CN205749569U - A kind of nano material mechanics performance in-situ test system - Google Patents
A kind of nano material mechanics performance in-situ test system Download PDFInfo
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- CN205749569U CN205749569U CN201620700597.5U CN201620700597U CN205749569U CN 205749569 U CN205749569 U CN 205749569U CN 201620700597 U CN201620700597 U CN 201620700597U CN 205749569 U CN205749569 U CN 205749569U
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Abstract
This utility model provides a kind of nano material mechanics performance in-situ test system, including scanning electron microscope, scans probe test unit, control unit and computer；Scanning probe test unit includes base, is located at the regulating platform of base upper surface side, is located at the measuring mechanism of base upper surface opposite side；Scanning electron microscope includes Electronic Speculum pole shoe, and regulating platform is provided with sample stage, X-axis adjusting means, Y-axis adjusting means, Z axis adjusting means；Measuring mechanism includes laser optical path adjusting means, the probe base being located on base, and the probe being located on probe base, and probe is positioned at below Electronic Speculum pole shoe, and laser optical path adjusting means is used for collimating and focusing on laser.This utility model truly achieves and scans the evolution process of sample micro structure under the mechanism of probe and sample and outfield physical mechanics effect in scanning electron microscope home position observation test process, and the micro image of chain of events and data of mechanical are transferred to the function of computer.
Description
Technical field
This utility model relates to microstructure performance detection apparatus technical field, particularly relates to a kind of nano material mechanics
Performance in-situ test system.
Background technology
During the progress and development of nanoscale science and technology, two class scientific instrument have played important impetus,
One class is the ultramicroscope using electron beam as probe, representative have transmission electron microscope (TEM) and scanning electron microscopy
Mirror (SEM)；Another kind of is the scanning probe microscopy (SPM) using solid needle point as probe, and representational have scanning-tunnelling to show
Micro mirror (STM) and atomic force microscope (AFM).
But be as micro-nano device fast development and on yardstick approaching to the nanometer limit, how to characterize micro-
Nanometer sized materials, structure and device act in outfield (stress field of electric field, thermal field and induction in such as device operation)
Under character, performance and variation tendency become study frontier and the focus in nanoscale science and technology field, with seek new material,
Further breakthrough in terms of new technique, new technology.
Realize physical property under outer field action of nano material, structure and device and microstructure dependency
Measure and characterize, need to realize reliable fixing, applying outer field action and the Trinitarian measurement of microexamination simultaneously.
The microcosmic such as current PSTM, atomic force microscope, scanning electron microscope, transmission electron microscope
Analyze and test instrunment has played important in terms of structure, pattern, composition and the performance test such as mechanics, electricity of nano material
Effect, becomes current people and probes into the main method of the various physical property of nano material.But, these instruments are only capable of nanometer material
Material carries out the measurement of single aspect, it is impossible to enough meets and handles sample simultaneously and measure, and the merit in situ, dynamically observed
Can, it is difficult to realize reliable fixing, applying outer field action and the Trinitarian measurement of microexamination.
Utility model content
The purpose of this utility model is to provide one and is capable of reliable fixing, applying External Force Acting and microexamination three
The in-situ test system measuring nanometer dynamic performance of position one.This utility model combines scanning electron microscope and scanning probe
The fresh approach of microtechnique development and technology, devise the scanning can being arranged in scanning electron microscope sample room and visit
Pin test cell, develops nano material mechanics performance based on scanning probe test function in scanning electron microscope sample room
Home position testing method.
