CN110763712A - Nondestructive measurement method for depth distribution of phase components of component - Google Patents
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- 239000010935 stainless steel Substances 0.000 description 3
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- 238000005464 sample preparation method Methods 0.000 description 1
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Abstract
According to the nondestructive measurement method for the phase component depth distribution of the component, a reflection type diffraction geometric layout formed by arranging a neutron source and a detector on the same side of a sample is used, and the position of a measuring point is selected and data signals are acquired through a four-dimensional table and the detector respectively, so that the nondestructive measurement of the phase component distribution of the component at different positions in the component is realized. And selecting a proper four-dimensional table and an installation mode according to practical conditions such as the specification and the weight of the sample to limit the size of the measuring point, collecting data signals of different measuring points in the sample by a detector, and analyzing to obtain corresponding phase and component information. The nondestructive measurement method for the component phase component depth distribution is suitable for nondestructive measurement of the component phase component distribution of different positions in a component-level sample.
Description
Technical Field
The invention belongs to the technical field of material microstructure analysis and detection, and particularly relates to a nondestructive measurement method for depth distribution of component phase components.
Background
The structural or functional engineering material contains various phases with different symmetries and corresponding components. These phases and components are often one of the determining factors for the physical or mechanical properties of the material. The material phases and compositions are in turn generally determined by the material preparation or post-treatment processes. Mastering material phase and component information is a key prerequisite for material process design and performance control. Therefore, in the field of material science, material phase and component test analysis become important links. At present, the phase structure analysis of materials is mainly based on diffraction methods, including X-ray, neutron, electron diffraction and the like. When an X-ray or neutron experiment test is adopted, powder or polycrystalline small blocks (generally with the weight of about 10 g and the volume within 1 cubic centimeter) are taken as samples, and full spectrum data at different angles are collected by a diffraction spectrometer. Then, the phase structure of the material is determined by fine adjustment and analysis aiming at the diffraction full spectrum data, and corresponding component information can be provided at the same time. When the electron diffraction method is adopted, the sample preparation process is more complicated, and the sample is generally thinned (to the micron level). The electron diffraction spot pattern obtained by the test is information of a space, and the phase structure cannot be uniquely determined in some cases. When the material composition is tested by spectroscopy, it is usually necessary to prepare a sample into a standard solution. In summary, the current methods for testing phase components are mainly focused on material-grade samples, and generally destructive sample preparation methods such as cutting, grinding or solution preparation are adopted. Due to the limitation of penetration capacity, X-rays can only nondestructively measure information such as phase components on the surface of the sample, but cannot penetrate into the sample to obtain data information such as depth distribution of the phase components. Neutrons have a certain penetration depth for most materials, but the existing neutron diffraction method is mainly suitable for phase composition testing of a small sample (gram-scale) of materials. There is currently no method available that can nondestructively measure the depth distribution of phase composition of part-scale large samples (typically tens of kilograms or more).
From the aspect of engineering application, the uniformity of the phase composition inside the part is one of the important factors influencing the overall service performance. Therefore, it is necessary to grasp the phase composition data information of different parts of the component to assist in the design of the component manufacturing process and the performance control. The existing phase composition testing method has the defects that the method is only suitable for small material samples and needs destructive sampling, and the like, and the nondestructive testing method for realizing the depth distribution of the phase composition of the large component-level samples has strong necessity under the technical background.
Disclosure of Invention
In view of the above, the present invention provides a nondestructive method for measuring the depth distribution of the phase composition of a component, which is suitable for large samples and non-destructive sampling.
