CN101042319A - In-situ measurement system of material micro-creep - Google Patents
In-situ measurement system of material micro-creep Download PDFInfo
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- CN101042319A CN101042319A CN 200710039639 CN200710039639A CN101042319A CN 101042319 A CN101042319 A CN 101042319A CN 200710039639 CN200710039639 CN 200710039639 CN 200710039639 A CN200710039639 A CN 200710039639A CN 101042319 A CN101042319 A CN 101042319A
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Abstract
This invention relates to one original measurement method and device for materials microscope worm change, which can get materials in thermal environment and mechanic force couple metal phase image in real time and adopts the image relative method based on digital image in data process terminal to get micro worm change in thermal environment. The original test device comprises load structure, heating furnace and control device, data acquire and process device, which realizes the real time original test with inertia protection gas to avoid specimen in high temperature to ensure specimen data accuracy.
Description
Technical field
The invention belongs to the material properties test technical field, relate to a kind of in-situ measuring method and device that is used for metal or nonmetallic materials micro-creep, especially can obtain the metallograph of material under thermal environment and mechanical force coupling condition by real-time in-situ, and obtain the microcreep distortion of material under the thermal environment based on the digital picture correlation method.
Background technology
Along with microcosmic, Jie's sight and the application of sight yardstick technology in microelectronic component, micromechanics of receiving, press for material deformation and the inefficacy evolutionary process understood under crystal grain and even the smaller szie, especially for the device and the microstructure that are operated under the thermal environment, need the creep failure characteristic of its microcosmic of scientific measurement, to satisfy the needs that design, manufacturing and reliability are safeguarded.In the face of this challenge, traditional experiment technology and means can't meet the demands, there is the incompatibility thermal environment in the experimental system of having developed, lacks real-time, the not high drawback of precision, therefore develop test method and the device that obtains the deformation of creep under the crystal particle scale under the thermal environment in real time, become needing badly of microelectronics and micro mechanical technology development.
" microspecimen high temperature creep property test unit " (application number: 200420080166.0) by Nanjing University of Technology's development, its function is to solve the problem of obtaining the bulk specimen performance data based on micro-test sample, can not realize the home position observation and the measurement of creep impairment process; The invention of University Of Tianjin " a kind of new engineering structure and material deformation are measured " (application number: 03128736.0), the deformation of body that only can finish under the room temperature is measured, be confined to room temperature environment, the oxidation difficulty that the high-temerature creep measurement brings can not be overcome, and creep and damage information under the micro-scale can not be provided." a kind of data auto-acquiring stretching creep deformation proving installation " (application number: 200520127714.5) of effluent south University of Science and Technology development, can be used for high temperature measurement, but adopted the extensometer method to obtain deformation data, belong to the direct measuring method category, measuring accuracy is the millimeter level, be confined to the macroscopic material test, can not provide the microcreep procedural information, more can not satisfy the microdeformation measurement requirement." microelectronics with material and soldered fitting creep strain proving installation " (application number 200410029947.1) of Beijing University of Technology invention, microscope is provided and has amplified camera function, can obtain the metallograph under the thermal environment, but the deformation of creep when being used for length is measured and is still had limitation, mainly be: the benchmark of surperficial method of scoring as distortion adopted in invention, when long under the thermal environment oxidation meeting of specimen surface cause precise decreasing, the frictional influence that the pulley load maintainer that adopts is introduced is not paid attention to yet, the ceramic edge infrared hot plate that invention is adopted also makes the device working temperature be limited to 150 degree, thereby is not suitable for higher temperature occasion and requirement.
Summary of the invention
Can not measure and the not high drawback of overall precision by real-time in-situ in order to overcome current material micro-creep test unit, the invention provides a kind of material creep behavior in-situ measurement system, this system not only can obtain the metallograph of material under thermal environment and mechanical force coupling condition by real-time in-situ, and obtain the microcreep distortion of material under the thermal environment based on the digital picture correlation method, to satisfy the further requirements of research and exploration of creep behaviour mechanism such as material property assessment and life prediction.