For achieving the above object, this utility model provides a kind of nano material mechanics performance in-situ test system, including
Scanning electron microscope, is located at the scanning probe test unit within the sample room of described scanning electron microscope, sweeps with described
Retouch the control unit that ultramicroscope is connected, and the meter being connected with described control unit with described scanning probe test unit
Calculation machine；Described scanning probe test unit includes base, is located at the regulating platform of described base upper surface side, is located at described base
The measuring mechanism of upper surface opposite side；Described scanning electron microscope includes that Electronic Speculum pole shoe, described regulating platform are provided with sample stage,
X-axis adjusting means that described sample stage moves along described regulating platform length direction can be made, described sample stage can be made along being perpendicular to institute
State regulating platform length direction and be perpendicular to the Y-axis adjusting means that the direction of described base upper surface is moved, and sample stage can be made
Along being perpendicular to the length direction of described regulating platform and being parallel to the Z axis adjusting means that the direction of described base upper surface is moved；X-axis
Be parallel to described regulating platform length direction and be parallel to described base upper surface, Y-axis be perpendicular to described regulating platform length direction and
Being perpendicular to the upper surface of described base, Z axis is perpendicular to regulating platform length direction and is parallel to described base upper surface, described sample
Platform surface is positioned at the plane that described X-axis is constituted with described Y-axis；Described measuring mechanism includes laser optical path adjusting means, is located at
Probe base on base, and it is located at the probe on described probe base, described probe is positioned at below described Electronic Speculum pole shoe, institute
State laser optical path adjusting means for collimating and focusing on laser.
Optionally, described X-axis adjusting means includes the X-axis lower guideway being fixed on described regulating platform upper surface, is located at described X
X-axis upper rail on axle lower guideway, described X-axis upper rail is provided with X-axis linear electric motors, one end of described X-axis linear electric motors and institute
Stating X-axis lower guideway to be connected, described X-axis linear electric motors are connected with described control unit.
Optionally, described Y-axis adjusting means includes the Y-axis lower guideway being fixed on described X-axis upper rail upper surface, is located at institute
Stating the Y-axis upper rail on Y-axis lower guideway, described Y-axis upper rail is provided with Y-axis linear electric motors, one end of described Y-axis linear electric motors with
Described Y-axis lower guideway connects, and described Y-axis linear electric motors are connected with described control unit.
Optionally, described Z axis adjusting means includes the Z axis lower guideway being fixed on described Y-axis upper rail upper surface, is located at institute
Stating the Z axis upper rail on Z axis lower guideway, described Z axis lower guideway is provided with Z axis linear electric motors, one end of described Z axis linear electric motors with
Described Z axis upper rail connects, and described Z axis linear electric motors are connected with control unit.
Optionally, X-axis piezoelectric ceramics, Y-axis piezoelectric ceramics and Z axis piezoelectricity pottery it are provided with between described regulating platform and sample stage
Porcelain, described X-axis piezoelectric ceramics is used for the displacement fine setting along X axis of the described sample stage, and described Y-axis piezoelectric ceramics is used for described sample
Platform is finely tuned along the displacement of Y-axis, and described Z axis piezoelectric ceramics is finely tuned along the displacement of Z-axis direction for described sample stage, described X-axis pressure
Electroceramics, Y-axis piezoelectric ceramics are connected with described control unit respectively with Z axis piezoelectric ceramics.
Optionally, described laser optical path adjusting means includes laser sight, reflecting mirror group, four-quadrant photo detector,
And regulate the second laser regulation of the first laser modulation device of described laser sight deflection, the regulation reflecting mirror group anglec of rotation
Device and the 3rd laser modulation device, regulate the 4th laser modulation device that described four-quadrant photo detector moves；Described laser aiming
Device is oppositely arranged with described four-quadrant photo detector, and described reflecting mirror is mounted on described laser sight and described four-quadrant light
Between electric explorer, and it is located at described sample stage table top just to position, described four-quadrant photo detector and described control unit
Being connected, described laser sight is connected with generating laser by optical fiber.
Optionally, described sample room is provided with hatch door, described hatch door be provided with Function Extension signal connect hole, signal wire interface,
Ground wire connects hole and optical fiber connects hole.
Optionally, the axis direction of the electron beam that described Electronic Speculum pole shoe is launched is 20 with the angle of described sample stage table top
～30 °, the tip of described electron beam is irradiated to the tip of described probe.
