CN106053504A - Novel contactless nondestructive method of measuring material hardness - Google Patents
Novel contactless nondestructive method of measuring material hardness Download PDFInfo
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- G01N23/2076—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions for spectrometry, i.e. using an analysing crystal, e.g. for measuring X-ray fluorescence spectrum of a sample with wavelength-dispersion, i.e. WDXFS
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Abstract
The invention relates to a novel contactless nondestructive method of measuring material hardness. The method is technically characterized in that GCr15 steel after being subjected to shot blasting of 0.50+0.30+0.15mmA is used as a studying object, the surface of the GCr15 steel has large residual pressure stress and refined tissue structure, the tissue structure can restore during high-temperature annealing, change of the tissue structure can be indirectly expressed actually through FWHM change, the residual pressure stress can be reduced, and lowering of surface hardness can be caused. Through change tendency of FWHM and the residual stress along with annealing time at different temperatures, a relational expression between the material surface hardness and the FWHM as well as the residual stress at different annealing temperatures is established. When hardness of same materials is tested, a hardness value can be acquired through calculation by measuring corresponding FWHM and residual stress through XRD technology and combining with the relational expression acquired. The method is an extension of XRD testing technology, and no contact with the sample occurs during testing, so that completely nondestructive testing is realized. The method is convenient, quick and more effectively and can be widely applied in measuring hardness of metal materials.
Description
Technical field
The present invention relates to the hardness using X-ray diffraction (XRD) technology to carry out measuring metallic materials, can be used for metal material
Material or component surface hardness contactless nondestructive measurement field.
Background technology
For setting up the relation between microstructure and residual stress and hardness, this method have employed has microcosmic
Organizational structure and residual stress gradient change shot-peening part top layer the most greatly carry out characterized by techniques.Shot-peening is with a large amount of bullets at a high speed
Ball bump material surface, produces bigger residual compressive stress at material surface, and surface layer grain size is diminished, micro-
Distortion increases, and the change of residual compressive stress and heterogeneous microstructure forms hardened layer on surface, both to material shot-peening layer
Hardness has been contributed, and plays good strengthening effect.Generally, when at high temperature annealing, the residual stress of shot-peening layer and
Heterogeneous microstructure all can change, and therefore brings the change of hardness, by setting up the variation relation between three, and can be real
The now accurate Characterization to hardness.
Generally, measure shot-peening layer hardness and all use conventional indentation method, the impression i.e. stayed on surface by hardness tester pressure head
Area, the degree of depth or size etc. judge the size of hardness.But the impression that this test process produces can to material or device (especially
Parts in being currently in use and thickness, the parts of small volume) itself cause damage, even lost efficacy.For avoiding this type of
The appearance of unfavorable phenomenon, this patent is taked XRD measuring technology, is devised a kind of contactless lossless hardness detection method, especially
It is suitable for the measurement with the material hardness of bigger residual compressive stress and heterogeneous microstructure change.XRD tests hardness technical essential
It is to set up XRD diffraction maximum halfwidth (FWHM) under material sample bead blasted surfaces different temperatures, pass between residual stress and hardness
It is formula: first, utilizes under XRD technical testing sample bead blasted surfaces different temperatures FWHM with the variation relation of annealing time, and survey
Anneal under amount different temperatures the hardness number after different time, set up under different temperatures between sample bead blasted surfaces FWHM and its hardness
Relational expression, owing to FWHM is the amount relevant with heterogeneous microstructure (mainly Boundary corrosion test and microcosmic distortion), be i.e. equivalent to
Establish the relational expression between material surface heterogeneous microstructure and its hardness；Second, utilize XRD stress survey technology, test
Under different temperatures, the residual compressive stress of sample bead blasted surfaces is with the variation relation of annealing time, the FWHM that the first step is obtained with
Relational expression between hardness is modified, and obtains the quantitative relationship that hardness is contributed by residual compressive stress.By setting up different materials
Shot-peening layer FWHM, relational expression between residual compressive stress and hardness, during the identical material hardness of follow-up measurement, only need to pass through
XRD technology obtains the numerical value of this material FWHM and residual compressive stress, gets final product this kind of material of accurate characterization or parts shot-peening layer is hard
The size of degree.The method is the most convenient effective but also belongs to entirely without contact Non-Destructive Testing, hardness measurement can be avoided completely to material
Material or the destruction of device.
