the observed value of computer programs point-by-point comparison diffracted intensity, with least square method adjustment structure atomic parameter and peak shape parameter, make to calculate peak shape and observe peak shape matching, the poor side's factor R of the weighted residual of figure wp is minimum.The theory point of full spectrum matching is:
(1) each diffraction peak all has certain shape and width, and available functions is simulated.If the peak shape function of area normalization is G k, subscript k represents a certain (HKL) crystal face diffraction, below all with.In diffraction peak certain (2 θ) ithe observed strength Y at some place ikbe expressed as:
Y ik=G iki k-formula (1)
Subscript i is illustrated in (2 θ) iplace, I kintegrated intensity for diffraction peak k
I k=SM kl kf k 2-formula (2)
M in formula k, L kand F kbe respectively multiplicity factor, the Lorentz lorentz's factor of diffracted ray k and comprise the structural amplitude of temperature factor, S is scale factor.
(2) whole diffraction spectra is the stack of each diffraction peak.Certain point (2 θ) in diffraction spectra ithe observed strength Y at place ibe expressed as
Y i = Y ib + Σ k Y ik -formula (3)
Y ibfor background intensity.
(3) according to certain model, can calculate each (2 θ) in whole diffraction spectra by formula (3) ithe diffracted intensity Y at place ic.Change each structural parameters in formula (3), can change each Y ic, make and each measured value Y iorelatively, by least square, make the M in following formula minimum, this is full spectrum matching.
M=∑ iw i(Y io-Y ic) 2-formula (4)
In formula, subscript o, c are expressed as measured value or calculated value, W i=[σ 2(Y i)+σ 2(B i)] -1for the weight factor obtaining by Poisson statistics, σ 2(B i) be conventionally decided to be 0, and σ 2(Y i) equal Y i 2therefore, W i=1/Y i.
(4) entirely compose the quality of matching, available R factor judgement, the conventional R factor has following several definition:
R p=∑ iy io-Y ic/ ∑ iy io-formula (5)
R wp=[∑ iw i(Y io-Y ic) 2/ ∑ iw iy io 2] 1/2-formula (6)
R b=R i=∑ ki ko-I kc/ ∑ I ko-formula (7)
Rexp=[(N-P)/∑ iw iy io 2] 0.5-formula (8)
G of F=∑ iw i(Y io-Y ic) 2/ (N-P)=(R wp/ R exp) 2-formula (9)
W in formula ifor the statistical weight factor, N is the number of diffraction spectra data point, and P is the number of the variable element in matching, and Gof F is the abbreviation of Goodness of Fitting.
At present, in steel, the mensuration of austenite content often adopts directly comparing method, during its specific requirement residual austenite quantitative analysis X-ray diffractometer method > > in standard GB/T8362-1987 and YB/T 5338-2006 < < steel is clear and definite, has regulation.But, while there is preferred orientation in sample, martensitic phase, austenite mutually in integrated intensity ratio between each diffracted ray by the allowed band exceeding in GB, thereby cause utilizing the result of calculation discreteness of directly comparing method very large.In addition, existing measuring method measuring result error is large, and if in steel, have third phase, as carbonide, need to know the volume fraction of third phase, and the volume fraction of third phase is difficult to obtain.Therefore,, while having third phase in steel, prior art is very scabrous.Therefore, need to study a kind of can be more accurately by the method that in the steel recording, austenite content and standard contrast, according to the less advantage of measuring error of Rietveld refine method, can utilize Rietveld refine method to obtain austenite content comparatively accurately.
Summary of the invention
Technical matters to be solved by this invention is, overcoming third phase in the large and steel sample of measuring result error in prior art can affect the shortcoming of measurement result, the measuring method of austenite content in a kind of steel that can improve measurement result accuracy is provided, the method is for the steel sample with texture, and can solve the problem that third phase brings.
In order to solve above technical matters, the invention provides the measuring method of austenite content in a kind of steel, comprise the steps:
Step 1: steel sample to be measured is polished step by step with abrasive paper for metallograph, be then polished to surfacing bright and clean;
Step 2: utilize X-ray diffractometer to obtain XRD collection of illustrative plates and the XRD data of the steel sample after step 1 polishing, steel sample after polishing is placed on clean sample stage, X-ray tube sends X ray and is irradiated on described steel sample, produce diffraction phenomena, with radiation detector, receive the x-ray photon of diffracted ray, after metering circuit is amplified processing, obtain corresponding XRD collection of illustrative plates and XRD data;
