CN109781516A - A kind of material strain original position EBSD observation test fixture and the test method - Google Patents
A kind of material strain original position EBSD observation test fixture and the test method Download PDFInfo
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- CN109781516A CN109781516A CN201811617915.1A CN201811617915A CN109781516A CN 109781516 A CN109781516 A CN 109781516A CN 201811617915 A CN201811617915 A CN 201811617915A CN 109781516 A CN109781516 A CN 109781516A
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Abstract
A kind of material strain original position EBSD observation test fixture of the invention and the test method, fixture include U-shaped folder head, clamping fixture and positioning bolt, and clamping fixture includes upper fixture and lower fixture, and upper fixture center is equipped with rectangular observation panel, for carrying out sample observation；Lower fixture, using bolt, is fixed for placing sample after upper fixture and lower fixture clamp sample by circular hole and collet.It when test, after sample installation is fixed, is first placed into stretching furnace after stretch observation imaging, finds region to be seen, carry out EBSD and observe imaging, repeat the above steps, complete material strain original position EBSD observation test.The method of the invention realizes the EBSD in situ observations under material strain, and the fixture is suitable for the sample of different-thickness and shape, determines size by fixture itself graduated scale while sample can be accurately positioned, and observes convenient for sample.
Description
Technical field:
The invention belongs to samples to stretch and EBSD observational technique field, and in particular to a kind of material strain original position EBSD observation
Test fixture and the test method.
Background technique:
EBSD technology is also referred to as electron backscatter diffraction (Electron Backscattered Diffraction, letter
Claim EBSD) or orientation mapping microtechnic (Orientation Imaging Microscopy, abbreviation OIM) etc..
Sample is tilted by high angle in scanning electron microscope, so that the signal EBSP of back scattering (i.e. diffraction) is abundant
Being consolidated to can be received by fluorescent screen (in microscope example room), and fluorescent screen is connected with a CCD camera, and EBSP can direct or warp
It is observed on fluorescent screen after amplification storage image, EBSD is not only capable of measuring each orientation shared ratio in the sample, moreover it is possible to know
These are orientated the distribution in microscopic structure in road, and the example that can be applied to orientation relationship measurement has: inferring between the second phase and matrix
Orientation relationship, the crystallography analysis of transcrystalline cracking, the integrality of monocrystal, EBSD measurement be every bit takes in sample
To, then the orientation difference of difference or different zones is also obtained with, it is brilliant so as to study the interfaces such as crystal boundary or phase boundary
The analysis of particle size and shape, the analysis of crystal boundary, subgrain and twin property.
The EBSD observation of material strain in drawing process: the laser high temperature imager of the function containing stretching/compressing may be implemented
The generation in materials microstructure/phase transition process and crack, trend and material at high temperature mechanical property under stress in hot environment
Observation and measurement.
In order to analyze tissue change of the metal in deformation process, tissue point is usually carried out under differently strained to sample
Analysis can observe the deformation behaviour of each phase in tissue, analyze stress distribution and microstructure evolution.Such as in TRIP steel, TRIP effect
Should guarantee the excellent mechanical property of TRIP steel, and TRIP effect is gradually occurred during sample deformation, therefore
Study it is differently strained under the conditions of in TRIP steel tissue morphology it is significant.Many researchers are to the differently strained condition of TRIP steel
Scientific and technical article is studied and delivered to undertissue's Evolution Mechanism, however, wherein most of changes due to observing position, can only obtain
To deformation to the universal law of tissue change, follow-up observation accurately cannot be carried out to specific organization, limit further group
Knit Evolution Mechanism research.So if the experimental method of effective tissue follow-up observation can be found, it will have to experimental study
Very big help.
The home position observation experiment of EBSD there are the problem of: traditional research technique is that stretch certain elongation percentage to test laggard
Row sampling, interception stretcher strain area carry out electrobrightening, observe under the EBSD function of scanning electron microscope sample, if it is desired to
Continue to observe material in the stress deformation row of such as 20%, 30%... sample tissue when breaking under stretching different elongation percentage
For, can only be carried out on different samples, thus can not accurate home position observation same position it is specific mutually or crystal grain is with stretching
The variation of deformation extent and the rule changed.
As described above, EBSD can only recording process, cannot achieve original position, traditional experimental method is to be stretched to sample
EBSD observation is carried out after certain ratio, but cannot achieve the continuous tracing and positioning under the different distortion amount of same position, is continued
It is difficult to find the position tested originally after stretching, does not accomplish original position.
People increasingly focus on the variation of material structure property in being subjected to deformation process at present, and material at high temperature
The structure property of deformation process changes, and it is desirable that is being subjected to certain high temperature to the progress EBSD observation of this process with study sample
The development law of undertissue, this research has very important realistic meaning, for example answers if can understand material under high temperature
Become rule, can steel design and process in by organization of regulation control come the coping behavior of controlled material, make steel certain
At a temperature of can also keep certain intensity and plasticity, be of great significance to the safety of the mankind, the safety of equipment.