The goal of the invention of the present invention is the deficiency overcoming conventional hardness measuring method, it is provided that one can accurate characterization material
The method of hardness, can avoid again the novel hardness test technology that measured material destroys completely.
Summary of the invention
The invention provides the new technique of a kind of contactless nondestructive measurement shot-peening layer hardness, hard at accurate characterization shot-peening layer
Degree is at the same time it can also be avoid the damage to test material completely.
The present invention is achieved by the following technical solutions, and concrete steps, work process and principle are as follows:
(1) choose GCr15 steel and be prepared as 30 × 10 × 5mm as original material3Sample, utilizes vapour-pressure type compressed air shotblasting machine to examination
Sample carries out composite shot blasting process, and composite shot blasting technique includes that three process, first operation shot peening strength are 0.50mmA, and second
Procedure shot peening strength is 0.30mmA, the shot media of twice shot-peening is constant (cast steel ball, a diameter of 0.6mm), three process
Shot peening strength is 0.15mmA, and the shot media of shot-peening is ceramic pellet for the third time, and particle diameter less (a diameter of 0.3mm), through three roads
Sample surfaces after operation shot-peening has the heterogeneous microstructure of bigger residual compressive stress and refinement.
(2) residual stress and annealing temperature and the relation of time are set up
Sample after shot-peening makes annealing treatment at different temperatures, at a certain temperature, prolongation in time, residual pressure
Stress can be gradually reduced, and can get residual compressive stress relation over time under different temperatures according to XRD test stress method,
Its test philosophy is, utilizes X diffraction stress analysis measuring method, in order to match with residual stress measurement, selects Fe (211) to spread out
Penetrating crystal face, X-ray elastic constant is S2/ 2=5.92 × 10-6MPa-1And S1=-1.28 × 10-6MPa-1, guarantee in the range of 2 θ
Diffraction maximum is complete.For abscissa and to have surveyed the residual compressive stress of correspondence be vertical coordinate to utilize annealing time under different temperatures, builds
Vertical relation between residual stress and annealing time.
(3) material X-ray diffraction, obtains diffraction line profile, sets up the relation of FWHM and annealing time.
Utilizing the annealing process the same with (2nd) step, utilize XRD method of testing to obtain diffraction line profile, its operation principle is,
X-ray bombardment is when crystalline material surface, when diffraction direction meets Bragg diffraction equation with diffraction crystal face, and corresponding diffraction
Peak arises that reinforcement, diffraction line profile are to be determined by the micro structure of crystalline material.According to the diffraction spectral line of test material, select Fe
(211) diffraction crystal face.Concrete test parameter is: tube voltage: 40Kv, tube current: 30mmA, Cu-KαRadiation, is filter plate with Ni,
To guarantee that the monochromaticity of diffracting X-rays, scanning step and speed are respectively set to 0.01 ° and 2 °/min, thus ensure that measurement
The reliability of result.FWHM is directly obtained by diffraction peak shape, diffraction maximum FWHM when utilizing different temperatures to anneal, indirectly characterize material
Under the different temperatures of material, bead blasted surfaces organizational structure is with the relation between annealing time.
(4) relation between material surface hardness and annealing time under different annealing temperature is set up
Its operation principle is, uses DHV-1000 type microhardness testers, according to the impression image analysis software carried, measures
Under different temperatures, bead blasted surfaces microhardness with the variation relation of annealing time, test condition is: imposed load 50g, keeps carrying
Lotus time 15s, in the microhardness of 3 points of surface random measurement, finally takes its meansigma methods and characterizes.
(5) relation between material surface XRD crest line FWHM and hardness under different annealing temperature is set up
Its operation principle is, utilizes FWHM and hardness number under the different temperatures of (3rd) step and (4th) pacing examination, sets up not
With relational expression between material surface XRD crest line FWHM and hardness under annealing temperature, compare under different annealing temperature hardness with
Relation between FWHM, carrys out the contribution to bead blasted surfaces hardness of the side light organizational structure.
(6) material bead blasted surfaces hardness and FWHM and the relation of residual stress under different annealing temperature are set up
By the relation between hardness when contrast high temperature and process annealing and FWHM, to residual stress under different temperatures to firmly
The contribution of degree explains, and is modified the relational expression between FWHM and hardness, introduces residual stress, the most indirectly in formula
Illustrate that organizational structure and residual stress have contribution to the size of hardness, and set up material bead blasted surfaces hardness and FWHM and remnants
The exact relationship formula of stress.When to identical testing material hardness, only need to be answered with remaining by the FWHM that XRD commercial measurement is corresponding
Power size, in conjunction with the relational expression obtained, i.e. can get hardness number.