To achieve the purpose, the nondestructive measuring method for the depth distribution of the component phase composition comprises the following steps:
a. measurement arrangement
Mounting a four-dimensional table on a sample table or a support frame, wherein a neutron source and a detector are arranged on the same side of a sample at an angle of more than or equal to 10 degrees to form a reflection type diffraction geometric layout;
b. sample mounting
Mounting and fixing a sample on a four-dimensional table, and setting the three-dimensional translation, rotation and other walking positions of the four-dimensional table to be in a return-to-zero state;
c. point selection
A radial collimator is arranged on the inner side of the detector, the size of a measuring point is limited by adopting the radial collimator and a slit at the front end of a neutron source, and the position of the measuring point is selected through three-way translation and autorotation operations of a four-dimensional table;
d. measurement of experiments
Starting a neutron source, collecting data signals from a selected measuring point through a detector, and transmitting the data signals to a computer for storage;
e. data processing
C, repeating the step c and the step d to measure data signals of measuring points at different positions in the sample, and storing and primarily processing the data signals;
f. measurement completion
And (3) closing the neutron source, unloading the sample from the four-dimensional table, cleaning a measurement field, and analyzing the measurement data through a program to obtain phase and component information corresponding to the measurement points at different positions.
In the step a, the four-dimensional table comprises an X-axis translation motor, a Y-axis translation motor, a Z-axis translation motor and a Z-axis rotation motor, and the power of the motors is more than or equal to 150 watts.
In the step a, the four-dimensional table is fixedly connected to the sample table or the support frame through the assembling holes, so that the four-dimensional table can be adapted to component samples with different sizes and weights.
In the step a, the center of the neutron source, the center of the detector and the center of the sample table are at the same horizontal height.
In the step a, the detector is arc-shaped and comprises a plurality of detection units.
The distance from each detection unit to the measuring point is equal.
In the step b, when the volume of the measured part sample is less than 1000 cubic centimeters and the weight is less than 10 kilograms, the four-dimensional table is directly arranged on the sample table, and the sample is arranged on the four-dimensional table.
In the step b, when the volume of the measured part sample is more than or equal to 1000 cubic centimeters and the weight of the measured part sample is more than or equal to 10 kilograms, the four-dimensional table is fixedly installed on the supporting frame, the supporting frame is fixedly connected on the fixing pile, the sample is further installed on the four-dimensional table, and the sample is integrally suspended and fixed above the sample table.
In the step b, the centers of the measuring points and the center of the sample table are positioned on the same vertical line.
The nondestructive measurement method for the depth distribution of the component phase components solves the problems that the existing phase component test method is only suitable for small material samples and needs destructive sampling, is suitable for nondestructive measurement of the distribution of the component phase components of different positions in component-level samples with different specifications and weights, and is further beneficial to helping the optimization design and the accurate performance control of the engineering component manufacturing process.
Drawings
FIG. 1 is a schematic diagram of an experimental layout of a nondestructive measurement method of depth distribution of phase composition of a part according to the present invention;
FIG. 2 is a schematic view of a suspended sample installation of the present invention;
FIG. 3 is a schematic diagram of a four-dimensional stage according to the present invention;
in the figure, 1, a sample table 2, a four-dimensional table 3, a sample 4, a neutron source 5, a slit 6, an incident beam 7, a measuring point 8, an emergent beam 9, a radial collimator 10, a detection unit 11, a detector 12, a connecting line 13, a computer 14, a support frame 15, a fixed pile 16, an assembly hole 17, an X-axis translation motor 18, a Y-axis translation motor 19, a Z-axis translation motor 20 and a Z-axis rotation motor are included.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
As shown in FIG. 1, the experimental layout of the nondestructive measurement method for depth distribution of phase composition of the component of the invention is as follows: mounting a four-dimensional table 2 on a sample table 1, and mounting a sample 3 on the four-dimensional table 2; the position of the measuring point 7 is selected through three-way translation and autorotation operations of the four-dimensional table 2; arranging the neutron source 4 and the detector 11 on the same side of the sample 3 to form a reflection type diffraction geometric layout; the detector 11 is arc-shaped and consists of a plurality of detection units 10, and the distance from each detection unit 10 to the measuring point 7 is equal; respectively installing a slit 5 and a radial collimator 9 at the front end of a neutron source 4 and the inner side of a detector 11; an incident beam 6 emitted by the neutron source 4 is irradiated on a measuring point 7 of the sample 3, and a signal of an emergent beam 8 is received by a detector 11 and is transmitted to a computer 13 for storage through a connecting line 12. The measuring method comprises the following steps:
a. measurement arrangement
A four-dimensional table 2 is arranged on a sample table 1 or a support frame 14, and a neutron source 4 and a detector 11 are arranged on the same side of a sample 3 at an angle of more than or equal to 10 degrees to form a reflection type diffraction geometric layout;
b. sample mounting
A sample 3 is fixedly arranged on a four-dimensional table 2, and the three-dimensional translation, the autorotation and other walking positions of the four-dimensional table 2 are set to be in a return-to-zero state;
c. point selection
A radial collimator 9 is arranged on the inner side of the detector 11, the size of the measuring point 7 is limited by the radial collimator 9 and a slit 5 at the front end of a neutron source 4, and the position of the measuring point 7 is selected through three-way translation and rotation operations of the four-dimensional table 2;
d. measurement of experiments
Starting the neutron source 4, collecting data signals from the selected measuring point 7 through the detector 11, and transmitting the data signals to the computer 13 for storage;
e. data processing
C, repeating the step c and the step d to measure data signals of measuring points 7 at different positions in the sample 3, and storing and primarily processing the data signals;
f. measurement completion
And (3) closing the neutron source 4, unloading the sample 3 from the four-dimensional table 2, cleaning a measurement site, and analyzing measurement data through a program to obtain phase and component information corresponding to the measurement points 7 at different positions.
As shown in FIG. 3, the four-dimensional stage 2 of the invention comprises an X-axis translation motor 17, a Y-axis translation motor 18, a Z-axis translation motor 19 and a Z-axis rotation motor 20, and the motor power is more than or equal to 150W, the motion functions of X, Y, Z three-way translation and rotation around the Z axis are realized through the drive of the four motors, and the four motors are connected and fixed on the sample stage 1 or the support frame 14 through the assembly holes 16 and can be adapted to component samples 3 with different sizes and weights.
In the step a, the center of the neutron source 4, the center of the detector 11 and the center of the sample table 1 are at the same horizontal height.
The detector 11 is arc-shaped and comprises a plurality of detecting units 10, and the distance from each detecting unit 10 to the measuring point 7 is equal.
In the step b, when the volume of the measured part sample 3 is less than 1000 cubic centimeters and the weight is less than 10 kilograms, the four-dimensional table 2 is directly arranged on the sample table 1, and the sample 3 is arranged on the four-dimensional table 2.
In the step b, when the volume of the measured part sample 3 is more than or equal to 1000 cubic centimeters and the weight of the measured part sample is more than or equal to 10 kilograms, the four-dimensional platform 2 is fixedly installed on the supporting frame 14 in a suspension type sample installation mode shown in fig. 2, the supporting frame 14 is fixedly connected on the fixing pile 15, the sample 3 is further installed on the four-dimensional platform 2, the sample 3 is integrally suspended and fixed above the sample platform 1, and the center of the measuring point 7 and the center of the sample platform 1 are positioned on the same vertical line.
According to the nondestructive measurement method for the phase component depth distribution of the part, the neutron source and the detector are arranged on the same side of the sample to form a reflection type diffraction geometric layout, the position of a measuring point in the sample is selected and data signals are acquired through the four-dimensional table and the detector respectively, destructive sampling is not needed, the sample is not damaged, and therefore nondestructive measurement of the phase component distribution of different positions in the part is achieved. Selecting a proper four-dimensional table and an installation mode thereof according to the practical conditions of the specification, the weight and the like of the component sample, selecting the position of a measuring point through three-dimensional translation and autorotation operation of the four-dimensional table, and selecting a proper radial collimator and a proper slit for limiting the size of the measuring point. Data signals of different measuring points in the sample are collected through a detector, transmitted to a computer for storage, and analyzed through a program to obtain corresponding phase and component information.
The nondestructive measurement method for the phase component depth distribution of the part is suitable for nondestructive measurement of phase component distribution of different positions in a part-level sample, and is further favorable for assisting in engineering part process design and performance control.