This utility model additionally provides one and utilizes nano material mechanics performance in-situ test system test nano material force
The method learning performance, described nano material mechanics performance in-situ test system includes scanning electron microscope, is located at described
Scanning probe test unit within the sample room of scanning electron microscope, visits with described scanning electron microscope and described scanning
The control unit that pin test cell is connected, and the computer being connected with described control unit；Described scanning probe test list
Unit includes base, is located at the regulating platform of described base upper surface side, is located at the measuring mechanism of described base upper surface opposite side；
Described scanning electron microscope includes that Electronic Speculum pole shoe, described regulating platform are provided with sample stage, and described sample stage can be made along described tune
X-axis adjusting means that joint platform length direction moves, described sample stage can be made along being perpendicular to described regulating platform length direction and vertical
The Y-axis adjusting means moved in the direction of described base upper surface, and sample stage can be made along the length being perpendicular to described regulating platform
Spend direction and be parallel to the Z axis adjusting means that the direction of described base upper surface is moved；X-axis is parallel to described regulating platform length side
To and be parallel to described base upper surface, Y-axis is perpendicular to described regulating platform length direction and is perpendicular to the upper table of described base
Face, Z axis is perpendicular to regulating platform length direction and is parallel to described base upper surface, described sample stage surface be positioned at described X-axis with
In the plane that described Y-axis is constituted；Described measuring mechanism includes laser optical path adjusting means, the probe base being located on base, with
And it is located at the probe on described probe base, described probe is positioned at below described Electronic Speculum pole shoe, described laser optical path adjusting means
For collimating and focusing on laser；The method of described test nano material mechanics performance comprises the following steps:
Regulation laser optical path adjusting means, makes laser focusing arrive the center of described four-quadrant photo detector；
Control X-axis adjusting means, Y-axis adjusting means and the position of Z axis adjusting means regulation sample stage, make on sample stage
Sample is positioned at immediately below described probe；
Evacuation, opens electron beam, focuses on electron beam to probe tip；
Control X-axis piezoelectric ceramics and the position of Y-axis piezoelectric ceramics regulation sample stage, make probe tip contact with sample；
The sample controlled on Z axis adjusting means regulation sample stage contacts with probe；
Control Z axis piezoelectric ceramics regulation sample stage, make probe to sample imposed load；
Obtain load value；When load value reaches desired value, control Z axis piezoelectric ceramics stop motion and return to original state；
Control computer recording and export the photosignal of four-quadrant photo detector and piezoelectric ceramics position in loading procedure
Move relation curve.
Optionally, sample is fixed on described sample stage, shuts the hatch door of scanning electron microscope, after evacuation, and scanning
The electron gun high voltage of ultramicroscope, then open electron beam, adjust scanning electron microscope duty, amplify in difference
Observe scanning probe microscopy under multiplying power and nano material is carried out the microprocess of Mechanics Performance Testing.
The specific embodiment provided according to this utility model, the utility model discloses techniques below effect:
X-axis in scanning probe test unit in the nano material mechanics performance in-situ test system that this utility model provides
Adjusting means, Y-axis adjusting means and Z axis adjusting means can regulate sample stage, it is also possible to fixing sample stage, it is achieved sample
Stable fixing；And change position owing to sample stage can also pass through X-axis adjusting means, Y-axis adjusting means and Z axis adjusting means
And angle of inclination, therefore it also is able to the effect realizing that sample is applied outfield；Owing to test system of the present utility model also includes
Scanning electron microscope, it is possible to by scanning electron microscope Real Time Observation micro-image.Therefore, this utility model provides
Test system is capable of reliable fixing, the applying outer field action to nano material and the Trinitarian measurement of microexamination.
This utility model also has a beneficial effect:
1, the overall structure of the scanning probe test unit in this utility model is according in scanning electron microscope sample room
Space, portion is designed, and volume is little, compact conformation, conveniently installs and dismantles, easy and simple to handle, and testing precision is high.It addition,
The sample stage of this scanning probe test unit and beam direction are the angle of 30 °, facilitate electron beam to test and manipulation process
Real-time monitored, it is to avoid blocked by other structures and affect the problem of real-time monitored, further increase measuring accuracy.
2, the scanning electron microscope sample room in this utility model devises some wiring holes, can not only realize scanning
The connection of probe test unit and external control unit outside, and can also the multiple additional thing such as attachment force field, electric field, thermal field, magnetic field
Reason field, it is achieved the expansion of Joint Systems Test function.
3, scanning electron microscope is combined by this utility model with scanning probe test unit, electron beam
Scanning imagery is handled can carry out simultaneously with scanning probe micro-nano, does not interfere with each other, it is achieved original position outfield physics truly
Performance test function.