Step 3: the XRD collection of illustrative plates that utilizes X-ray analysis software to obtain step 2 carries out qualitative analysis of phase, determines in steel sample whether have martensite, austenite and the third phase except martensite and austenite, if there not being third phase, enters next step;
Step 4: according to the result of step 3, utilize Findit2008 software to derive corresponding martensite and austenitic cif data file in output storehouse, and the reference data during using cif data file as matching;
Step 5: open MAUD software, by needed cif data file and XRD data importing in MAUD software;
Step 6: click " compute spectra " icon in MAUD software, XRD collection of illustrative plates and matching collection of illustrative plates appear in the software upper right corner, matching collection of illustrative plates utilizes the cif data and the XRD data that in step 5, import to carry out matching, then increases the intensity of matching collection of illustrative plates;
Step 7: manually adjust martensite and austenitic cell parameter;
Step 8: XRD collection of illustrative plates is carried out to back end correction;
Step 9: " basic phase " icon of clicking in MAUD software is finely tuned martensite and austenitic crystal cell parameter again, and austenite is carried out to " microstructure " refine;
Step 10: martensite is carried out to texture refine mutually with austenite;
Step 11: click " refinement wizard " icon in MAUD software, then click " Quantitative analysis ", then click " go ", XRD collection of illustrative plates is carried out to refine, MAUD software carries out refine automatically, and after refine finishes, software interface will show refine error;
Step 12: click " sample " in software interface, click again " Edit the selected object of the visible list ", in " phase " hurdle, select " Austenite ", in " Volume fraction " and " Weight fraction " hurdle, can distinguish show sample in austenitic volume fraction and massfraction.
The technical scheme that the present invention further limits is:
In abovementioned steps 3,, there is third phase in the qualitative analysis of phase to XRD collection of illustrative plates in analysis result, carry out following steps:
Step 4: according to the result of step 3, utilize Findit2008 software to derive the cif data file of martensite, austenite and third phase corresponding in output storehouse, and using described cif data file the reference data during as matching;
Step 5: open MAUD software, by needed cif data file and XRD data importing in MAUD software;
Step 6: click " compute spectra " icon in MAUD software, XRD collection of illustrative plates and matching collection of illustrative plates appear in the software upper right corner, matching collection of illustrative plates utilizes the cif data and the XRD data that in step 5, import to carry out matching, then increases the intensity of matching collection of illustrative plates;
Step 7: the cell parameter of manually adjusting martensite, austenite and third phase;
Step 8: XRD collection of illustrative plates is carried out to back end correction;
Step 9: " basic phase " icon of clicking in MAUD software is finely tuned martensite, austenite and third phase cell parameter again, and austenite is carried out to " microstructure " refine;
Step 10: martensite, austenite and third phase are carried out to texture refine mutually;
Step 11: click " refinement wizard " icon in MAUD software, then click " Quantitative analysis ", then click " go ", XRD collection of illustrative plates is carried out to refine, MAUD software carries out refine automatically, and after refine finishes, software interface will show refine error;
Step 12: click " sample " in software interface, click again " Edit the selected object of the visible list ", in " phase " hurdle, select " Austenite ", in " Volume fraction " and " Weight fraction " hurdle, can distinguish show sample in austenitic volume fraction and massfraction.
Further, in abovementioned steps 2, utilize X-ray diffractometer to adopt step-scan pattern or continuous sweep pattern to the scan mode of steel sample, the sweep velocity of continuous sweep pattern is set to be not more than 1 °/min, and sweep limit 2 θ of continuous sweep pattern are set to 40 °-120 °.