Design of the present invention is as follows: the heating furnace that will develop voluntarily places on the loading frame; Thermopair and sample directly weld, and sample connects to be placed on by pull rod screw up and down and adds in the electrothermal stove; Sample is applied the needed load of test by lever principle, can accurately measure the magnitude of load that is applied on the sample by force transducer; In heating furnace, feed inert gas by gas shield device, oxidized and influence the precision of experimental data when the high-temerature creep to prevent sample; Drive a small-sized observation port in the middle of the heating furnace, obtain test material microdeformation structure and morphology in the sample experimentation, realized the real-time in-situ measurement by long-focus high-power microscope and digital CCD device; Simultaneously this data transmission is arrived data processing terminal, by related software the relevant search of related variation unique point is calculated, thereby obtain the little microdeformation amount of material grains yardstick, reach real-time in-situ and measure and high-precision purpose based on the diffusing class of numeral correlation method.
The technical solution adopted in the present invention is: a kind of in-situ measurement system of material micro-creep is characterized in that described in-situ measurement device comprises that load maintainer, heating furnace and control device, data obtain and treating apparatus;
Described load maintainer comprises: be fixed on the loading frame 7 on the air cushion vibration isolators 13, linear bearing 33 is connected on the crossbeam 35 of loading frame 7, lever 34 above the crossbeam, the positive left-hand thread 32 in linear bearing 33, upper end below the crossbeam, upper connecting rod 31 connect successively, connect successively between lower link 14, the positive left-hand thread 29 in lower end, force transducer 1 ball angle 40 and the base plate 41, lever about 34 hangs with balanced weight 5 respectively and is loaded with the counterweight suspension rod 37 that loads counterweight 39, and the upper and lower side of sample 30 is fixed by upper and lower pull bar 31,14;
Described heating furnace and control device comprise: a centre has the heating furnace 6 of observation port 51, link to each other with the temperature controller 42 in the electric cabinet 3, one group of output terminal of temperature controller 42 is by thermopair 2 and sample 30 welding, and the terminal box 16 on another group output terminal and the furnace wall is joined;
Described data are obtained and treating apparatus comprises: be connected white light source 8 and three-dimensional regulation platform 11 on the air cushion vibration isolators 8, long-focus high-power microscope 9 and digital CCD10 are fixed on the three-dimensional regulation platform 11, and digital CCD is connected on the data processing terminal 12 by data line;
The center of the optical center of long-focus microscope 9 and the observation port of heating furnace 51.
Described heating furnace 6 comprises: pipe core 19, twine heating wire 18 in the thread groove of pipe core 19, insulation material 17 densifications be arranged in heating wire 18 around; Run through the furnace wall from pipe core 19 and have observation port 51, one water collar 20 is set on observation port 51 excircles, water collar 20 is welded on the furnace wall, water inlet pipe 21 and rising pipe 24 are welded on the water collar 20, be provided with fused quartz glass 22 in the water collar 20 with observation port 51 sealings, a back-up ring 23 of sealing fused quartz glass 22 is threaded with water collar 20, and the heating furnace bottom has furnace bottom baffle plate 25 to link to each other with gland bonnet 26 with the furnace wall, accompanies asbestos layer 15 between baffle plate 25 and the furnace wall.
Said sample 30 can be positioned in the pipe core 19, and fixedly the upper and lower pull bar 31,14 of sample 30 stretches in the pipe core 19, and said heating furnace pipe core can be a ceramic pipe.
Described heating furnace and control device also comprise an inert gas bottle 4, pass furnace bottom gland bonnet 26 by snorkel 27 and link to each other with heating furnace 6.
Beneficial effect
The present invention can obtain the metallograph of material under thermal environment and mechanical force coupling condition by real-time in-situ, and takes to obtain the distortion of the microcreep under the material grains yardstick under the thermal environment based on the digital picture correlation method at data processing terminal 12.The observation port that adds electrothermal stove has been realized the real-time in-situ of sample is measured; Thermopair and sample directly weld, and can accurately measure the temperature of sample itself; Force transducer can accurately measure the size that is applied to load on the sample; Be connected with inert protective gas in the stove and can prevent that sample is at high temperature oxidized to guarantee the accuracy of sample data.