4, the scanning probe scanning probe test unit in this utility model can be carried out more easily according to experiment demand
Change, it is achieved material nano material mechanics performance under different loads, different method of testing and different probe pressure head effect is surveyed
Examination function.
Accompanying drawing explanation
In order to be illustrated more clearly that this utility model embodiment or technical scheme of the prior art, below will be to embodiment
The accompanying drawing used required in is briefly described, it should be apparent that, the accompanying drawing in describing below is the most of the present utility model
Some embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to according to
These accompanying drawings obtain other accompanying drawing.
Fig. 1 is the scanning probe test unit three-dimensional structural representation in this utility model；
Fig. 2 is the scanning probe test unit plan structure schematic diagram in this utility model；
Fig. 3 is that the needle point scanning probe in the scanning probe test unit in this utility model contacts partial enlargement with sample
Figure；
Fig. 4 is the scanning probe test unit middle probe needle point in this utility model, sample and scanning electron microscope electron beam angle
Degree schematic diagram；
Fig. 5 is the scanning electron microscope sample room structural representation in this utility model；
Fig. 6 is the three-dimensional appearance image of this utility model scanning probe test in-situ test groove structure；
Fig. 7 is that the scanning probe in this utility model carries out the scanogram in original position manipulation process to nano-particle；
Fig. 8 is two ends fixed pattern nano wire three-point bending procedure charts；
Fig. 9 is two ends free type nano wire three-point bending procedure charts；
Figure 10 is photosignal output and the piezoelectric ceramics displacement of the four-quadrant photo detector of nano material in-situ test
Graph of relation；
Figure 11 is the force-displacement curve of this utility model nano silver wire three-point bend test in situ and output.
Detailed description of the invention
Below in conjunction with the accompanying drawing in this utility model embodiment, the technical scheme in this utility model embodiment is carried out
Clearly and completely describe, it is clear that described embodiment is only a part of embodiment of this utility model rather than whole
Embodiment.Based on the embodiment in this utility model, those of ordinary skill in the art are not under making creative work premise
The every other embodiment obtained, broadly falls into the scope of this utility model protection.
As Figure 1-5, this utility model provides a kind of nano material mechanics performance in-situ test system, including scanning
Ultramicroscope 1, is located at the scanning probe test unit 2 within sample room 11 of scanning electron microscope 1, shows with scanning electron
The control unit that micro mirror 1 is connected with scanning probe test unit 2, and the computer being connected with control unit；Scanning probe
Test cell 2 includes base 21, is located at the regulating platform 22 of base 21 upper surface side, is located at the survey of base 21 upper surface opposite side
Measuring mechanism；Scanning electron microscope 1 includes that Electronic Speculum pole shoe 12, regulating platform 22 are provided with sample stage 23, and sample stage 23 can be made along tune
X-axis adjusting means 24 that joint platform 22 length direction moves, sample stage 23 can be made along being perpendicular to regulating platform 22 length direction and vertical
In the Y-axis adjusting means 25 that the direction of base 21 upper surface is moved, and sample stage 23 can be made along the length being perpendicular to regulating platform 22
Spend direction and be parallel to the Z axis adjusting means 26 that the direction of base 21 upper surface is moved；X-axis is parallel to regulating platform 22 length direction
And it being parallel to base 21 upper surface, Y-axis is perpendicular to regulating platform 22 length direction and is perpendicular to the upper surface of base 21, and Z axis is vertical
In regulating platform 22 length direction and be parallel to base 21 upper surface, sample stage 23 surface is positioned at the plane that X-axis is constituted with Y-axis；
Measuring mechanism includes laser optical path adjusting means 27, the probe base 28 being located on base 21, and is located on probe base 28
Probe 281, probe 281 is positioned at below Electronic Speculum pole shoe 12, and laser optical path adjusting means 27 is used for collimating and focusing on laser.
