CN110927201A - DIC-based thermal expansion phase change measurement method - Google Patents
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Abstract
The invention relates to a thermal expansion phase change measuring method based on DIC, and belongs to the field of detection and analysis. The invention provides a thermal expansion phase change measuring method based on DIC (digital computer) in order to solve the problems of expensive equipment and complex operation of the conventional phase change device and to more accurately and conveniently determine the phase change point of a material. The method is based on a hot stage microscope, controls the heating and cooling processes through a control program of the hot stage microscope, continuously photographs a sample in the heating and cooling processes through the microscope by adopting a high-speed camera through an image photographing control program, keeps a certain distance between a lens and the surface of a material, obtains a strain field on the surface of the sample through a DIC (digital image computer) method, obtains average strain values of the sample in each direction of each point, draws a thermal expansion curve of the sample by taking the average strain values as the expansion amount of the material, and has the advantages of simple equipment and accurate and reliable measurement results.
Description
Technical Field
The invention relates to a thermal expansion phase change measuring method based on DIC, and belongs to the field of detection and analysis.
Background
In the process of gradually increasing the temperature of the material, especially the metal material, the internal microstructure, such as the size, the morphology, the element distribution and the like of the crystal grains, can be gradually changed. When the temperature reaches a certain value, the material is subjected to phase change, the internal crystal structure is changed, and important influences are caused on various properties of the material. In the case of steel materials, the austenite transformation temperature varies depending on factors such as the chemical composition of the inside of the material and the heat treatment state. The phase transformation point is an important characteristic parameter of material characteristics, and has important significance for engineering application, so that specific phase transformation tests are required to be carried out on different materials to measure the specific phase transformation point.
At present, methods for measuring the phase change point mainly include: 1. differential scanning calorimetry, namely heating (or cooling) a sample to be measured and another reference sample under the same condition by means of a synchronous thermal analyzer, and judging the state of a substance according to the change relation (DSC curve) of the temperature difference and the temperature or the time of the two samples; 2. the continuous temperature raising metallographic method includes selecting quenching temperature range and determining the interval of quenching temperature to be 10 deg.c. Heating, preserving heat, then quenching with water, and finally observing the tissue change of the samples with different quenching temperatures under an optical microscope; 3. a calculation method, which is used for calculating a phase change point according to the influence of each element on the phase change temperature; 4. the X-ray method comprises the steps of respectively measuring diffraction spectra of a sample at different temperatures by changing the temperature of the sample, and carrying out phase analysis to find out the temperature range of phase change; 5. acoustic emission method; 6. resistance method; 7. an expansion method; the measuring principle of the expansion method is that a phase change point is obtained by analyzing and obtaining the expansion curve of a material in the continuous heating process according to the difference of the thermal expansion coefficients of different phases and the volume change generated in the phase change process.
The thermal expansion test is to perform a baseline test firstly, then test the sample according to a sample + correction mode, and finally import the test data into professional thermal analysis software. Analyzing the change of a heating and cooling thermal expansion curve through software, and analyzing by using a peak value or tangent method to obtain a phase change point of the material; the instantaneous thermal expansion coefficient of any temperature point and the average thermal expansion coefficient of any temperature interval can be calculated by software.
The existing phase change test method depends on professional instruments and equipment, the measurement cost is high, and the data processing is complex.
Disclosure of Invention
The invention provides a thermal expansion phase change measuring method based on DIC (digital computer) in order to solve the problems of expensive equipment and complex operation of the conventional phase change device and to more accurately and conveniently determine the phase change point of a material. This patent is based on hot stage microscope, through hot stage microscope's control program control heating and cooling process, through image shooting control program, adopt high-speed camera to pass through the microscope and carry out continuous shooting to the sample in heating and the cooling process, and keep camera lens and material surface distance certain, obtain the strain field on sample surface through the DIC method, thereby obtain the average strain value of sample each point in all directions, draw its thermal expansion curve with the expansion of this average strain value as the material, have equipment simply, the accurate reliable advantage of measuring result.
The purpose of the invention is realized by the following technical scheme.
The invention discloses a thermal expansion phase change measuring method based on DIC, which comprises the following steps:
heating and cooling the material through a hot stage microscope to enable the material to generate phase change, photographing the material through the microscope by adopting a high-speed camera, and acquiring time, temperature and phase change conditions at each temperature in the heating and cooling process through DIC (digital image computer).
And step two, extracting a relation curve of the strain and the time according to the shot image.
DIC methods were used. The captured image is processed by software. And taking the first image as a reference, acquiring the strain of each point corresponding to each image, namely a strain field, and calculating the average strain corresponding to each direction. And meanwhile, according to the sampling frequency adopted during shooting and the starting difference time of the two control programs, the heating time corresponding to each image is obtained, and a relation curve of average strain and time is drawn.
