Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. To this end, an object of the present invention is to provide a method for measuring the austenite content in steel.
The technical scheme of the invention is as follows, and the method for measuring the austenite content in the steel is characterized by comprising the following steps:
S1, polishing a steel sample to be tested step by using metallographic sand paper, and then polishing until the surface is flat and smooth;
S2, obtaining an X-ray diffraction pattern and X-ray diffraction data of the steel sample polished in the step S1 by using an X-ray diffractometer;
S3, performing qualitative analysis on the X-ray diffraction pattern obtained in the step S2 by utilizing X-ray analysis software, and determining whether martensite, austenite and a third phase except the martensite and the austenite exist in the steel sample, if the third phase does not exist, entering the next step;
S41, according to the result of the step S3, utilizing Findit2008 software to export cif data files of corresponding martensite and austenite in an output library, and taking the cif data files as reference data in fitting;
S51, opening TOPAS software, clicking a Load SCAN FILES icon in the TOPAS software, and importing a diffraction data original file;
S61, importing the required cif data files into TOPAS software;
S71, selecting an original file, and firstly selecting a light pipe diffraction ray type of 'Emission Profile'. Lam;
s81, selecting 'Background', carrying out back correction on an X-ray diffraction pattern, selecting 'Chebychev' polynomials as 'refine', selecting 'order' series, and then selecting '1/X Bkg' to be set as 'refine';
S91, selecting an Instrument, filling in Primary radius and secondary radius, selecting a detector type, and further selecting a slit specification;
s101, selecting Corrections, namely selecting Zero error and SAMPLE DISPLACEMENT in PEAK SHIFT, setting LP factor Value in INTENSITY CORRECTIONS to 0, code to Fix and Absorption in Sample Convolutions to refine;
s111, selecting Miscellaneous, and setting '1' for 'Conv.Steps' and 'Value';
S121, clicking 'Austenite structure' and 'MARTENSTITE STRUCTURE' in TOPAS software sets 'refine' for austenite and martensite unit cell parameters;
s131, setting the atomic occupation 'Code' in the austenitic and martensitic structures as 'Fix'
S141, clicking a Run icon in TOPAS software to refine the X-ray diffraction pattern, automatically refining the TOPAS software, and displaying a refining error by a software interface after finishing the refining;
S151, clicking the sample in the software interface, and clicking the Rpt/Text to respectively display the volume fraction and the mass fraction of the austenite in the sample.
In step S3, the third phase is present in the analysis result of the qualitative analysis of the X-ray diffraction pattern, and the following steps are performed:
s42, according to the result of the S3, utilizing Findit2008 software to derive cif data files of corresponding martensite, austenite and third phases in the output library, and taking the cif data files as reference data in fitting;
S52, opening TOPAS software, and importing the required cif data files and X-ray diffraction data into the TOPAS software;
S62, manually adjusting unit cell parameters of martensite, austenite and a third phase;
s72, selecting an original file, and firstly selecting a light pipe diffraction ray type of 'Emission Profile'. Lam;
S82, selecting 'Background', carrying out back correction on an X-ray diffraction pattern, selecting 'Chebychev' polynomials as 'refine', selecting 'order' series, and then selecting '1/X Bkg' to be set as 'refine';
S92, selecting an Instrument, filling in Primary radius and secondary radius, selecting a detector type point detector, and further selecting a slit specification;
S102, selecting Corrections, namely selecting Zero error and SAMPLE DISPLACEMENT in PEAK SHIFT respectively, setting LP factor Value in INTENSITY CORRECTIONS to 0, code to Fix, and setting Absorption in Sample Convolutions to refine;
S112, selecting Miscellaneous, and setting Value in Conv.Steps to be 1;
S122, clicking 'Austenite structure', 'MARTENSTITE STRUCTURE', 'third phase' in TOPAS software sets 'refine' for austenite and martensite and third phase unit cell parameters;
s132, setting the atomic occupation 'Code' of austenite, martensite and a third phase structure as 'Fix';
S142, clicking a Run icon in TOPAS software to refine the X-ray diffraction pattern, automatically refining the TOPAS software, and displaying a refining error by a software interface after finishing the refining;
S152, clicking the sample in the software interface, and clicking the Rpt/Text to respectively display the volume fraction and the mass fraction of austenite, martensite and a third phase in the sample.