But current scanning electron microscope cannot achieve this research, because EBSD is mounted in one in scanning electron microscope
A component, current scanning electron microscope cannot achieve the EBSD home position observation under drawing by high temperature.If it is desired under observation specific condition such as
The deformation and its differentiation of the material of (100~1200 DEG C) under specific temperature, it is necessary to such as there is stretch function by other equipment
High temperature Laser Scanning Confocal Microscope realize.And the existing main problem of high-temp in-situ stretching at present is as follows:
(1) the size limitation of laboratory sample:
The thickness range of laboratory sample requires to be 1.2mm~2mm, and existing tensile sample scale diagrams are as shown in figure 3, big
In 2mm, the stretching experiment less than 1.2mm can not be observed.The reason is as follows that:
The fixed sample end of equipment is U-shaped folder head, full-size is 2mm between collet, and therefore, the most thick 2mm that can only sandwich is thick
Laboratory sample.
Objective lens used in high temperature observation are routinely 20 times of camera lenses, and image-forming range 22.5mm, focal length is up to
0.8 mm, super go beyond the scope just exceed the maximum focal length of object lens, can not blur-free imaging.Carrying out high temperature, room temperature original position stretching
In experimentation, with the progress of stretching, sample parallel-segment is elongated along Impact direction, while thickness is thinned, when sample surfaces arrive
After the distance of camera lens exceeds 0.8mm range, object lens will be unable to blur-free imaging, therefore the sample minimum thickness of equipment requirement cannot be small
In 1.2mm.
As shown in figure 4, as seen from the figure, experiment steel is being drawn for the real-time micro-organization chart of sample drawing process in the prior art
Constriction, height of specimen decline occur for sample during stretching, and height of specimen is lower than the maximum imaging focal plane of objective lens, leads to sample
Product can not blur-free imaging, stretcher strain details is smudgy.And fuzzy region is the position of this experiment actual needs observation, because
Equipment design cause experimentation can not all-the-way tracking, significantly limit the application of equipment.
(2) thermocouple is fixed difficult, and temperature control precision is unstable
When carrying out tensile test at high temperature, for the surface temperature of real-time monitoring sample, by thermo-electric metal piece with resistance to
The fine wire of high temperature is bundled in the back side of sample parallel-segment, in the prior art thermocouple and sample connection schematic diagram such as Fig. 5 (a)
With shown in 5 (b)；But there are the following problems for operation in this way:
I. it is easy the observation surface contamination that sample is polished；
If the ii. thin wire material non-refractory of binding thermocouple used, be easy during tensile test at high temperature and
Thermocouple is melted together, and therefore, it is necessary to extra purchase high temperature resistant thin wire or other high temperature resistant filament materials, increases experiment
Cost and risk；
Iii. because thermocouple and sample are to be linked together by iron wire, and thermocouple plate makes because multiple, duplicate
With, surface irregularity, the case where causing thermocouple and sample surfaces that poor contact is locally present, temperature control precision is unstable
It is fixed.
(3) high temperature observation can not be carried out to film sample, steel wire class sample.Because the limitation that equipment itself designs, leads
Sample design can only can not be fixed in furnace body wire sample at sample shape as shown in Figure 2 by cause, therefore nothing
Method carries out tensile test at high temperature research.And it is directed to film-form sample, it is ultra-thin and can not process because thickness is generally in 0.1mm or so
The shape and size that forming apparatus requires, therefore also it is unable to complete tensile test at high temperature observation.
Summary of the invention:
The purpose of the present invention is overcoming above-mentioned the shortcomings of the prior art, a kind of material strain original position EBSD observation is provided
Test fixture and the test method, cooperate the stretching module of laser confocal microscope, while can be by fixture and sample together
It is put into scanning electron microscope, scanning electron microscopic observation and the synchronous progress of EBSD home position observation is realized, two experimental facilities is organically combined
Come, perfectly solves the EBSD observation problem in situ of room temperature, high temperature tension test.
To achieve the above object, the invention adopts the following technical scheme:
A kind of material strain original position EBSD observation test fixture, for clamping thin slice/membranous metal sample or wire
Sample, including collet, clamping fixture and positioning bolt, in which:
The collet is U-shaped folder head, and the U-shaped folder head clamping end surfaces are equipped with circular hole, for fixing with clamping fixture；
The clamping fixture includes upper fixture and lower fixture, and the upper fixture includes upper fixture clamping end, described
Upper fixture clamps end surfaces and is equipped with circular hole, and the upper fixture center is equipped with rectangular observation panel, for carrying out sample observation；
The lower fixture specifically includes lower fixture clamping end and lower fixture parallel-segment, under described for placing sample
Fixture clamps end surfaces and is equipped with circular hole；
The U-shaped folder head clamps end surfaces circular hole, and upper fixture clamps end surfaces circular hole and lower fixture clamping end surfaces circle
Hole aperture is consistent, after the upper fixture and lower fixture clamping sample, using positioning bolt, is fixed by circular hole and collet,
In:
When the material strain original position EBSD observation test fixture clamping wire sample, the lower fixture is flat
Row section both ends are equipped with wire sample fixed end, are fastened for wire sample.
The thin slice/membranous metal sample thickness is 0.01~5mm.
The U-shaped folder head width of rebate is 5mm.
For the upper fixture with a thickness of 1-2mm, lower jaw thickness is 1-2mm.
