CN106840852B - A kind of more atmosphere in situ environment stress gauges of modularization wide temperature range - Google Patents
A kind of more atmosphere in situ environment stress gauges of modularization wide temperature range Download PDFInfo
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- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
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Abstract
A kind of more atmosphere in situ environment stress gauges of modularization wide temperature range, including Mechanical loading module, alternating temperature module, optical imagery and locating module, atmosphere module and sensing system, the deformeter can switch high temperature refrigerated module and realize mechanical test under wide temperature range extreme temperature, it can be passed through different atmosphere in sealing shell and realize uniaxial in-situ mechanical test under more atmospheres, can realize displacement measurement, temperature measurement and mechanical meaurement immediately.The deformeter has modularization mainly for synchrotron radiation in-situ mechanical experimental design, and wide temperature range, multi-environment, multi- scenarios method carry out the characteristics of mechanics, displacement, temperature measurement and feedback immediately.
Description
Technical field
The present invention relates to fields of measurement, and in particular to a kind of more atmosphere in situ environment stress gauges of modularization wide temperature range, it can be with
Switch high temperature refrigerated module and realize mechanical test under wide temperature range extreme temperature, different atmosphere realization can be passed through in sealing shell
Uniaxial in-situ mechanical test under more atmospheres, can realize displacement measurement, temperature measurement and mechanical meaurement immediately.This is answered
Become instrument mainly for synchrotron radiation and electron microscope in-situ mechanical experimental design, there is modularization, it is wide temperature range, multi-environment, more
Field coupling carries out the characteristics of mechanics, displacement, temperature measurement and feedback immediately.
Background technique
The physical and chemical performance of atoms outermost electronics structure substantial connection material, and change atom by applying elastic strain
Between distance influence outer electronic structure again, therewith, realize the change to the physics, chemical property of material.Therefore, by applying bullet
Property strain for the physics of controllable, reversible, quantitative controlled material, chemical property provide new approaches, i.e., so-called " elastic strain
Engineering ", and elastic strain engineering further investigate essential in-situ mechanical loading equipemtn and realize to apply elastic strain
The correlated performance of material is monitored simultaneously.
On the other hand, the Service Environment of material is diversified, including hot environment, low temperature environment, dry environment, wet
Environment, by stress, be powered etc. including, if it is desired to the military service behavior of research material under these circumstances, it is necessary to test
In give material similar experiment condition, additionally need microscopy apparatus to material microstructure to provide grinding in terms of mechanism
Study carefully.Therefore, the additional characterization equipment of the experimental facilities in situ of multi-environment multi- scenarios method is the necessary condition of investigation of materials.
In addition, the means for being conventionally used to characterization microstructure have transmission electron microscope (TEM) for microscopy apparatus, pass
The X-ray diffraction (XRD) of system, electron backscatter diffraction (EBSD), neutron diffraction etc..If it is intended to accurately obtaining microcosmic in material
Structure, including crystal orientation, defect, twin etc., it is necessary to very high spatial resolution is right in intra-die range scale
Defect is characterized and is identified.Obviously, the resolution ratio of neutron diffraction and traditional XRD cannot be met the requirements, although TEM resolution ratio
Very high but efficiency is very low, and it is extremely difficult to obtain the defects of a wide range of distribution.The spatial resolution of EBSD very it is high still
It is difficult to quantitatively characterize local Strain Distribution, and very high to sample surfaces requirement, sample preparation is a problem.These set simultaneously
It is standby to need high vacuum environment to be tested, for providing with former Service Environment quite or the experiment condition of target detection is not
Reality.
In view of the limitation of above traditional characterization technique, in recent years, the X-ray microbeam diffraction (μ XRD) based on synchrotron radiation
Technology rapidly develops, spatial resolution and angular resolution respectively reached submicron-scale (M.Kunz, N.Tamura,
K.Chen, et al, Review of Scientific Instruments, 2009) and~0.01 ° (N.Tamura,
A.A.MacDowell, R.S.Celestre, et al., Applied Physics Letters, 2002) rank.For sample
Size, sample (18) surface etc. are also without strict requirements, it is possible to reduce influence factor is introduced in sample making course.Since X is penetrated
Line penetration capacity is stronger than electronics, can carry out nondestructive analysis to some multilayer film heterojunction structures.Synchrotron radiation light source brightness is very high,
Than bright 100,000,000 times of common XRD light source or more, thus enough diffraction informations can be collected within a very short time, have very high
Time and spatial resolution.Since the shape of Laue diffraction spot is very sensitive to the variation of lattice constant, thus to part
The resolution ratio of strain is very high by (~10‐4)(J.D.Budai,W.Yang,N.Tamura,et al.,Nature Materials,
2003), so that the Laue diffraction technology based on synchrotron radiation has very real meaning to the research that material microstructure develops
Justice.But studied currently based on synchrotron radiation X micro-diffractive material, need experimental bench to provide experiment condition, it is instantly existing
Experimental bench only has single warm table and cooling bench, lacks the in-situ mechanical experimental bench that can be realized multi-environment multi- scenarios method.
