CN108956665B - Neutron measurement method for microstructure research of brittle material - Google Patents
Neutron measurement method for microstructure research of brittle material Download PDFInfo
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Abstract
The invention discloses a neutron measurement method for microstructure research of a brittle material, which realizes measurement of neutron small-angle scattering signals of the brittle material under different strains in the process of carrying out Brazilian experiments by reasonably configuring relative position relations of various measurement devices and layout and introducing a discrete strain calculation method, and can effectively ensure the consistency of neutron measurement areas of a measured sample under different strain states. The method is used in cooperation with a neutron small-angle scattering spectrometer, can be used for carrying out Brazilian experiments on brittle materials such as ceramics and polymers and detecting the microscopic deformation, cracking damage and damage processes of the materials on line, and is beneficial to the analysis and research of mechanical properties and damage mechanisms of the materials.
Description
Technical Field
The invention belongs to the technical field of environmental loading in neutron small-angle scattering application, and particularly relates to a neutron measurement method for microstructure research of a brittle material.
Background
The neutron small-angle scattering technology has nondestructive detection and deep penetration characteristics, and is an effective method for researching internal microstructure information of materials such as precipitated phases of metals, configurations of macromolecules and biomolecules, and internal dopants of the materials. The Brazilian experiment is a common experimental method for researching the characteristics of the brittle material such as tensile strength, breaking strain, creep deformation, fatigue and the like, and is widely used for measuring mechanical properties of ceramics, polymers and the like. The Brazilian experiment has the difficulty in measuring the tiny strain of the brittle material, and the speckle strain gauge is a general method for measuring the strain in the current Brazilian experiment due to the advantages of high measuring precision, quick detection, convenience in operation and the like. The working principle of the speckle strain gauge is that the high-resolution camera tracks the speckles on the surface of a measured sample in real time in the deformation process of a measured object, and then the strain analysis is carried out by a digital image processing method. When the speckle strain gauge is used, the camera is required to face the surface of a measured object, and the surface is also a measuring surface facing neutron beam in neutron small-angle scattering measurement, so that when a Brazilian experiment is carried out in the neutron small-angle scattering measurement process, the placing position of the camera coincides with the neutron beam, the problem that the neutron beam is shielded by the camera is caused, and the Brazilian experiment cannot be carried out in the neutron small-angle scattering experiment based on the reason.
Disclosure of Invention
The invention aims to provide a neutron measurement method for microstructure research of a brittle material.
The invention discloses a neutron measurement method for microstructure research of a brittle material, which is characterized in that measurement equipment adopted in the measurement method and the connection relation thereof are as follows: installing an upper pressure head and a lower pressure head of the special fixture for Brazilian experiments on a mechanical loading device, and placing a sample to be measured between the upper pressure head and the lower pressure head; fixing the mechanical loading device on the horizontal rotating platform to enable the center of the tested sample to be positioned on the extension line of the rotating shaft of the horizontal rotating platform; the horizontal rotating platform is arranged on a sample platform of the neutron small-angle scattering spectrometer, so that a sample to be measured is positioned right in front of a neutron detector of the neutron small-angle scattering spectrometer; a camera of the speckle strain gauge is placed on the left side or the right side of the sample table according to the on-site condition of the neutron small-angle scattering spectrometer; the centers of the tested sample, the neutron detector and the camera of the speckle strain gauge are at the same horizontal height; the signal lines of the mechanical loading device, the neutron detector, the camera of the speckle strain gauge and the neutron monitor of the neutron small-angle scattering spectrometer are connected to the control computer;
the measuring method comprises the following steps:
a. parameter initialization and sample initial state measurement: setting the number of single-step neutrons measured by a neutron small-angle scattering spectrometer and the diameter D of a samplesSample information parameter related to the thickness of the sample, and current strain parameter T of the measured samplecAnd controlling the current position A of the horizontal rotary tablerIs zero; starting a neutron monitor to count measuring neutrons, and starting a neutron detector to measure a scattering signal of a measured sample to obtain a measurement result of the initial state of the sample;