The invention has the beneficial effects as follows: the method for contactless Non-Destructive Testing hardness proposed by the invention, be completely eliminated
The infringement to material of the conventional hardness method of testing.Compared with tradition blasting technology, the material after test hardness is especially become
The serviceability of product parts is entirely without impact.
Accompanying drawing explanation
Fig. 1: in annealing process, GCr15 steel bead blasted surfaces Fe (211) face FWHM is over time
Fig. 2: under different temperatures, GCr15 steel surface residual stress is with the change of annealing time
Fig. 3: when GCr15 steel is annealed under different temperatures, bead blasted surfaces microhardness is over time
During the annealing of Fig. 4: different temperatures, GCr15 steel bead blasted surfaces hardness is with the change of FWHM
Detailed description of the invention
Following example are provided in conjunction with present disclosure:
(1) original material bead
Selecting the trade mark is GCr15 steel, Technology for Heating Processing: oil quenching after 840 DEG C of heating 15min, keeps 120min at 200 DEG C
Annealing.Cut into a size of through line: 30 × 20 × 5mm3.Utilize pneumatic type compressed air shotblasting machine, sample carried out composite shot blasting process,
Shot-blast process includes three process: first operation shot peening strength is 0.50mmA, and second operation work shot peening strength is 0.30mmA,
The shot media of twice shot-peening is constant (cast steel ball, a diameter of 0.6mm), and three process shot peening strength is 0.15mmA, for the third time
The shot media of shot-peening is ceramic pellet, particle diameter less (a diameter of 0.3mm).
(2) annealing
Annealing sample at different temperatures, annealing temperature is respectively as follows: 300 DEG C, 400 DEG C, 500 DEG C and 600 DEG C, protects
The temperature time changes between 0-120min.
(3) X-ray diffraction spectral line gathers
X-ray diffractometer is utilized to gather different annealing temperature and the bead blasted surfaces diffraction spectral line of time, tube voltage: 40Kv,
Tube current: 30mmA, Cu-KαRadiation, is filter plate with Ni, to guarantee that the monochromaticity of diffracting X-rays, scanning step and speed are divided
It is not set to 0.01 ° and 2 °/min.By FWHM under diffraction spectral line acquisition different annealing temperature with the variation relation of annealing time,
As shown in Figure 1.
(4) test of residual stress
Utilizing X diffraction stress analysis instrument to measure, select Fe (211) diffraction crystal face, X-ray elastic constant is S2/ 2=
5.92×10-6MPa-1And S1=-1.28 × 10-6MPa-1, in the range of 2 θ, guarantee that diffraction maximum is complete.Utilize and move back under different temperatures
Fire the time be abscissa and surveyed correspondence residual compressive stress be vertical coordinate, set up between residual stress and annealing time
Relation, as shown in Figure 2.
(5) hardness measurement
Use DHV-1000 type microhardness testers, according to the impression image analysis software carried, measure and spray under different temperatures
Ball surface microhardness with the variation relation of annealing time, test condition is: imposed load 50g, keeps load-time 15s,
The microhardness of 3 points of surface random measurement, finally takes its meansigma methods and characterizes.Bead blasted surfaces microhardness under different temperatures
With annealing time variation relation as shown in Figure 3.