Summary of the invention
In order to cope with existing deficiency, the purpose of the present invention is to provide a kind of more atmosphere in situ environments of modularization wide temperature range
Stress gauge, the deformeter can switch high temperature refrigerated module and realize mechanical test under wide temperature range extreme temperature, can be closed outer
It is passed through different atmosphere in shell and realizes uniaxial in-situ mechanical test under more atmospheres, can realize that displacement measurement, temperature are surveyed immediately
Amount and mechanical meaurement.The deformeter has a modularization mainly for synchrotron radiation in-situ mechanical experimental design, wide temperature range, more
Environment, multi- scenarios method carry out the characteristics of mechanics, displacement, temperature measurement and feedback immediately.
In order to reach the goals above, the present invention adopts the following technical scheme:
A kind of more atmosphere in situ environment stress gauges of modularization wide temperature range, comprise the following modules: Mechanical loading module: including double
To the pull head 15 arranged in opposite directions, speed-changing gear box 32 and the driving motor 16 of screw rod 4, slide bar 5 and fixed 18 both ends of sample, institute
The contour installation parallel with slide bar 5 of reverse-flighted screw 4 is stated, passes through 15 pedestal 23 of pull head jointly, and both ends are pierced by sealing shell 1 and fix
On sealing shell 1, one end that reverse-flighted screw 4 is pierced by sealing shell 1 passes through shaft coupling and speed-changing gear box 32 and driving electricity
Machine 16 is connected；The pull head 15 is divided into 5 layers of structure, L-type bearing panel 20 including tabletting 26, for carrying tabletting 26,
Alternating temperature module 25, heat insulation layer 24 and pedestal 23, tabletting 26 are fixed on L-type bearing panel 20, are designed using sinking to property, are guaranteed
Upper surface and bearing panel 20 flush, and tabletting 26 maximizes X-ray and electron beam incident angle, bearing panel with a thickness of 1~2mm
20 points are two components, the vertical part 20-2 of the horizontal part 20-1 combined with tabletting 26 and L-type, vertical part and water
Flat component leads to recirculated water by two tooth wedgings at vertical part, horizontal part upper surface fin is reinforced；When sample 18 is thin
Having a size of 10mm*20mm when film sample；When to stretch sample, shape is to stretch sample shape, i.e. intermediate elongated, the flat width in both ends, both ends
For rough surface；The displacement range of the Mechanical loading module is 10mm to 20mm, and precision is 1 μm, can apply strain and be up to
100%, can applied force be 0~1kN；
Alternating temperature module: including temperature feedback system, high-temperature heating module and sub-cooled module, extent of alternating temperature are as follows: low
Warm refrigerating module is liquid nitrogen boiling point to room temperature, and being heated at high temperature module is room temperature to 1000 DEG C；It is heated at high temperature module and sub-cooled
Module is that rectangle plate 28 designs, as limit, the other side when long side side processes two chamferings for being embedded in pull head 15
Limit realized by positioning pin 31；Wherein refrigerated module structure is sandwich structure, fixes coiling by two pieces of metal plates
Copper pipe 27；Refrigerated module connects with external liquid nitrogen, and by valve 9-1 folding by flow control temperature, thermocouple 12 is provided instead
Present model.High temperature module connects with external power supply, and by relay 9-2 control resistance wire heating, thermocouple 12 provides feedback signal；
It is ± 1 DEG C that alternating temperature module, which can control precision,.