Preferably, the specific content of the step S2 is that a polished steel sample is placed on a cleaned sample table, an X-ray tube of an X-ray diffractometer emits X-rays and irradiates the steel sample to generate diffraction phenomenon, a radiation detector of the X-ray diffractometer receives X-ray photons of the diffraction lines, and corresponding X-ray diffraction patterns and X-ray diffraction data are obtained after amplification treatment of a measuring circuit.
Preferably, in the step S2, a step-and-scan mode is adopted for scanning the steel sample by using an X-ray diffractometer, a cobalt target is adopted for an X-ray light tube target, the working voltage is 35kV, the working current is 40ma, the scanning range of 2Θ is 50 ° -120 °, the scanning mode is a step-and-step mode, the step size is 0.02 °, and the scanning speed is 0.5 °/min.
Compared with the prior art, the invention has the following beneficial effects:
According to the invention, a Rietveld method is adopted for a steel sample with preferred orientation, and TOPAS (total internal reflection) finishing software is utilized for carrying out structural finishing on an X-ray diffraction pattern, so that the accuracy of a test result can be improved when the austenite content in steel is calculated.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
A method for measuring austenite content in steel according to an embodiment of the present invention is described below with reference to fig. 1 of the accompanying drawings, including the steps of:
S1, polishing a steel sample to be tested step by using metallographic sand paper, and polishing the steel sample until the surface is smooth and clean, wherein the metallographic sand paper is special sand paper used for polishing when being applied to metallographic analysis of a physical laboratory, is applicable to a metallographic grinder and belongs to waterproof sand paper.
And S2, obtaining an X-ray diffraction pattern and X-ray diffraction data of the steel sample polished in the step S1 by using an X-ray diffractometer. The X-ray diffractometer is a large-scale analysis instrument for carrying out qualitative and quantitative analysis on solid substances, particularly crystalline substances, and representing microstructure, and is widely applied to various discipline fields. The wavelength of the X-ray is similar to the space between the atomic planes in the crystal, the crystal can be used as a space diffraction grating of the X-ray, namely, when a beam of X-ray irradiates an object, the X-ray is scattered by atoms in the object, each atom generates scattered waves, the waves interfere with each other, diffraction is generated as a result, the intensity of the ray is enhanced in certain directions as a result of superposition of the diffracted waves, the intensity of the ray is weakened in other directions, and the diffraction result is analyzed to obtain the crystal structure.
The method comprises the specific steps of placing a polished steel sample on a cleaned sample table, emitting X rays by an X-ray tube of an X-ray diffractometer and irradiating the X rays on the steel sample to generate diffraction phenomenon, receiving X-ray photons of the diffraction rays by a radiation detector of the X-ray diffractometer, amplifying the X-ray photons by a measuring circuit to obtain corresponding X-ray diffraction patterns and X-ray diffraction data, wherein a scanning mode of the X-ray diffractometer on the steel sample adopts a step scanning mode, an X-ray light tube target adopts a cobalt target, the working voltage is 35kV, the working current is 40mA, the scanning range of 2Θ is 50-120 degrees, the scanning mode is a step mode, and the scanning speed is 0.02 degrees per minute.
And S3, performing qualitative analysis on the X-ray diffraction pattern obtained in the step S2 by utilizing X-ray analysis software, and determining whether martensite, austenite and a third phase except the martensite and the austenite exist in the steel sample, if the third phase does not exist, entering the next step.