The U-shaped folder head is equipped with collet or gasket so that collet size be suitable for thickness range 0.01~5mm to
Test specimens are fixed.
The collet or gasket material is No. 45 steel.
The collet tail end is that cylindric, described cylindric tail end is arranged for screw thread, is used for and experimental rig carries out
Tighten fixation.
The clamping fixture is in use, pass through upper fixture and the fitting of lower fixture, specially upper fixture clamping end and lower folder
Have clamping end fitting, makes sample to be tested is firm to fix.
The lower fixture parallel-segment midpoint is equipped with thermocouple slot, and for placing thermocouple, the slot is deep
Degree≤thermoelectricity dual thickness, after guaranteeing that sample is fixed, thermocouple comes into full contact with sample, carries out temperature measurement, and protect sample
Water holding placing flat is convenient for sample observation.
The upper fixture observation panel two sides are equipped with scale, form graduated scale, including scale starting point and scale terminal,
In sample drawing process, the graduated scale horizontally slips as sample stretches, size observation, survey when stretching for sample
Amount and positioning, wherein the two sides graduated scale scale is oppositely arranged, i.e. side graduated scale scale starting point and opposite scale
Ruler scale terminal is corresponding.
The upper fixture and lower fixture are equipped with cut-off point, carry out stretched operation convenient for sample.
The upper fixture cut-off point is arranged in scale final position.
The lower fixture cut-off point is arranged in parallel segment length one third position.
A kind of material strain original position EBSD observation test method, using above-mentioned fixture, specifically includes the following steps:
Step 1, sample is installed:
(1) it opens and is copolymerized burnt microexamination equipment, and after confirming stretching furnace non-vacuum, open bell, sample is installed,
Wherein:
When for thin sheet film sample: the positioning bolt at left and right sides of specimen holder being unclamped, sheet metal specimens are put into fixture
In, after being adjusted to optimum position, the positioning bolt of the left and right sides is tightened, fixture is put into stretching furnace sample storehouse, sample installation
It finishes.
When for wire sample: the positioning bolt at left and right sides of specimen holder being unclamped, by wire sample or so two
Side is respectively wound around the wire sample fixed end of specimen holder, completes wire sample and fixes；
(2) thermocouple plate fitting is set to specimen surface；
(3) stretching module of specimen holder and stretching furnace is connected:
(4) drive rod bolt on the left of collet tail end on the left of specimen holder and stretching furnace is tightened into fixation, by a clamping fixture left side
Side is protruded on the left of specimen holder in U-shaped folder head, and positioning bolt is inserted into, and is completed fixed on the left of sample；
(5) left side fixture is moved in stretching furnace, and will be driven on the right side of collet tail end on the right side of specimen holder and stretching furnace
Bar bolt tightens fixation, will be protruded on the right side of specimen holder in U-shaped folder head on the right side of clamping fixture, is inserted into positioning bolt, adjusting sample
After level, screwed in place bolt is completed to fix on the right side of sample, adjusts sample position in furnace, be in sample among observation window
Position, sample are installed；
Step 2, sample is stretched observes with EBSD:
(1) loading force and displacement are zeroed by Compression and Expansion controller, and input the loading force range that experiment needs
And the experiment parameters such as loading speed；
(2) bell is covered, guarantees leakproofness, opens gas control unit, opens inert gas passage control valve, is taken out true
Sky, is passed through inert gas, vacuumizes be passed through operation with inert gas repeatedly for three times, guarantees the intracorporal degree of purity of experimental furnace；
(3) experimental arrangement is worked out, starts to test；Observe drawing process in sample localized variation, treat viewing area into
Row positioning is imaged with stretching；
(4) after testing, the fixture with tensile sample is taken out；
(5) it will be put on sample platform of scanning electronic microscope with the fixture of tensile sample, vert after 70 degree, EBSD probe is protruded into
In sample bin；
(6) sample region to be seen is found, electron beam is treated into observation experiment area and is scanned, generates EBSD observation figure
Picture；
(7) after scanning electron microscope Germicidal efficacy, the fixture with tensile sample is taken out, laser co-focusing is placed again into
In microscope stretching furnace, the left and right center that even wall bar makes sample be located at om observation window is adjusted；
(8) it determines Experimental Area, stretches certain ratio again, repeat 4-8 experimental procedure, measure different elongation percentage respectively
The strained situation of the identical structure (same position) of lower material；
(9) experiment terminates, and is arranged and is analyzed to experimental result, and material strain original position EBSD observation test is completed.
In the step 1 (2), the specific modes of emplacement of thermocouple plate are as follows: thermocouple plate is inserted into thermocouple slot, adjustment
Position guarantees that thermocouple plate uniformly contacts sample, so that thermocouple plate real-time and accurate measurement specimen temperature.
In the step 2 (3), by the graduated scale of specimen holder treat viewing area carry out positioning with stretch imaging.
In the step 2 (6), the localization region of previewing when stretching observation is found by the graduated scale of specimen holder,
Carry out EBSD scanning imagery.
In the step 2 (8), the area of the sample for needing to observe is found by the graduated scale of specimen holder, is scanned
Imaging.