This utility model is by being integrated into scanning electron microscope 1 sample by the scanning probe microscopy unit of compact conformation
In room 11, it is utilized respectively function and scanning probe microscopy that sample microcosmic tested by scanning electron microscope 1 and sample is carried out
The function of the test such as micro-scale mechanics, electricity, constituent material original position, online morphology feature are integrated with physical property
Analysis of test system.Scanning electron microscope 1 is combined by this utility model with scanning probe test unit 2,
Electron beam scanning imaging is handled can carry out simultaneously with scanning probe micro-nano, does not interfere with each other, it is achieved outside original position truly
Field quantitative measurement function.The overall structure of scanning probe test unit 2 is internal according to scanning electron microscope 1 sample room 11
Space is designed, and volume is little, compact conformation, conveniently installs and dismantles, easy and simple to handle, and testing precision is high.This practicality
The probe 281 of novel middle scanning probe test unit 2 can be replaced easily according to experiment demand, it is achieved material is in difference
Quantitative measurement function under load, different method of testing and different physical field effect.This system structure is compact, operation letter
Just, organically combine the test function of scanning electron microscope 1 and scanning probe microscopy, can be widely applied to micro-nano
Bar-shaped, filamentary material, the thin-film material of yardstick, the microstructure of the materials such as micro-nano granules, the one of the performance such as mechanics, electricity
Change in site measurement.
As the optional embodiment of one, X-axis adjusting means 24 includes being fixed on to be led under the X-axis of regulating platform 22 upper surface
Rail 241, the X-axis upper rail 242 being located on X-axis lower guideway 241, X-axis upper rail 242 is provided with X-axis linear electric motors 243, X-axis straight line
One end of motor 243 is connected with X-axis lower guideway 241, and X-axis linear electric motors 243 are connected with control unit.Control unit controls X
Axle linear electric motors 243 move, owing to one end of X-axis linear electric motors 243 is connected with X-axis lower guideway 241, and therefore X-axis linear electric motors
The athletic meeting of 243 drives X-axis upper rail 242 to translate, then also sample stage 23 will be driven to put down along X-axis by X-axis upper rail 242
Move, it is achieved that sample stage 23 is along the movement of X-axis.
As the optional embodiment of one, Y-axis adjusting means 25 includes the Y-axis being fixed on X-axis upper rail 242 upper surface
Lower guideway 251, the Y-axis upper rail 252 being located on Y-axis lower guideway 251, Y-axis upper rail 252 is provided with Y-axis linear electric motors 253, Y-axis
The other end of linear electric motors 253 is connected with Y-axis lower guideway 251, and Y-axis linear electric motors 253 are connected with control unit.Control unit
Control Y-axis linear electric motors 253 to move, owing to the other end of Y-axis linear electric motors 253 is connected with Y-axis lower guideway 251, therefore Y-axis
The athletic meeting of linear electric motors 253 drives Y-axis upper rail 252 to translate, then also will drive sample stage by Y-axis upper rail 252
23 translate along Y-axis, it is achieved that sample stage 23 is along the movement of Y-axis.
As the optional embodiment of one, Z axis adjusting means 26 includes the Z axis being fixed on Y-axis upper rail 252 upper surface
Lower guideway 261, the Z axis upper rail 262 being located on Z axis lower guideway 261, Z axis lower guideway 261 is provided with Z axis linear electric motors 263, Z axis
The other end of linear electric motors 263 is connected with Z axis upper rail 262, and Z axis linear electric motors 263 are connected with control unit.Control unit
Controlling Z axis linear electric motors 263 to move, owing to the other end of Z axis linear electric motors 263 is connected with Z axis upper rail 262, therefore Z axis is straight
The athletic meeting of line motor 263 drives Z axis upper rail 262 to translate, then also will drive sample stage 23 by Z axis upper rail 262
Translate along Z axis, it is achieved that sample stage 23 is along the movement of Z axis.
As the optional embodiment of one, between regulating platform 22 and sample stage 23, it is provided with X-axis piezoelectric ceramics 231, Y-axis pressure
Electroceramics 232 and Z axis piezoelectric ceramics 233, X-axis piezoelectric ceramics 231 is used for the sample stage 23 displacement fine setting along X axis, Y-axis piezoelectricity
Pottery 232 is finely tuned along the displacement of Y-axis for sample stage 23, and Z axis piezoelectric ceramics 233 is used for the sample stage 23 displacement along Z-axis direction
Fine setting, X-axis piezoelectric ceramics 231, Y-axis piezoelectric ceramics 232 are connected with control unit respectively with Z axis piezoelectric ceramics 233.By control
Unit processed controls X-axis piezoelectric ceramics 231 and realizes X with Y-axis piezoelectric ceramics 232, and Y-direction displacement is finely tuned, and Z axis piezoelectric ceramics 233 is real
Existing Z-direction displacement fine setting.Under scanning electron microscope image formation state, observe probe 281 sample is carried out microcell mechanics, calorifics
Deng performance test, real time record sample structural information under outer field action and performance change, pass through information processing system simultaneously
The voltage signal receiving four-quadrant photo detector carries out Treatment Analysis, i.e. can get the microcell mechanics of sample, calorifics etc.