Example 1:
aiming at a stainless steel cylinder sample with the diameter of 6 cm, the height of 10 cm and the weight of 2kg, the method for the nondestructive measurement of the phase composition depth distribution of the part comprises the following specific steps:
(a) measurement arrangement
And resetting the sample table 1 to zero, and installing and fixing the four-dimensional table 2 on the sample table 1. For the sample used in the present embodiment, the power of the X-axis translation motor 17, the Y-axis translation motor 18, the Z-axis translation motor 19, and the Z-axis rotation motor 20 in the four-dimensional stage 2 is 200 watts. The neutron source 4 and the detector 11 are arranged on the same side of the sample table 1 at an angle of 30 degrees to form a reflection type diffraction geometric layout. When the detector is arranged, the distances between all the detection units 10 in the detector 11 and the center of the sample table 1 are kept equal; meanwhile, the center of the neutron source 4, the center of the detector 11 and the center of the sample table 1 are at the same horizontal height.
(b) Sample mounting
And (3) installing and fixing the sample 3 on the four-dimensional table 2, and setting the three-dimensional translation, rotation and other walking positions of the four-dimensional table 2 to be in a return-to-zero state. The center of the sample table 1 and the center of the sample 3 are at the same level by lifting the sample table 1. According to a pre-planned test path, the test path is composed of a plurality of test points to be measured. The measuring point 7 of the sample 3 is brought substantially to the first position of the predetermined test path by the three-way translation and rotation operation of the four-dimensional stage 2.
(c) Point selection
According to the practical conditions of sample specification, a preset testing path and the like, an appropriate radial collimator 9 and a slit 5 are selected for size limitation of the testing point 7. For the sample used in this example, the dimensions of the measuring point 7 are 2 mm. The radial collimator 9 and the slit 5 are mounted and positioned so that the center of the radial collimator 9 and the center of the slit 5 are at the same level as the center of the measuring point 7. And confirming and selecting the position of the measuring point 7 through three-way translation and rotation operations of the four-dimensional table 2.
(d) Measurement of experiments
The neutron source 4 is turned on to emit an incident beam 6 which passes through the slit 5 and impinges on a measurement point 7 of the sample 3. Outgoing beams 8 from measuring points 7 in different directions pass through a radial collimator 9 and are collected by a detection unit 10 at a corresponding position of a detector 11. Data signals from selected stations 7 are collected by detector 11 and transmitted via connection 12 to computer 13 for storage.
(e) Data processing
And c, repeating the step c, and selecting the next position of the measuring point 7 through the three-way translation and autorotation operation of the four-dimensional table 2. For the samples used in this example, one measurement point was taken every 10 mm along the height and diameter of the stainless steel cylinder, respectively. Step d is repeated, and the data signal from the measuring point 7 at the position is collected by the detector 11 and transmitted to the computer 13 for storage. In this cycle, data signals of the test points 7 on all the predetermined test paths of the sample 7 are measured and obtained. The data signals are subjected to preliminary processing to form a complete set of one-dimensional data results.
(f) Measurement completion
Confirming that the measuring points 7 on all the preset testing paths are measured. The neutron source 4 is turned off, the sample 3 is unloaded from the four-dimensional stage 2, and the measurement site is cleaned. The data results obtained by the preliminary processing are further analyzed by the computer 13 in combination with a program, and phase and component information corresponding to the measuring points at different positions is obtained. And finally, obtaining the phase composition distribution data of different positions of the part sample. For the samples used in the embodiment, a series of experimental data corresponding to different measuring point positions are analyzed by adopting a professional program, and the result shows that the phases of the stainless steel cylinder at different depth positions are all single face-centered cubic gamma iron phases.
Example 2:
example 1 is mainly directed to the case when the specification and weight of the sample 3 are compared to match the space of the sample stage 1. If this is not the case, i.e. the sample 3 is of a larger size or heavier (e.g. volume 1000 cc. or more and weight 10 kg. or more), a suspended sample mounting method is used. In this case, the support frame 14 is connected and fixed on the fixing pile 15, and the four-dimensional table 2 is installed and fixed on the support frame 14; the sample 3 is arranged on the four-dimensional table 2, the sample 3 is integrally hung on the sample table 1, and the center of the measuring point 7 and the center of the sample table 1 are positioned on the same vertical line. The other measurement steps were in accordance with example 1.
