CN108956665A - A kind of neutron measurement method for fragile material Study on Microstructure - Google Patents
A kind of neutron measurement method for fragile material Study on Microstructure Download PDFInfo
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- CN108956665A CN108956665A CN201810396123.XA CN201810396123A CN108956665A CN 108956665 A CN108956665 A CN 108956665A CN 201810396123 A CN201810396123 A CN 201810396123A CN 108956665 A CN108956665 A CN 108956665A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/201—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by measuring small-angle scattering
- G01N23/202—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by measuring small-angle scattering using neutrons
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Abstract
The invention discloses a kind of neutron measurement methods for fragile material Study on Microstructure, this method is a variety of measuring devices of reasonable disposition and by way of being laid out its relative positional relationship and introducing discrete strain calculation method, it realizes and carries out differently strained lower neutron small angle scattering signal measurement during carrying out Brazilian test to fragile material, while can effectively ensure that the consistency in the sample neutron measurement region under strain conditions.This method cooperates neutron small angle scattering spectrometer to use, on-line checking material microdeformation, crack and damage and destructive process while capable of carrying out Brazilian test to fragile materials such as ceramics, macromolecules, helps to carry out characteristic of material mechanics, damage mechanisms analysis and research.
Description
Technical field
The invention belongs to the environment loading technique fields in neutron small angle scattering application, and in particular to one kind is used for brittleness material
Expect the neutron measurement method of Study on Microstructure.
Background technique
Small-angle neutron scattering has non-destructive testing and deep penetration characteristic, be study the precipitated phase of metal, macromolecule and
The effective ways of the material internals Microstructure Informations such as configuration, the material internal dopant of biomolecule.Brazilian test is that research is crisp
Property material the characteristics such as tensile strength, breaking strain, creep, fatigue universal experimental method, be widely used in measurement ceramics, high score
The mechanical properties such as son.The difficult point of Brazilian test is the measurement of fragile material small strain, and speckle deformeter is due to its test essence
The advantages that degree is high, detection is quick, easy to operate, is the universal method of strain measurement in current Brazilian test.Speckle deformeter
Working principle is real by being carried out during measurand deforms by speckle of the high-resolution video camera to sample surface
When track, then strain analysis is carried out by digital image processing method.Need video camera towards tested when using speckle deformeter
Subject surface, and the surface be also neutron small angle scattering measurement neutron streaming towards measuring surface, therefore, in neutron small angle scattering
When carrying out Brazilian test in measurement process, the placement position of video camera is overlapped with neutron streaming, and video camera is caused to block neutron beam
Flow problem, for these reasons, Brazilian test can not carry out in neutron small angle scattering experiment.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of neutron measurements for fragile material Study on Microstructure
Method.
Neutron measurement method for fragile material Study on Microstructure of the invention, its main feature is that, the measurement side
The measuring device and its connection relationship used in method is as follows: the seaming chuck of Brazilian test special fixture, push-down head are installed to power
It learns on loading device, sample is placed between seaming chuck, push-down head；Mechanical loading unit is fixed on horizontal rotating table
On, it is in sample center on the extended line of horizontal rotating table rotary shaft；Horizontal rotating table is mounted on neutron small angle scattering
On the sample stage of spectrometer, sample is made to be in the front of the neutron detector of neutron small angle scattering spectrometer；Speckle deformeter
Video camera the left or right side of sample stage is placed on according to neutron small angle scattering spectrometer field condition；Sample, neutron are visited
Survey device, the center of video camera of speckle deformeter is in same level height；Mechanical loading unit, neutron detector, speckle are answered
Become the video camera of instrument, the signal wire of the neutron monitor of neutron small angle scattering spectrometer is connected to control computer；
The measurement method the following steps are included:
A. parameter initialization and sample initial state measure: the single step neutron measurement number of setting neutron small angle scattering spectrometer measurement, sample
Product diameter DsWith the sample message parameter of thickness of sample, the current dependent variable parameter T of sample is initializedcIt is revolved with controlled level
The current location A of turntablerIt is zero；Starting neutron monitor counts measurement neutron, starts neutron detector to detected sample
The scattered signal of product measures, and obtains the measurement result of sample initial state；
B. controlled level turntable is to strain loading position: video camera from controlled level turntable to speckle deformeter placement side
To rotation fixed angle θ, make the camera lens of sample surfaces face video camera；
C. the calculating of the discrete strain parameter of Brazilian test: according to target strain parameter TsWith current dependent variable TcCalculate load strain
Measure Tl, triadic relation are as follows: Tl=Ts-Tc, further calculate load deformation quantity LΔ, LΔWith load dependent variable TlWith sample diameter Ds's
Relationship are as follows: LΔ=Tl×Ds；
D. strain loading and measurement: by TcNumerical value be assigned to nearest dependent variable Tc-last；Control mechanics loading device is to detected sample
Product carry out Mechanical loading, load deflection LΔ, the practical deformation of speckle strain-ga(u)ge measurement and feedback sample in loading procedure
Measure Lr；After the completion of load, current dependent variable T is updatedcParameter, calculation formula are as follows: Tc = Tc-last+Lr/Ds；Judge that Mechanical loading fills
Whether be single-ended loading method, be to control the sample stage of small-angle scattering spectrometer to be moved upwardly or downwardly 0.5 times of L if settingΔ。
E. controlled level turntable is to neutron measurement position: controlled level turntable returns to zero position, makes sample surfaces face
To neutron incidence beam direction；
F. neutron scattering signal measurement of the sample under strain loading: starting neutron monitor counts measurement neutron
Number, starting neutron detector measure scattered signal of the sample under the strain regime；Whether judge measurement experiment
It completes, is to jump to g, otherwise goes to step b, next strain point load is carried out to sample；
G. measurement terminates, and saves the test of the Mechanical loading data of mechanical loading unit and the neutron detector of the small angular spectrum instrument of neutron
As a result；
In the step a, the diameter of sample is greater than neutron streaming diameter of section.