Optical imagery and locating module: optical imagery and locating module include visual light imaging and positioning and black light
Imaging and positioning, the visual light imaging and positioning mainly include reflective mirror 30 and microscope 10, and reflective mirror 30 includes difference
The first reflective mirror 30-1 being arranged at angle with horizontal plane α, the second reflective mirror 30-2 for being β with the first reflective mirror 30-1 angle
And the third reflective mirror 30-3 of 30 ° of sample oblique upper；Wherein the relationship of α and β isReflective mirror 30 be located at it is relatively fixed with microscope 10 in sealing shell 1,
10 horizontal direction face reflective mirror 30 of microscope obtains 18 information of sample from reflective mirror 30；The camera lens of microscope 10 passes through close
It seals shell 1 to be inserted into, and in surrounding rubber-coated 11, is also able to achieve between camera lens and sample 18 to guarantee air-tightness and guarantee
Relative motion；Reflective mirror 30 and the camera lens of microscope 10 are relatively fixed, are able to confirm that sample when sample 18 appears in the visual field
18 on synchrotron radiation sample stage horizontal direction position.When adjustment short transverse, when keeping sample 18 clear, i.e. confirmatory sample 18
Short transverse position；The black light of the black light imaging and positioning is primarily referred to as synchrotron radiation Laue X-ray and electricity
Beamlet, window of the upper cover plate of sealing shell 1 as black light；Upper cover plate is divided into 3 layers, hollow out among upper and lower plates, and two
Plate hollow part accommodates graphite flake 29, and graphite flake 29 and upper and lower plates are sealed by organic resin；
Atmosphere module: including tentatively dehumidifying and filter assemblies, air inlet flow-disturbing component, Vacuum filtration device 17 and more gas
Atmosphere mixing chamber 7 installs gas flowmeter and air pressure feedback control valve 6 and flow-disturbing net conduct after more atmosphere mixing chambers 7
Air inlet flow-disturbing component, the horizontal fin of 1 inwall processing of sealing shell；Using activated carbon coating, as tentatively being removed in sealing shell 1
Wet and filter assemblies；Pass through the folding of the air pressure feedback control valve 6 of barometer 14；Vacuum filtration device 17 and atmosphere mixing
Room 7 is distributed in 1 two sides of sealing shell；
Sensing system: mechanics sensing, displacement measurement and feedback, temperature measurement and feedback, barometric surveying and dry and wet are realized
Degree measurement；Mechanics sensing relies on piezoelectric transducer 22, and the piezoelectric transducer 22 is fixed on the drawing opposite with L-type bearing panel 20
On first 15 23 step of pedestal, 20 lower end of bearing panel is contacted with piezoelectric transducer 22, and 20 section of L-type bearing panel is laid flat
" mutual " character form structure is presented with 15 pedestal 23 of pull head in L-type, directly passes through piezoelectric transducer 22 in Mechanical loading and measures pulling force；
Displacement measurement uses contact type measurement, and displacement sensor two parts are respectively placed on the support frame 19 being fixed on pull head 15；
Temperature measurement in order to increase accuracy using thermocouple 12 contact 18 surface of sample directly measure surface temperature, wherein wire around
At spring like, guarantee that vibration causes temperature measurement inaccurate when 12 detecting head of thermocouple and 18 surface of sample will not be because of loads；Together
Shi Wendu measurement also includes for monitoring temperature in shell, and air pressure and the measurement of humidity are then directed to shell vivo environment, to shell
Interior temperature, humidity and the measurement of air pressure are surveyed by the temperature and dry hygrometer 13 and barometer 14 for being fixed on shell side
Amount.
20 lower surface of L-type bearing panel is contacted with alternating temperature module 25, as thermal conductive surface, alternating temperature module 25 and pull head 15
Heat insulation layer 24 is placed between pedestal 23, positioning pin 31 is interted between heat insulation layer 24 and L-type bearing panel 20, is used for alternating temperature module 25
Limit.
15 entire length of pull head is twice or more of height, and the height of pull head 15 is the axis and pull head of reverse-flighted screw 4
1.5 to 2 times of distance between 15 bottom surface.
Support frame as described above 19 is substantially reduced heat transfer with 15 contact portion cushioning heat insulation layer 24 of pull head using intermediate hollow out.
24 surface of internal insulation of the pull head 15 processes through-hole array, under conditions of guaranteeing mechanical strength, further
Reduce thermal conductivity coefficient.
Temperature feedback is the resistance wire power adjusted in high-temperature heating module for high-temperature heating module, and is directed to low temperature
Refrigerating module is then the flow velocity for adjusting liquid nitrogen in copper pipe 27.