b. controlling the horizontal rotation table to the strain loading position: controlling the horizontal rotating platform to rotate for a fixed angle theta towards the placing direction of the camera of the speckle strain gauge, so that the surface of the sample is opposite to the lens of the camera;
c. calculation of discrete strain parameters for brazilian experiments: according to the target strain parameter TsAnd the current dependent variable TcCalculating the loading dependent variable TlThe three relations are as follows: t isl=Ts-TcFurther calculating the loading deformation quantity LΔ，LΔAnd the loading dependent variable TlAnd sample diameter DsThe relationship of (1) is: l isΔ=Tl×Ds；
d. Strain loading and measurement: will TcIs assigned to the most recent dependent variable Tc-last(ii) a Controlling a mechanical loading device to mechanically load the tested sample, wherein the loading displacement is LΔAnd the actual deformation L of the tested sample is measured and fed back by the speckle strain gauge in the loading processr(ii) a After the loading is finished, updating the current dependent variable TcParameters and a calculation formula are as follows: t isc= Tc-last+Lr/Ds(ii) a Judging whether the mechanical loading device is in a single-end loading mode, if so, controlling the sample stage of the small-angle scattering spectrometer to move upwards or downwards by 0.5 times LΔ。
e. Controlling the horizontal rotating table to a neutron measurement position: controlling the horizontal rotating platform to return to a zero position, so that the surface of the sample faces to the neutron incident beam flow direction;
f. measuring a neutron scattering signal of a tested sample under strain loading: starting a neutron monitor to count measuring neutrons, and starting a neutron detector to measure a scattering signal of the measured sample in the strain state; judging whether the measurement experiment is finished, if so, jumping to step g, otherwise, turning to step b, and carrying out next strain point loading on the sample to be measured;
g. after the measurement is finished, storing the mechanical loading data of the mechanical loading device and the test result of the neutron detector of the neutron small-angle spectrometer;
in the step a, the diameter of the detected sample is larger than the diameter of the section of the neutron beam.
In the step b, the horizontal rotating platform is a high-precision low-vibration rotating platform.
In the step d, the mechanical loading device is in a double-end synchronous loading mode or a single-end loading mode, and the two loading output ends of the mechanical loading device in the double-end synchronous loading mode move at the same speed and in opposite directions; when the mechanical loading device adopting the single-end loading mode is used, the sample table has a lifting function.
The neutron measurement method for microstructure research of the brittle material realizes measurement of neutron small-angle scattering signals under different strains of the brittle material in the process of carrying out Brazilian experiments by reasonably configuring a plurality of measurement devices and arranging the relative position relationship of the measurement devices and introducing a discrete strain calculation method; secondly, aiming at the problem that the position relation between a detected sample and a neutron beam current is changed in the non-in-situ mechanical loading process, the invention adopts a mode of lifting compensation of a bidirectional synchronous loading mechanical loading device or a sample platform on the position of the detected sample to eliminate the influence of mechanical loading on the position of the detected sample, and simultaneously, a high-precision low-vibration rotating platform is selected to reduce the position error caused by the rotary switching of the position of the sample, and the consistency of neutron measurement areas of the detected sample in different strain states can be effectively ensured by the combined use of the two means; finally, each time of strain loading of the mechanical loading device, the speckle strain gauge starts a new round of strain tracking, and the strain tracking is not related to the speckle state of the surface of the sample at the last time.
The neutron measurement method for the microstructure research of the brittle material is suitable for measuring the internal microstructure and evolution information of the ceramic, polymer and other materials in the process of carrying out the standard mechanical property test of the brittle material, namely a Brazilian experiment, provides an effective test method for obtaining a microstructure corresponding to the macroscopic characteristics of fracture, fatigue and the like of the brittle material, and solves the problem that the Brazilian experiment cannot be carried out in the process of measuring a neutron small-angle scattering signal of the brittle material.