Performance, it is thus achieved that structure more accurate.
As the optional embodiment of one, laser optical path adjusting means 27 includes laser sight 271, reflecting mirror group,
Four-quadrant photo detector 272, and the first laser modulation device 273 of regulation laser sight 271 deflection, regulation reflecting mirror group
Second laser modulation device 274 and the 3rd laser modulation device 275 of the anglec of rotation, regulation four-quadrant photo detector 272 moves
4th laser modulation device 276；Laser sight 271 is oppositely arranged with four-quadrant photo detector 272, and reflecting mirror is mounted on laser
Between sight 271 and four-quadrant photo detector 272, and it is located at sample stage 23 table top just to position, four-quadrant photodetection
Device 272 is connected with control unit, and laser sight 271 is connected with generating laser 29 by optical fiber.Laser passes through laser
Sight 271 is irradiated into the laser optical path of scanning probe test unit 2, and the first reflecting mirror 277 in reflecting mirror group,
The multiple reflections of the second reflecting mirror 278 in probe 281, reflecting mirror group is irradiated to the photosensitive area of four-quadrant photo detector 272.
Regulate the second laser modulation device the 274, the 3rd laser modulation device the 275, first laser modulation device 273 and the 4th laser modulation device successively
276 adjust respectively the anglec of rotation of first reflecting mirror the 277, second reflecting mirror 278, the incoming position of laser sight 271, four
Limit, as the displacement of photodetector 272, makes laser focusing to optimum state and be in four limits as photodetector 272 photosensitive area
The most central.Guarantee focusing and the collimation of light path, provide safeguard for measuring accuracy.
As the optional embodiment of one, sample room 11 is provided with hatch door 17, and hatch door 17 is provided with Function Extension signal and connects
Hole 13, signal wire interface 14, ground wire connects hole 15 and optical fiber connects hole 16.Sample room 11 hatch door 17 of scanning electron microscope 1 has
There are some wiring holes, it is simple to scanning probe test unit 2 couples and functions expanding with external control unit outside.Wherein Function Extension
Signal connects hole 13 can connect the outfields such as the field of force, electric field, thermal field, magnetic field, it is achieved the expansion of Joint Systems Test function；Holding wire
Interface 14 uses self-feeding type connector binding post, connects internal SPM test cell and external control unit outside, controls SPM test single
The operation of unit；Ground wire connects hole 15 for discharging unnecessary electric charge, reduces Electronic Speculum imaging interference, improves image quality；Optical fiber connects hole
Outside laser is imported the light path part of sample room 11 inner scanning probe test unit 2 by 16.
As the optional embodiment of one, the folder of the electron beam 121 that Electronic Speculum pole shoe 12 is launched and sample stage 23 table top
Angle is 20～30 °, and the tip of electron beam 121 is irradiated to the tip of probe 281.In order to ensure that test system can be carried out in situ
Observation, probe 281 is positioned at the underface of Electronic Speculum pole shoe 12, and scans sample stage 23 and the electron beam 121 of probe test unit 2
Axis direction is 20～30 ° of angles, makes electron beam 121 can shine directly into the end of probe 281 needle point.When test, protect
Holding needle point static, electron beam 121 focuses on the basis of needle point end.During mobile example platform 23 position, electron beam 121
The relative movement between needle point and sample can be observed clearly.