In abovementioned steps 6, the method that increases the intensity of matching collection of illustrative plates is: in the drop-down menu of MAUD software, select " Diffraction Instrument " option, then select " Intensity (the scalefactor) " option in " Diffraction Instrument " option, click and increase icon.
In abovementioned steps 7, in MAUD software drop-down menu, click martensite option, adjust cell parameter a value, martensitic matching collection of illustrative plates peak position and actual collection of illustrative plates are coincide; In MAUD software drop-down menu, click austenite option, adjust austenitic cell parameter a value, itself and actual collection of illustrative plates are coincide.
In abovementioned steps 9, the method of austenite being carried out to " microstructure " refine is: click the austenite option in MAUD software drop-down menu, select " microstructure " option in austenite option, by progressively reducing or increase austenite grain size, austenite grain size is carried out to manual refine, make the diffraction peak width of matching collection of illustrative plates consistent with actual collection of illustrative plates.
In abovementioned steps 10, in " Phases " of MAUD software page, click martensitic phase, click " Edit the selected object of the visible list ", select " Advanced Models " option, then in " Texture " item, select " Harmonic " option, click " Options " option, in " Sample symmetry " frame in described " Options " option, select " m3m ", martensite is carried out to texture refine; In " Phases " of MAUD software page, click austenite phase, click " Edit the selected object of the visible list ", select " Advanced Models " option, then in " Texture " item, select " Harmonic " option, click " Options " option, in " Sample symmetry " frame in described " Options " option, select " m3m ", austenite is carried out to texture refine.
In above technical scheme, can use prior art with radiation detector, to receive the x-ray photon of diffracted ray, through metering circuit, amplify and process, obtain corresponding XRD collection of illustrative plates and XRD data, and use prior art to utilize X-ray analysis software to carry out qualitative analysis of phase to XRD collection of illustrative plates.
The invention has the beneficial effects as follows: the present invention adopts Rietveld refine method to have following advantage: (1) Rietveld refine method can solve the insurmountable problem of some classic methods, the problem that comprises overlap of peaks, solid solution problem, the different problems of grain size, preferred orientation problem and containing the problem of amorphous; (2) Rietveld refine method can be revised a plurality of phases simultaneously, and, while there is third phase (as carbonide) in XRD collection of illustrative plates, still can obtain austenitic content, only the crystal structure of third phase need to be imported and revises; (3) what Rietveld refine method was done is structure refinement, when doing quantitative test, does not need to understand the formula of quantitative calculating; (4) the present invention adopts Rietveld method, utilizes MAUD refine software to carry out structure refinement to XRD collection of illustrative plates, can improve the accuracy of test findings; (5) the present invention, by the refine of " basicphase " module, adjusts the cell parameter of martensite and austenite cif file; (6) the present invention, by the refine of " microstructure " module, adjusts the grain size of martensite and austenite cif file, makes matching collection of illustrative plates and actual collection of illustrative plates meet better.
Accompanying drawing explanation
Fig. 1 is the XRD collection of illustrative plates that utilizes X-ray diffractometer to obtain of the present invention.
Fig. 2 is the refine matching collection of illustrative plates of the present invention to 1# sample.
Fig. 3 is the refine error of the present invention to 1# sample.
Fig. 4 is the austenite content that the present invention obtains after to the refine of 1# sample.
Fig. 5 is the refine matching collection of illustrative plates of the present invention to 2# sample.
Fig. 6 is the refine error of the present invention to 2# sample.
Fig. 7 is the austenite content that the present invention obtains after to the refine of 2# sample.
Embodiment
Embodiment 1
The measuring method of austenite content in a kind of steel that the present embodiment provides, its operation steps is as follows:
Step 1: steel sample to be measured is polished step by step with abrasive paper for metallograph, be then polished to surfacing bright and clean; If specimen surface is more coarse, in process of the test, easily there is re-diffraction, affect XRD graph-spectrum quality.