The neutron measurement method for microstructure research of the brittle material is used together with a neutron small-angle scattering spectrometer, can be used for carrying out Brazilian experiments on the brittle materials such as ceramics and polymers and simultaneously carrying out on-line detection on the microstructure of the materials, and is beneficial to analysis and research on mechanical properties of the brittle materials and damage cracking mechanisms.
Drawings
FIG. 1 is a schematic view of a measuring apparatus layout of a neutron measuring method for microstructure study of brittle materials according to the present invention;
FIG. 2 is a schematic diagram of the operation of the neutron measurement method for microstructure study of brittle materials according to the present invention;
in the figure, 1, an upper pressure head 2, a lower pressure head 3, a mechanical loading device 4, a sample to be measured 5, a horizontal rotating platform 6, a sample platform 7, a neutron detector 8, a camera 9, a neutron monitor 10 and a control computer are arranged.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
As shown in fig. 1, the layout of the measuring apparatus of the neutron measuring method for microstructure study of brittle materials of the present invention is as follows: installing an upper pressure head 1 and a lower pressure head 2 of the special fixture for Brazilian experiments on a mechanical loading device 3, and placing a sample 4 to be measured between the upper pressure head 1 and the lower pressure head 2; fixing the mechanical loading device 3 on the horizontal rotating platform 5 to enable the center of the tested sample 4 to be positioned on the extension line of the rotating shaft of the horizontal rotating platform 5; the horizontal rotating platform 5 is arranged on a sample platform 6 of the neutron small-angle scattering spectrometer, so that the sample 4 to be measured is positioned right in front of a neutron detector 7 of the neutron small-angle scattering spectrometer; a camera 8 of the speckle strain gauge is arranged on the left side of the sample table 6; the centers of the tested sample 4, the neutron detector 7 and the camera 8 of the speckle strain gauge are at the same horizontal height; the signal lines of the mechanical loading device 3, the neutron detector 7, the camera 8 of the speckle strain gauge and the neutron monitor 9 of the neutron small-angle scattering spectrometer are connected to a control computer 10.
Example 1
As shown in fig. 2, in the present embodiment, the mechanical loading device 3 of the neutron measurement method for microstructure research of a brittle material is a loading mode with a fixed upper end and a fixed lower end, and the sample stage 6 has a lifting function, and the measurement method includes the following steps:
a. parameter initialization and sample initial state measurement: setting the number of single-step neutrons measured by a neutron small-angle scattering spectrometer and the diameter D of a samplesInitializing the current dependent variable parameter T of the tested sample 4 according to the sample information parameter of the sample thicknesscAnd controlling the current position A of the horizontal rotation table 5rIs zero; starting a neutron monitor 9 to count the measurement neutrons, and starting a neutron detector 7 to measure the scattering signals of the sample 4 to be measured to obtain the measurement result of the initial state of the sample;
b. controlling the horizontal rotation stage 5 to the strain loading position: controlling the horizontal rotating platform 5 to rotate to the left by a fixed angle theta to enable the surface of the sample to be over against a lens of a camera 8 of the speckle strain gauge;
c. calculation of discrete strain parameters for brazilian experiments: according to the target strain parameter TsAnd the current dependent variable TcCalculating the loading dependent variable TlThe three relations are as follows: t isl=Ts-TcFurther calculating the loading deformation quantity LΔ，LΔAnd the loading dependent variable TlAnd sample diameter DsThe relationship of (1) is: l isΔ=Tl×Ds；
d. Strain loading and measurement: will TcIs assigned to the most recent dependent variable Tc-last(ii) a Controlling the mechanical loading device 3 to mechanically load the tested sample 4, wherein the loading displacement is LΔAnd the actual deformation L of the tested sample 4 is measured and fed back by the speckle strain gauge in the loading processr(ii) a After the loading is finished, updating the current dependent variable TcParameters and a calculation formula are as follows: t isc= Tc-last+Lr/Ds(ii) a Judging whether the mechanical loading device 3 is in a single-end loading mode, if so, controlling the sample stage 6 of the small-angle scattering spectrometer to move downwards by 0.5 times LΔ。
e. Controlling the horizontal rotating table 5 to a neutron measurement position: controlling the horizontal rotary table 5 to return to a zero position to enable the surface of the sample to face the neutron incident beam flow direction;
f. and (3) measuring a neutron scattering signal of the tested sample 4 under strain loading: starting a neutron monitor 9 to count the measurement neutrons, and starting a neutron detector 7 to measure the scattering signals of the sample 4 under the strain state; judging whether the measurement experiment is finished, if so, jumping to step g, otherwise, turning to step b, and carrying out next strain point loading on the sample 4 to be measured;
g. after the measurement is finished, storing the mechanical loading data of the mechanical loading device 3 and the test result of the neutron detector 7 of the neutron small-angle spectrometer;
in the step a, the diameter of the detected sample 4 is larger than the diameter of the section of the neutron beam.