In the step b, horizontal rotating table is high-precision, low vibration turntable.
In the step d, mechanical loading unit is the synchronous loading method of both-end or single-ended loading method, and both-end is synchronous to be added
The load output both ends of the mechanical loading unit of load mode are synchronized, counter motion；It is filled using the Mechanical loading of single-ended loading method
When setting, sample stage has elevating function.
Neutron measurement method for fragile material Study on Microstructure of the invention is set by a variety of measurements of reasonable disposition
The standby mode with its relative positional relationship of layout and the discrete strain calculation method of introducing, realizes and is carrying out Brazil to fragile material
Differently strained lower neutron small angle scattering signal measurement is carried out in experimentation；Secondly, for quilt during ex situ Mechanical loading
The problem of sample and neutron streaming positional relationship change, the present invention is using bi-directional synchronization load mechanical loading unit or sample stage
The mode of heave compensation is carried out to sample position, is influenced with eliminating Mechanical loading to sample position bring, simultaneously
By selection high-precision, low vibration turntable to reduce the location error that sample position rotation switching introduces, the connection of two kinds of means
Close the consistency using the sample neutron measurement region that can effectively ensure that under strain conditions；Finally, Mechanical loading fills
The strain loading each time set, speckle deformeter start the strain tracking of a new round, the sporadophyric with last sample surfaces
State and onrelevant, discrete strain calculation method realize the accumulation function of multiple strain loading, solve because sample position switches
Caused by speckle tracking lose and the problem of introduce strain measurement error.
Neutron measurement method for fragile material Study on Microstructure of the invention is suitable for the materials such as ceramics, macromolecule
Expect in the standard Mechanics Performance Testing for carrying out fragile material --- during Brazilian test, measures its internal microstructure and drill
Become information, provide effective test method for corresponding micromechanisms of macroscopic propertieies such as fracture, the fatigues of acquisition fragile material,
Solve the problems, such as that fragile material can not carry out Brazilian test during neutron small angle scattering signal measurement.
Neutron measurement method cooperation neutron small angle scattering spectrometer for fragile material Study on Microstructure of the invention makes
With, on-line checking is carried out to the microstructure of material while can the fragile materials such as ceramics, macromolecule be carried out with Brazilian test,
Help to carry out fragile material mechanics characteristic, damage cracking mechanism analysis and research.
Detailed description of the invention
Fig. 1 is that the measuring device of the neutron measurement method for fragile material Study on Microstructure of the invention is laid out signal
Figure；
Fig. 2 is the operation schematic diagram of the neutron measurement method for fragile material Study on Microstructure of the invention；
In figure, 1. seaming chuck, 2. push-down head, 3. mechanical loading unit, 4. sample, 5. horizontal rotating table, 6. sample stage 7.
8. video camera of neutron detector, 9. neutron monitor 10. controls computer.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples.
As shown in Figure 1, the measuring device cloth of the neutron measurement method for fragile material Study on Microstructure of the invention
Office is as follows: the seaming chuck 1 of Brazilian test special fixture, push-down head 2 being installed on mechanical loading unit 3, sample 4 is put
It sets between seaming chuck 1, push-down head 2；Mechanical loading unit 3 is fixed on horizontal rotating table 5, is made at 4 center of sample
In on the extended line of 5 rotary shaft of horizontal rotating table；Horizontal rotating table 5 is mounted on the sample stage 6 of neutron small angle scattering spectrometer, is made
Sample 4 is in the front of the neutron detector 7 of neutron small angle scattering spectrometer；The video camera 8 of speckle deformeter is placed on
The left side of sample stage 6；Sample 4, neutron detector 7, speckle deformeter video camera 8 center be in same level height
Degree；Mechanical loading unit 3, neutron detector 7, the video camera 8 of speckle deformeter, neutron small angle scattering spectrometer neutron monitor
9 signal wire is connected to control computer 10.