Specifically, iron and steel are refined from iron ore, also called iron-carbon alloy, and are alloys composed of iron (Fe) and carbon (C), silicon (Si), manganese (Mn), phosphorus (P), sulfur (S), and other small amounts of elements (Cr, V, etc.). By adjusting the content of various elements in the steel and the heat treatment process (four fires: quenching, annealing, tempering and normalizing), various metallographic structures can be obtained, so that the steel has different physical properties. In the Fe-Fe 3 C system, iron-carbon alloys of various compositions can be formulated, which differ in their equilibrium structure at different temperatures, but consist of several basic phases (ferrite F, austenite A and cementite Fe 3 C). These basic phases are combined in the form of a mechanical mixture, forming a metallographic structure that is rich in iron and steel.
Austenite is a lamellar microstructure of steel, and austenite generally consists of equiaxed polygonal grains with twins within the grains. The austenite grains immediately after the heating transformation are relatively fine, and the grain boundaries have an irregular arc shape. After a period of heating or heat preservation, the grains will grow up and the grain boundaries may tend to flatten. In the iron-carbon phase diagram, austenite is a high-temperature phase, exists above the critical point A1 temperature, and is formed by reverse eutectoid transformation of pearlite. Ni, mn, etc. can stabilize austenite at room temperature when enough chemical elements to enlarge the austenite phase region are added to the steel, such as austenitic steel. Ferrite changes to austenite at 912 to 1394 ℃, changing from a body centered cubic structure to a face centered cubic structure. The austenite strength is lower but its carbon dissolution capacity is greater (2.04% of carbon can be dissolved at 1146 ℃). Austenitic series stainless steels are commonly used in the food industry and surgical equipment.
Martensite is formed by rapid cooling (quenching) of austenite, in which case the carbon atoms in solution in the austenite do not have time to diffuse out of the unit cell. When austenite reaches the martensite transformation temperature (Ms), martensite transformation starts to occur, and the parent phase austenite structure starts to be unstable. At a temperature below Ms, which remains unchanged, a small portion of the austenitic structure rapidly changes, but does not continue. Only when the temperature is further reduced, more austenite is transformed into martensite. Finally, the temperature reaches the martensitic transformation end temperature Mf, and the martensitic transformation ends.
Martensite differs from austenite in that martensite is a body-centered square structure and austenite is a face-centered cubic structure. The austenite to martensite transformation requires only little energy because the transformation is diffusion-free and only a rapid and minute atomic rearrangement.
And S41, according to the result of the step S3, utilizing Findit2008 software to derive cif data files of corresponding martensite and austenite in the output library, taking cif data files as reference data in fitting, wherein Findit is inorganic crystal structure database query software.
S51, opening TOPAS software, clicking a Load SCAN FILES icon in the TOPAS software, and importing a diffraction data original file, wherein an X-ray diffraction pattern and a pattern to be fitted appear below the software, and the TOPAS-Academic software is full spectrum analysis software which is specially used for education scientific research units and is introduced by Australia Coelho Software company on the basis of Bruker-TOPAS software and is used for carrying out high-level analysis on X-ray diffraction (XRD) spectrum lines and sample crystal structures.
S61, importing the required cif data files into TOPAS software;
S71, selecting an original file, and firstly selecting a light pipe diffraction ray type of 'Emission Profile'. Lam;
s81, selecting 'Background', carrying out back correction on an X-ray diffraction pattern, selecting 'Chebychev' polynomials as 'refine', selecting 'order' series, and then selecting '1/X Bkg' to be set as 'refine';
S91, selecting an Instrument, filling in Primary radius and secondary radius, selecting a detector type, and further selecting a slit specification;
s101, selecting Corrections, namely selecting Zero error and SAMPLE DISPLACEMENT in PEAK SHIFT, setting LP factor Value in INTENSITY CORRECTIONS to 0, code to Fix and Absorption in Sample Convolutions to refine;
s111, selecting Miscellaneous, and setting '1' for 'Conv.Steps' and 'Value';
S121, clicking 'Austenite structure' and 'MARTENSTITE STRUCTURE' in TOPAS software sets 'refine' for austenite and martensite unit cell parameters;
s131, setting the atomic occupation 'Code' in the austenitic and martensitic structures as 'Fix'
S141, clicking a Run icon in TOPAS software to refine the X-ray diffraction pattern, automatically refining the TOPAS software, and displaying a refining error by a software interface after finishing the refining;
S151, clicking the sample in the software interface, and clicking the Rpt/Text to respectively display the volume fraction and the mass fraction of the austenite in the sample.