This utility model additionally provides one and utilizes scanning electron microscope 1 and scanning probe microscopy combined test system
The method of test nano ZnO, scanning electron microscope 1 includes sweeping with scanning probe microscopy combined test system
Retouch ultramicroscope 1, be located at the scanning probe test unit 2 within sample room 11 of scanning electron microscope 1, with scanning electron
The control unit that microscope 1 is connected with scanning probe test unit 2, and the computer being connected with control unit；Scanning is visited
Pin test cell 2 includes base 21, is located at the regulating platform 22 of base 21 upper surface side, is located at base 21 upper surface opposite side
Measuring mechanism；Scanning electron microscope 1 includes that Electronic Speculum pole shoe 12, regulating platform 22 are provided with sample stage 23, can make sample stage 23 edge
X-axis adjusting means 24 that regulating platform 22 length direction moves, sample stage 23 can be made along being perpendicular to regulating platform 22 length direction and hanging down
The straight Y-axis adjusting means 25 moved in the direction of base 21 upper surface, and sample stage 23 can be made along being perpendicular to regulating platform 22
Length direction and be parallel to the Z axis adjusting means 26 that the direction of base upper surface is moved；X-axis is parallel to regulating platform 22 length direction
And it being parallel to base 21 upper surface, Y-axis is perpendicular to regulating platform 22 length direction and is perpendicular to the upper surface of base 21, and Z axis is vertical
In regulating platform 22 length direction and be parallel to base 21 upper surface, sample stage 23 surface is positioned at the plane that X-axis is constituted with Y-axis；
Measuring mechanism includes laser optical path adjusting means 27, the probe base 28 being located on base 21, and is located on probe base 28
Probe 281, probe 281 is positioned at below Electronic Speculum pole shoe 12, and laser optical path adjusting means 27 is used for collimating and focusing on laser；Test
The method of nano ZnO comprises the following steps:
S1: regulation laser optical path adjusting means 27, makes laser focusing to the center of four-quadrant photo detector 272；
S2: control X-axis adjusting means 24, Y-axis adjusting means 25 and Z axis adjusting means 26 and regulate the position of sample stage 23,
The sample on sample stage 23 is made to be positioned at immediately below probe 281；
S3: evacuation, high voltage, open electron beam 121, and focus on the basis of probe 281 tip；
S4: control X-axis piezoelectric ceramics 231 and Y-axis piezoelectric ceramics 232 regulate the position of sample stage 23, makes probe 281 most advanced and sophisticated
Contact with sample；
S5: the sample that control Z axis adjusting means 26 regulates on sample stage 23 contacts with probe 281；
S6: control Z axis piezoelectric ceramics 233 and regulate sample stage 23, make probe 281 to sample imposed load；
S7: obtain load value；When load value is equal to desired value, controls Z axis piezoelectric ceramics 233 stop motion and return to initial
State；
S8: control computer recording and export photosignal and the piezoelectric ceramics of four-quadrant photo detector in loading procedure
Displacement relation curve.
The scanning electron microscope 1 that utilizes provided the following detailed description of this utility model combines survey with scanning probe microscopy
The concrete steps of the method for test system test nano ZnO:
1, preparation:
Click scan ultramicroscope 1 controls " Vent " button on software, lays down vacuum, then opens sample room 11
Hatch door, follows the steps below:
1.1 scanning probe test unit 2 are installed: utilize double end attachment screw will scanning probe test unit 2 base 21 with
In electron microscope sample room 11, original sample stage links together, and by original sample in electron microscope sample room 11
Scanning probe test unit 2 is fixed by the spinfunction of sample platform, prevents the unstable vibration in test process.Then scanning is visited
Self-locking aggregating cable connectors in pin test cell 2 is connected with the signal wire interface on hatch door, connects external control by wire
Unit.
1.2 samples and sample stage 23 are installed: after sample prepares, and are fixed on sample stage 23 by sample with conductive tape.
Then sample stage 23 is fixed in sample stage 23 mounting seat above Z axis piezoelectric ceramics 233 by trip bolt, and adjusts
The position of sample.
1.3 probes 281 and probe base 28 are installed: select suitable probe 281 according to testing requirement and be fixed in
On probe base 28, screw is then utilized probe base 28 to be arranged on the side of pedestal, as illustrated in fig. 1 and 2.
1.4 connect laser: by optical fiber interface reserved in scanning electron microscope 1 sample room 11 and laser sight 271
Interface connects, and optical fiber connects the external generating laser in hole 29 by optical fiber.
2, debugging process:
After preparation completes, progressively open test system control unit, generating laser 29 and computer and control
Software, proceeds by the debugging of scanning probe test unit 2.