Step 2: utilize X-ray diffractometer to obtain XRD collection of illustrative plates and the XRD data of the steel sample after step 1 polishing, steel sample after polishing is placed on clean sample stage, X-ray tube sends X ray and is irradiated on described steel sample, produce diffraction phenomena, with radiation detector, receive the x-ray photon of diffracted ray, after metering circuit is amplified processing, obtain corresponding XRD collection of illustrative plates and XRD data; Due to Rietveld refine method having relatively high expectations to the quality of data, utilize X-ray diffractometer to adopt step-scan pattern or continuous sweep pattern to the scan mode of steel sample, the sweep velocity of continuous sweep pattern is set to be not more than 1 °/min, and the XRD collection of illustrative plates signal to noise ratio (S/N ratio) obtaining is like this higher.In addition, the diffraction peak number of participation matching requires many as far as possible.The diffraction peak number that participates in matching is more, and result of calculation is more accurate.Therefore,, in order to improve the accuracy of measurement, sweep limit 2 θ of continuous sweep pattern are set to 40 °-120 °.
Step 3: the XRD collection of illustrative plates that utilizes X-ray analysis software to obtain step 2 carries out qualitative analysis of phase, determines in steel sample whether have martensite, austenite and the third phase except martensite and austenite, if there not being third phase, enters next step.
Step 4: according to the result of step 3, utilize Findit2008 software to derive corresponding martensite and austenitic cif data file in output storehouse, and the reference data during using cif data file as matching.
Step 5: open MAUD software, by needed cif data file and XRD data importing in MAUD software.
Step 6: click " compute spectra " icon in MAUD software, there is XRD collection of illustrative plates and matching collection of illustrative plates in the software upper right corner, matching collection of illustrative plates utilizes the cif data and the XRD data that in step 5, import to carry out matching, then increase the intensity of matching collection of illustrative plates, in the drop-down menu of MAUD software, select " Diffraction Instrument " option, then select " Intensity (the scalefactor) " option in " Diffraction Instrument " option, click and increase icon.The intensity object that increases matching collection of illustrative plates is when subsequent manual is adjusted cell parameter, can more clearly find out whether matching collection of illustrative plates peak position and actual XRD collection of illustrative plates coincide.
Step 7: manually adjust martensite and austenitic cell parameter, click martensite option in MAUD software drop-down menu, adjust cell parameter a value, martensitic matching collection of illustrative plates peak position and actual collection of illustrative plates are coincide; In MAUD software drop-down menu, click austenite option, adjust austenitic cell parameter a value, itself and actual collection of illustrative plates are coincide.
Step 8: XRD collection of illustrative plates is carried out to back end correction; While utilizing MAUD software to carry out refine, should first carry out step (6) and step (7), and then carry out back end correction, can not start just to carry out back end correction most.Otherwise when in steel, austenite content is lower, austenite diffraction peak has very easily been deducted in back end makeover process as back end intensity.
Step 9: " basic phase " icon of clicking in MAUD software is finely tuned martensite and austenitic crystal cell parameter again, and austenite is carried out to " microstructure " refine; While utilizing MAUD software to carry out refine, should note, MAUD software can not carry out automatic refine to the content of Micro Phases, when if in steel, austenite content is lower, need carry out manual refine, the method of austenite being carried out to " microstructure " refine is: click the austenite option in MAUD software drop-down menu, select " microstructure " option in austenite option, by progressively reducing or increase austenite grain size, austenite grain size is carried out to manual refine, make the diffraction peak width of matching collection of illustrative plates consistent with actual collection of illustrative plates.