The shell long side inner wall of the sealing shell 1 has two sliding rail carryings and the horizontal movement of gentle support frame 19, close
Width, length and the height for closing shell 1 are 5 times or more of the width of alternating temperature module 25, length and height.
Microscope 10 is installed in the 1 long side side of sealing shell, and microscope 10 and horizontal direction are in 45 degree of reflective mirror 30
Relatively fixed, 10 tail portion of microscope is fixed on small-sized displacement platform, is then fixed on outer base, microscope imaging is in external
On screen.
The deformeter is used not only for experiment of machanics under synchrotron radiation, also can be used under electron microscope testing,
For testing under electron microscope, installation microscope 10 is not needed.
Compared to the prior art compared with the present invention has following advantage:
(1) there is the universality that can be used under synchrotron radiation and microscope.
(2) modularized design has complete test macro, can carry out mechanics, displacement, temperature survey immediately and in high precision
The characteristics of amount and feedback.
(3) can carry out the test under wide temperature range extreme temperature, realize carried out on a laboratory apparatus simultaneously low temperature and
High temperature experiment.
(4) it can simulate and carry out the test under multi-environment atmosphere.
(5) individual mechanical test, Li Re-coupling measurement can be carried out, Li-heat-atmosphere coupling measurement realizes experiment
The diversity of implementation.
(6) imaging and positioning system for having gathered visible light and black light may be implemented to observe in real time in experimentation,
Solve the problems, such as that synchrotron radiation is limited and in closed lab space how and meanwhile carry out X-ray scanning and realize home position observation.
Detailed description of the invention
Fig. 1 is deformeter overall structure of the present invention and arrangement.
Fig. 2 is pull head side sectional view.
Fig. 3-1 is alternating temperature module top view.
Fig. 3-2 is L-type bearing panel lower surface bottom view.
Fig. 3-3 is sealing shell upper cover explosive view.
Fig. 3-4 is microscope and reflective mirror layout drawing.
Specific embodiment
Below in conjunction with drawings and the specific embodiments, present invention is further described in detail.
A kind of more atmosphere in situ environment stress gauges of modularization wide temperature range as shown in Figure 1, comprise the following modules:
Mechanical loading module: including reverse-flighted screw 4, slide bar 5 and fixed 18 both ends of sample pull head 15 positioned opposite,
Speed-changing gear box 32, driving motor 16, the displacement range of Mechanical loading module are 10mm to 20mm, and precision is 1 μm, can apply and answer
Change be up to 100%, can applied force be 0~1kN.The contour installation parallel with slide bar 5 of reverse-flighted screw 4, jointly across pull head 15
Pedestal 23, and both ends are pierced by sealing shell 1 and are fixed on sealing shell 1, one end that reverse-flighted screw 4 is pierced by sealing shell 1 is logical
Shaft coupling is crossed to be connected with speed-changing gear box 32 and driving motor 16.As shown in Fig. 2, the pull head 15 is divided into 5 layers of structure,
L-type bearing panel 20, alternating temperature module 25, heat insulation layer 24 and pedestal 23 including tabletting 26, for carrying tabletting 26.Tabletting 26
It is fixed on L-type bearing panel 20, is designed using sinking to property, guarantee that upper surface and bearing panel 20 flush, 26 thickness of tabletting is about
For 1~2mm, X-ray and electron beam incident angle are maximized, is fixed respectively with sunk screw on four angles, L-type bearing panel 20 divides
For two components horizontal part 20-1 combined with tabletting 26 and the vertical part 20-2 of L-type, vertical part and horizontal part
By two tooth wedgings, while leading to recirculated water at vertical part, horizontal part upper surface fin is reinforced.When sample 18 is film sample
Having a size of 10mm*20mm；When for general stretching sample, shape is general stretching sample common shape, and centre is for test section field width
1mm, long 10mm, thick 0.5mm, both ends are rough surface.
Alternating temperature module: including temperature feedback system, high-temperature heating module and sub-cooled module, extent of alternating temperature are as follows: low
Warm refrigerating module is liquid nitrogen boiling point to room temperature, and being heated at high temperature module is room temperature to 1000 DEG C.As shown in figure 3-1, it is heated at high temperature mould
Block and sub-cooled module are that rectangle plate 28 designs, and long side side processes two chamferings for conduct when being embedded in pull head 15
The limit of limit, the other side is realized by positioning pin 31.Wherein refrigerated module structure is sandwich structure, by two pieces of metal plates
Fix the copper pipe 27 of coiling.Refrigerated module connects with external liquid nitrogen, passes through flow control by flowmeter and valve 9-1 folding
Temperature, thermocouple 12 provide feedback model.High temperature module connects with external power supply, by relay 9-2 control resistance wire heating, heat
Galvanic couple 12 provides feedback signal.It is ± 1 DEG C that alternating temperature module, which can control precision,.