Beneficial effects of the present invention:
(1) material strain original position EBSD of the invention observation test fixture is designed using hollow round hole, overcomes stretching
The problem of constriction causes camera lens that can not capture sample deformation in the process, can small range clearly observe drawing process crack propagation, disconnected
It splits the in situ of equal behaviors and overall process occurs.
(2) material strain original position EBSD of the invention observation test fixture is specifically for spies such as thin sheet film sample, steel wires
The laboratory holder of different sample carry out thin sheet film, the experiment of wire sample correlation home position observation can smoothly.
(3) the material strain original position EBSD observation test fixture invented is equipped with scale: separately designing quarter in fixture two sides
Ruler is spent, with the progress of drawing process, side is mobile to left and right for graduated scale, captures, can be stretched in real time by objective lens
The length variation of sample in the process, measurement is more accurate, and the function is more significant to film sample, which also has fixed
Position function, can assistant experiment sample carry out the Germicidal efficacy that subsequent EBSD etc. needs record position.
(4) it is tested using EBSD observation test fixture in material strain original position of the invention, can be realized sample chamber
The home position observation of temperature and the EBSD of drawing by high temperature process；And the success rate of experiment and the utilization rate of equipment are improved, and widen
The use scope of equipment.
Experimental method of the invention devises ultra-thin sample, the room temperature of film sample and wire sample and high temperature and sees
It examines and uses fixture, which has the variation of sample real time length in simple to operation, recordable drawing process, can be to sample position
The function of being recorded organically combines laser confocal microscope and scanning electron microscope, realizes drawing process EBSD
Home position observation experimental program, the application and EBSD for greatly expanding room temperature and drawing by high temperature module solve original position stretching
Problem.
Detailed description of the invention:
Fig. 1 is that the material strain original position EBSD of embodiment 1 observes test fixture structural schematic diagram, and Fig. 1 (a) is that fixture is whole
Body structural schematic diagram (b) is fixture main view；
Fig. 2 is that the material strain original position EBSD of embodiment 2 observes test fixture structural schematic diagram, and Fig. 2 (a) is that fixture is whole
Body structural schematic diagram (b) is upper fixture structural schematic diagram, (c) is lower clamp structure schematic diagram；
Wherein, 1-U type collet, 2- positioning bolt, 3-1 thin sheet of metal sample, 3-2 wire sample, 4- graduated scale, on 5-
Fixture, fixture under 6-, 7 thermocouple slots, 8- gasket, 9- wire sample fixed end；
Fig. 3 is the tensile sample scale diagrams used in the prior art；
Fig. 4 is the real-time micro-organization chart of sample drawing process in the prior art；As seen from the figure, steel is tested during stretching
Constriction, specimen height decline occur for sample, and specimen height is lower than the maximum imaging focal plane of objective lens, causes sample clear
Clear imaging, stretcher strain details is smudgy；
Fig. 5 is thermocouple in the prior art and sample connection schematic diagram；
Fig. 6 is the room temperature confocal microscopy view in embodiment 1 under sample different stretch deflection, in which: (a) stretcher strain
Amount is 10%, and (b) stretcher strain amount is 20%, and (c) stretcher strain amount is 30%, and (d) stretcher strain amount is 40%；
Fig. 7 is EBSD (KAM) figure in embodiment 2 under sample high temperature after different distortion amount, wherein Fig. 7 (a) deflection is
KAM distribution map under 10% EBSD in situ, Fig. 7 (b) deflection are KAM distribution map under 20% EBSD in situ, Fig. 7 (c) deformation
Amount is KAM distribution map under 30% EBSD in situ, KAM distribution map under the EBSD in situ that Fig. 7 (d) deflection is 40%；
Specific embodiment:
Below with reference to embodiment, the present invention is described in further detail.