Step 10: martensite is carried out to texture refine mutually with austenite; In " Phases " of MAUD software page, click martensitic phase, click " Edit the selected object of the visible list ", select " Advanced Models " option, then in " Texture " item, select " Harmonic " option, click " Options " option, in " Sample symmetry " frame in described " Options " option, select " m3m ", martensite is carried out to texture refine; In " Phases " of MAUD software page, click austenite phase, click " Edit the selected object of the visible list ", select " Advanced Models " option, then in " Texture " item, select " Harmonic " option, click " Options " option, in " Sample symmetry " frame in described " Options " option, select " m3m ", austenite is carried out to texture refine.
Step 11: click " refinement wizard " icon in MAUD software, then click " Quantitative analysis ", then click " go ", XRD collection of illustrative plates is carried out to refine, MAUD software carries out refine automatically, and after refine finishes, software interface will show refine error.
Step 12: click " sample " in software interface, click again " Edit the selected object of the visible list ", in " phase " hurdle, select " Austenite ", in " Volume fraction " and " Weight fraction " hurdle, can distinguish show sample in austenitic volume fraction and massfraction.
If in step 3,, there is third phase in the qualitative analysis of phase to XRD collection of illustrative plates in analysis result, carry out following steps:
Step 4: according to the result of step 3, utilize Findit2008 software to derive the cif data file of martensite, austenite and third phase corresponding in output storehouse, and using described cif data file the reference data during as matching;
Step 5: open MAUD software, by needed cif data file and XRD data importing in MAUD software;
Step 6: click " compute spectra " icon in MAUD software, XRD collection of illustrative plates and matching collection of illustrative plates appear in the software upper right corner, matching collection of illustrative plates utilizes the cif data and the XRD data that in step 5, import to carry out matching, then increases the intensity of matching collection of illustrative plates;
Step 7: the cell parameter of manually adjusting martensite, austenite and third phase;
Step 8: XRD collection of illustrative plates is carried out to back end correction;
Step 9: " basic phase " icon of clicking in MAUD software is finely tuned martensite, austenite and third phase cell parameter again, and austenite is carried out to " microstructure " refine;
Step 10: martensite, austenite and third phase are carried out to texture refine mutually;
Step 11: click " refinement wizard " icon in MAUD software, then click " Quantitative analysis ", then click " go ", XRD collection of illustrative plates is carried out to refine, MAUD software carries out refine automatically, and after refine finishes, software interface will show refine error;
Step 12: click " sample " in software interface, click again " Edit the selected object of the visible list ", in " phase " hurdle, select " Austenite ", in " Volume fraction " and " Weight fraction " hurdle, can distinguish show sample in austenitic volume fraction and massfraction.
According to above step, sample adopts 9Ni steel plate, selects two kinds of different heat treating regimes, and mark specimen coding is 1# and 2#.Sample is polished to surfacing light after all polishing step by step with abrasive paper for metallograph again.The XRD-7000 type X-ray diffraction analysis instrument that X-ray diffraction analysis adopts Japanese Shimadzu company to produce, Cu-K αradiation, graphite curved-crystal monochromator, tube voltage 40kV, tube current 30mA, sweep limit is 40~120 °.Scan pattern is continuous sweep, and sweep velocity is 1 °/min, and step-length is 0.02 °.Before using, whether first inspection apparatus is normal, open successively circulating condensing water power source switch and panel-switch, to control water loop temperature, open X-ray diffractometer host switch, the sample stage of cleaning X-ray diffractometer, puts into specimen holder by the steel sample of having polished, and shuts main frame door, and open X-ray tube high pressure and start steel sample to scan, the XRD collection of illustrative plates measuring is as shown in Figure 1.
Use MAUD software to carry out Rietveld refine to 1#, 2# sample.According to step (1) to step (11), XRD collection of illustrative plates is carried out to refine, comprise background, scaling factor, microstructure, cell parameter, texture etc.After refine finishes, as shown in Figures 2 and 3, its refine error meets refine requirement for the refine result that software provides and error, and Rw(is Rwp)≤15%.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.