Optical imagery and locating module: optical imagery and locating module include visual light imaging and positioning and black light
Imaging and positioning, it is seen that light imaging mainly includes reflective mirror 30 and microscope 10 with positioning.As shown in Figure 3-4, reflective mirror 30
Including the first reflective mirror 30-1 being arranged at angle with horizontal plane α, and that the first reflective mirror 30-1 angle is β is second anti-
The light microscopic 30-2 and third reflective mirror 30-3 of 30 ° of sample oblique upper.Wherein the relationship of α and β isα=60 °, β=64 ° are used herein.Reflective mirror 30 is located at sealing shell 1
It is interior relatively fixed with microscope 10.10 horizontal direction face reflective mirror 30 of microscope obtains 18 information of sample from reflective mirror 30.
The camera lens of microscope 10 is inserted by sealing shell 1, and in surrounding rubber-coated 11, to guarantee air-tightness and guarantee camera lens
Relative motion is also able to achieve between sample 18.Reflective mirror 30 and the camera lens of microscope 10 are relatively fixed, when sample 18 appears in
The position of the horizontal direction on synchrotron radiation sample stage of sample 18 can be confirmed when in the visual field.When adjustment short transverse, make sample
18 it is clear when, can confirm short transverse position.Black light imaging and the black light of positioning are primarily referred to as synchrotron radiation labor
X-ray in distress and electron beam.Window of the upper cover plate of sealing shell 1 as black light.As shown in Fig. 3-3, upper cover plate is total
Be divided into 3 layers, hollow out among upper and lower plates, two plate hollow parts accommodate graphite flake 29, graphite flake 29 and upper and lower plates by organic resin into
Row sealing, graphite window size are 3cm*5cm.
Atmosphere module: including tentatively dehumidifying and filter assemblies, air inlet flow-disturbing component, Vacuum filtration device 17 and more gas
Atmosphere mixing chamber 7 installs gas flowmeter and air pressure feedback control valve 6 and flow-disturbing net conduct after more atmosphere mixing chambers 7
Air inlet flow-disturbing component, the horizontal fin of 1 inwall processing of sealing shell, fin clearance are 2~3mm, and with a thickness of 1~2mm, width is
3~5mm, using activated carbon coating, as tentatively dehumidifying and filter assemblies in shell.Pass through the air pressure feedback control of barometer 14
The folding of valve 6.Vacuum filtration device 17 and atmosphere mixing chamber 7 are distributed in 1 two sides of sealing shell.
Sensing system: mechanics sensing, displacement measurement and feedback, temperature measurement and feedback, barometric surveying, humidity are realized
Measurement.Mechanics sensing relies on piezoelectric transducer 22, and the piezoelectric transducer 22 is fixed on the pull head opposite with L-type bearing panel 20
On 15 23 step of pedestal, 20 lower end of bearing panel is contacted with piezoelectric transducer 22, and 20 section of L-type bearing panel is the L laid flat
" mutual " character form structure is presented with 15 pedestal 23 of pull head in type, directly passes through piezoelectric transducer 22 in Mechanical loading and measures pulling force.Position
Shift measurement uses contact type measurement, and displacement sensor two parts are respectively placed on the support frame 19 being fixed on pull head 15.Temperature
Degree measurement directly measures surface temperature to increase accuracy using the contact of thermocouple 12 18 surface of sample, and wherein wire is coiled into
Spring like guarantees that vibration causes temperature measurement inaccurate when 12 detecting head of thermocouple and 18 surface of sample will not be because of loads.Simultaneously
Temperature measurement also includes for monitoring temperature in shell, and air pressure and the measurement of humidity are then directed to shell vivo environment, in shell
Temperature, humidity and the measurement of air pressure are measured by the temperature and dry hygrometer 13 and barometer 14 for being fixed on shell side
20 lower surface of L-type bearing panel is contacted with alternating temperature module 25, as thermal conductive surface.Alternating temperature module 25 and pull head 15
Heat insulation layer 24 is placed between pedestal 23, positioning pin 31 is interted between heat insulation layer 24 and L-type bearing panel 20, is used for alternating temperature module 25
Limit.