Embodiment 1
A kind of material strain original position EBSD observation test fixture, shown in overall structure diagram such as Fig. 1 (a), main view
Figure is as shown in Fig. 1 (b), for clamping thin slice/membranous metal sample, including U-shaped folder head 1, clamping fixture and positioning bolt 2,
In:
The U-shaped folder head 1 clamps end surfaces and is equipped with circular hole, for fixing with clamping fixture；
The clamping fixture includes upper fixture 5 and lower fixture 6, and the upper fixture 5 includes 5 clamping end of upper fixture, institute
The upper fixture 5 stated clamps end surfaces and is equipped with circular hole, and 5 center of upper fixture is equipped with rectangular observation panel, for carrying out sample sight
It examines；
The lower fixture 6 is used to place sample, specifically includes lower 6 clamping end of fixture and lower 6 parallel-segment of fixture, described
Lower fixture 6 clamps end surfaces and is equipped with circular hole；
The U-shaped folder head 1 clamps end surfaces circular hole, and upper fixture 5 clamps end surfaces circular hole and lower fixture 6 clamps end surfaces
Circular hole aperture is consistent, after the upper fixture 5 and lower fixture 6 clamping sample, is clamped by 5 clamping end of upper fixture and lower fixture 6
End fitting, using positioning bolt 2, is fixed by circular hole and collet, makes sample to be tested is firm to fix；
The present embodiment is taken from potassium steel hot rolled steel plate, sample thickness 0.8mm, sample overall length Lt=using sample
57mm, distance Lr=42mm between the two pin hole centers of circle, the parallel segment length Lc=27mm of sample, distance Lr=between the two pin hole centers of circle
42mm sample parallel-segment width b=2, clamping end width B=15mm, clamping end pin hole diameter is D=5mm, transition arc radius
R=5mm；
1 width of rebate of U-shaped folder head is 5mm；
The upper fixture 5 is with a thickness of 1.5mm, and lower fixture 6 is with a thickness of 1.5mm；
The U-shaped folder head 1 is equipped with No. 45 steel plate washers 8, fixes so that sample is firm；
The collet tail end is that cylindric, described cylindric tail end is arranged for screw thread, is used for and experimental rig carries out
Tighten fixation；
The 6 parallel-segment midpoint of lower fixture is equipped with thermocouple slot 7, for placing thermocouple, the slot
Depth≤thermoelectricity dual thickness, after guaranteeing that sample is fixed, thermocouple comes into full contact with sample, carries out temperature measurement, and make sample
It keeps horizontal positioned, is convenient for sample observation；
The 5 observation panel two sides of upper fixture are equipped with scale, form graduated scale 4, including scale starting point and scale end
Point, in sample drawing process, the graduated scale 4 horizontally slips as sample stretches, and size when stretching for sample is seen
It examines, measure and positioning, wherein it is oppositely arranged, i.e. 4 scale starting point of side graduated scale and opposite that ruler scale is drawn in the two sides
4 scale terminal of graduated scale is corresponding；
The upper fixture 5 and lower fixture 6 are equipped with cut-off point, carry out stretched operation convenient for sample, wherein upper fixture 5
Cut-off point is arranged in scale final position；Lower 6 cut-off point of fixture is arranged in parallel segment length one third position.
A kind of material strain original position EBSD observation test method, using above-mentioned fixture, specifically includes the following steps:
Before experiment, the viewing surface of tensile sample is ground and mechanically polished one by one using abrasive paper for metallograph, it later will examination
Sample is placed in alcohol, clean using cleaned by ultrasonic vibration and be dried, will before testing since experimental temperature is room temperature
Viewing surface has carried out electrobrightening to show its microscopic structure.
Step 1, sample is installed:
(1) it opens and is copolymerized burnt microexamination equipment, and after confirming stretching furnace non-vacuum, bell is opened, by specimen holder
The positioning bolt 2 of the tool left and right sides unclamps, and sheet metal specimens fixture is put into stretching furnace sample storehouse, after being adjusted to optimum position,
The positioning bolt 2 of the left and right sides is tightened, sample installs；
2) thermocouple plate is inserted into thermocouple slot 7, adjusts position, guarantee that thermocouple plate uniformly contacts sample, so that hot
Galvanic couple piece real-time and accurate measurement specimen temperature；
(3) stretching module of specimen holder and stretching furnace is connected:
Drive rod bolt on the left of collet tail end on the left of specimen holder and stretching furnace is tightened into fixation, will be stretched on the left of clamping fixture
Enter on the left of specimen holder in U-shaped folder head 1, be inserted into positioning bolt 2, completes fixed on the left of sample；
Left side fixture is moved in stretching furnace, and by drive rod spiral shell on the right side of collet tail end on the right side of specimen holder and stretching furnace
Bolt tightens fixation, will be protruded on the right side of specimen holder in U-shaped folder head 1 on the right side of clamping fixture, is inserted into positioning bolt 2, adjusting sample water
After flat, screwed in place bolt 2 is completed to fix on the right side of sample, adjusts sample position in furnace, sample is made to be in observation window interposition
It sets, sample is installed；
Step 2, sample is stretched observes with EBSD:
(1) loading force and displacement are zeroed by Compression and Expansion controller, and input the loading force range that experiment needs
And the experiment parameters such as loading speed；
(2) bell is covered, guarantees leakproofness, opens gas control unit, opens inert gas passage control valve, is taken out true
Sky, is passed through inert gas, vacuumizes be passed through operation with inert gas repeatedly for three times, guarantees the intracorporal degree of purity of experimental furnace；
(3) experimental arrangement is worked out, room temperature tensile is carried out with the rate of extension of 2mm/min, starts to test；Observe drawing process
The localized variation of middle sample, by the graduated scale 4 of specimen holder treat viewing area carry out positioning with stretch imaging；
(4) after testing, after waiting in-furnace temperature to be reduced to room temperature, the fixture with tensile sample is taken out；
(5) it will be put on sample platform of scanning electronic microscope with the fixture of tensile sample, vert after 70 degree, EBSD probe is protruded into
In sample bin；
(6) interested localization region when stretching is observed is found by the graduated scale 4 of specimen holder, electron beam is treated into sight
It examines test block to be scanned, generates EBSD and observe image；
(7) after scanning electron microscope Germicidal efficacy, the fixture with tensile sample is taken out, laser co-focusing is placed again into
In microscope stretching furnace, the left and right center that even wall bar makes sample be located at om observation window is adjusted；
(8) by graduated scale 4, the Experimental Area that need to be observed is found, stretches certain ratio again, repeats 4-8 experiment step
Suddenly, the strain feelings of the identical structure of material (same position) under 10%, 20%, 30% and 40% different elongation percentage are measured respectively
Condition；
(9) experiment terminates, and is arranged and is analyzed to experimental result, completes material strain original position EBSD observation test, no
With the room temperature confocal microscopy view under stretcher strain amount as shown in fig. 6, specially materials microstructure deforms schematic diagram, wherein Fig. 6
(a) stretcher strain amount is 10%；Fig. 6 (b) stretcher strain amount is that 20%, Fig. 6 (c) stretcher strain amount is that 30%, Fig. 6 (d) is stretched
Deflection is 40%, by the micrograph to potassium steel room temperature tensile process it has been observed that experiment structure of steel is single austenite
Tissue, as shown in Fig. 6 (a)；Since austenite stacking fault energy is lower, be also easy to produce fault, thus observe in austenite crystal there is
A large amount of twins, during stretching, when sample institute's tension stress is greater than yield strength, and obvious plastic deformation takes place, crystal grain
Inside starts the Zona transformans for occurring significantly being parallel to each other, as shown in white circle part in Fig. 6 (b), Fig. 6 (c) and Fig. 6 (d)
Display: with continuing for drawing process, sample deformation degree is increasing, and Zona transformans is also more and more, big and deep change
Shape band is more and more significant, and the Zona transformans direction generated in different crystal grain is different, but substantially all at 45 ° point of tensile stress direction
Cloth.