The concrete implementation method of the second step is as follows:
step 2.1: and (4) image numbering.
The images are numbered in order according to the order in which they were taken.
Step 2.2: an analysis area is set.
And drawing an analysis area by adopting drawing software according to the quality of the shot picture, and removing the image edge and the rest non-interested area.
Step 2.3: and setting analysis parameters.
DIC analysis parameters including subset radius, subset spacing, number of iterations, and multi-point tracking parameters are set. The setting of the parameters should be decided according to the calculation precision requirement and the computer performance.
Step 2.4: the average strain is extracted.
According to the analysis result of the software, firstly, the displacement field corresponding to each image is extracted, and after the displacement field is confirmed to be accurate, the corresponding strain field is obtained through calculation according to the displacement field. After averaging the strains at each point according to the strain field in the analysis area, the average values of the main strains Exx and Eyy in the analysis area are obtained, respectively.
Step 2.5: drawing a curve of the relation between strain and time
According to the test time corresponding to each image, the average value of the main strains Exx and Eyy is used as the strain corresponding to the image, and a strain-time relation curve is drawn.
And step three, drawing a relation curve of average strain and temperature in the thermal expansion process.
Step 3.1: and (5) drawing a temperature-time relation curve.
And drawing a theoretical temperature-time relation curve according to the heating and cooling programs programmed in the test, and drawing a corresponding real temperature-time relation curve in the test process according to the measurement result of the thermocouple in the test.
Step 3.2: the average strain is plotted against temperature.
And calculating the temperature corresponding to the shooting time of each image according to the temperature-time relation curve, and drawing the average strain-temperature relation curve by combining the calculated average strain.
And step four, determining the temperature of the phase change critical point.
And C, according to the average strain-temperature relation curve in the thermal expansion process obtained in the step three, performing linear fitting on the thermal expansion stage without phase change in the average strain-temperature relation curve by a tangent line method, wherein the tangent point of the fitted linear line and the fitted curve is the phase change critical point, so that the phase change measuring method in the thermal expansion process is realized.
Has the advantages that:
1. the traditional phase change point measurement method depends on special equipment, and the measurement of the phase change critical point is greatly limited. The thermal expansion phase change measurement method based on DIC disclosed by the invention is based on a DIC processing method, can measure the phase change critical point and the phase change volume fraction of a material in the heating process on the basis of a high-temperature metallographic stage without modifying and upgrading equipment, and has the characteristics of low cost, convenience in operation and the like.
2. The thermal expansion phase change measuring method based on DIC disclosed by the invention adopts the average strain and temperature relation curve obtained by measurement to replace the traditional linear expansion amount and temperature relation curve method, so that the real situation of the material in the phase change process can be reflected better, and the measured result is more accurate and reliable. The obtained metallographic image is combined with the phase change point measurement, and the obtained result is more real and visual.
3. The metal phase change measuring method based on the DIC method provided by the invention can obtain a corresponding thermal expansion curve of a material by shooting a micrograph of a sample in a heating process on the basis of a high-temperature metallographic hot stage and performing subsequent processing through corresponding DIC software, so that the phase change point of the material is obtained through calculation and analysis by a thermal expansion method. The method has the advantages of simple operation, no need of equipment modification and the like, and has wide application value.
Drawings
FIG. 1 is a flow chart of a thermal expansion phase transition measurement method based on DIC according to the present disclosure;
FIG. 2 is a high temperature hot stage phase diagram;
FIG. 3 is a diagram of DIC software processing area;
FIG. 4 is a graph of displacement distribution measured using DIC analysis software;
FIG. 5 is E as measured by DIC analysis softwarexxDistributing a strain field;
FIG. 6 is E as measured by DIC analysis softwareyyDistributing a strain field;
FIG. 7 is a graph of mean strain versus time measured using DIC;
FIG. 8 is a graph of actual temperature versus time;
FIG. 9 is a schematic diagram illustrating the measurement of the critical point of phase transition on the average strain versus temperature curve during thermal expansion by using the tangent method;
FIG. 10 is a schematic diagram of a method for measuring the critical point of phase change by using a tangent method;
Detailed Description
For a better understanding of the objects and advantages of the present invention, reference should be made to the following detailed description taken in conjunction with the accompanying drawings and examples.
The method for measuring the phase change critical point of the 45CrNiMoV high-strength steel comprises the following steps:
step one, sample preparation.
The overall flow of the DIC-based thermal expansion phase transition measurement method is shown in FIG. 1.