15 entire length of pull head is twice or more of height, and the height of pull head 15 is the axis and pull head of reverse-flighted screw 4
1.5 to 2 times of distance between 15 bottom surface.
Support frame as described above 19 is substantially reduced heat transfer with 15 contact portion cushioning heat insulation layer 24 of pull head using intermediate hollow out.
24 surface of internal insulation of the pull head 15 processes through-hole array, under conditions of guaranteeing mechanical strength, further
Reduce thermal conductivity coefficient.
Temperature feedback is the resistance wire power adjusted in high-temperature heating module for high-temperature heating module, and is directed to low temperature
Refrigerating module is then the flow velocity for adjusting liquid nitrogen in copper pipe 27.
The shell long side inner wall of the sealing shell 1 has two sliding rail carryings and the horizontal movement of gentle support frame 19, close
Width, length and the height for closing shell 1 are 5 times or more of the width of alternating temperature module 25, length and height.
Microscope 10 is installed in the 1 long side side of sealing shell, and microscope 10 and horizontal direction are in 45 degree of reflective mirror 30
Relatively fixed, 10 tail portion of microscope is fixed on small-sized displacement platform, is then fixed on outer base, microscope imaging is in external
On screen.
The deformeter is used not only for experiment of machanics under synchrotron radiation, also can be used under electron microscope testing,
For testing under electron microscope, installation microscope 10 is not needed.
The operation principle of the present invention is that: strip standard specimen is used first, is placed on the recessed of 20 upper surface of L-type bearing panel
Slot installs tabletting 26, entire sample stage is installed on synchrotron radiation sample stage, finds the position of sample 18 accurately under synchrotron radiation
It sets.Then the camera lens of microscope 10 is inserted into together with reflective mirror 30, first vertically draws high and axially moves horizontally, substantially determine sample 18
Then position in the horizontal direction moves up and down the camera lens and reflective mirror 30 of microscope 10, until 18 lower surface of sample is clear.It connects
Unload standard specimen.Strip is made in laboratory sample 18, is placed on the groove of 20 upper surface of L-type bearing panel, tabletting 26 is installed,
It realizes the fixation to 18 both ends of sample, alternating temperature module 25 is installed, by this 20 following table of L-type bearing panel of one side face with chamfering
It is fixed to be inserted into positioning pin 31 for the following insertion of the position-limited edge, that is, Fig. 3-2 in face.If it is low temperature test is carried out, then by low temperature
Then the copper pipe 27 of module and liquid nitrogen the pipeline shell that is connected out close thermocouple 12 and 18 intimate surface contact of sample close
The upper cover for closing shell 1, to carrying out vacuum drying in shell.It tests, then connects heating wire outside power supply pass-out shell if it is high temperature, it will
Thermocouple 12 and 18 intimate surface contact of sample, then close the upper cover of sealing shell 1.It is extracted then according to environment needed for testing
Vacuum is simultaneously passed through required gas, can be without vacuum drying, by barometer, thermometer and dry hygrometer to shell under high temperature experiment
Interior environment is monitored.Revolving speed by controlling motor 16 is monitored loading speed, while piezoelectric transducer 22 is recorded
The size of stress, the displacement sensor being mounted on support frame 19 then writes displacement, while testing number to synchrotron radiation
According to being acquired.It is possible thereby to realize the uniaxial in-situ mechanical experiment of primary more atmosphere wide temperature ranges.
The sample stage, which can be also placed under electron microscope, simultaneously uses, and does not need installation microscope 10 at this time, remaining step
It is rapid to be same as above.