Claims (7)

1. a measuring method for austenite content in steel, is characterized in that: comprise the steps:
Step 1: steel sample to be measured is polished step by step with abrasive paper for metallograph, be then polished to surfacing bright and clean;
Step 2: utilize X-ray diffractometer to obtain XRD collection of illustrative plates and the XRD data of the steel sample after step 1 polishing, steel sample after polishing is placed on clean sample stage, X-ray tube sends X ray and is irradiated on described steel sample, produce diffraction phenomena, with radiation detector, receive the x-ray photon of diffracted ray, after metering circuit is amplified processing, obtain corresponding XRD collection of illustrative plates and XRD data;
Step 3: the XRD collection of illustrative plates that utilizes X-ray analysis software to obtain step 2 carries out qualitative analysis of phase, determines in steel sample whether have martensite, austenite and the third phase except martensite and austenite, if there not being third phase, enters next step;
Step 4: according to the result of step 3, utilize Findit2008 software to derive corresponding martensite and austenitic cif data file in output storehouse, and using described cif data file the reference data during as matching;
Step 5: open MAUD software, by needed cif data file and XRD data importing in MAUD software;
Step 6: click " compute spectra " icon in MAUD software, XRD collection of illustrative plates and matching collection of illustrative plates appear in the software upper right corner, described matching collection of illustrative plates utilizes the cif data and the XRD data that in step 5, import to carry out matching, then increases the intensity of matching collection of illustrative plates;
Step 7: manually adjust martensite and austenitic cell parameter;
Step 8: XRD collection of illustrative plates is carried out to back end correction;
Step 9: " basic phase " icon of clicking in MAUD software is finely tuned martensite and austenitic crystal cell parameter again, and described austenite is carried out to " microstructure " refine;
Step 10: martensite is carried out to texture refine mutually with austenite;
Step 11: click " refinement wizard " icon in MAUD software, then click " Quantitative analysis ", then click " go ", XRD collection of illustrative plates is carried out to refine, MAUD software carries out refine automatically, and after refine finishes, software interface will show refine error;
Step 12: click " sample " in software interface, click again " Edit the selected object of the visible list ", in " phase " hurdle, select " Austenite ", in " Volume fraction " and " Weight fraction " hurdle, can distinguish show sample in austenitic volume fraction and massfraction.
2. according to the measuring method of austenite content in the steel described in claim 1, it is characterized in that: in described step 3, the qualitative analysis of phase to XRD collection of illustrative plates, exists third phase in analysis result, carries out following steps:
Step 4: according to the result of step 3, utilize Findit2008 software to derive the cif data file of martensite, austenite and third phase corresponding in output storehouse, and using described cif data file the reference data during as matching;
Step 5: open MAUD software, by needed cif data file and XRD data importing in MAUD software;
Step 6: click " compute spectra " icon in MAUD software, XRD collection of illustrative plates and matching collection of illustrative plates appear in the software upper right corner, described matching collection of illustrative plates utilizes the cif data and the XRD data that in step 5, import to carry out matching, then increases the intensity of matching collection of illustrative plates;
Step 7: the cell parameter of manually adjusting martensite, austenite and third phase;
Step 8: XRD collection of illustrative plates is carried out to back end correction;
Step 9: " basic phase " icon of clicking in MAUD software is finely tuned martensite, austenite and third phase cell parameter again, and described austenite is carried out to " microstructure " refine;
Step 10: martensite, austenite and third phase are carried out to texture refine mutually;
Step 11: click " refinement wizard " icon in MAUD software, then click " Quantitative analysis ", then click " go ", XRD collection of illustrative plates is carried out to refine, MAUD software carries out refine automatically, and after refine finishes, software interface will show refine error;
Step 12: click " sample " in software interface, click again " Edit the selected object of the visible list ", in " phase " hurdle, select " Austenite ", in " Volume fraction " and " Weight fraction " hurdle, can distinguish show sample in austenitic volume fraction and massfraction.
3. according to the measuring method of austenite content in the steel described in claim 1, it is characterized in that: in described step 2, utilize X-ray diffractometer to adopt step-scan pattern or continuous sweep pattern to the scan mode of steel sample, the sweep velocity of described continuous sweep pattern is set to be not more than 1 °/min, and sweep limit 2 θ of described continuous sweep pattern are set to 40 °-120 °.
4. according to the measuring method of austenite content in the steel described in claim 1, it is characterized in that: in described step 6, the method that increases the intensity of matching collection of illustrative plates is: in the drop-down menu of MAUD software, select " Diffraction Instrument " option, then select " Intensity (scale the factor) " option in described " Diffraction Instrument " option, click and increase icon.
5. according to the measuring method of austenite content in the steel described in claim 1, it is characterized in that: in described step 7, in MAUD software drop-down menu, click martensite option, adjust cell parameter a value, martensitic matching collection of illustrative plates peak position and actual collection of illustrative plates are coincide; In MAUD software drop-down menu, click austenite option, adjust austenitic cell parameter a value, itself and actual collection of illustrative plates are coincide.
6. according to the measuring method of austenite content in the steel described in claim 1, it is characterized in that: in described step 9, the method of described austenite being carried out to " microstructure " refine is: click the austenite option in MAUD software drop-down menu, select " microstructure " option in described austenite option, by progressively reducing or increase austenite grain size, austenite grain size is carried out to manual refine, make the diffraction peak width of matching collection of illustrative plates consistent with actual collection of illustrative plates.
7. according to the measuring method of austenite content in the steel described in claim 1, it is characterized in that: in described step 10, in " Phases " of MAUD software page, click martensitic phase, click " Edit the selected object of the visible list ", select " Advanced Models " option, then in " Texture " item, select " Harmonic " option, click " Options " option, in " Sample symmetry " frame in described " Options " option, select " m3m ", martensite is carried out to texture refine; In " Phases " of MAUD software page, click austenite phase, click " Edit the selected object of the visible list ", select " Advanced Models " option, then in " Texture " item, select " Harmonic " option, click " Options " option, in " Sample symmetry " frame in described " Options " option, select " m3m ", austenite is carried out to texture refine.
CN201310618760.4A 2013-11-27 2013-11-27 The measuring method of austenite content in a kind of steel Active CN103604821B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310618760.4A CN103604821B (en) 2013-11-27 2013-11-27 The measuring method of austenite content in a kind of steel