(6) material bead blasted surfaces hardness and X diffraction crest line FWHM and the relational expression of residual stress are set up
The data obtained according to Fig. 1 and Fig. 3, set up different temperatures annealing time 18CrNiMo7-6 steel bead blasted surfaces hardness with
The change of FWHM, as shown in Figure 4.From fig. 4, it can be seen that when there is higher value in FWHM, hardness corresponding at each temperature and
FWHM is approximately line relationship, and this is owing to residual stress declines rapidly at Initial Annealing, and the most linearly change (Fig. 4
Shown in), now shot-peening organizational structure (representing with FWHM, crystallite dimension and the value of micro-distortion can be drawn by the value of FWHM)
Change at Initial Annealing the change of hardness contributed and accounts for leading, the linear change of residual stress also determines firmness change simultaneously
Do not deviate by linear change；Simultaneously in the diagram it is also found that when temperature is higher, hardness and FWHM are approximately linear relationship,
But at low temperatures, corresponding for less FWHM hardness number can deviate considerably from change straight line.The hardness of shot-peening material surface is not only and group
Knit structure relevant, the most relevant with residual stress.Shot-peening layer Boundary corrosion test increases after annealing, microcosmic distortion reduces, and therefore causes
The reduction of FWHM value；There is also bigger and stable residual compressive stress after process annealing certain time simultaneously, now residual pressure should
Power becomes big to the contribution of hardness, and both common effects still can make the value that hardness holding is bigger, and the least FWHM is corresponding
Hardness can be contributed increasing to deviate original linear relationship because of residual compressive stress by hardness number, and hardness number is to higher value
Deviation, the least deviation of annealing temperature is the most obvious.And residual compressive stress drops to the least value after high annealing, to the contribution of hardness very
Little, it might even be possible to ignore, therefore the contribution of hardness is accounted for definitely leading by shot-peening layer tissue structure, therefore during high annealing hardness and
Between FWHM value the most linear, hardness number deviation less.For less FWHM value region, the deviation of corresponding hardness number
Can along with the increase departure degree of annealing temperature more and more less, this also further illustrate high annealing after organizational structure to hardness
Contribution occupies leading position.By the analytic explanation to Fig. 4, the change of approximate description hardness can be carried out in the material with its FWHM
Trend,
But its change in value of accurate expression can not be carried out with linear relationship simply, especially bigger to residual compressive stress
Material.The change of accurate description material hardness it is also contemplated that the impact of residual compressive stress, according to this feature and the data of Fig. 4
Can approximate and obtain material hardness and its FWHM and the relational expression model of residual stress, as shown in formula (1):
HV=aFWHM (deg.)+b+0.1RS (1)
In formula 1, a, b are the parameter (can according to the temperature that use be determined by experiment) relevant with temperature, and RS is residual pressure
Stress absolute value (in the calculating of this formula, FWHM and residual stress only take its numerical value, do not consider its measurement unit).This formula is at relatively low temperature
It is the most accurate to express time less with FWHM.
Measurement result shows, by hardness and FWHM and the relational expression of residual stress, in conjunction with XRD measuring technology, Ke Yijing
Really obtain the hardness number of material, simultaneously for material itself entirely without damage, and easily operate, be particularly suitable for various metal material
Or the measurement of Prefabricated parts hardness.
Claims (5)
1. a method for new non-contact non-destructive testing material hardness, is characterized in that using XRD method to test corresponding diffraction surfaces
FWHM and residual stress characterize the hardness of material.Wherein, utilize FWHM to represent the heterogeneous microstructure tribute to material hardness
Offer；When utilizing residual stress to characterize hardness number, only use its numerical value, do not consider its measurement unit.
The most according to claim 1, material residual stress and annealing temperature and the relation of time, the sample after shot-peening are initially set up
Product make annealing treatment at different temperatures, and at a certain temperature, prolongation in time, residual compressive stress can be gradually reduced, root
Can get residual compressive stress relation over time under different temperatures according to XRD test stress method, its test philosophy is, utilizes
X diffraction stress analysis measuring method, in order to match with residual stress measurement, selects Fe (211) diffraction crystal face, and X-ray is elastic
Constant is S2/ 2=5.92 × 10-6MPa-1And S1=-1.28 × 10-6MPa-1, in the range of 2 θ, guarantee that diffraction maximum is complete.Measure
The residual compressive stress that under different temperatures, annealing time is corresponding, sets up the change between residual stress and annealing temperature and time and closes
System.
The most according to claim 1, also need to obtain diffraction line profile by XRD measuring technology, set up FWHM and annealing time
Relation.Utilize the annealing process the same with described in claim 2, utilize XRD method of testing to obtain diffraction line profile, its operation principle
It is that x-ray bombardment is when crystalline material surface, when diffraction direction meets Bragg diffraction equation with diffraction crystal face, accordingly
Diffraction maximum arises that reinforcement, diffraction line profile are to be determined by the micro structure of crystalline material.According to the diffraction spectral line of test material, choosing
Select Fe (211) diffraction crystal face.Concrete test parameter is: tube voltage: 40Kv, tube current: 30mmA, Cu-KαRadiation, is filter with Ni
Wave plate, to guarantee that the monochromaticity of diffracting X-rays, scanning step and speed are respectively set to 0.01 ° and 2 °/min, thus ensure that
The reliability of measurement result.FWHM can be obtained by diffraction peak shape, utilize the FWHM of different temperatures difference annealing time diffraction maximum,
Under the indirect different temperatures characterizing material, materials microstructure is with the variation relation between annealing temperature and time.
4. set up the relation between material surface hardness and annealing time under different annealing temperature.Its operation principle is, uses
DHV-1000 type microhardness testers, according to the impression image analysis software carried, measure material surface under different temperatures micro-firmly
Degree with annealing temperature and the variation relation of time, test condition is: imposed load 50g, keep load-time 15s, on surface with
The microhardness of 3 points measured by machine, finally takes its meansigma methods and characterizes.
The most according to claim 1, the pass between material surface XRD crest line FWHM and hardness under different annealing temperature is first set up
System.Utilize FWHM and hardness number under the different temperatures of (3rd) step and (4th) pacing examination, set up material list under different annealing temperature
Relational expression between face FWHM and its hardness, compares the relation between hardness and FWHM under different annealing temperature, carrys out side light
The organizational structure contribution to bead blasted surfaces hardness.In conjunction with claim 2, by hardness when contrast high temperature and process annealing and FWHM
Between relation, the contribution of hardness is modified by residual stress under different temperatures, introduces in hardness and FWHM relational expression
Residual stress, finally set up the exact relationship formula between material hardness and FWHM and residual stress: HV=aFWHM+b+0.1RS,
I.e. have expressed the contribution that organizational structure and residual stress are common to hardness level.When to identical testing material hardness, only need to lead to
Cross FWHM corresponding to XRD commercial measurement and residual stress size, in conjunction with the relational expression obtained, hardness number can be calculated, and
Realize the most contactless non-destructive.
The invention has the beneficial effects as follows: the method for contactless Non-Destructive Testing hardness proposed by the invention, be completely eliminated tradition
Infringement to material during hardness test.Compared with tradition blasting technology, for the material especially finished product zero after test hardness
The serviceability of part, entirely without impact, has obvious advantage.
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| CN106596307A (en) * | 2016-12-26 | 2017-04-26 | 西北工业大学 | Component fatigue limit distribution calculation method based on residual stress and microhardness layer |
| CN106769574A (en) * | 2017-03-25 | 2017-05-31 | 西安科技大学 | Hardware residual stress and case hardness relation test device and method |
| CN109388878A (en) * | 2018-09-30 | 2019-02-26 | 北京航空航天大学 | A kind of Prediction method for fatigue life comprehensively considering shot-peening effect |
| CN110568001A (en) * | 2019-08-14 | 2019-12-13 | 武汉科技大学 | Method for determining stress relief annealing temperature of cold-bending thick-wall section steel corner |
| CN113340754A (en) * | 2021-05-31 | 2021-09-03 | 东风商用车有限公司 | Temperature field measuring method and manufacturing method of needle valve and needle valve body |
| CN113574368A (en) * | 2019-03-25 | 2021-10-29 | 新东工业株式会社 | Method for manufacturing reference sheet for measuring X-ray residual stress and reference sheet for measuring X-ray residual stress |
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| CN106769574A (en) * | 2017-03-25 | 2017-05-31 | 西安科技大学 | Hardware residual stress and case hardness relation test device and method |
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| CN109388878A (en) * | 2018-09-30 | 2019-02-26 | 北京航空航天大学 | A kind of Prediction method for fatigue life comprehensively considering shot-peening effect |
| CN113574368A (en) * | 2019-03-25 | 2021-10-29 | 新东工业株式会社 | Method for manufacturing reference sheet for measuring X-ray residual stress and reference sheet for measuring X-ray residual stress |
| CN110568001A (en) * | 2019-08-14 | 2019-12-13 | 武汉科技大学 | Method for determining stress relief annealing temperature of cold-bending thick-wall section steel corner |
| CN110568001B (en) * | 2019-08-14 | 2021-09-03 | 武汉科技大学 | Method for determining stress relief annealing temperature of cold-bending thick-wall section steel corner |
| CN113340754A (en) * | 2021-05-31 | 2021-09-03 | 东风商用车有限公司 | Temperature field measuring method and manufacturing method of needle valve and needle valve body |
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