In the step S3, the X-ray diffraction pattern is subjected to a qualitative analysis, and if a third phase exists in the analysis result, the following steps are performed:
s42, according to the result of the S3, utilizing Findit2008 software to derive cif data files of corresponding martensite, austenite and third phase in the output library, and taking cif data files as reference data in fitting;
S52, opening TOPAS software, and importing the required cif data files and X-ray diffraction data into the TOPAS software;
S62, manually adjusting unit cell parameters of martensite, austenite and a third phase;
s72, selecting an original file, and firstly selecting a light pipe diffraction ray type of 'Emission Profile'. Lam;
S82, selecting 'Background', carrying out back correction on an X-ray diffraction pattern, selecting 'Chebychev' polynomials as 'refine', selecting 'order' series, and then selecting '1/X Bkg' to be set as 'refine';
S92, selecting an Instrument, filling in Primary radius and secondary radius, selecting a detector type point detector, and further selecting a slit specification;
S102, selecting Corrections, namely selecting Zero error and SAMPLE DISPLACEMENT in PEAK SHIFT respectively, setting LP factor Value in INTENSITY CORRECTIONS to 0, code to Fix, and setting Absorption in Sample Convolutions to refine;
S112, selecting Miscellaneous, and setting Value in Conv.Steps to be 1;
S122, clicking 'Austenite structure', 'MARTENSTITE STRUCTURE', 'third phase' in TOPAS software sets 'refine' for austenite and martensite and third phase unit cell parameters;
s132, setting the atomic occupation 'Code' of austenite, martensite and a third phase structure as 'Fix';
S142, clicking a Run icon in TOPAS software to refine the X-ray diffraction pattern, automatically refining the TOPAS software, and displaying a refining error by a software interface after finishing the refining;
S152, clicking the sample in the software interface, and clicking the Rpt/Text to respectively display the volume fraction and the mass fraction of austenite, martensite and a third phase in the sample.
The invention discloses a method for measuring the austenite content in steel, which adopts a Rietveld method for a steel sample with preferred orientation, and utilizes TOPAS finishing software to carry out structural finishing on an X-ray diffraction pattern, so that the accuracy of a test result can be improved when the austenite content in the steel is calculated.
Rietveld in 1967 proposed a method of structural refinement with full spectrum fitting, starting a new period of fundamental revolution in the processing of diffraction data. The Rietveld method is a method of full spectrum fitting, i.e., using the data spectrum of each step over the diffraction spectrum. And adjusting the structural atomic parameters and the peak type parameters by using a least square method to enable the fit between the calculated peak type and the observed peak type, namely, the weighted residual variance factor Rwp of the graph to be minimum.
The measured intensity y i at a certain 2Θ i point on the diffraction pattern is formed by the joint participation of Bragg reflections, and the calculated intensity y ik is caused by factors such as the structural factor F k 2 value calculated by accumulating the contributions of Bragg reflections in the adjacent range of the structural model, and can be expressed as
Wherein S is a scale factor;
K represents the Bragg reflection Miller index h, K, l;
p K is the preferred orientation function;
F k is the structural factor of the K-th Bragg reflection;
L k contains Lorentz polarization and multiple factors;
Φ is a reflection peak type function;
a is an absorption factor, and the effective absorption factor A is changed according to the geometric design of the diffractometer;
s r is a surface roughness factor;
e is a extinction factor;
yb i is the back intensity at point i.
In the process of fitting full spectrum by using least square method, the residual error value in the following formula is required to reach the minimum value
S=Σiwi[yi-yik]2 (2)
W i is a weight factor
The Rietveld finishing method has the advantages of no need of standard sample correction, high precision, high speed, no difficulty caused by spectrum peak overlapping due to phase increase, capability of correcting systematic errors caused by factors such as preferred orientation, linewidth and the like.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.