Embodiment 1
As shown in Fig. 2, the Mechanical loading dress of the neutron measurement method for fragile material Study on Microstructure in the present embodiment
3 are set as the fixed lower end loading method in upper end, sample stage 6 has elevating function, the measurement method the following steps are included:
A. parameter initialization and sample initial state measure: the single step neutron measurement number of setting neutron small angle scattering spectrometer measurement, sample
Product diameter DsWith the sample message parameter of thickness of sample, the current dependent variable parameter T of sample 4 is initializedcIt is revolved with controlled level
The current location A of turntable 5rIt is zero；Starting 9 pairs of measurement neutrons of neutron monitor count, and starting neutron detector 7 is to tested
The scattered signal of sample 4 measures, and obtains the measurement result of sample initial state；
B. controlled level turntable 5 is to strain loading position: controlled level turntable 5 rotates fixed angle θ to the left, makes sample
The camera lens of the video camera 8 of surface face speckle deformeter；
C. the calculating of the discrete strain parameter of Brazilian test: according to target strain parameter TsWith current dependent variable TcLoad is calculated to answer
Variable Tl, triadic relation are as follows: Tl=Ts-Tc, further calculate load deformation quantity LΔ, LΔWith load dependent variable TlWith sample diameter Ds
Relationship are as follows: LΔ=Tl×Ds；
D. strain loading and measurement: by TcNumerical value be assigned to nearest dependent variable Tc-last；Control mechanics loading device 3 is to tested
Sample 4 carries out Mechanical loading, load deflection LΔ, the reality of speckle strain-ga(u)ge measurement and feedback sample 4 in loading procedure
Deformation quantity Lr；After the completion of load, current dependent variable T is updatedcParameter, calculation formula are as follows: Tc = Tc-last+Lr/Ds；Judge that mechanics adds
It carries and sets whether 3 be single-ended loading method, be to control the sample stage 6 of small-angle scattering spectrometer to move downward 0.5 times of LΔ。
E. controlled level turntable 5 is to neutron measurement position: controlled level turntable 5 returns to zero position, makes sample surfaces
Towards neutron incidence beam direction；
F. neutron scattering signal measurement of the sample 4 under strain loading: starting 9 pairs of measurement neutrons of neutron monitor are counted
Number, starting neutron detector 7 measure scattered signal of the sample 4 under the strain regime；Judging measurement experiment is
No completion is to jump to g, otherwise goes to step b, carries out next strain point load to sample 4；
G. measurement terminates, and saves the survey of the Mechanical loading data of mechanical loading unit 3 and the neutron detector 7 of the small angular spectrum instrument of neutron
Test result；
In the step a, the diameter of sample 4 is greater than neutron streaming diameter of section.
In the step b, horizontal rotating table 5 is high-precision, low vibration turntable.
Embodiment 2
The basic phase of embodiment of the neutron measurement method and embodiment 1 for fragile material Study on Microstructure of the present embodiment
Together, the video camera 8 for the speckle deformeter being a difference in that in the present embodiment is placed on the right side of sample stage 6, mechanical loading unit 3
For the fixed upper end loading method in lower end.
Step b are as follows: controlled level turntable 5 to strain loading position: controlled level turntable 5 rotates fixed angles to the right
θ is spent, the camera lens of the video camera 8 of sample surfaces face speckle deformeter is made；
Step d are as follows: strain loading and measurement: by TcNumerical value be assigned to nearest dependent variable Tc-last；Control mechanics loading device 3
Mechanical loading, load deflection L are carried out to sample 4Δ, speckle strain-ga(u)ge measurement and feedback sample 4 in loading procedure
Practical deformation quantity Lr；After the completion of load, current dependent variable T is updatedcParameter, calculation formula are as follows: Tc = Tc-last+Lr/Ds；Judgement
Whether mechanical loading unit 3 is single-ended loading method, is to control the sample stage 6 of small-angle scattering spectrometer to move upwards 0.5 times
LΔ。
Embodiment 3
The present embodiment for fragile material Study on Microstructure neutron measurement method and embodiment and embodiment 1 it is basic
It is identical, it is a difference in that mechanical loading unit is the synchronous loading method of both-end.
Step d are as follows: strain loading and measurement: by TcNumerical value be assigned to nearest dependent variable Tc-last；Control mechanics load dress
It sets 3 pairs of samples 4 and carries out Mechanical loading, load deflection LΔ, speckle strain-ga(u)ge measurement and feedback detected sample in loading procedure
The practical deformation quantity L of product 4r；After the completion of load, current dependent variable T is updatedcParameter, calculation formula are as follows: Tc = Tc-last+Lr/Ds。
Claims (4)
1. a kind of neutron measurement method for fragile material Study on Microstructure, which is characterized in that in the measurement method
The measuring device and its connection relationship of use are as follows:
The seaming chuck (1) of Brazilian test special fixture, push-down head (2) are installed on mechanical loading unit (3), by sample
(4) it is placed between seaming chuck (1), push-down head (2)；Mechanical loading unit (3) is fixed on horizontal rotating table (5), make by
Sample (4) center is on the extended line of horizontal rotating table (5) rotary shaft；Horizontal rotating table (5) is mounted on the small angle of neutron and dissipates
It penetrates on the sample stage (6) of spectrometer, sample (4) is made to be in the front of the neutron detector (7) of neutron small angle scattering spectrometer；
The video camera (8) of speckle deformeter is placed on the left or right side of sample stage (6) according to neutron small angle scattering spectrometer field condition；
Sample (4), neutron detector (7), speckle deformeter the center of video camera (8) be in same level height；Mechanics adds
Carry set (3), neutron detector (7), the video camera (8) of speckle deformeter, neutron small angle scattering spectrometer neutron monitor (9)
Signal wire be connected to control computer (10)；
The measurement method the following steps are included:
Parameter initialization and sample initial state measure: the single step neutron measurement number of setting neutron small angle scattering spectrometer measurement, sample
Diameter DsWith the sample message parameter of thickness of sample, the current dependent variable parameter T of sample (4) is initializedcIt is revolved with controlled level
The current location A of turntable (5)rIt is zero；Starting neutron monitor (9) counts measurement neutron, starts neutron detector (7)
The scattered signal of sample (4) is measured, the measurement result of sample initial state is obtained；
Controlled level turntable (5) is to strain loading position: video camera (8) of the controlled level turntable (5) to speckle deformeter
Placement direction rotate fixed angle θ, make the camera lens of sample surfaces face video camera (8)；
The calculating of the discrete strain parameter of Brazilian test: according to target strain parameter TsWith current dependent variable TcCalculate load dependent variable
Tl, triadic relation are as follows: Tl=Ts-Tc, further calculate load deformation quantity LΔ, LΔWith load dependent variable TlWith sample diameter DsPass
System are as follows: LΔ=Tl×Ds；
Strain loading and measurement: by TcNumerical value be assigned to nearest dependent variable Tc-last；Control mechanics loading device (3) is to detected sample
Product (4) carry out Mechanical loading, load deflection LΔ, the reality of speckle strain-ga(u)ge measurement and feedback sample (4) in loading procedure
Border deformation quantity Lr；After the completion of load, current dependent variable T is updatedcParameter, calculation formula are as follows: Tc = Tc-last+Lr/Ds；Judge mechanics
Whether loading device (3) is single-ended loading method, is to control the sample stage (6) of small-angle scattering spectrometer to be moved upwardly or downwardly
0.5 times of LΔ；
Controlled level turntable (5) is to neutron measurement position: controlled level turntable (5) returns to zero position, makes sample surfaces face
To neutron incidence beam direction；
Neutron scattering signal measurement of the sample (4) under strain loading: starting neutron monitor (9) carries out measurement neutron
It counts, starting neutron detector (7) measures scattered signal of the sample (4) under the strain regime；Judgement measurement
Whether experiment is completed, and is to jump to g, otherwise goes to step b, carries out next strain point load to sample (4)；
Measurement terminates, the neutron detector (7) of the Mechanical loading data and small angular spectrum instrument of neutron of preservation mechanical loading unit (3)
Test result.
2. a kind of neutron measurement method for fragile material Study on Microstructure according to claim 1, feature
Be: in step a, the diameter of sample (4) is greater than neutron streaming diameter of section.
3. a kind of neutron measurement method for fragile material Study on Microstructure according to claim 1, feature
Be: in stepb, horizontal rotating table (5) is high-precision, low vibration turntable.
4. a kind of neutron measurement method for fragile material Study on Microstructure according to claim 1, feature
Be: in step d, mechanical loading unit (3) is the synchronous loading method of both-end or single-ended loading method, the synchronous load side of both-end
The load output both ends of the mechanical loading unit (3) of formula are synchronized, counter motion；Use the mechanical loading unit of single-ended loading method
(3) when, sample stage (6) has elevating function.
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| CN201810396123.XA CN108956665B (en) | 2018-04-28 | 2018-04-28 | Neutron measurement method for microstructure research of brittle material |
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| CN111307572A (en) * | 2020-04-03 | 2020-06-19 | 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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| CN108956665B (en) | 2020-10-23 |
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