Claims (9)
1. a kind of more atmosphere in situ environment stress gauges of modularization wide temperature range, it is characterised in that: comprise the following modules: Mechanical loading mould
Block: pull head (15), the speed-changing gear box arranged in opposite directions including reverse-flighted screw (4), slide bar (5) and fixed sample (18) both ends
(32) and driving motor (16), the reverse-flighted screw (4) contour installation parallel with slide bar (5) passes through the bottom of pull head (15) jointly
Seat (23), and both ends are pierced by sealing shell (1) and are fixed on sealing shell (1), reverse-flighted screw (4) is pierced by sealing shell (1)
One end be connected with speed-changing gear box (32) and driving motor (16) by shaft coupling；The pull head (15) one is divided into 5 layers
Structure, L-type bearing panel (20), alternating temperature module (25), heat insulation layer (24) including tabletting (26), for carrying tabletting (26) with
And pedestal (23), tabletting (26) are fixed on L-type bearing panel (20), are designed using sinking to property, guarantee upper surface and loading end
Plate (20) flushes, and tabletting (26) maximizes X-ray and electron beam incident angle, bearing panel (20) are divided into two with a thickness of 1~2mm
The vertical part (20-2) of a component, the horizontal part (20-1) combined with tabletting (26) and L-type, vertical part and level
Component leads to recirculated water by two tooth wedgings at vertical part, horizontal part upper surface fin is reinforced；When sample (18) are thin
Having a size of 10mm*20mm when film sample；When to stretch sample, shape is to stretch sample shape, i.e. intermediate elongated, the flat width in both ends, both ends
For rough surface；The displacement range of the Mechanical loading module is 10mm to 20mm, and precision is 1 μm, can apply strain and be up to
100%, can applied force be 0~1kN；
Alternating temperature module: including temperature feedback system, high-temperature heating module and sub-cooled module, extent of alternating temperature are as follows: low temperature cold
But module is liquid nitrogen boiling point to room temperature, and being heated at high temperature module is room temperature to 1000 DEG C；It is heated at high temperature module and sub-cooled module
It is rectangle plate (28) design, as limit, the other side when long side side processes two chamferings for being embedded in pull head (15)
Limit rely on positioning pin (31) Lai Shixian；Wherein refrigerated module structure is sandwich structure, fixes disk by two pieces of metal plates
Around copper pipe (27)；Refrigerated module connects with external liquid nitrogen, passes through flow control temperature, thermocouple by valve (9-1) folding
(12) feedback model is provided；High temperature module connects with external power supply, by relay (9-2) control resistance wire heating, thermocouple
(12) feedback signal is provided；It is ± 1 DEG C that alternating temperature module, which can control precision,；
Optical imagery and locating module: optical imagery includes that visual light imaging and positioning and black light are imaged with locating module
With positioning, the visual light imaging and positioning mainly include reflective mirror (30) and microscope (10), and reflective mirror (30) includes point
The first reflective mirror (30-1) not being arranged at angle with horizontal plane a, and that the first reflective mirror (30-1) angle is β is second reflective
Mirror (30-2) and the third reflective mirror (30-3) of 30 ° of sample oblique upper；Wherein the relationship of α and β be 2/ (√ 3sin (alpha+beta))=
1/(2cosβ)；Reflective mirror (30) is located at, microscope (10) horizontal direction relatively fixed with microscope (10) in sealing shell (1)
Face reflective mirror (30), from acquisition sample (18) information in reflective mirror (30)；The camera lens of microscope (10) passes through sealing shell (1)
Insertion, and it is rubber-coated (11) in surrounding, phase is also able to achieve between camera lens and sample (18) to guarantee air-tightness and guarantee
To movement；Reflective mirror (30) and the camera lens of microscope (10) are relatively fixed, are able to confirm that when sample (18) appears in the visual field
The position of sample (18) horizontal direction on synchrotron radiation sample stage；When adjustment short transverse, when keeping sample (18) clear, i.e.,
Confirmatory sample (18) short transverse position；The black light of the black light imaging and positioning is primarily referred to as synchrotron radiation Laue
X-ray and electron beam, window of the upper cover plate of sealing shell (1) as black light；Upper cover plate is divided into 3 layers, up and down
Hollow out among plate, two plate hollow parts accommodate graphite flake (29), and graphite flake (29) and upper and lower plates are sealed by organic resin；
Atmosphere module: including tentatively dehumidifying and filter assemblies, air inlet flow-disturbing component, Vacuum filtration device (17) and more atmosphere
Mixing chamber (7) installs gas flowmeter and air pressure feedback control valve (6) and flow-disturbing net after more atmosphere mixing chambers (7)
As air inlet flow-disturbing component, the horizontal fin of sealing shell (1) inwall processing；Using activated carbon coating, as sealing shell (1)
Interior preliminary dehumidifying and filter assemblies；Pass through the folding of the air pressure feedback control valve (6) of barometer (14)；Vacuum filtration device
(17) and atmosphere mixing chamber (7) is distributed in sealing shell (1) two sides；
Sensing system: realize that mechanics sensing, displacement measurement and feedback, temperature measurement and feedback, barometric surveying and humidity are surveyed
Amount；Mechanics sensing relies on piezoelectric transducer (22), and the piezoelectric transducer (22) is fixed on opposite with L-type bearing panel (20)
On pedestal (23) step of pull head (15), bearing panel (20) lower end is contacted with piezoelectric transducer (22), L-type bearing panel (20)
Section is the L-type laid flat, and " mutual " character form structure is presented with pull head (15) pedestal (23), is directly passed by piezoelectricity in Mechanical loading
Sensor (22) measures pulling force；Displacement measurement uses contact type measurement, and displacement sensor two parts, which are respectively placed in, is fixed on pull head
(15) on the support frame (19) on；Temperature measurement is direct using thermocouple (12) contact sample (18) surface in order to increase accuracy
Surface temperature is measured, wherein wire is coiled into spring like, guarantees that thermocouple (12) detecting head and sample (18) surface will not be because of
Vibration causes temperature measurement inaccurate when load；Temperature measurement simultaneously also includes for monitoring temperature in shell, air pressure and humidity
Measurement be then directed to shell vivo environment, to the measurement of shell body temperature, humidity and air pressure by being fixed on the gas of shell side
Temperature and dry hygrometer (13) and barometer (14) measure.
2. the more atmosphere in situ environment stress gauges of a kind of modularization wide temperature range according to claim 1, it is characterised in that: described
L-type bearing panel (20) lower surface is contacted with alternating temperature module (25), as thermal conductive surface, alternating temperature module (25) and pull head (15) pedestal
(23) heat insulation layer (24) are placed between, intert positioning pin (31) between heat insulation layer (24) and L-type bearing panel (20), are used for alternating temperature
The limit of module (25).
3. the more atmosphere in situ environment stress gauges of a kind of modularization wide temperature range according to claim 1, it is characterised in that: described
Pull head (15) entire length is twice or more of height, and the height of pull head (15) is axis and pull head (15) of reverse-flighted screw (4)
1.5 to 2 times of distance between bottom surface.
4. the more atmosphere in situ environment stress gauges of a kind of modularization wide temperature range according to claim 1, it is characterised in that: described
Support frame (19) is substantially reduced heat transfer with pull head (15) contact portion cushioning heat insulation layer (24) using intermediate hollow out.
5. the more atmosphere in situ environment stress gauges of a kind of modularization wide temperature range according to claim 1, it is characterised in that: described
Heat insulation layer (24) the surface processing through-hole array of pull head (15) further decreases thermal conductivity system under conditions of guaranteeing mechanical strength
Number.
6. the more atmosphere in situ environment stress gauges of a kind of modularization wide temperature range according to claim 1, it is characterised in that: temperature
Feedback is the resistance wire power adjusted in high-temperature heating module for high-temperature heating module, and is then for sub-cooled module
Adjust the flow velocity of liquid nitrogen in copper pipe (27).
7. the more atmosphere in situ environment stress gauges of a kind of modularization wide temperature range according to claim 1, it is characterised in that: described
The shell long side inner wall of sealing shell (1) has two sliding rail carryings and the horizontal movement of gentle support frame (19), sealing shell (1)
Width, length and height be 5 times or more of the width of alternating temperature module (25), length and height.
8. the more atmosphere in situ environment stress gauges of a kind of modularization wide temperature range according to claim 1, it is characterised in that: described
Microscope (10) are installed in sealing shell (1) long side side, and microscope (10) and horizontal direction are opposite in 45 degree of reflective mirror (30)
Fixed, microscope (10) tail portion is fixed on small-sized displacement platform, is then fixed on outer base, microscope imaging is in external screen
On curtain.
9. the more atmosphere in situ environment stress gauges of a kind of modularization wide temperature range according to claim 1, it is characterised in that: described
The more atmosphere in situ environment deformeters of modularization wide temperature range are used not only for experiment of machanics under synchrotron radiation, also can be used in electronics
It is tested under microscope, for testing under electron microscope, does not need installation microscope (10).
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| CN113514319B (en) * | 2021-05-10 | 2022-06-14 | 吉林大学 | In-situ static-dynamic fatigue mechanical property testing instrument in scanning electron microscope |
| CN113702153B (en) * | 2021-08-13 | 2022-04-19 | 北京科技大学 | Material structure performance in-situ detection equipment with wide temperature range characteristic |
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