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310618760.4A CN103604821B (en) 2013-11-27 2013-11-27 The measuring method of austenite content in a kind of steel

Publications (2)

Publication Number Publication Date
CN103604821A true CN103604821A (en) 2014-02-26
CN103604821B CN103604821B (en) 2016-04-27

Family

ID=50123065

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310618760.4A Active CN103604821B (en) 2013-11-27 2013-11-27 The measuring method of austenite content in a kind of steel

Country Status (1)

Country Link
CN (1) CN103604821B (en)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104062310A (en) * 2014-05-23 2014-09-24 武汉钢铁(集团)公司 Method for precisely measuring residual austenite content of steel and iron materials
WO2016166704A1 (en) * 2015-04-16 2016-10-20 King Abdullah University Of Science And Technology X-ray diffraction imaging of material microstructures
CN106290358A (en) * 2016-07-22 2017-01-04 武汉钢铁股份有限公司 The measuring method of residual austenite content in carbide-containing ferrous materials
CN108802075A (en) * 2018-06-26 2018-11-13 湘潭大学 The measurement method of each phase content in a kind of sherardised coating
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
CN109187608A (en) * 2018-09-21 2019-01-11 首钢集团有限公司 The method being precipitated using Nb in X-ray diffractometer quantitatively characterizing micro alloyed steel
CN109738466A (en) * 2018-12-04 2019-05-10 江苏省沙钢钢铁研究院有限公司 A method of residual austenite content in measurement steel is analyzed based on Full _ pattern fitting
CN110243850A (en) * 2019-07-12 2019-09-17 上海交通大学 The method of hydroxyapatite content in full spectrum refine measurement bata-tricalcium phosphate
CN112730488A (en) * 2021-02-04 2021-04-30 洛阳Lyc轴承有限公司 Calibration method for measuring residual austenite of steel grade by X-ray diffraction method
CN116559210A (en) * 2023-03-21 2023-08-08 南京海关工业产品检测中心 Mineral product phase detection method and system

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
LUCA LUTTEROTTI: "Total pattern fitting for the combined size–strain–stress–texture determination", 《NUCLEAR INSTRUMENTS AND METHODS IN PHYSICS RESEARCH B》, no. 268, 4 October 2009 (2009-10-04) *
李琪等: "Rietveld方法在钢中残余奥氏体定量测定中的应用", 《物理测试》, vol. 26, no. 4, 31 July 2008 (2008-07-31) *
王海涛: "高能球磨制备不锈钢纳米晶粉体及其放电等离子烧结研究", 《中国优秀硕士学位论文全文数据库 工程科技1辑》, no. 5, 15 May 2013 (2013-05-15) *
王锐: "Rietveld精修定量分析钢中残余奥氏体", 《物理测试》, vol. 26, no. 4, 31 July 2008 (2008-07-31) *