Embodiment 2
A kind of material strain original position EBSD observation test fixture, overall structure diagram such as Fig. 2 (a) is shown, is used for
Clamp wire sample, including U-shaped folder head 1, clamping fixture and positioning bolt 2, in which:
The U-shaped folder head 1 clamps end surfaces and is equipped with circular hole, for fixing with clamping fixture；
The clamping fixture includes upper fixture 5 and lower fixture 6, shown in 5 structural schematic diagram of upper fixture such as Fig. 2 (b), lower folder
Have shown in 6 structural schematic diagrams such as Fig. 2 (c), the upper fixture 5 includes 5 clamping end of upper fixture, 5 clamping end of upper fixture
Surface is equipped with circular hole, and 5 center of upper fixture is equipped with rectangular observation panel, for carrying out sample observation；
The lower fixture 6 is used to place sample, specifically includes lower 6 clamping end of fixture and lower 6 parallel-segment of fixture, described
Lower fixture 6 clamps end surfaces and is equipped with circular hole, and the 6 parallel-segment both ends of lower fixture are equipped with wire sample fixed end 9, are used for
Wire sample is fastened；
The U-shaped folder head 1 clamps end surfaces circular hole, and upper fixture 5 clamps end surfaces circular hole and lower fixture 6 clamps end surfaces
Circular hole aperture is consistent, after the upper fixture 5 and lower fixture 6 clamping sample, is clamped by 5 clamping end of upper fixture and lower fixture 6
End fitting, using positioning bolt 2, is fixed by circular hole and collet, makes sample to be tested is firm to fix；
The present embodiment is taken from trip590 cold rolling wire, steel wire diameter 2.3mm using sample；
1 width of rebate of U-shaped folder head is 5mm；
The upper fixture 5 is with a thickness of 1.5mm, and lower fixture 6 is with a thickness of 1.5mm；
The U-shaped folder head 1 is equipped with No. 45 steel plate washers, fixes so that sample is firm；
The collet tail end is that cylindric, described cylindric tail end is arranged for screw thread, is used for and experimental rig carries out
Tighten fixation；
The 6 parallel-segment midpoint of lower fixture is equipped with thermocouple slot 7, for placing thermocouple, the slot
Depth≤thermoelectricity dual thickness, after guaranteeing that sample is fixed, thermocouple comes into full contact with sample, carries out temperature measurement, and make sample
It keeps horizontal positioned, is convenient for sample observation；
The 5 observation panel two sides of upper fixture are equipped with scale, form graduated scale 4, including scale starting point and scale end
Point, in sample drawing process, the graduated scale 4 horizontally slips as sample stretches, and size when stretching for sample is seen
It examines, measure and positioning, wherein it is oppositely arranged, i.e. 4 scale starting point of side graduated scale and opposite that ruler scale is drawn in the two sides
4 scale terminal of graduated scale is corresponding；
The upper fixture 5 and lower fixture 6 are equipped with cut-off point, carry out stretched operation convenient for sample, wherein upper fixture 5
Cut-off point is arranged in scale final position；Lower 6 cut-off point of fixture is arranged in parallel segment length one third position.
A kind of material strain original position EBSD observation test method, using above-mentioned fixture, specifically includes the following steps:
The viewing surface of tensile sample is ground and mechanically polished one by one using abrasive paper for metallograph before experiment, later by sample
It is placed in alcohol clean using cleaned by ultrasonic vibration and is dried；
Step 1, sample is installed:
(1) it opens high temperature and is copolymerized burnt microexamination equipment, and after confirming high temperature furnace non-vacuum, open bell, will try
Positioning bolt 2 at left and right sides of sample fixture unclamps, and the wire of specimen holder will be respectively wound around at left and right sides of wire sample
Sample fixed end is completed wire sample and is fixed；
2) thermocouple plate is inserted into thermocouple slot 7, adjusts position, guarantee that thermocouple plate uniformly contacts sample, so that hot
Galvanic couple piece real-time and accurate measurement specimen temperature.
