CN109187607A - A kind of method that the full pole figure of X-ray diffraction tests Koln coefficient in zircaloy - Google Patents
A kind of method that the full pole figure of X-ray diffraction tests Koln coefficient in zircaloy Download PDFInfo
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- CN109187607A CN109187607A CN201811091058.6A CN201811091058A CN109187607A CN 109187607 A CN109187607 A CN 109187607A CN 201811091058 A CN201811091058 A CN 201811091058A CN 109187607 A CN109187607 A CN 109187607A
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
Abstract
The purpose of the present invention is to provide a kind of method of Koln coefficient in X-ray diffraction analysis technical testing zircaloy, specific steps are as follows: (1) sample preparation, sampling and testing face is parallel with rolling surface, and has marked the direction of sample；(2) sample of well cutting is polished；(3) it mechanically polishes, until reaching surface generation mirror effect；(4) cleaning sample and drying；(5) it is observed using X-ray diffraction analysis technology, obtains the X-ray diffraction pole figure of sample；(6) the corresponding diffracted intensity value of corresponding orientation is obtained according to the X-ray diffraction pole figure of sample, the basal plane Koln coefficient on three directions is obtained by integral.The method test speed is fast, can test in the case where existing zircaloy standard specimen and obtain the Koln coefficient of material macro-regions, it is grain-oriented to solve the problems, such as that current EBSD technology can only characterize material domain.
Description
Technical field
The invention belongs to zircaloy technical field of performance test, and in particular to a kind of full pole figure test zirconium conjunction of X-ray diffraction
The method of Koln coefficient in gold.
Background technique
Texture has an important influence to the orientation of the hydride in zircaloy, and its also with the mechanical property of alloy, spoke
It is contacted according to existing between performance and corrosive nature.Therefore, for the control in the test and process of the texture of zircaloy
It is extremely important.Koln coefficient (Kearns factor) is the index that related scientific research worker defines, to describe zircaloy
And Texture Information in other hexagonal closed-packeds.Koln coefficient quantitatively can provide Patterns for Close-Packed Hexagonal Crystal standard shaft c, i.e. basal plane
Volume fraction in different directions.By Texture Information, material processing can be adjusted correspondingly, so as to improve
Material property.Currently, the method for test zircaloy Koln coefficient mainly passes through Electron Back-scatter Diffraction Analysis Technique (EBSD),
But using the method for EBSD with significant limitation, it is very high for the quality requirement of sample first, it is desirable that shows that nothing is answered
Power residual.This just needs related scientific research worker to remove sample by the method for electrolytic etching, vibropolish and ion etching
The stressor layers on surface, these methods are not only higher to operator's technical requirements, but also increase many cost inputs.In addition, by
In the limitation of relevant device, EBSD method can only test the Texture Information of microcosmos area, and (general word test zone is about 1 square
Millimeter), this is obviously unreasonable for the application of alloy in engineering.
X-ray diffraction (XRD) pole figure method tests Koln coefficient technology, is the data acquisition material provided by XRD pole figure
A kind of calculation method of Koln coefficient.Using the crystal grain that can mainly obtain macro-regions the advantages of the method test material texture
It is orientated (can generally test the material texture information of 400 square millimeters of areas), XRD method is suitble to believe the texture of material entirety
Breath measures, and obtains the statistical value of a marcotexture, more can comprehensively reflect all different Texture Informations of material.Separately
Outside, the method sample preparation requires low, it may not be necessary to electrolytic etching, it is only necessary to simply be polished sample surfaces and mechanical
Polishing can be to test, and the Texture Information of quick obtaining material.
Summary of the invention
The purpose of the present invention is to provide a kind of method of Koln coefficient in X-ray diffraction analysis technical testing zircaloy,
The method test speed is fast, can test in the case where existing zircaloy standard specimen and obtain the Koln coefficient of material macro-regions,
It is grain-oriented to solve the problems, such as that current EBSD technology can only characterize material domain.
Technical solution of the present invention is as follows:
A kind of method that the full pole figure of X-ray diffraction tests Koln coefficient in zircaloy, which is characterized in that specific steps are such as
Under:
(1) sample preparation, using linear cutting equipment to the sample to be analyzed, sample size: rolling direction is Y-direction, ruler
Very little is 10-22mm, is laterally X-direction, and having a size of 10-20mm, Z-direction takes thickness of sample (thickness of sample cannot be greater than 15mm),
That is sampling and testing face is parallel with rolling surface, and has marked the direction of sample, the surface that the rolling surface is X, Y-direction is constituted；
(2) sample of the well cutting in step (1) is successively passed through 150#, 320#, 800#, 2000# sand paper to polish,
The process ground is firmly light as far as possible and uniform, to guarantee that sample surfaces do not introduce new texture；
(3) sample polished in step (2) is mechanically polished, until reaching surface generation mirror effect；
(4) successively with clear water and dehydrated alcohol that sample clean is clean and dry；
(5) it is observed using X-ray diffraction analysis technology, obtain the pole figure of sample: its principle is to be placed in X-ray detector
Meet on 2 positions θ of Bragg equation, sample does Space Rotating around incidence point, enters the crystal grain in all orientation all successively
Its diffracted intensity is measured to be detected by the detector in diffraction orientation；If there are texture in sample, diffracted intensity can be with
The orientation of sample and change, due to diffracted intensity can be proportional to occur diffraction crystal face Polar orderatim；Intensity is divided into difference
Grade, according to its corresponding azimuth mark on stereogram, to obtain the X-ray diffraction pole figure of sample；
(6) corresponding orientation (under different α and β angles) corresponding diffracted intensity value is finally obtained according to the pole figure of sample,
The basal plane Koln coefficient on three directions is obtained by integral.
As a preferred technical scheme:
The zircaloy is Zr-4 alloy (Zr-1.2wt%Sn-0.2wt%Fe-0.1wt%Cr).
Use SiO2Suspension mechanically polishes the sample polished in step (2).
Step (5) carries out X-ray diffraction analysis and needs using zirconium standard specimen, preparation method are as follows: utilizes hydraulic press by pure zirconium
Powder is suppressed, pressure 800MPa, is obtained with a thickness of 3mm, and diameter is the cylindrical type standard specimen of 25mm, carries out X-ray to it and spreads out
Penetrate analysis.
Sample is made into α angular turn around X-axis or Y-axis in step (5) test process, and makees β angular turn about the z axis,
- 75 ° of middle α=0 °, -360 ° of β=0 °.
The advantage of the method for the invention is to prepare that sample is simple, and the marcotexture suitable for high-volume material measures, and
And this method can obtain the Texture Information of material macroscopic view, obtain the statistical value of material texture, for commenting for material macro property
Valence has one's own knack.
Detailed description of the invention
Fig. 1 x-ray pole figure measuring device schematic diagram.
Fig. 2 Koln coefficient Computing Principle schematic diagram.
Specific embodiment
Obtaining embodiment with pole figure with reference to the accompanying drawing, the present invention will be described in detail.
Embodiment
1. sample preparation
(1) using linear cutting equipment to the sample to be analyzed, sample size: (rolling direction is denoted as the side Y to 15mm
To), 10mm (laterally, be denoted as X-direction), 0.5mm (normal direction is denoted as Z-direction, i.e. thickness of strip direction), sampling and testing face with roll
Face processed is parallel, and has marked the direction of sample, the surface that the rolling surface is X, Y-direction is constituted；
(2) sample surfaces that cutting obtains in step (1) are successively used into 150#, 320#, 800#, 2000# sand paper pre-grinding, obtained
The zircaloy sample arrived；
(3) SiO is used2Suspension mechanically polishes the sample surfaces of pre-grinding in step (2), pays attention in polishing process
Force should keep uniform and should not be too large, and cause texture to change in order to avoid introducing stress；
(4) successively use water and washes of absolute alcohol clean and dry in sample after polishing.
2. being observed using X-ray diffraction analysis technology
(1) test apparatus mainly has X-ray diffractometer (the present embodiment test is spread out using Rigaku/max-2400 type X-ray
Penetrate instrument), zirconium powder standard specimen tilts sample stage, DIFFRACplus TEXEVAl processing software.
(2) XRD analysis needs to deduct back end, therefore to prepare the standard specimen of zirconium.Pure zirconium powder is suppressed using hydraulic press,
Pressure is about 800MPa, is obtained with a thickness of 3mm, and diameter is the cylindrical type standard specimen of 25mm or so, and X-ray diffraction point is carried out to it
Analysis.
(3) zircaloy sample is placed on inclination sample stage, and its rolling direction is made to be parallel to the water for tilting sample stage
Square to.
(4) use the schematic diagram of X-ray diffractometer measurement zircaloy plate basal plane pole figure as shown in Figure 1, the device can be with
Diffracted intensity is recorded in the 2 θ diffraction locations of certain { HKL } crystal face.Test radiates sample using single CuK α radiation, surveys
Sample is made into α angular turn around X-axis or Y-axis during examination, and make about the z axis β angular turn (minimum angles of rotation can from
Row setting), the diffracted intensity of sample { HKL } crystal face at different (α, β).
(5) DIFFRAC is then usedplusTEXEVAl software is modified its result with zirconium powder standard specimen, and exports examination
Test data, i.e., the diffracted intensity value of different (α, β) and its respective direction.
(6) schematic diagram calculation of Koln coefficient is as shown in Fig. 2, crystal grain basal plane normal direction and three reference directions (X, Y, the sides Z
To) angle be respectively α, α1, α2, then have the Koln coefficient of normal plane according to the definition of Koln coefficient are as follows:
Wherein I is diffracted intensity, β angle when β is measurement, i.e., around the normal rotational angle of sample, due to reduction of a fraction, at this time
Calculating can not consider β specific value.
Verifying: according to above-mentioned steps, Zr-4 sheet alloy normal direction plane texture Koln coefficient is measured.Pass through X-ray pole figure method
It is as shown in table 1 to measure Zr-4 alloy strip steel rolled stock plate texture initial data.After obtaining the test data of pole figure method of testing, normal direction is substituted into
In the integral formula (1) of Koln coefficient fz.The Excel of the operation of initial data is shown in Table 2.As shown in table 2, to every in initial data
The corresponding measurement data of angle [alpha] of one column carries out summation operation and trigonometric function operation respectively, has obtained under different measurement angle α
Integral result of the corresponding β in 0~360 °, then by integral result of the β in 0~360 ° under all different test angle α
It sums, obtains molecule and the corresponding integral result of denominator in formula (1), molecule and denominator are divided by, acquired results are
The sample is in angular extensions alpha: the fz=0.6896 tested in 0~75 °, β: 0~360 °.
Koln coefficient fz=0.633 is tested by EBSD Eulerian angles method of testing, the two result is almost the same.
1 X-ray pole figure method of table tests Zr-4 sheet alloy texture initial data
The Excel table of the calculating Koln coefficient of table 2
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of method of Koln coefficient in full pole figure test zircaloy of X-ray diffraction, which is characterized in that specific step is as follows:
(1) sample preparation, using linear cutting equipment to the sample to be analyzed, sample size: rolling direction is Y-direction, having a size of
10-22mm is laterally X-direction, and having a size of 10-20mm, thickness of sample direction is Z-direction, having a size of no more than 15mm；Sampling is surveyed
Examination face is parallel with rolling surface, and has marked the direction of sample, the surface that the rolling surface is X, Y-direction is constituted；
(2) sample of the well cutting in step (1) is successively passed through 150#, 320#, 800#, 2000# sand paper to polish；
(3) sample polished in step (2) is mechanically polished, until reaching surface generation mirror effect；
(4) successively with clear water and dehydrated alcohol that sample clean is clean and dry；
(5) it is observed using X-ray diffraction analysis technology, obtains the pole figure of sample: X-ray detector being placed in and meets Prague side
On 2 positions θ of journey, sample does Space Rotating around incidence point, and the crystal grain in all orientation is made all to enter diffraction orientation successively, thus
It is detected by the detector, measures its diffracted intensity；If there are texture in sample, diffracted intensity can with the orientation of sample and
Variation, since diffracted intensity can be proportional to the Polar orderatim of generation diffraction crystal face；Intensity is divided into different grades, according to its phase
The azimuth mark answered is on stereogram, to obtain the X-ray diffraction pole figure of sample；
(6) the corresponding diffracted intensity value of corresponding orientation is finally obtained according to the pole figure of sample, is obtained on three directions by integral
Basal plane Koln coefficient.
2. according to the method for Koln coefficient in the full pole figure test zircaloy of X-ray diffraction described in claim 1, it is characterised in that:
The zircaloy is Zr-1.2wt%Sn-0.2wt%Fe-0.1wt%Cr.
3. according to the method for Koln coefficient in the full pole figure test zircaloy of X-ray diffraction described in claim 1, it is characterised in that:
Use SiO2Suspension mechanically polishes the sample polished in step (2).
4. according to the method for Koln coefficient in the full pole figure test zircaloy of X-ray diffraction described in claim 1, it is characterised in that:
Zirconium standard specimen needed for step (5) carries out X-ray diffraction analysis the preparation method comprises the following steps: pure zirconium powder is suppressed using hydraulic press, press
Power is 800MPa, is obtained with a thickness of 3mm, and diameter is the cylindrical type standard specimen of 25mm, carries out X-ray diffraction analysis to it.
5. according to the method for Koln coefficient in the full pole figure test zircaloy of X-ray diffraction described in claim 1, it is characterised in that:
Sample is made into α angular turn around X-axis or Y-axis in step (5) test process, and makees β angular turn about the z axis, wherein α=0 °-
75 °, -360 ° of β=0 °.
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Cited By (2)
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| CN110361404A (en) * | 2019-07-11 | 2019-10-22 | 合肥工业大学 | The acquisition device and acquisition methods of crystalline mi texture orientation |
| CN113533400A (en) * | 2021-07-06 | 2021-10-22 | 合肥工业大学 | High-speed and accurate X-ray texture testing method for extruded bar |
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Application publication date: 20190111 |