Description of drawings
Fig. 1 is a material micro-creep in-situ measurement device assembling synoptic diagram
Wherein: 1. force cell, 2. thermopair, 3. electric cabinet, 4. inert gas bottle, 5. balanced weight, 6. add electrothermal stove, 7. loading frame, 8. white light source, 9. long-focus high-power microscope, 10. digital CCD, 11. three-dimensional regulation platforms, 12. data processing terminals, 13. air cushion vibration isolators.
Fig. 2 is a heating electric cooker structure synoptic diagram
14. lower link, 15. asbestos layers, 16. terminal boxes, 17. insulation materials, 18. heating wire, 19. pipe cores, 20. water collars, 21. water inlet pipes, 22. fused quartz glass, 23. back-up rings, 24. rising pipes, 25. furnace bottom baffle plates, 26. gland bonnets, 27. snorkels, 51. observation ports.
Fig. 3 is a loading frame assembling synoptic diagram
28. left lever, the positive and negative threaded rod in 29. upper ends, 30. samples, 31. upper connecting rods, the positive and negative threaded rod in 32. lower ends, 33. linear bearings, 34. levers, 35. crossbeams, 36. right columns, 37. counterweight suspension rods, 38. adjusting handles, 39. counterweights, 40. ball angles, 41. base plates.
Fig. 4 is electric cabinet panel synoptic diagram
42. temperature controller, 43. reometers, 44. power Displaying Meters, 45. power switches, 46. heater switch, 47. heated condition pilot lamp.
Fig. 5 is a three-dimensional regulation platform assembling synoptic diagram
48. vertical adjusting handle, 49. vertical direction setting nuts, 50. lateral adjustments handles.
Fig. 6 is a 316L stainless steel diffusion welding joint sample
Fig. 7 is the different microscopic appearance characteristic patterns constantly of sample
Fig. 8 is the test findings data and curves figure of unique point A
Embodiment
Below by accompanying drawing and corresponding embodiment material micro-creep behavior in-situ measurement device is described.
Material creep behavior in-situ measurement system device is formed by equipment assembling connection as shown in Figure 1, mainly is made up of loading frame 7, heating furnace 6, white light source 8, long-focus high-power microscope 9 and digital CCD10, three-dimensional regulation platform 11, data processing terminal 12 and force transducer 1, thermopair 2, switch cabinet 3 and inert gas bottle 4.Whole device all places on the air cushion vibration isolators 13.
As shown in Figure 1 and Figure 2, material creep behavior in-situ measurement system device annexation is as follows: loading frame 7, white light source 8, three-dimensional regulation platform 11 all are connected by the group hole on screw and the air cushion vibration isolators 13; Long-focus high-power microscope 9 and digital CCD are by being bolted on the three-dimensional regulation platform 11; Temperature controller 42 in the electricity cabinet 3 has two groups of output terminals, and one group of output terminal is by thermopair 2 and sample 30 welding, and another group output terminal links to each other with the terminal box 16 that adds electrothermal stove 6; Terminal box 16 and furnace wall screw attachment, insulation material 17 densifications are around high temperature resistant pipe core 19, heating wire 18 is wound in pipe core 19 thread grooves, between water collar 20 and the furnace wall, connect by spot welding between water inlet pipe 21 and rising pipe 24 and the water collar 20, back-up ring 23 and water collar 20 are by thread connection; Be connected by the counterbore screw between furnace bottom baffle plate 25 and furnace wall and the gland bonnet 26, the centre accompanies asbestos layer 15; Thermopair 2 and snorkel 27 penetrate in the furnace chamber by the aperture on gland bonnet 26 and the furnace bottom baffle plate 25.
The electricity cabinet panel is provided with heater switch 46 and power switch 45, warranty test personnel's Electrical Safety as shown in Figure 4; Can set the Temperature numerical that test needs as required by control knob on temperature controller 44 control panels, treat that temperature tends to be balanced after adjusting; Power Displaying Meter 44 has accurately shown the real load that is applied on the sample; Reometer 43 and heated condition pilot lamp 47 be the circuit state in the monitoring test process in real time.
Add electrothermal stove operating voltage 220V, its advantage is: firing rate is fast, the control accuracy height, and security is good, at the bottom of the manufacturing cost; Maximum temperature can reach 900 ℃.Realized the real-time in-situ of sample is measured by the observation port of fused quartz glass 22 sealings; Cold water jacket can be avoided the too high destruction of causing the camera lens that adjusts the telescope to one's eyes of furnace wall temperature; Be connected with blanket gas in the stove and can prevent that sample is at high temperature oxidized to guarantee the accuracy of sample data.
As shown in Figure 3: left column 28 is connected by the counterbore screw retention with negative 41 with crossbeam 35 with right column 36; According to order from top to bottom: be between lever 34, upper connecting rod 31, sample 30, lower link 14, the positive left-hand thread 29 in lower end, force transducer 1, ball angle 40 and the base plate 41 and be threaded; As linear bearing 33 by screw retention on crossbeam 35; Lever about 34 ends hang with balanced weight 5 and counterweight suspension rod 37 respectively.
Loading frame constitutes basic framework by left column 28, right column 36, crossbeam 35 and base plate 41.Its rated load is 200Kg.Linear bearing 33 and ball angle 40 guarantee load vertical with sample to neutrality; The positive left-hand thread 32 in upper end is consistent with the observation port center with positive left-hand thread 29 adjusting sample centers, lower end; Compare with direct loading or motor loading, adopt lever principle to load the vibration that has reduced the number of counterweight 39 and avoided system.
As shown in Figure 5, the three-dimensional regulation platform has lateral adjustments handle 50, vertical adjusting handle 48 and vertical direction setting nut 49, and its principle is all based on the screw thread transmission.Consistent by regulating its position and then can adjusting the microscope center with the observation port center.
Embodiment
The preparation of sample
Sample is chosen 316L stainless steel diffusion welding welding joint, 1100 ℃ of welding temperatures, and pressure 10MPa, temperature retention time 2 hours, size is as shown in Figure 6.The blank that the preparation sample is chosen is that diameter is that φ 80mm, length are the 316L stainless steel bar of 45mm, chamfering 1mm, and face of weld is through after the grinding, and roughness is at 0.6～1.2 μ m.Before welding, clean being welded part with acetone soln in the ultrasonic washing instrument, remove surperficial grease, oxide film and other dirt.Used sample is that the warp cutting processing makes from this weldment, adds man-hour, guarantees that weld seam is positioned at the center of sample.
The test procedure of this measuring system is as follows:
1. the pilot system devices needed is assembled according to connected mode shown in Figure 1, regulate the air cushion vibration isolators and make it to be up to the standard
2. the sample two ends that prepare are coupled together with last lower link respectively, thermopair is passed to weld behind the aperture on the furnace bottom gland bonnet 26 then and put on sample one side
3. above-mentioned combiner is passed from the furnace chamber lower end, and will go up lower link and connect, rotation adjusting handle 38 will add electrothermal stove to be fixed, and the positive left-hand thread of regulating upper and lower side makes the sample center consistent with the observation port center, and makes the side observation port dorsad that is welded with thermopair
4. after snorkel being passed another aperture on the furnace bottom gland bonnet 26, fill up asbestos 15 at furnace bottom baffle plate 25 inner chambers, gland bonnet and lower bolster are fastening
5. calculating the required counterweight number that applies as required and according to the lever ratio, and add counterweight or select suitable counterweight size and number according to power Displaying Meter 44 shown magnitudes of load. this test imposed load is 700N
6. regulate the three-dimensional regulation platform, make microscope camera lens center consistent with the observation port center; Regulate the position of microscope focal length and white light source 8, until obtaining distinct image at data processing terminal
7. open the valve on the inert gas bottle 4, in furnace chamber, feed inert gas by snorkel 27
8. as shown in Figure 4, turn on the power switch 45 and electric furnace heater switch 46 successively, 400 ℃ of the temperature that test needs are set on temperature controller 44 control panels, treat that temperature tends to be balanced from the back temperature of adjusting.Reometer 43 and heated condition pilot lamp 47 circuit state in can the monitoring test process
9. feed tap water toward water inlet 21,, guarantee that the microscope camera lens is not heated the electric stove wall temperatures involved the furnace wall surface cooling
10. according to testing requirements, took the picture of a sample microscopic appearance feature every 12 hours, Fig. 7 is wherein four
11. a series of pictures that obtains can be calculated the microdeformation of a certain unique point of material by digital picture relevant treatment software at data processing terminal 12.As selected point A, obtain result as shown in Figure 8.
Claims (5)
1, a kind of in-situ measurement system of material micro-creep is characterized in that, described in-situ measurement device comprises that load maintainer, heating furnace and control device, data obtain and treating apparatus;
Described load maintainer comprises: be fixed on the loading frame 7 on the air cushion vibration isolators 13, linear bearing 33 is connected on the crossbeam 35 of loading frame 7, lever 34 above the crossbeam, the positive left-hand thread 32 in linear bearing 33, upper end below the crossbeam, upper connecting rod 31 connect successively, connect successively between lower link 14, the positive left-hand thread 29 in lower end, force transducer 1 ball angle 40 and the base plate 41, lever about 34 hangs with balanced weight 5 respectively and is loaded with the counterweight suspension rod 37 that loads counterweight 39, and the upper and lower side of sample 30 is fixed by upper and lower pull bar 31,14;
Described heating furnace and control device comprise: a centre has the heating furnace 6 of observation port 51, link to each other with the temperature controller 42 in the electric cabinet 3, one group of output terminal of temperature controller 42 is by thermopair 2 and sample 30 welding, and the terminal box 16 on another group output terminal and the furnace wall is joined;
Heating furnace 6 is connected on the loading frame 7 by the adjusting handle 38 that is arranged on the loading frame 7, and sample 30 sides place in the heating furnace;
Described data are obtained and treating apparatus comprises: be connected white light source 8 and three-dimensional regulation platform 11 on the air cushion vibration isolators 8, long-focus high-power microscope 9 and digital CCD10 are fixed on the three-dimensional regulation platform 11, and digital CCD is connected on the data processing terminal 12 by data line;
The center of the optical center of long-focus microscope 9 and the observation port of heating furnace 51.
2, the in-situ measurement system of material micro-creep as claimed in claim 1, described heating furnace 6 comprises: pipe core 19, twine heating wire 18 in the thread groove of pipe core 19, insulation material 17 densifications be arranged in heating wire 18 around, it is characterized in that, observation port 51 runs through the furnace wall from pipe core 19, one water collar 20 is set on observation port 51 excircles, water collar 20 is welded on the furnace wall, water inlet pipe 21 and rising pipe 24 are welded on the water collar 20, be provided with fused quartz glass 22 in the water collar 20 with observation port 51 sealings, a back-up ring 23 of sealing fused quartz glass 22 is threaded with water collar 20, the heating furnace bottom has furnace bottom baffle plate 25 to link to each other with gland bonnet 26 with the furnace wall, accompanies asbestos layer 15 between baffle plate 25 and the furnace wall.
3, the in-situ measurement system of material micro-creep as claimed in claim 1 or 2 is characterized in that, described heating furnace and control device also comprise an inert gas bottle 4, passes furnace bottom gland bonnet 26 by snorkel 27 and links to each other with heating furnace 6.
4, the in-situ measurement system of material micro-creep as claimed in claim 2 is characterized in that, the pipe core of heating furnace is a ceramic pipe.
5, the in-situ measurement system of material micro-creep as claimed in claim 1 or 2 is characterized in that, said sample 30 is positioned in the pipe core 19, and fixedly the upper and lower pull bar 31,14 of sample 30 stretches in the pipe core 19.
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