(3) specimen holder is connect with the stretching module of drawing by high temperature furnace:
Drive rod bolt on the left of collet tail end on the left of specimen holder and drawing by high temperature furnace is tightened into fixation, by a clamping fixture left side
Side is protruded on the left of specimen holder in U-shaped folder head 1, and positioning bolt 2 is inserted into, and is completed fixed on the left of sample；
Left side fixture is moved in high temperature furnace, and will be driven on the right side of collet tail end on the right side of specimen holder and drawing by high temperature furnace
Bar bolt tightens fixation, will be protruded on the right side of specimen holder in U-shaped folder head 1 on the right side of clamping fixture, is inserted into positioning bolt 2, adjusts examination
After sample is horizontal, screwed in place bolt 2 is completed to fix on the right side of sample, adjusts sample position in furnace, be in sample in observation window
Between position, sample is installed；
Step 2, sample drawing by high temperature and EBSD are observed:
(1) loading force and displacement are zeroed by Compression and Expansion controller, and input the loading force range that experiment needs
And the experiment parameters such as loading speed；
(2) bell is covered, guarantees leakproofness, opens gas control unit, opens inert gas passage control valve, is taken out true
Sky, is passed through inert gas, vacuumizes be passed through operation with inert gas repeatedly for three times, guarantees the intracorporal degree of purity of experimental furnace；
(3) experimental arrangement to be worked out, starts to test, drawing by high temperature is carried out with the rate of extension of 2mm/min, temperature is 300 DEG C,
Stretcher strain amount is 10%, observes the localized variation of sample in drawing process, treats observation area by the graduated scale 4 of specimen holder
Domain carries out positioning and is imaged with high temperature；
(4) after testing, after waiting in-furnace temperature to be reduced to room temperature, the fixture with tensile sample is taken out；
(5) it will be put on sample platform of scanning electronic microscope with the fixture of tensile sample, vert after 70 degree, EBSD probe is protruded into
In sample bin；
(6) interested localization region when high temperature observation is found by the graduated scale 4 of specimen holder, electron beam is treated into sight
It examines test block to be scanned, generates EBSD and observe image；
(7) after scanning electron microscope Germicidal efficacy, the fixture with tensile sample is taken out, it is total to be placed again into high-temperature laser
In focusing microscope stretching furnace, the left and right center that even wall bar makes sample be located at om observation window is adjusted；
(8) by graduated scale 4, the Experimental Area that need to be observed is found, stretches certain ratio again, repeats 4-8 experiment step
Suddenly, respectively measurement stretcher strain amount be 10%, 20%, 30% with 40% material identical structure (same position) strained situation；
Measurement result is as follows:
Black line-big angle crystal boundary in Fig. 7, shade indicate deformation extent size.KAM figure is commonly used to disclose local position
The case where wrong (local misorientation) and strain energy (strain energy), as in some crystal grain of qualitative analysis
The orientation change of gradient in portion, as dependent variable is increased to 40% by 10%, KAM distribution map under the EBSD in situ that deflection is 10%
As shown in Fig. 7 (a), KAM distribution map such as Fig. 7 (b) is shown under the EBSD in situ that deflection is 20%, the original position that deflection is 30%
Under EBSD shown in KAM distribution map such as Fig. 7 (c), under the EBSD in situ that deflection is 40% shown in KAM distribution map such as Fig. 7 (d), by
, as it can be seen that deformation extent constantly increases, the orientation change of gradient of intra-die gradually increases for this, and concentrates on crystal boundary area or lean on smectic
Battery limit (BL) domain；
(9) experiment terminates, and is arranged and is analyzed to experimental result, and material strain original position EBSD observation test is completed.
Claims (6)
1. a kind of material strain original position EBSD observes test fixture, which is characterized in that for clamping thin slice/membranous metal sample
Or wire sample, including collet, clamping fixture and positioning bolt, in which:
The collet is U-shaped folder head, and the U-shaped folder head clamping end surfaces are equipped with circular hole, for fixing with clamping fixture；
The clamping fixture includes upper fixture and lower fixture, and the upper fixture includes upper fixture clamping end, the upper folder
Tool clamping end surfaces are equipped with circular hole, and the upper fixture center is equipped with rectangular observation panel, for carrying out sample observation；
The lower fixture specifically includes lower fixture clamping end and lower fixture parallel-segment, the lower fixture for placing sample
It clamps end surfaces and is equipped with circular hole；
The U-shaped folder head clamps end surfaces circular hole, and upper fixture clamps end surfaces circular hole and lower fixture clamps end surfaces circular hole hole
Diameter is consistent, after the upper fixture and lower fixture clamping sample, using positioning bolt, is fixed by circular hole and collet, in which:
When the material strain original position EBSD observation test fixture clamping wire sample, the lower fixture parallel-segment
Both ends are equipped with wire sample fixed end, are fastened for wire sample.
2. a kind of material strain original position EBSD according to claim 1 observes test fixture, which is characterized in that described
Thin slice/membranous metal sample thickness is 0.01~5mm.