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104062310A (en) * 2014-05-23 2014-09-24 武汉钢铁(集团)公司 Method for precisely measuring residual austenite content of steel and iron materials
WO2016166704A1 (en) * 2015-04-16 2016-10-20 King Abdullah University Of Science And Technology X-ray diffraction imaging of material microstructures
CN106290358A (en) * 2016-07-22 2017-01-04 武汉钢铁股份有限公司 The measuring method of residual austenite content in carbide-containing ferrous materials
CN106290358B (en) * 2016-07-22 2018-08-24 武汉钢铁有限公司 The measurement method of residual austenite content in carbide-containing steel material
CN108802075A (en) * 2018-06-26 2018-11-13 湘潭大学 The measurement method of each phase content in a kind of sherardised coating
CN108802075B (en) * 2018-06-26 2023-09-15 湘潭大学 Method for measuring content of each phase in powder zinc impregnation layer
CN109187608A (en) * 2018-09-21 2019-01-11 首钢集团有限公司 The method being precipitated using Nb in X-ray diffractometer quantitatively characterizing micro alloyed steel
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
CN109738466B (en) * 2018-12-04 2021-05-14 江苏省沙钢钢铁研究院有限公司 Method for analyzing and measuring content of residual austenite in steel based on full-spectrum fitting
CN109738466A (en) * 2018-12-04 2019-05-10 江苏省沙钢钢铁研究院有限公司 A method of residual austenite content in measurement steel is analyzed based on Full _ pattern fitting
CN110243850A (en) * 2019-07-12 2019-09-17 上海交通大学 The method of hydroxyapatite content in full spectrum refine measurement bata-tricalcium phosphate
CN110243850B (en) * 2019-07-12 2022-02-25 上海交通大学 Method for determining hydroxyapatite content in beta-tricalcium phosphate through full-spectrum fine modification
CN112730488A (en) * 2021-02-04 2021-04-30 洛阳Lyc轴承有限公司 Calibration method for measuring residual austenite of steel grade by X-ray diffraction method
CN112730488B (en) * 2021-02-04 2023-09-22 洛阳Lyc轴承有限公司 Calibration method for measuring residual austenite in steel by X-ray diffraction method
CN116559210A (en) * 2023-03-21 2023-08-08 南京海关工业产品检测中心 Mineral product phase detection method and system
CN116559210B (en) * 2023-03-21 2024-04-30 南京海关工业产品检测中心 Mineral product phase detection method and system

Also Published As

Publication number Publication date
CN103604821B (en) 2016-04-27

Similar Documents

Publication Publication Date Title
CN103604821B (en) The measuring method of austenite content in a kind of steel
CN103808743B (en) A kind of method adopting austenite content in X-ray diffraction commercial measurement steel
US11841334B2 (en) Quantitative phase analysis device, quantitative phase analysis method, and non-transitory computer-readable storage medium storing quantitative phase analysis program
US11402341B2 (en) Quantitative phase analysis device for analyzing non-crystalline phases, quantitative phase analysis method for analyzing Non-Crystalline phases, and non-transitory computer-readable storage medium storing quantitative phase analysis program for analyzing Non-Crystalline Phases
CN103076308B (en) Laser-induced breakdown spectroscopy overlapped peak resolution method
CN108693205A (en) Detection device for multi metallic elements fast detector in a kind of portable soil of sample spin
CN106124542A (en) A kind of Multifunctional X-ray direction finder and method
WO2021196416A1 (en) Optical fiber raman system and method for online detection of tungsten flotation concentrate grades
Markovic et al. Assessing non-linear models for galaxy clustering I: unbiased growth forecasts from multipole expansion
CN105651801A (en) Online analysis method for ore pulp minerals
CN104007075B (en) Method and system for detecting crystal growth environment by using terahertz time-domain spectroscopy technology
TWI479176B (en) Method for acquiring nuclide activity with high nuclide identification ability applicable to spectroscopy from sodium iodide detector
CN114972185A (en) Powder X-ray diffraction pattern expectation maximization algorithm full-spectrum line fitting method based on statistical modeling
CN114295598B (en) Method for discriminating zircon raw rock type by using zircon lattice damage
CN208568641U (en) Detection device for multi metallic elements fast detector in a kind of portable soil of sample spin
Dai et al. Cost normalization for global capital projects benchmarking
CN105738392A (en) Method of measuring cell parameters of SAPO-11 molecular sieve
CN102566321B (en) Method for monitoring offset of focal length of lithography machine
CN103604820A (en) Method for improving XRD experiment precision
Neuling et al. Rietveld analysis for energy dispersive X-ray diffraction under high pressure with synchrotron radiation
Pázsit et al. Ringhals Diagnostics and Monitoring, Annual Research Report 2016-17
CN114705704A (en) Method for measuring austenite content in steel
Lucas Developing and Validating a Standard Operating Procedure for Quantitative Analysis using Central Washington University's X-ray Diffractometer
CN103940838A (en) X-ray phase analysis method for metal material
Kalaycıoğlu Indicator-based evaluation of inter-linkages between different sustainable development objectives (INDI-LINK)

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant