CN106556535B - A kind of mechanic property test method based on mechanics sensor - Google Patents
A kind of mechanic property test method based on mechanics sensor Download PDFInfo
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- CN106556535B CN106556535B CN201610984204.2A CN201610984204A CN106556535B CN 106556535 B CN106556535 B CN 106556535B CN 201610984204 A CN201610984204 A CN 201610984204A CN 106556535 B CN106556535 B CN 106556535B
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- 239000000523 sample Substances 0.000 claims abstract description 96
- 238000012360 testing method Methods 0.000 claims abstract description 33
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- 229910052710 silicon Inorganic materials 0.000 claims abstract description 17
- 239000010703 silicon Substances 0.000 claims abstract description 17
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 18
- 238000011065 in-situ storage Methods 0.000 claims description 16
- 238000001514 detection method Methods 0.000 claims description 14
- 229910052697 platinum Inorganic materials 0.000 claims description 9
- 238000004062 sedimentation Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 6
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- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N3/02—Details
- G01N3/06—Special adaptations of indicating or recording means
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
- G01N2203/0016—Tensile or compressive
- G01N2203/0017—Tensile
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0069—Fatigue, creep, strain-stress relations or elastic constants
- G01N2203/0075—Strain-stress relations or elastic constants
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/0641—Indicating or recording means; Sensing means using optical, X-ray, ultraviolet, infrared or similar detectors
Abstract
The invention discloses a kind of mechanic property test method based on mechanics sensor, step includes：Testing sample is placed on sample deposition, mechanics inductor is put into and fixes, silicon wafer is fixed on to the sample deposition on mobile platform top；The first T-shaped groove is etched on mechanics inductor with focused ion beam, etches the second T-shaped groove on silicon；The I type convex samples being adapted with groove are etched on testing sample simultaneously；By tungsten tipped probe it is Nian Jie with sample after transport into I type grooves it is fixed, tungsten tipped probe is separated with sample by electron beam irradiation；Start the video recording of electron microscope, mobile X-axis mobile platform, until I type convex samples are pulled off；The pulling force data that multiframe consecutive image and mechanics inductor in video recording measure, obtains the mechanical property and stress-strain diagram of testing sample.The present invention is realized to performance tests such as the extension test of material and mechanics while carried out.
Description
Technical field
The present invention relates to test equipment technology, more particularly to a kind of mechanical property based on mechanics sensor to survey
Method for testing.
Background technology
Nano material and nanometer technology are that various countries are paid special attention to and one of the research field paid attention in recent years.When the chi of material
It is very little when narrowing down to Nano grade, its physical property, chemical property, and other properties can greatly difference with it is even complete
Full difference is with it in macro-size（Micron millimeter rank）Under the every characteristic showed.And nanoscale imparting is all kinds of
The special performance of material, increasing scientific research personnel and mechanism is also attracted to be engaged in nanometer material science research and technological development work
Make.
By taking carbon nano-tube material as an example.CNT is typical monodimension nanometer material, it have other many materials without
Excellent mechanics, electricity, thermal property and the chemical property that method matches in excellence or beauty；And all kinds of researchs, including composite, catalysis, electricity
The focus and emphasis research object of the research fields such as chemistry, various kinds of sensors.It there is now thousands upon thousands R＆D institutions and personnel
Studied and product development application study in the basic property for specializing in CNT.Although now many enterprises and research aircraft
Structure has had the technology and ability that manufacture produces a large amount of CNTs, but they clearly can not nearly all produce to them
The performance of CNT make one and correctly, accurately assess, particularly mechanical property.Because the diameter chi of CNT
It is very little very small, it is several nanometers to several tens of nanometers scope, and existing tester can not be completed to Nano grade or micron level
Material carries out extension test, and evaluation and the sign of mechanical property.
Therefore, prior art has yet to be improved and developed.
The content of the invention
In view of above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of mechanical property based on mechanics sensor
Can method of testing, it is intended to which solving tester in the prior art can not complete to evaluate the mechanical property of CNT and table
The defects of sign.
Technical scheme is as follows：
A kind of mechanic property test method based on mechanics sensor, wherein, it the described method comprises the following steps：
S1, testing sample is placed on to sample deposition, and mechanics sensor is fixed on SEM original position
Sample deposition side at the top of the X-axis mobile platform of detection means, testing sample is positioned over sample deposition, and by silicon wafer
Piece is fixed on the nearly sample deposition end on Z axis mobile platform top；Wherein, SEM in situ detection device includes setting
The Y-axis mobile platform on pedestal is put, the X-axis mobile platform being arranged on Y-axis mobile platform, and the Z axis being arranged on pedestal
Mobile platform, the sample deposition are arranged on the nearly Z axis mobile platform end on X-axis mobile platform top；
S2, the first T-shaped groove etched on mechanics sensor by focused ion beam, and etch second on silicon
T-shaped groove, the first T-shaped groove and the described second T-shaped groove composition I type grooves；By focused ion beam in testing sample
On etch the I type convex samples being adapted with the I types groove；
S3, by tungsten tipped probe it is Nian Jie with I type convex samples after, I type convex samples are transported into I type grooves it is fixed,
And tungsten tipped probe is separated with I type convex samples by electron beam irradiation；
S4, the video recording for starting electron microscope, and to specify translational speed to move X-axis mobile platform, until I types is raised
Shape sample pulls off；
The pulling force data that S5, the multiframe consecutive image in video recording and mechanics sensor measure, obtains testing sample
Mechanical property and load-deformation curve.
The mechanic property test method based on mechanics sensor, wherein, the step S2 is specifically included：
S21, the first T-shaped groove etched on mechanics sensor by focused ion beam；
S22, etch the second T-shaped groove on silicon by focused ion beam；
S23, the I type convex samples being adapted with the I types groove are etched on testing sample by focused ion beam
Product.
The mechanic property test method based on mechanics sensor, wherein, the step S3 is specifically included：
S31, after tungsten tipped probe is contacted with I type convex samples, by platinum sedimentation by tungsten tipped probe and I type convex samples
Product are bonded, and I type convex samples are transported to one end and are fixed on the described second T-shaped groove by mobile tungsten tipped probe；
S32, the abutting edge by focused ion beam irradiation tungsten tipped probe and I type convex samples, tungsten tipped probe and I types is raised
Shape sample separates；
S33, I type convex samples are fixed on by the described second T-shaped groove by platinum sedimentation；
S33, mobile X-axis mobile platform and Y-axis mobile platform, the other end of I type convex samples is fixed on described the
One T-shaped groove, and the field section of I type convex samples will be fixed on by the described first T-shaped groove by platinum sedimentation.
The mechanic property test method based on mechanics sensor, wherein, the translational speed is 0.3-0.7nm/s.
The mechanic property test method based on mechanics sensor, wherein, the translational speed is 0.5nm/s.
The mechanic property test method based on mechanics sensor, wherein, the top length of the first T-shaped groove is
15 microns, bottom lengths be 2 microns, width be 6 microns, depth be 4 microns.
The mechanic property test method based on mechanics sensor, wherein, the top length of the second T-shaped groove is
15 microns, bottom lengths be 2 microns, width be 6 microns, depth be 4 microns.
The mechanic property test method based on mechanics sensor, wherein, the length of the I types convex sample is 20
Micron, width are 4 microns, thickness is less than 1 micron.
Mechanic property test method provided by the present invention based on mechanics sensor, step include：Testing sample is put
Put in sample deposition, be put into mechanics sensor and fix, silicon wafer is fixed on to the sample deposition on mobile platform top；With poly-
Pyrophosphate ion beam etches the first T-shaped groove on mechanics sensor, etches the second T-shaped groove on silicon；Simultaneously to be measured
The I type convex samples being adapted with groove are etched on sample；By tungsten tipped probe it is Nian Jie with sample after transport into I type grooves it is solid
It is fixed, tungsten tipped probe is separated with sample by electron beam irradiation；The video recording of startup electron microscope, mobile X-axis mobile platform, until
I type convex samples are pulled off；The pulling force data that multiframe consecutive image and mechanics sensor in video recording measure, is obtained
The mechanical property and load-deformation curve of testing sample.The present invention realizes to be surveyed to performances such as the extension test of material and mechanics
Examination is carried out simultaneously.
Brief description of the drawings
Fig. 1 is the flow chart of the mechanic property test method preferred embodiment of the present invention based on mechanics sensor.
Fig. 2 is the structural representation of SEM in situ detection device in the present invention.
Embodiment
The present invention provides a kind of tensile test method based on atomic force microscope probe, to make the purpose of the present invention, skill
Art scheme and effect are clearer, clear and definite, and the present invention is described in more detail below.It should be appreciated that tool described herein
Body embodiment only to explain the present invention, is not intended to limit the present invention.
Fig. 1 and Fig. 2 are please also refer to, wherein Fig. 1 is the Mechanics Performance Testing side of the present invention based on mechanics sensor
The flow chart of method preferred embodiment, Fig. 2 are the structural representation of SEM in situ detection device in the present invention.Such as figure
Shown in 1 and Fig. 2, the mechanic property test method based on mechanics sensor, including：
Step S1, testing sample is placed on sample deposition, and mechanics sensor is fixed on SEM
Sample deposition side at the top of the X-axis mobile platform of in situ detection device, testing sample is positioned over sample deposition, and will
Silicon wafer is fixed on the nearly sample deposition end on Z axis mobile platform top；Wherein, SEM in situ detection device bag
The Y-axis mobile platform being arranged on pedestal is included, the X-axis mobile platform being arranged on Y-axis mobile platform, and be arranged on pedestal
Z axis mobile platform, the sample deposition are arranged on the nearly Z axis mobile platform end on X-axis mobile platform top；
Step S2, the first T-shaped groove is etched on mechanics sensor by focused ion beam, and etched on silicon
Second T-shaped groove, the first T-shaped groove and the described second T-shaped groove composition I type grooves；By focused ion beam to be measured
The I type convex samples being adapted with the I types groove are etched on sample；
Step S3, by tungsten tipped probe it is Nian Jie with I type convex samples after, I type convex samples are transported into I type grooves solid
It is fixed, and separated tungsten tipped probe with I type convex samples by electron beam irradiation；
Step S4, the video recording of electron microscope is started, and to specify translational speed to move X-axis mobile platform, until by I types
Convex sample pulls off；
Step S5, the pulling force data that multiframe consecutive image and mechanics sensor in video recording measure, obtains treating test sample
The mechanical property and load-deformation curve of product
More specifically, as shown in Fig. 2 the SEM in situ detection device includes：
Base 10；
Y-axis mobile platform 200, the Y-axis mobile platform 200 are arranged on the base 10；
X-axis mobile platform 100, the X-axis mobile platform 100 are arranged on the Y-axis mobile platform 200, and are moved in Y-axis
Mobile 100 on moving platform；
Sample deposition 110, the sample deposition 110 are arranged on the top of X axles mobile platform 100；
Mechanics sensor 120, the mechanics sensor 120 are arranged on the side of the sample deposition 110;
Z axis mobile platform 300, the Z axis mobile platform 300 are arranged on base 10, and are made relative to the base 10
Rise or fall motion；
Silicon wafer 310, the silicon wafer 310 are arranged on the nearly sample deposition end on the top of Z axis mobile platform 3000；
Pressure is provided with the X-axis mobile platform 100, the Y-axis mobile platform 200 and axle mobile platform 300 described in Z
Electric sub-prime control unit；The piezoelectricity sub-prime control unit includes the elongation piezoelectricity pottery directly proportional to electric-field intensity square
Porcelain.
Wherein, after applying voltage on the piezoelectricity sub-prime control unit, piezoelectric ceramics can extend, so as to drive the X-axis
Mobile platform 100, the Y-axis mobile platform 200 or axle mobile platform 300 described in Z move, and the elongation of piezoelectric ceramics and electricity
Field intensity square is directly proportional.
In embodiments of the present invention, the step S2 is specifically included：
Step S21, the first T-shaped groove is etched on mechanics sensor 120 by focused ion beam；
Step S22, the second T-shaped groove is etched on silicon by focused ion beam；
Step S23, it is raised that the I types being adapted with the I types groove are etched on testing sample by focused ion beam
Shape sample.
Further, the step S3 is specifically included：
Step S31, it is by platinum sedimentation that tungsten tipped probe and I types is raised after tungsten tipped probe is contacted with I type convex samples
Shape sample is bonded, and I type convex samples are transported to one end and are fixed on the described second T-shaped groove by mobile tungsten tipped probe；
Step S32, by the abutting edge of focused ion beam irradiation tungsten tipped probe and I type convex samples, by tungsten tipped probe and I types
Convex sample separates；
Step S33, I type convex samples are fixed on by the described second T-shaped groove by platinum sedimentation；
Step S33, mobile X-axis mobile platform and Y-axis mobile platform, are fixed on institute by the other end of I type convex samples
The first T-shaped groove is stated, and the field section of I type convex samples will be fixed on by the described first T-shaped groove by platinum sedimentation.
Specifically, the x-axis translational speed is 0.3-0.7nm/s；0.5nm/s is preferably embodiment.
Further, the top length of the described first T-shaped groove is 15 microns, bottom lengths are 2 microns, width is 6 micro-
Rice, depth are 4 microns.
Further, the top length of the described second T-shaped groove is 15 microns, bottom lengths are 2 microns, width is 6 micro-
Rice, depth are 4 microns.
Further, the length of the I types convex sample is 20 microns, width is 4 microns, thickness is less than 1 micron.
Preferably, X-axis moving range of the X-axis mobile platform 100 under roughcast formula is 0-8 mm, X-axis coarse motion speed
For 0.4 mm/s, X-axis Minimum sliding distance is 0.01 um；The X-axis movement model of the X-axis mobile platform 100 in the fine mode
It is 0.1 nm to enclose for 0-20 um, X-axis Minimum sliding distance；Y-axis moving range of the Y-axis mobile platform 200 under roughcast formula
For 0-8 mm, Y-axis coarse motion speed is 0.4 mm/s, and Y-axis Minimum sliding distance is 0.01 um；The Y-axis mobile platform 200 exists
Y-axis moving range under fine pattern is 0-20 um, and Y-axis Minimum sliding distance is 0.1 nm；The Z axis mobile platform 300 exists
Z axis moving range under roughcast formula is 0-8 mm, and Z axis translational speed is 0.4 mm/s, and Z axis Minimum sliding distance is 0.01 um；
The Z axis moving range of the Z axis mobile platform 300 in the fine mode is 0-20 um, and Z axis Minimum sliding distance is 0.1 nm.
SEM in situ detection device of the present invention, which is one, to be realized to material by nanometer
Yardstick is observed to the dynamic in-situ of centimeter scale, the precision apparatus that can be tested simultaneously performances such as its physics again.At present
There is no the in-situ monitoring that any set of device can realize nano-scale and cm size simultaneously, less with carrying between two yardsticks
Dynamic transition in situ.Extension test is realized using the SEM in situ detection device as carrier, it is acceptable while right
The performances such as its mechanics are tested.
Why SEM in situ detection device of the present invention is better than existing similar device, be because
Its unique piezoelectricity sub-prime control unit design so that its controllable displacement range can be continuously from microcosmic Nano grade transition
To micron/centimetre rank of macroscopic view, otherwise and other existing any SEM Platform Designings can be only done nanometer
Displacement on yardstick, or can be only done the displacement of micron/mm-scale, controllable motion is on microcosmic and macro-size
Separated, thus when doing material properties test, Line Continuity dynamic measuring control can not be entered to same position or material.Need especially
It is proposed, platform moving displacement resolution ratio can reach Ethylmercurichlorendimide（10-10m）Rank, equivalent to the distance of several atoms, this is also
The controllable minimum length scope of the mankind at present.
SEM in situ detection device of the present invention simultaneously can applying power is minimum arrives nN ranks, be up to
10 N, for test object material, the scope of this applying power, which can cover the almost present mankind, to be manufactured
All intensity material.SEM in situ detection device not only tests nanotube, the performance of nanometer wire, goes back
Micron and the sample of Centimeter Level, such as micrometer fibers or film can be tested.Material is also accurately controlled to be continuously completed
Realize that the continuity from microcosmic perturbation to macroscopic appearance truly is moved to the displacement movement of millimeter again from nanometer to micron
State monitors, and realtime graphic and data result synchronism output.
In summary, the mechanic property test method provided by the present invention based on mechanics sensor, step include：It will treat
Test sample product are placed on sample deposition, are put into mechanics sensor and fix, the sample that silicon wafer is fixed on to mobile platform top is put
Put area；The first T-shaped groove is etched on mechanics sensor with focused ion beam, etches the second T-shaped groove on silicon；Together
When the I type convex samples being adapted with groove are etched on testing sample；By tungsten tipped probe it is Nian Jie with sample after transport to I types
It is fixed in groove, tungsten tipped probe is separated with sample by electron beam irradiation；Start the video recording of electron microscope, mobile X-axis movement
Platform, until I type convex samples are pulled off；The pulling force that multiframe consecutive image and mechanics sensor in video recording measure
Data, obtain the mechanical property and load-deformation curve of testing sample.The present invention realizes the extension test and mechanics to material
Carried out simultaneously Deng performance test.
It should be appreciated that the application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can
To be improved or converted according to the above description, all these modifications and variations should all belong to the guarantor of appended claims of the present invention
Protect scope.
Claims (8)
1. a kind of mechanic property test method based on mechanics sensor, it is characterised in that the described method comprises the following steps：
S1, testing sample is placed on to sample deposition, and mechanics inductor is fixed on SEM in situ detection
Sample deposition side at the top of the X-axis mobile platform of device, testing sample is positioned over sample deposition, and silicon wafer is consolidated
Due to the nearly sample deposition end on Z axis mobile platform top；Wherein, SEM in situ detection device includes being arranged on
Y-axis mobile platform on pedestal, the X-axis mobile platform being arranged on Y-axis mobile platform, and the Z axis movement being arranged on pedestal
Platform, the sample deposition are arranged on the nearly Z axis mobile platform end on X-axis mobile platform top；
S2, the first T-shaped groove etched on mechanics inductor by focused ion beam, and it is T-shaped to etch second on silicon
Groove, the first T-shaped groove and the described second T-shaped groove composition I type grooves；Lost by focused ion beam on testing sample
Carve the I type convex samples being adapted with the I types groove；
S3, by tungsten tipped probe it is Nian Jie with I type convex samples after, I type convex samples are transported into I type grooves fixed, and led to
Electron beam irradiation is crossed to separate tungsten tipped probe with I type convex samples；
S4, the video recording for starting electron microscope, and to specify translational speed to move X-axis mobile platform, until by I type convex samples
Product pull off；
The pulling force data that S5, the multiframe consecutive image in video recording and mechanics inductor measure, obtains the mechanics of testing sample
Performance and load-deformation curve.
2. the mechanic property test method according to claim 1 based on mechanics sensor, it is characterised in that the step S2
Specifically include：
S21, the first T-shaped groove etched on mechanics inductor by focused ion beam；
S22, etch the second T-shaped groove on silicon by focused ion beam；
S23, the I type convex samples being adapted with the I types groove are etched on testing sample by focused ion beam.
3. the mechanic property test method according to claim 2 based on mechanics sensor, it is characterised in that the step S3
Specifically include：
S31, after tungsten tipped probe is contacted with I type convex samples, tungsten tipped probe and I type convex samples are glued by platinum sedimentation
Connect, and I type convex samples are transported to one end and are fixed on the described second T-shaped groove by mobile tungsten tipped probe；
S32, the abutting edge by focused ion beam irradiation tungsten tipped probe and I type convex samples, by tungsten tipped probe and I type convex samples
Product separate；
S33, I type convex samples are fixed on by the described second T-shaped groove by platinum sedimentation；
S33, mobile X-axis mobile platform and Y-axis mobile platform, it is T-shaped to be fixed on described first by the other end of I type convex samples
Groove, and the field section of I type convex samples will be fixed on by the described first T-shaped groove by platinum sedimentation.
4. the mechanic property test method according to claim 3 based on mechanics sensor, it is characterised in that the mobile speed
Spend for 0.3-0.7nm/s.
5. the mechanic property test method according to claim 4 based on mechanics sensor, it is characterised in that the mobile speed
Spend for 0.5nm/s.
6. the mechanic property test method according to claim 2 based on mechanics sensor, it is characterised in that the first T
The top length of type groove is 15 microns, bottom lengths are 2 microns, width is 6 microns, and depth is 4 microns.
7. the mechanic property test method according to claim 2 based on mechanics sensor, it is characterised in that the 2nd T
The top length of type groove is 15 microns, bottom lengths are 2 microns, width is 6 microns, and depth is 4 microns.
8. the mechanic property test method according to claim 2 based on mechanics sensor, it is characterised in that the I types are convex
The length for playing shape sample is 20 microns, width is 4 microns, thickness is less than 1 micron.
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| US8499645B2 (en) * | 2007-02-21 | 2013-08-06 | The Board Of Trustees Of The University Of Illinois | Stress micro mechanical test cell, device, system and methods |
| CN101109687B (en) * | 2007-07-20 | 2010-06-02 | 北京工业大学 | Testing device for force-electricity property under nanowire original position stretching in transmission electron microscope |
| CN101261206B (en) * | 2008-01-30 | 2010-11-03 | 吉林大学 | Material nanometer dynamic performance test two freedom degree loading unit |
| CN105158073A (en) * | 2015-09-22 | 2015-12-16 | 哈尔滨工业大学 | Carbon nano tube end and carbon fiber surface grafting strength measuring method |
| CN105300794B (en) * | 2015-09-23 | 2018-04-27 | 上海大学 | The parallel stretching test system of nanofiber and method |
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