Aiming at 45CrNiMoV used in the test, according to the size required by a ZEISS metallographic phase hot stage, firstly, the 45CrNiMoV is processed by adopting a wire cutting method
The size of the DIC tracing point is determined by obtaining a flat observation surface by adopting methods of mechanical grinding, polishing and the like, and keeping a certain grinding trace as a DIC tracing point with the shape basically unchanged in the heating and cooling processes. The requirement is that before the test, the surface oxidation and corrosion areas of the material are completely removed, the parallelism of the upper end surface and the lower end surface of the sample is better, and the texture and the characteristic points which can be identified and can be kept unchanged in the heating and cooling process are uniformly distributed on the observation surface of the sample.
And step two, metallographic phase hot table test and image acquisition.
Using the sample prepared in step one, it was heated and cooled in a metallographic hot stage while capturing images observed in the microscope using software, as shown in fig. 2.
The concrete implementation method of the second step is as follows:
step 2.1: a test environment was prepared.
And (3) placing the sample prepared in the first step into a heating cavity of a metallographic hot stage microscope, and adjusting the height of the sample by using an eyepiece until the surface of the sample in the visual field is clear and distinguishable. According to the observation image in the visual field, the position of the sample is adjusted at the same time, the region observed in the microscope is ensured to be typical and clear, and the influence of mechanical grinding marks is eliminated. The safety of the equipment is ensured by connecting the circulating water pump. Pumping the experimental cavity to a vacuum environment to 10E by using a mechanical pump and a molecular pump-4Pa, ensuring that the sample can not generate oxidation reaction with air in the heating and cooling processes.
Step 2.2: heating and cooling procedures.
The control program for heating and cooling the sample is written by software. The heating rate and the cooling rate are determined according to the high-temperature metallographic hot stage equipment, and the ZEISS metallographic hot stage microscope used in the test has the maximum heating rate of 100K/s and the maximum cooling rate of 500K/s. The heating rate used in this test was 10K/min, the cooling rate 200K/min, and the holding time 3 min. According to the literature referred to, the austenite transformation temperature of 45CrNiMoV material is determined to be about 790 ℃, so the austenite transformation temperature is set to 1000 ℃.
Step 2.3: and adjusting the camera shooting parameters.
Firstly, the object distance is adjusted to ensure that the characteristics in the visual field are clear, and the object distance is adjusted according to the expansion amount of the sample in the heating process, so that the definition in the visual field is always ensured to be consistent, and the distance between the lens and the sample is ensured to be unchanged. The method comprises the steps of acquiring a real-time picture through software, previewing a shot image before a test, adjusting the brightness of the image by adopting automatic exposure or manual exposure, and adjusting the color tone of a visual field by adopting automatic white balance or manual white balance. The sampling frequency was adjusted to 0.1 based on the heating and cooling rates tested.
Step 2.4: the test apparatus was started.
The control of the test equipment is divided into two parts, one part is heating and cooling control, the other part is an image shooting control program, the two parts of control programs are started simultaneously when the test equipment is started, and the starting difference time of the two parts of programs is recorded. In the test, the heating program is started first, and the image shooting control program is started after 10 seconds.
And step three, extracting a relation curve of the strain and the time according to the shot image.
And performing software processing on the shot images by using NCORR open source software by adopting a DIC method. And taking the first image as a reference, acquiring a strain field corresponding to each image, and calculating the average strain corresponding to each point in each direction. And meanwhile, according to the sampling frequency adopted during shooting and the starting difference time of a control program, the heating time corresponding to each image is obtained, and a relation curve of average strain and time is drawn.
The concrete implementation method of the third step is as follows:
step 3.1: and (4) image numbering.
According to the sequence of image shooting, the images are numbered in sequence, the specific rule of the numbering is 'name _ XX.ext', wherein 'XX' is the sequence corresponding to the images and the numbering is carried out from 00. ". ext" is the image extension, and the image format used in this experiment is jpg. In the case of a small number of images extracted in the present experiment, the number of 110 analyzed images was numbered by using a manual number method.
Step 3.2: an analysis area is set.
According to the quality of the shot picture, drawing an analysis area by adopting drawing software such as Photoshop and the like, and removing the image edge and the rest of non-interested areas. The analysis area used in this experiment was a white rectangular area, as shown in fig. 3.
Step 3.3: and setting analysis parameters.
DIC analysis parameters including subset radius, subset spacing, number of iterations, and multi-point tracking parameters are set. The parameters are set according to the calculation accuracy requirement and the computer performance, and the specific analysis parameters used in the test are "Subset Radius 100", "Subset Spacing 10", "Diff Norm C/O1E-06", "operation # C/O50" and "Num threads 4".
Step 3.4: the average strain is extracted.
According to the software analysis result, firstly, the displacement field corresponding to each image is extracted, as shown in fig. 4, after the displacement field is confirmed to be accurate, the strain of each corresponding point, namely the strain field, is obtained through calculation according to the displacement field. According to the strain field in the analysis area, after the strain of each point is averaged, the main strain E in the analysis area is obtainedxxAnd EyyThe average values of (2) are shown in FIGS. 5 and 6.
Step 3.5: drawing a curve of the relation between strain and time
According to the test time corresponding to each image, the main strain E is calculatedxxAnd EyyThe average value of (d) is taken as the strain corresponding to the image, and a strain-time relationship curve is plotted, as shown in fig. 7.
And step four, drawing an average strain and temperature curve in the thermal expansion process.
Step 4.1: and (5) drawing a temperature-time relation curve.
Theoretical temperature versus time curves were plotted based on the heating and cooling program programmed at the time of the experiment, as shown in fig. 8. And according to the measurement result of the thermocouple in the test, drawing a corresponding real temperature and time relation curve in the test process.
Step 4.2: the average strain is plotted against temperature.
And calculating the temperature corresponding to the shooting time of each image according to the temperature-time relation curve, and drawing the average strain-temperature relation curve by combining the calculated average strain.
And step five, determining the temperature of the phase change critical point by adopting a tangent method.
According to the average strain-temperature relation curve in the thermal expansion process obtained in the fourth step, a tangent line method is adopted, as shown in fig. 9, linear fitting is performed on the thermal expansion stage without phase change in the average strain-temperature relation curve, the tangent point of the fitted linear line and curve is a phase change critical point, as shown in fig. 10, and then comparison is performed with the phase change critical point in the consulted literature data, so that good coincidence is found, and the phase change measuring method in the thermal expansion process is realized.
The above detailed description is intended to illustrate the objects, aspects and advantages of the present invention, and it should be understood that the above detailed description is only exemplary of the present invention and is not intended to limit the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (2)
1. A thermal expansion phase change measuring method based on DIC is characterized in that: the method comprises the following steps:
heating and cooling a material through a hot stage microscope to enable the material to generate phase change, photographing the material through the microscope by adopting a high-speed camera, and acquiring time, temperature and phase change conditions at each temperature in the heating and cooling process through DIC (digital image computer);
secondly, extracting a relation curve of strain and time according to the shot image;
DIC methods were used. Processing the shot images by using software, taking the first image as a reference, acquiring the strain of each point corresponding to each image, namely a strain field, and calculating the average strain corresponding to each point in each direction; and meanwhile, according to the sampling frequency adopted during shooting and the starting difference time of the two control programs, the heating time corresponding to each image is obtained, and a relation curve of average strain and time is drawn.
2. The DIC-based thermal expansion phase transition measurement method of claim 1, wherein: the concrete implementation method of the second step is as follows:
step 2.1: numbering the images;
numbering the images in sequence according to the sequence of the images;
step 2.2: setting an analysis area;
drawing an analysis area by adopting drawing software according to the quality of the shot picture, and removing the image edge and the rest non-interested areas;
step 2.3: setting analysis parameters;
setting DIC analysis parameters including the radius of the subset, the spacing of the subset, the iteration times and multipoint tracking parameters; the setting of the parameters is determined according to the calculation precision requirement and the computer performance;
step 2.4: extracting average strain;
according to the analysis result of the software, firstly extracting the displacement field corresponding to each image, and calculating according to the displacement field to obtain a corresponding strain field after confirming that the displacement field is accurate; according to the strain field in the analysis area, after the strain of each point is averaged, the main strain E in the analysis area is respectively obtainedxxAnd EyyAverage value of (d);
step 2.5: drawing a curve of the relation between strain and time
According to the test time corresponding to each image, the main strain E is calculatedxxAnd EyyTaking the average value of the strain data as the strain corresponding to the image, and drawing a strain-time relation curve;
step three, drawing a relation curve of average strain and temperature in the thermal expansion process;
step 3.1: drawing a temperature-time relation curve;
drawing a theoretical temperature-time relation curve according to a heating and cooling program compiled in the test, and drawing a corresponding real temperature-time relation curve in the test process according to the measurement result of the thermocouple in the test;
step 3.2: drawing a relation curve of average strain and temperature;
calculating the temperature corresponding to the shooting time of each image according to the temperature-time relation curve, and drawing the relation curve of the average strain and the temperature by combining the average strain obtained by calculation;
step four, determining the temperature of the phase change critical point;
and C, according to the average strain-temperature relation curve in the thermal expansion process obtained in the step three, performing linear fitting on the thermal expansion stage without phase change in the average strain-temperature relation curve by a tangent line method, wherein the tangent point of the fitted linear line and the fitted curve is the phase change critical point, so that the phase change measuring method in the thermal expansion process is realized.
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