In the step b, the horizontal rotary table 5 is a high-precision low-vibration rotary table.
Example 2
The neutron measurement method for microstructure research of brittle materials in this embodiment is basically the same as the embodiment of embodiment 1, except that the camera 8 of the speckle strain gauge in this embodiment is placed on the right side of the sample stage 6, and the mechanical loading device 3 is a loading mode in which the lower end is fixed and the upper end is fixed.
The step b is as follows: controlling the horizontal rotation stage 5 to the strain loading position: controlling the horizontal rotating platform 5 to rotate to the right side by a fixed angle theta, so that the surface of the sample is just opposite to a lens of a camera 8 of the speckle strain gauge;
step d is: strain loading and measurement: will TcIs assigned to the most recent dependent variable Tc-last(ii) a Controlling the mechanical loading device 3 to mechanically load the tested sample 4, wherein the loading displacement is LΔAnd the actual deformation L of the tested sample 4 is measured and fed back by the speckle strain gauge in the loading processr(ii) a After the loading is finished, updating the current dependent variable TcParameters and a calculation formula are as follows: t isc= Tc-last+Lr/Ds(ii) a Judging whether the mechanical loading device 3 is in a single-end loading mode, if so, controlling the sample stage 6 of the small-angle scattering spectrometer to move upwards by 0.5 times LΔ。
Example 3
The neutron measurement method for microstructure research of brittle materials in this example is basically the same as that in example 1 in the embodiment, except that the mechanical loading device is a double-end synchronous loading mode.
Step d is: strain loading and measurement: will TcIs assigned to the most recent dependent variable Tc-last(ii) a Controlling the mechanical loading device 3 to mechanically load the tested sample 4, wherein the loading displacement is LΔAnd the actual deformation L of the tested sample 4 is measured and fed back by the speckle strain gauge in the loading processr(ii) a After the loading is finished, updating the current dependent variable TcParameters and a calculation formula are as follows: t isc= Tc-last+Lr/Ds。
Claims (4)
1. A neutron measurement method for microstructure research of brittle materials is characterized in that measurement equipment and connection relations thereof adopted in the measurement method are as follows:
an upper pressure head (1) and a lower pressure head (2) of the special clamp for Brazilian experiments are arranged on a mechanical loading device (3), and a sample (4) to be tested is placed between the upper pressure head (1) and the lower pressure head (2); fixing the mechanical loading device (3) on the horizontal rotating table (5) to enable the center of the tested sample (4) to be positioned on the extension line of the rotating shaft of the horizontal rotating table (5); the horizontal rotating platform (5) is arranged on a sample platform (6) of the neutron small-angle scattering spectrometer, so that a tested sample (4) is positioned right in front of a neutron detector (7) of the neutron small-angle scattering spectrometer; a camera (8) of the speckle strain gauge is placed on the left side or the right side of the sample table (6) according to the on-site condition of the neutron small-angle scattering spectrometer; the centers of a tested sample (4), a neutron detector (7) and a camera (8) of the speckle strain gauge are at the same horizontal height; the signal lines of the mechanical loading device (3), the neutron detector (7), the camera (8) of the speckle strain gauge and the neutron monitor (9) of the neutron small-angle scattering spectrometer are connected to a control computer (10);
the measuring method comprises the following steps:
a. parameter initialization and sample initial state measurement: setting the number of single-step neutrons measured by a neutron small-angle scattering spectrometer and the diameter D of a samplesSample information parameter related to the thickness of the sample, and the current strain parameter T of the tested sample (4) is initializedcAnd controlling the current position A of the horizontal rotation table (5)rIs zero; starting a neutron monitor (9) to count measuring neutrons, and starting a neutron detector (7) to measure a scattering signal of a measured sample (4) to obtain a measurement result of a sample initial state;
b. controlling the horizontal rotating platform (5) to a strain loading position: controlling the horizontal rotating platform (5) to rotate for a fixed angle theta towards the placing direction of a camera (8) of the speckle strain gauge, so that the surface of the sample is opposite to a lens of the camera (8);
c. calculation of discrete strain parameters for brazilian experiments: according to the target strain parameter TsAnd the current dependent variable TcCalculating the loading dependent variable T1The three relations are as follows: t is1＝Ts-TcFurther calculating the loading deformation quantity LΔ，LΔAnd the loading dependent variable T1And sample diameter DsThe relationship of (1) is: l isΔ＝T1×Ds；
d. Strain loading and measurement: will TcIs assigned to the most recent dependent variable Tc-last(ii) a Controlling a mechanical loading device (3) to mechanically load a tested sample (4), wherein the loading displacement is LΔAnd the actual deformation L of the tested sample (4) is measured and fed back by the speckle strain gauge in the loading processr(ii) a After the loading is finished, updating the current dependent variable TcParameter(s)The calculation formula is as follows: t isc＝Tc-last+Lr/Ds(ii) a Judging whether the mechanical loading device (3) is in a single-end loading mode, if so, controlling the sample stage (6) of the small-angle scattering spectrometer to move upwards or downwards by 0.5 times of LΔ；
e. Controlling the horizontal rotating platform (5) to a neutron measurement position: controlling the horizontal rotating platform (5) to return to a zero position, so that the surface of the sample faces to the neutron incident beam flow direction;
f. measuring the neutron scattering signal of the tested sample (4) under the strain loading: starting a neutron monitor (9) to count the measurement neutrons, and starting a neutron detector (7) to measure the scattering signal of the measured sample (4) in the strain state; judging whether the measurement experiment is finished, if so, jumping to step g, otherwise, turning to step b, and carrying out next strain point loading on the sample (4) to be measured;
g. and after the measurement is finished, storing the mechanical loading data of the mechanical loading device (3) and the test result of the neutron detector (7) of the neutron small-angle spectrometer.
2. A neutron measurement method for microstructure studies of brittle materials according to claim 1, characterized in that: in the step a, the diameter of the tested sample (4) is larger than the section diameter of the neutron beam current.
3. A neutron measurement method for microstructure studies of brittle materials according to claim 1, characterized in that: in step b, the horizontal rotary table (5) is a high-precision, low-vibration rotary table.
4. A neutron measurement method for microstructure studies of brittle materials according to claim 1, characterized in that: in the step d, the mechanical loading device (3) is in a double-end synchronous loading mode or a single-end loading mode, and the two ends of the loading output of the mechanical loading device (3) in the double-end synchronous loading mode move in the same speed and in the opposite directions; when the mechanical loading device (3) adopting the single-end loading mode is used, the sample table (6) has the lifting function.
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| CN111307572B (en) * | 2020-04-03 | 2022-10-28 | 中国工程物理研究院核物理与化学研究所 | Small-angle neutron scattering-based filled rubber structure network evolution determination method |
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