CN109141706A - The method for detecting macromolecule material product remnants principal stress - Google Patents
The method for detecting macromolecule material product remnants principal stress Download PDFInfo
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- CN109141706A CN109141706A CN201710507705.6A CN201710507705A CN109141706A CN 109141706 A CN109141706 A CN 109141706A CN 201710507705 A CN201710507705 A CN 201710507705A CN 109141706 A CN109141706 A CN 109141706A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L5/00—Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes
- G01L5/0047—Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes measuring forces due to residual stresses
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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 present invention relates to high molecular material stress measurement fields, disclose a kind of method for detecting macromolecule material product remnants principal stress, this method carries out quantitative detection using remaining principal stress of the Two dimensional X ray diffraction method to macromolecule material product, wherein, the high molecular material includes crystalline region and amorphous area, and in the presence of residual stress, the dependent variable of the crystalline region and amorphous area is equal.Two dimensional X ray diffraction method is successfully applied to the detection of the remaining principal stress of common macromolecule engineering material by method provided by the invention, the limitation that conventional two-dimensional X-ray diffraction method is only used for the residual stress of detection Polycrystalline Metals material is broken, detection method is simply controllable, it is applied widely, detection error is small, has broad application prospects.
Description
Technical field
The present invention relates to high molecular material stress measurement fields, and in particular, to a kind of detection macromolecule material product is residual
The method of remaining principal stress.
Background technique
Currently, to the research of macromolecule residual stress, there are mainly four types of methods: first is that Birefringence Method, passes through optical instrument
It can be directly observed the distribution situation of stress, however this method is only limitted to transparent material, especially transparent membrane, using ten
Dividing has limitation；Second is that layer removes method, it is big to measure stress by its bending deformation situation after Material Physics is removed one layer
It is small, however this method can be only applied to plate material, analyze in practical applications plate stress using less；Third is that chemical
Material is immersed in chemical reagent by sonde method, this method, since the big material of stress is easier corrosion cracking, can be led to
It crosses the corrosion with standard sample to compare to estimate stress intensity range, complicated operation for the method, and is not capable of measuring multiple
The sample of miscellaneous shape；Fourth is that boring method, this method is used for reference from metal material, has widest applicability, however
High molecular material has a crystalline region and amorphous area two-phase, usually has certain elasticity, thus the result measured in this way with
Hole depth increases, error also will increase, while this method is also only limitted to simple shape and the biggish drilling operation that carries out
Material.Chinese patent CN105651440A discloses a kind of by punching quantitative detection macromolecule material product residual stress
Method improves the accuracy of this method by the coefficient in amendment Stress calculation.
And widely used another kind nondestructive determination --- the X-ray diffraction method in metal material, it is multiple to be capable of measuring shape
The stress of miscellaneous metal parts or very thin composite coating, the principle of X-ray diffraction method is according to the crystal in sample in stress
Acting on lower interplanar distance can change, so that the angle of diffraction measured can deviate, can be calculated by this bias
The strain of crystalline region out, to calculate stress with Hooke's law.United States Patent (USP) US4686631 and US5414747 disclose this side
Application of the method on polycrystalline solids and polycrystal film, figure layer.However it is different from metal material, it is usually contained in high molecular material
A large amount of amorphous area can not obtain the stress of material entirety by the strain of crystalline region, and high molecular material does not have metal material
The high angle peak needed in measurement, therefore currently can not be also widely used in the measurement of high molecular material residual stress.
Summary of the invention
The purpose of the invention is to overcome existing macromolecule stress detection to have, limitation, error are big, operate
The defects of complicated, provides a kind of method for detecting macromolecule material product remnants principal stress, and this method is non-destructive testing, is applicable in
Range is wide, largely compensates for the deficiency of existing macromolecule stress mornitoring method.Meanwhile hard high molecular material crystalline region and
The it is proposed of amorphous area contoured die of equal strain rate type for X-ray method to be applied to the common macromolecule engineering material in part.
To achieve the goals above, the present invention provides a kind of method for detecting macromolecule material product remnants principal stress, should
Method carries out quantitative detection using remaining principal stress of the Two dimensional X ray diffraction method to macromolecule material product, wherein the height
Molecular material includes crystalline region and amorphous area, and in the presence of residual stress, the dependent variable of the crystalline region and amorphous area is equal.
The method of the detection macromolecule material product remnants principal stress provided according to the present invention, using two-dimentional X x ray diffraction
Method carries out quantitative detection to the remaining principal stress of macromolecule material product, using contoured die of equal strain rate type, according to macromolecule material product
Whole modulus and Poisson's ratio can calculate macromolecule material product residual stress size and remaining principal stress it is big
Small and direction, what it is suitable for various shapes includes crystalline region and amorphous area, and in the presence of residual stress, the crystalline region and amorphous
The detection of the remaining principal stress of the equal macromolecule material product of the dependent variable in area.
Two dimensional X ray diffraction method is successfully applied to the remnants of common macromolecule engineering material by method provided by the invention
The office that conventional two-dimensional X-ray diffraction method is only used for the residual stress of detection Polycrystalline Metals material has been broken in the detection of principal stress
It is sex-limited, make it possible the non-destructive testing of macromolecule material product remnants principal stress, detection method is simply controllable, is applicable in model
Enclose wide, detection error is small, largely improves the accuracy of existing macromolecule material product stress mornitoring method and easy to operate
Property.It has broad application prospects.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Detailed description of the invention
Fig. 1 is sample when carrying out quantitative detection using remaining principal stress of the Two dimensional X ray diffraction method to macromolecule material product
The schematic diagram of product direction of rotation and diffraction vector distribution；
Fig. 2 is to carry out quantitative inspection to the remaining principal stress of macromolecule material product using a peacekeeping Two dimensional X ray diffraction method
Detector collects the schematic diagram of diffraction vector distribution when survey.
Description of symbols
S1S2S3, sample stage rotate tilt coordinates system S1-S2, specimen surface plane
S3, specimen surface normal θ, Bragg angle
ω, the included angle of incident X-rays and sample surfaces, sample rotates angle
ψ, sample inclination angle γ, diffraction ring deflection
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value, these ranges herein
Or value should be understood as comprising the value close to these ranges or value.For numberical range, the endpoint value of each range it
Between, can be combined with each other between the endpoint value and individual point value of each range, and individually between point value and obtain one
Or multiple new numberical ranges, these numberical ranges should be considered as specific open herein.
The present invention provides a kind of method for detecting macromolecule material product remnants principal stress, this method is penetrated using two dimension X
Line diffraction approach carries out quantitative detection to the remaining principal stress of macromolecule material product, wherein the high molecular material includes crystalline region
And amorphous area, and in the presence of residual stress, the dependent variable of the crystalline region and amorphous area is equal.
According to the present invention, the high molecular material includes crystalline region and amorphous area, and the crystalline region is arranged in crystalline substance by macromolecular chain
For lattice structure as framework ingredient, molecule interchain has stronger mechanics to interact, and the amorphous area is wound in a jumble by macromolecular chain
It is formed, intermolecular interaction is not strong, is in rubbery state at room temperature, is filled among crystalline region skeleton, such structure is able to
In the presence of residual stress, dependent variable is equal and stress etc., and then makes two for the crystalline region and amorphous area for making the high molecular material
Dimension X-ray diffraction method carries out quantitative detection for the remaining principal stress of the macromolecule material product and is possibly realized.
According to the present invention, in order to further increase the standard that the Two dimensional X ray diffraction method detects macromolecule material product
Exactness allows the macromolecule material product to obtain the integrated stress of the macromolecule material product by the strain of crystalline region,
The high molecular material is preferably hypocrystalline hard high molecular material.It is the elastic material of skeleton, hypocrystalline relative to rubbery state
Hard high molecular material is filled in it by the hard skeleton of crystal zone formation, amorphous area, can make the hypocrystalline hard high in this way
For molecular material product after the machining such as pressure processing, the dependent variable of crystalline region and the dependent variable of amorphous area are equal.
According to the present invention, the glass transition temperature of the amorphous area of the high molecular material is lower, is at room temperature rubber
State, Young's modulus is very low, and the Young's modulus of crystalline region is very high, usually the tens of amorphous area times even hundred times, in order to make
The crystalline region and amorphous area for stating high molecular material be not in the case where residual stress is equal, it is possible to have identical dependent variable makes institute
The integrated stress of the macromolecule material product, the high score can be obtained by the strain of crystalline region by stating macromolecule material product
The glass transition temperature of sub- material is preferably shorter than 25 DEG C, and the Young's modulus of the high molecular material is preferably 1-2GPa.
According to the present invention, in order to ensure that the macromolecule material product is sufficiently large by the hard skeleton area of crystal zone formation,
The crystallinity of the high molecular material is preferably greater than 20%
According to the present invention, the high molecular material for meeting above-mentioned condition can be polyolefin or polyester, it is preferable that institute
Stating high molecular material can be polyethylene or polypropylene.Polyethylene and polyacrylic molecular formula long-chain linear structure or branching knot
Structure is typical crystalline polymer.In the solid state, crystalline portion coexists with unformed.Crystallinity regards processing conditions and original
Treatment conditions and it is different, the macromolecule material can be controlled by the degree of branching of regulation polyethylene molecule and polypropylene molecule
The crystallinity and crystalline region of material are distributed, so that meeting the remaining principal stress of macromolecule material product of the present invention can use
Two dimensional X ray diffraction method detects.
According to the present invention, the Poisson's ratio for meeting the high molecular material of above-mentioned condition can be 0.3-0.6.Poisson's ratio refers to
For material when unidirectional tension or in compression, the ratio of the absolute value of transverse normal strain and axial normal strain is also named transversely deforming system
Number, it is the elastic constant for reflecting material transversely deforming.
According to the present invention, in order to make macromolecule material product generate residual stress, the detection macromolecule material product is residual
The method of remaining principal stress can also include: before detecting the macromolecule material product remnants principal stress, by the macromolecule
Material product is carried out at a temperature of close to molten condition along machine direction stretch and/or along the processing of vertical machine direction stretch.When
After the macromolecule material product carries out above-mentioned stretch processing, due to strand in a stretched state crystallisation by cooling and be locked,
Biggish residual stress will be remained.
According to the present invention, in order to make detector receive the macromolecule material product generated under X-ray diffraction it is each
The diffraction ring in a direction improves test data to obtain the diffraction information of the macromolecule material product in all directions
Accuracy, the method for the detection macromolecule material product remnants principal stress can also include in different rotation angle and inclining
Under oblique angle, the crystal face diffraction information of the macromolecule material product is acquired.
According to the present invention it is possible to realize the diffraction information received in all directions by rotation to sample and inclination.
As shown in Fig. 1 (a), S1S2S3Indicate that sample stage rotates tilt coordinates system, wherein S1-S2Representing sample surface plane, S3Represent examination
Sample surface normal direction, θ indicate that Bragg angle, ω indicate that the angle of incident X-rays and sample surfaces, φ indicate sample rotates angle,
ψ indicates sample inclination angle, and γ indicates diffraction ring deflection.When sample is in S1S2S3In coordinate system along different directions rotation and/
Or when inclination, shown in the two-dimensional projection of diffraction space such as Fig. 1 (b), two-dimensional detector can be according to the different directions being collected into
Diffraction ring distortion obtain selected (HKL) crystal face the angle of diffraction variation or interplanar distance variation, thus in conjunction with the height
The Young's modulus and Poisson's ratio of molecular material product, using Stress calculation software, fitting obtains this macromolecule material product
Remaining principal stress size and Orientation.
According to the present invention, described to be determined using remaining principal stress of the Two dimensional X ray diffraction method to macromolecule material product
Amount detection is omited with the conventional method for carrying out quantitative detection using remaining principal stress of the Two dimensional X ray diffraction method to metal product
Different, sample stage rotates in the parameter setting of angle and tilt angle the main distinction when detecting, specifically, the detection
The method of macromolecule material product remnants principal stress the following steps are included:
(1) macromolecule material product to be measured is put into sample stage, adjustment X-ray incoming position to sample to be tested surface is adjusted
Whole two-dimensional detector corner to a sample diffraction ring reaches two-dimensional detector center position, sets X-ray detection analysis system
Parameter up and down threshold, acquire the X-ray diffraction ring spectrogram of sample；
(2) diffraction for choosing highest angle diffraction peak or the corresponding crystal face of high angle diffraction maximum (HKL) as test is brilliant
Face, test obtain the X-ray diffraction ring peak position 2 of the crystal face (HKL) for the macromolecule material product that two-dimensional detector receives
θHKLOffset, strain value is calculated by bragg's formula；
(3) multiple sample inclination angle ψ and sample rotates azimuth are setSample stage is set to incline by the multiple samples set
Oblique angle ψ and sample rotates azimuthIt is tilted and is rotated, successively collect (HKL) crystal face of macromolecule material product not
X-ray diffraction ring spectrogram on equidirectional repeats step (2), obtains the high molecular material system that two-dimensional detector receives
The offset and strain value of the X-ray diffraction ring peak position of (HKL) crystal face of product in different directions；
(4) (HKL) crystal face for the macromolecule material product being collected into according to step (3) two-dimensional detector is in different directions
On X-ray diffraction ring peak position offset and strain value, fitting obtain the macromolecule material product principal stress size
The direction and.
According to the present invention, when choosing the diffraction crystal face as test in step (2), highest angle diffraction peak can be chosen
Or the corresponding crystal face of high angle diffraction maximum (HKL).When the corresponding crystal face (HKL) in highest angle diffraction peak is without adjacent dry
When disturbing diffraction ring, then diffraction crystal face of the corresponding crystal face (HKL) in the highest angle diffraction peak as test is chosen；When it is described most
When the corresponding crystal face of high angle diffraction maximum (HKL) has adjacent interference diffraction ring, then choose than low next of interference diffraction ring angle
Diffraction crystal face of the corresponding crystal face of diffraction maximum (HKL) of the independent diffraction ring of a high angle as test.
According to the present invention, Fig. 2 is the comparison that diffraction information is received with a peacekeeping two-dimensional x-ray receiver.In sample space
In, the direction of corresponding (HKL) the crystal face diffraction of all crystallite orientations of sample is provided, qualitative (HKL) crystal face diffraction vectors are obtained
Spatial distribution map.With dimension X-ray receiver, each sample inclination angle can only measure a point diffraction, as an example,
It is only measured in 7 point diffractions (as shown in the upper right side Fig. 2) with 7 different inclinations angle, and with two-dimensional x-ray receiver, each
On a sample inclination angle, a large amount of point diffraction (as shown in the lower right Fig. 2) can be measured, for identical 7 sample inclinations
Angle, Two dimensional X ray diffraction method can be collected into more diffraction datas.Therefore, significant with two-dimentional diffraction system data collection time
It reduces, and the diffraction maximum offset of sample different directions can be counted, obtain the spatial distribution of sample strain.
According to the present invention, in step (3), the setting means of the sample inclination angle ψ can be according to the sample of actual test
Diffracted intensity and peak position within the scope of 0-70 ° according to be angularly equidistant setting, for example, the sample inclination angle ψ can be set
It is 0 °, 15 °, 30 ° and 45 °, the sample inclination angle ψ can also be set as 0 °, 20 °, 40 ° and 60 °；The sample rotates side
Parallactic angleSetting means equally can according to the diffracted intensity and peak position of the sample of actual test within the scope of 0-360 ° according to
It is angularly equidistant setting.When rotation or inclination sample stage, sample stage is tilted according to preset inclination angle ψ first, so
Sample stage is planar successively rotated in sample stage upper surface to preset rotational orientation angle again afterwardsInclination every time
After sample stage, all repeat above-mentioned planar successively to rotate sample stage to preset rotation in sample stage upper surface
Turn azimuthThe step of, so alternately, until sample stage tilt angle reaches maximum setting inclination angle ψ, obtain multiple groups
Diffraction ring datagram.
Under preferable case, the sample rotates azimuthIt can be 0 °, 45 °, 90 °, 135 °, 180 °, 225 °, 270 °
With 315 °, the macromolecule material product (HKL) crystal face can be collected in this way at each specific sample inclination angle ψ
Equally distributed eight different rotational orientation anglesA large amount of diffraction ring information on direction, can ensure that the two-dimensional x-ray is answered
The reliability of power measurement result.
In a preferred embodiment, the macromolecule material product be 7cm × 7cm × 0.2cm (it is long × wide ×
It is high) polypropylene material, the polyacrylic Young's modulus is 1400MPa, Poisson's ratio 0.41, using biaxial orientation stretching machine to described
Polypropylene material is stretched, and is elongated with the speed of 300% deflection per second to five times at 155 DEG C along machine direction (MD),
After being heated to 173 DEG C, elongated with same tensile speed to the biaxial tension obtained after seven times perpendicular to machine direction (TD)
Film carries out quantitative detection to the polyacrylic remaining principal stress using Two dimensional X ray diffraction method, in detection process, first
It adjusts X-ray incidence angle and detector acceptance angle is 13 °, acquire sample diffraction ring at this time.Choose the second high angle in the visual field
Diffraction crystal face of corresponding (060) crystal face of diffraction maximum as test, test obtain the macromolecule that two-dimensional detector receives
2 θ of the angle of diffraction of the X-ray diffraction ring peak position of (060) crystal face of material product060Offset.Then by sample stage around S3Axis,
Rotational orientation angle is pressed in sample stage planeIt is successively rotated simultaneously for 0 °, 45 °, 90 °, 135 °, 180 °, 225 °, 270 ° and 315 °
The acquisition of diffraction loop data is carried out, 8 diffraction ring datagrams are obtained, then by sample stage around S1Axis tilts 20 ° clockwise, repeats
Above-mentioned steps, by sample stage around S3Axis presses rotational orientation angle in sample stage planeFor 0 °, 45 °, 90 °, 135 °, 180 °,
225 °, 270 ° and 315 ° successively rotate and carry out diffraction ring data acquisition, obtain 8 diffraction ring datagrams again, then again will
Sample stage is around S1Axis tilts 40 ° clockwise, then by sample stage around S3Axis presses rotational orientation angle in sample stage planeFor
0 °, 45 °, 90 °, 135 °, 180 °, 225 °, 270 ° and 315 ° successively rotates and carries out diffraction ring data acquisition, obtains 8 again
Diffraction ring datagram is opened, gained 24 is finally opened into diffraction ring datagram and imports Stress calculation software, according to used polypropylene
The Young's modulus and Poisson's ratio of material product obtain the stress Value Data of test point.
The present invention will be described in detail by way of examples below.
In following embodiment, Two dimensional X ray diffraction analysis is in the model Bruker for being purchased from Brooker company
It is carried out on the Two dimensional X ray diffraction instrument of D8DISCOVE；Stress calculation software is Bruker DIFFRAC.LEPTOS；Biaxial tension
Machine is test-type Br ü ckner Karo IV biaxial orientation stretching machine.
In following embodiment, polypropylene material is that the trade mark produced purchased from Hunan Chang Sheng petrochemical industry Co., Ltd is the poly- of T38f
Propylene material, the Young's modulus of the polypropylene material are 1400MPa, and Poisson's ratio 0.41, glass transition temperature is about -5 DEG C,
The crystallinity of the polypropylene material is about 40%.
In following embodiment, the polyethylene material is the PE100 polyvinyl piping materials produced purchased from oil of SPC material YH041,
Outer diameter is 4cm.The Young's modulus of the polyethylene material is 1200MPa, and Poisson's ratio 0.41, glass transition temperature is about -78
DEG C, the crystallinity of the polyethylene pipe material is about 62%.
Reference Example 1
Systematic error when this Reference Example is used to test using this method detection polypropylene material remnants principal stress.
It takes a small amount of corundum powder to be laid on the sample stage for being stained with double-sided adhesive, adjusts X-ray incident angle and detector connects
Receiving angle is 13 degree, acquires the X-ray diffraction ring spectrogram of sample, is chosen brilliant closest to (012) of polypropylene (060) crystal face
Diffraction crystal face of the face (2 angles θ are about 25.6 degree) as test, then by sample stage around S3Axis, by rotation in sample stage plane
AzimuthDiffraction ring data acquisition is successively rotated and carries out for 0 °, 45 °, 90 °, 135 °, 180 °, 225 °, 270 ° and 315 °,
8 diffraction ring datagrams are obtained, then by sample stage around S1Axis tilts 20 ° clockwise, repeats the above steps, by sample stage around
S3Axis presses rotational orientation angle in sample stage planeIt is successively revolved for 0 °, 45 °, 90 °, 135 °, 180 °, 225 °, 270 ° and 315 °
Turn and carry out diffraction ring data acquisition, 8 diffraction ring datagrams is obtained again, then again by sample stage around S1Axis inclines clockwise
Oblique 40 °, then by sample stage around S3Axis presses rotational orientation angle in sample stage planeFor 0 °, 45 °, 90 °, 135 °, 180 °,
225 °, 270 ° and 315 ° successively rotate and carry out diffraction ring data acquisition, 8 diffraction ring datagrams are obtained again, finally by institute
It obtains 24 diffraction ring datagrams and imports Bruker DIFFRAC.LEPTOS Stress calculation softwares, the selection for setting data calculates
Range are as follows: the start angle for integrating 2Theta is 25 °, and the angle at the end of 2Theta is 26.3 °, and the segmentation of 2Theta counts step
A length of 0.05 °, Gamma initial calculation angle is -125 °, and Gamma angle at the end is -55 °, and diffraction arc is divided into 14 subregions,
Give up the data point that diffracted intensity is lower than maximum intensity 20%.According to the system strain value being calculated, polypropylene material is utilized
Young's modulus and Poisson's ratio, systematic error when obtaining detection polypropylene material remnants principal stress are -3.7MPa.
Reference Example 2
Systematic error when this Reference Example is used to test using this method detection polyethylene material remnants principal stress.
It takes a small amount of corundum powder to be laid on the sample stage for being stained with double-sided adhesive, adjusts X-ray incident angle and detector connects
Receiving angle is 18 degree, acquires the X-ray diffraction ring spectrogram of sample, is chosen brilliant closest to (104) of polyethylene (040) crystal face
Diffraction crystal face of the face (2 angles θ are about 35.1 degree) as test.Then by sample stage around S1Axis tilts 22.5 ° clockwise, by sample
Sample platform is around S3Axis presses rotational orientation angle in sample stage planeIt is 0 °, 45 °, 90 °, 135 °, 180 °, 225 °, 270 ° and 315 °
Diffraction ring data acquisition is successively rotated and carried out, 8 diffraction ring datagrams are obtained, gained 8 is opened into diffraction ring datagram and is imported
Bruker DIFFRAC.LEPTOS Stress calculation software, sets the selection computer capacity of data are as follows: integrate the starting of 2Theta
Angle is 33.7 °, and the angle at the end of 2Theta is 36.4 °, and the segmentation statistics step-length of 2Theta is 0.05 °, Gamma starting meter
Calculating angle is -114 °, and Gamma angle at the end is -64 °, and diffraction arc is divided into 10 subregions, gives up diffracted intensity lower than maximum
The data point of intensity 20%.It is obtained according to the system strain value being calculated using the Young's modulus and Poisson's ratio of polyethylene material
It is -2.2MPa to systematic error when detecting polyethylene material remnants principal stress.
Reference Example 3
Systematic error when this Reference Example is used to test using this method detection polypropylene material remnants principal stress.
According to the method for Reference Example 1, the difference is that, the mode of sample rotates are as follows: setting sample stage inclination angle ψ is followed successively by
0 °, 10 °, 20 °, 30 ° and 40 °, by sample stage around S3 axis under each tilt angle, rotation side is pressed in sample stage plane
Parallactic angleIt is successively rotated for 0 °, 45 °, 90 °, 135 °, 180 °, 225 °, 270 ° and 315 ° and carries out diffraction ring data acquisition, respectively
8 diffraction ring datagrams are obtained, gained 40 is finally opened into diffraction ring datagram and imports Bruker DIFFRAC.LEPTOS stress
It is poly- to obtain detection using the Young's modulus and Poisson's ratio of polypropylene material according to the system strain value being calculated for software for calculation
Systematic error when propylene material remnants principal stress is -8.6MPa.
Embodiment 1
Polypropylene material is cut into the polypropylene material of 7cm × 7cm × 0.2cm (length × width × height) after 230 DEG C squeeze out in flakes,
The polypropylene material is stretched using biaxial orientation stretching machine, is become at 155 DEG C along machine direction (MD) with per second 300%
The speed of shape amount is elongated to five times, the size of the central location of the polypropylene material after taking the stretching be 5cm × 5cm ×
The sample of 0.03cm (length × width × height), is adsorbed on sample stage with deionized water, adjusts X-ray incident angle and detector
Receiving angle is 13 degree, acquires the X-ray diffraction ring spectrogram of sample, and it is corresponding to choose the second high angle diffraction maximum in the visual field
(060) diffraction crystal face of the crystal face as test.Then by sample stage around S3Axis presses rotational orientation angle in sample stage plane
Diffraction ring data acquisition is successively rotated and carried out for 0 °, 45 °, 90 °, 135 °, 180 °, 225 °, 270 ° and 315 °, 8 is obtained and spreads out
Loop data figure is penetrated, then by sample stage around S1Axis tilts 20 ° clockwise, repeats the above steps, by sample stage around S3Axis, in sample
Rotational orientation angle is pressed in platform planeIt successively rotates and spreads out for 0 °, 45 °, 90 °, 135 °, 180 °, 225 °, 270 ° and 315 °
Loop data acquisition is penetrated, 8 diffraction ring datagrams are obtained again, then again by sample stage around S1Axis tilts 40 ° clockwise, then
By sample stage around S3Axis presses rotational orientation angle in sample stage planeFor 0 °, 45 °, 90 °, 135 °, 180 °, 225 °, 270 ° and
315 ° successively rotate and carry out diffraction ring data acquisition, obtain 8 diffraction ring datagrams again, gained 24 is finally opened diffraction
Loop data figure imports Bruker DIFFRAC.LEPTOS Stress calculation software, sets the selection computer capacity of data are as follows: integral
The start angle of 2Theta is 24.5 °, and the angle at the end of 2Theta is 26.8 °, and the segmentation statistics step-length of 2Theta is
0.05 °, Gamma initial calculation angle is -125 °, and Gamma angle at the end is -55 °, and diffraction arc is divided into 14 subregions, gives up
Diffracted intensity is lower than the data point of maximum intensity 20%.Using the Young's modulus and Poisson's ratio of used polypropylene material, obtain
The stress Value Data of test point, the results are shown in Table 1.
Embodiment 2
Polypropylene material is cut into the polypropylene of 7cm × 7cm × 0.0025cm (length × width × height) after 230 DEG C squeeze out in flakes
Material, stretches the polypropylene material using biaxial orientation stretching machine, along machine direction (MD) with per second 300% at 155 DEG C
The speed of deflection is elongated to five times, after being heated to 173 DEG C, is being drawn perpendicular to machine direction (TD) with same tensile speed
The biaxially oriented film obtained after growing to seven times, the size of the central location of the polypropylene material after taking the stretching be 5cm ×
The sample of 5cm × 0.0025cm (length × width × height), is adsorbed on sample stage with deionized water, adjusts X-ray incident angle
It is 13 degree with detector receiving angle, it is corresponding to choose the second high angle diffraction maximum in the visual field for collected sample diffraction ring
(060) diffraction crystal face of the crystal face as test.Then by sample stage around S3Axis presses rotational orientation angle in sample stage planeFor
0 °, 45 °, 90 °, 135 °, 180 °, 225 °, 270 ° and 315 ° successively rotates and carries out diffraction ring data acquisition, obtains 8 diffraction
Loop data figure, then by sample stage around S1Axis tilts 20 ° clockwise, repeats the above steps, by sample stage around S3Axis, in sample
Rotational orientation angle is pressed in platform planeIt successively rotates and spreads out for 0 °, 45 °, 90 °, 135 °, 180 °, 225 °, 270 ° and 315 °
Loop data acquisition is penetrated, 8 diffraction ring datagrams are obtained again, then again by sample stage around S1Axis tilts 40 ° clockwise, then
By sample stage around S3Axis presses rotational orientation angle in sample stage planeFor 0 °, 45 °, 90 °, 135 °, 180 °, 225 °, 270 ° and
315 ° successively rotate and carry out diffraction ring data acquisition, obtain 8 diffraction ring datagrams again, gained 24 is finally opened diffraction
Loop data figure imports Bruker DIFFRAC.LEPTOS Stress calculation software, sets the statistical of data are as follows: integral
The start angle of 2Theta is 24.5 °, and the angle at the end of 2Theta is 26.8 °, and the segmentation statistics step-length of 2Theta is 0.05 °,
Gamma initial calculation angle is -125 °, and Gamma angle at the end is -55 °, and diffraction arc is divided into 14 subregions, and it is strong to give up diffraction
Degree is lower than the data point of maximum intensity 20%.Using the Young's modulus and Poisson's ratio of used polypropylene material, test point is obtained
Stress Value Data, the results are shown in Table 1.
Embodiment 3
The segment that the PE100 polyvinyl piping materials that outer diameter is 4cm are cut into 12cm long is fixed on sample stage, its tube wall is made
Highest point X-ray incidence point.It adjusts X-ray incident angle and detector receiving angle is 18 degree, collect sample diffraction
Ring chooses diffraction crystal face of corresponding (040) crystal face in highest angle diffraction peak as test in the visual field.Then by sample stage around
S1 axis tilts 22.5 ° clockwise, and sample stage is pressed rotational orientation angle around S3 axis in sample stage planeFor 0 °, 45 °, 90 °,
135 °, 180 °, 225 °, 270 ° and 315 ° successively rotate and carry out diffraction ring data acquisition, obtain 8 diffraction ring datagrams,
Gained 8 is opened into diffraction ring datagram and imports Bruker DIFFRAC.LEPTOS Stress calculation software, sets the selection meter of data
Calculate range are as follows: the start angle for integrating 2Theta is 33.7 °, and the angle at the end of 2Theta is 36.4 °, and the segmentation of 2Theta is united
A length of 0.05 ° of step counting, Gamma initial calculation angle is -114 °, and Gamma angle at the end is -64 °, and diffraction arc is divided into 10
Subregion gives up the data point that diffracted intensity is lower than maximum intensity 20%.Utilize the Young's modulus and pool of used polyethylene material
Loose ratio obtains the stress Value Data of test point, and the results are shown in Table 1.
Embodiment 4
According to the method for embodiment 2, the difference is that, the mode of sample rotates are as follows: setting sample stage inclination angle ψ is followed successively by
0 °, 10 °, 20 °, 30 ° and 40 °, by sample stage around S3 axis under each tilt angle, rotation side is pressed in sample stage plane
Parallactic angleIt is successively rotated for 0 °, 45 °, 90 °, 135 °, 180 °, 225 °, 270 ° and 315 ° and carries out diffraction ring data acquisition, respectively
8 diffraction ring datagrams are obtained, gained 40 is finally opened into diffraction ring datagram and imports Bruker DIFFRAC.LEPTOS stress
Software for calculation obtains the stress Value Data of test point, as a result using the Young's modulus and Poisson's ratio of used polypropylene material
As shown in table 1.
Table 1
It can be seen that the present invention using Two dimensional X ray diffraction method to the residual of macromolecule material product by the result of table 1
It is non-destructive testing that remaining principal stress, which carries out quantitative detection, and systematic error is smaller, and accuracy is higher, applied widely, largely more
The deficiency of existing macromolecule stress mornitoring method, the proposition of hard high molecular material crystalline region and amorphous area contoured die of equal strain rate type are mended
For X-ray method to be applied to the common macromolecule engineering material in part, has broken conventional two-dimensional X-ray diffraction
Method is only used for the limitation of the residual stress of detection Polycrystalline Metals material.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.Of the invention
, can be with various simple variants of the technical solution of the present invention are made in range of the technology design, including each technical characteristic is with any
Other suitable methods are combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, are belonged to
In protection scope of the present invention.
Claims (9)
1. a kind of method for detecting macromolecule material product remnants principal stress, which is characterized in that this method is spread out using two-dimensional x-ray
It penetrates method and quantitative detection is carried out to the remaining principal stress of macromolecule material product, wherein the high molecular material includes crystalline region and non-
Crystalline region, and in the presence of residual stress, the dependent variable of the crystalline region and amorphous area is equal.
2. according to the method described in claim 1, wherein, the high molecular material is hypocrystalline hard high molecular material, preferably
Ground, the glass transition temperature of the high molecular material are lower than 25 DEG C, and the Young's modulus of the high molecular material is 1-2GPa.
3. method according to claim 1 or 2, wherein the high molecular material is polyolefin or polyester.
4. method according to claim 1 or 2, wherein the high molecular material is polyethylene or polypropylene.
5. method according to claim 1 or 2, wherein the method also includes: detecting the macromolecule material product
Before remaining principal stress, the macromolecule material product is carried out along machine direction stretch and/or along vertical machine direction stretch
Processing.
6. method according to claim 1 or 2, wherein the method includes adopting under different rotation angles and inclination angle
Collect the crystal face diffraction information of the macromolecule material product.
7. method according to claim 1 or 2, wherein the described method comprises the following steps:
(1) macromolecule material product to be measured is put into sample stage, adjustment X-ray incoming position to sample to be tested surface, adjustment two
Dimension detector corner to a sample diffraction ring reaches two-dimensional detector center position, sets the ginseng of X-ray detection analysis system
Threshold above and below number, acquires the X-ray diffraction ring spectrogram of sample；
(2) the diffraction crystal face of highest angle diffraction peak or the corresponding crystal face of high angle diffraction maximum (HKL) as test is chosen, is surveyed
Examination obtains 2 θ of X-ray diffraction ring peak position of the crystal face (HKL) for the macromolecule material product that two-dimensional detector receivesHKL's
Strain value is calculated by bragg's formula in offset；
(3) multiple sample inclination angle ψ and sample rotates azimuth are setMake sample stage by the multiple sample inclination angle ψ set
With sample rotates azimuthIt is tilted and is rotated, successively collect (HKL) crystal face of macromolecule material product in different directions
On X-ray diffraction ring spectrogram, repeat step (2), obtain the macromolecule material product that two-dimensional detector receives
(HKL) offset and strain value of the X-ray diffraction ring peak position of crystal face in different directions；
(4) X of (HKL) crystal face for the macromolecule material product being collected into according to step (3) two-dimensional detector in different directions
The offset and strain value of x ray diffraction ring peak position, fitting obtain the macromolecule material product remaining principal stress size and
Direction.
8. according to the method described in claim 7, wherein, in step (3), the setting means of the sample inclination angle ψ is in 0-
Within the scope of 70 ° according to be angularly equidistant setting；The sample rotates azimuthSetting means be pressed within the scope of 0-360 °
It is set according to being angularly equidistant.
9. according to the method described in claim 8, wherein, the sample rotates azimuthFor 0 °, 45 °, 90 °, 135 °, 180 °,
225 °, 270 ° and 315 °.
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| CN113433150A (en) * | 2021-06-29 | 2021-09-24 | 北京科技大学 | Method for determining rock sealing stress |
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