3. a kind of material strain original position EBSD according to claim 1 observes test fixture, which is characterized in that described
Collet tail end is that cylindric, described cylindric tail end is arranged for screw thread, tightens fixation for carrying out with experimental rig.
4. a kind of material strain original position EBSD according to claim 1 observes test fixture, which is characterized in that described
Lower fixture parallel-segment midpoint is equipped with thermocouple slot, for placing thermocouple, the socket depth≤thermoelectricity dual thickness,
After guaranteeing that sample is fixed, thermocouple comes into full contact with sample, carries out temperature measurement, and sample is made to keep horizontal positioned, is convenient for
Carry out sample observation.
5. a kind of material strain original position EBSD according to claim 1 observes test fixture, which is characterized in that described
Upper fixture observation panel two sides are equipped with scale, form graduated scale, including scale starting point and scale terminal, sample drawing process
In, the graduated scale horizontally slips as sample stretches, size observation, measurement and positioning when stretching for sample,
In, the two sides graduated scale scale is oppositely arranged, i.e. side graduated scale scale starting point and opposite graduated scale scale terminal
It is corresponding.
6. a kind of material strain original position EBSD observes test method, using fixture described in claim 1, which is characterized in that tool
Body the following steps are included:
Step 1, sample is installed:
(1) it opens and is copolymerized burnt microexamination equipment, and after confirming stretching furnace non-vacuum, open bell, sample is installed,
In:
When for thin sheet film sample: the positioning bolt at left and right sides of specimen holder being unclamped, sheet metal specimens fixture is put into drawing
Furnace sample storehouse is stretched, after being adjusted to optimum position, tightens the positioning bolt of the left and right sides, sample installs；
When for wire sample: the positioning bolt at left and right sides of specimen holder being unclamped, by left and right sides of wire sample points
It is not wrapped in the wire sample fixed end of specimen holder, completes wire sample and fixes；
(2) thermocouple plate fitting is set to specimen surface；
(3) stretching module of specimen holder and stretching furnace is connected:
(4) drive rod bolt on the left of collet tail end on the left of specimen holder and stretching furnace is tightened into fixation, will be stretched on the left of clamping fixture
Enter on the left of specimen holder in U-shaped folder head, be inserted into positioning bolt, completes fixed on the left of sample；
(5) left side fixture is moved in stretching furnace, and by drive rod spiral shell on the right side of collet tail end on the right side of specimen holder and stretching furnace
Bolt tightens fixation, will protrude on the right side of clamping fixture on the right side of specimen holder in U-shaped folder head, is inserted into positioning bolt, and adjusting sample is horizontal
Afterwards, screwed in place bolt is completed to fix on the right side of sample, adjusts sample position in furnace, sample is made to be in observation window middle position,
Sample is installed；
Step 2, sample is stretched observes with EBSD:
(1) loading force and displacement are zeroed by Compression and Expansion controller, and input loading force range and add that experiment needs
Carry the experiment parameters such as rate；
(2) bell is covered, guarantees leakproofness, opens gas control unit, inert gas passage control valve is opened, vacuumizes, is led to
Enter inert gas, vacuumize be passed through operation with inert gas repeatedly for three times, guarantees the intracorporal degree of purity of experimental furnace；
(3) experimental arrangement is worked out, starts to test；The localized variation for observing sample in drawing process, treats viewing area and is determined
Position is imaged with stretching；
(4) after testing, the fixture with tensile sample is taken out；
(5) it will be put on sample platform of scanning electronic microscope with the fixture of tensile sample, vert after 70 degree, EBSD probe is protruded into sample
In storehouse；
(6) sample region to be seen is found, electron beam is treated into observation experiment area and is scanned, EBSD is generated and observes image；
(7) after scanning electron microscope Germicidal efficacy, the fixture with tensile sample is taken out, it is micro- to be placed again into laser co-focusing
In mirror stretching furnace, the left and right center that even wall bar makes sample be located at om observation window is adjusted；
(8) it determines Experimental Area, stretches certain ratio again, repeat 4-8 experimental procedure, measure material under different elongation percentage respectively
Expect the strained situation of same position；
(9) experiment terminates, and is arranged and is analyzed to experimental result, and material strain original position EBSD observation test is completed.
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| CN110823678A (en) * | 2019-11-25 | 2020-02-21 | 北京北冶功能材料有限公司 | High-temperature tensile test device and method for metal filaments |
| CN110954563A (en) * | 2019-12-10 | 2020-04-03 | 北京航空航天大学 | Device and method for in-situ observation of rheological behavior of semi-solid metal alloy |
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| CN112359182B (en) * | 2020-11-09 | 2021-08-20 | 燕山大学 | Make things convenient for high temperature singly to draw sample quenching treatment's anchor clamps |
| CN112359182A (en) * | 2020-11-09 | 2021-02-12 | 燕山大学 | Make things convenient for high temperature singly to draw sample quenching treatment's anchor clamps |
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| CN114062135A (en) * | 2021-11-16 | 2022-02-18 | 武汉工程大学 | Rock strain data correction method of high-temperature triaxial testing machine |
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| CN115266423A (en) * | 2022-08-10 | 2022-11-01 | 哈尔滨工业大学 | Penetration test device |
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