The present invention is not limited to the above-described embodiments, and those skilled in the art will be able to make various modifications without creative efforts from the above-described conception, and fall within the scope of the present invention.
Claims (11)
1. A nondestructive measurement method for component phase component depth distribution is characterized by comprising the following steps:
a. measurement arrangement
The four-dimensional table (2) is arranged on the sample table (1) or the support frame (14), and the neutron source (4) and the detector (11) are arranged on the same side of the sample (3) to form a reflection type diffraction geometric layout;
b. sample mounting
The sample (3) is installed and fixed on the four-dimensional table (2), and the three-dimensional translation displacement and the self-rotation displacement of the four-dimensional table (2) are set to be in a return-to-zero state;
c. point selection
A radial collimator (9) is arranged on the inner side of the detector (11), the size of a measuring point (7) is limited by the radial collimator (9) and a slit (5) at the front end of a neutron source (4), and the position of the measuring point (7) is selected through three-way translation and rotation operations of a four-dimensional table (2);
d. measurement of experiments
Starting a neutron source (4), collecting data signals from a selected measuring point (7) through a detector (11), and transmitting the data signals to a computer (13) for storage;
e. data processing
C, repeating the step c and the step d to measure data signals of measuring points (7) at different positions in the sample (3), and storing and primarily processing the data signals;
f. measurement completion
And (3) closing the neutron source (4), unloading the sample (3) from the four-dimensional table (2), cleaning a measurement site, and analyzing measurement data to obtain phase and component information corresponding to the measurement points (7) at different positions.
2. The method for the nondestructive measurement of the phase composition depth distribution of the component according to claim 1, wherein in the step a, the neutron source (4) and the detector (11) are arranged on the same side of the sample (3) at an angle of 10 degrees or more.
3. The method for nondestructive measurement of component phase composition depth distribution according to claim 1, wherein in the step a, the four-dimensional stage (2) comprises an X-axis translation motor (17), a Y-axis translation motor (18), a Z-axis translation motor (19) and a Z-axis rotation motor (20).
4. The method for nondestructive measurement of component phase composition depth distribution according to claim 2, wherein in step a, the power of the X-axis translation motor (17), the power of the Y-axis translation motor (18), the power of the Z-axis translation motor (19) and the power of the Z-axis rotation motor (20) are all equal to or more than 150 watts.
5. The method for the nondestructive measurement of the phase composition depth distribution of the component according to claim 1, wherein in the step a, the four-dimensional table (2) is fixedly connected to the sample table (1) or the support frame (14) through the assembling hole (16).
6. The method for nondestructive measurement of phase composition depth distribution of parts according to claim 1, wherein in step a, the center of the neutron source (4), the center of the detector (11) and the center of the sample stage (1) are all at the same level.
7. The method for non-destructive measurement of the depth distribution of the phase composition of a component according to claim 1, characterized in that: in the step a, the detector (11) is arc-shaped and comprises a plurality of detection units (10).
8. The method for non-destructive measurement of the depth distribution of the phase composition of a component according to claim 1, characterized in that: the distance between each detection unit (10) and the measuring point (7) is equal.
9. The method for the nondestructive measurement of the phase composition depth distribution of the part according to claim 1, wherein in the step b, when the measured part sample (3) has a volume of less than 1000 cubic centimeters and a weight of less than 10 kilograms, the four-dimensional stage (2) is directly mounted on the sample stage (1), and the sample (3) is mounted on the four-dimensional stage (2).
10. The method for nondestructive measurement of component phase composition depth distribution of the component according to claim 1, wherein in the step b, when the measured component sample (3) has a volume of more than or equal to 1000 cubic centimeters and a weight of more than or equal to 10 kilograms, the four-dimensional table (2) is fixedly installed on the support frame (14), the support frame (14) is fixedly connected to the fixing pile (15), the sample (3) is installed on the four-dimensional table (2), and the sample (3) is integrally suspended and fixed above the sample table (1).
11. The method for the nondestructive measurement of the phase composition depth distribution of the component according to claim 7, wherein in the step b, the center of the measuring point (7) and the center of the sample stage (1) are on the same vertical line.
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