2.1 optical path adjustings: laser is irradiated into the laser optical path of scanning probe test unit 2 by laser sight 271, and
The multiple reflections of the second reflecting mirror 278 in the first reflecting mirror 277 in reflecting mirror group, probe 281, reflecting mirror group irradiates
Photosensitive area to four-quadrant photo detector 272.Regulate successively the second laser modulation device 274, the 3rd laser modulation device 275,
One laser modulation device 273 and the 4th laser modulation device 276 adjust the rotation of first reflecting mirror the 277, second reflecting mirror 278 respectively
Angle, the incoming position of laser sight 271, four limits, as the displacement of detector, make laser focusing to optimum state and be in four
Limit is the most central as photosensitive area.
2.2 sample displacement coarse adjustment: utilize control unit to control X-axis adjusting means 24, Y-axis adjusting means 25 and Z axis respectively
Adjusting means 26, drives the motion of each axle drive rod to realize the coarse adjustment of sample displacement.Repeatedly adjust the displacement of each axle, make sample gradually
Approaching probe 281 and be positioned at the underface of probe 281, and distance is the nearest, the speed approached is the least.When the two distance reaches default
During value, each driving motor is automatically stopped motion.
After sample displacement coarse tuning process completes, shut scanning electron microscope 1 sample room 11 hatch door, click on computer and control
" Pump " button on software, evacuation, then add high pressure, open electron beam 121, enter on the basis of probe 281 needle point tip
Line focusing, carries out following operation under the real-time monitored of electron beam 121:
2.3 sample displacement fine settings: utilize electron beam 121 to find target sample, control X-axis pressure by control unit after determining
Electroceramics 231, Y-axis piezoelectric ceramics 232 realize sample displacement fine setting, and sample progressively moves to the underface of probe 281.
3, test process: preset less " Setpoint " value, slowly drives three Z axis to drive motor, makes probe
281 slowly approach with sample and contact with each other.Then target setting " Setpoint " value (desired value), and set control software
In each parameter in " force curve " module, click on " Start ", Z axis piezoelectric ceramics 233 starts elongation, and target sample is executed by probe 281
Add load.Load reach " Setpoint " value after Z axis piezoelectric ceramics 233 stop motion return to original state, simultaneous computer
Record and export the photosignal curve of output in loading procedure.The least " Setpoint " value and target " Setpoint "
Value is force value.
After this test process completes, it is right that the fine setting of repeat the above steps 2.3 sample displacement and step 3 test process just can realize
Multiple samples are tested.In test process, utilize electron beam 121 that target sample carries out real-time monitored in situ, and acquisition should
During scanning electron microscope 1 picture.
4, process is exited: after all having tested, returned to by this each element of test system successively according to the step of inverted order
Original state, takes out scanning probe test unit 2, closes generating laser 29, control unit and computer control software.
5, data convert, calculate process: first received by the PSD four-quadrant photo detector 272 that pressure hard substrate obtains
To T-B magnitude of voltage and Z axis piezoelectric ceramics 233 voltage value signal relation curve be converted into the force-displacement curve of three-point bending, tool
Body method is: according to piezoelectric ceramics characteristic, voltage signal is converted into displacement signal, due to scanning probe 281 needle point pressure hard base
Ground, compression distance is the least relative to cantilever beam 241 amount of bow, and displacement can be regarded as the amount of bow of scanning micro cantilever probe,
The amount of bow of the cantilever beam under this active force, is obtained scanning the size of the power of micro cantilever probe by Hooke's law,
Corresponding force-displacement curve during pressing hard substrate to scanning probe 24.
The T-B magnitude of voltage the most again the PSD four-quadrant photo detector 272 that nano wire three-point bending obtains received
With " power-displacement " curve that Z axis piezoelectric ceramics 233 voltage value signal relation curve is converted into nano wire three-point bending, specifically side
Method is: according to piezoelectric ceramics characteristic, voltage signal is converted into displacement signal, probe pressure hard substrate and pressure nano wire and carries out three
During point bending, at identical T-B, represent that the flexibility of scanning micro cantilever probe is the same, can by the relation between both
To calculate the size of corresponding power, and then obtain " power-displacement " curve.Owing to the displacement of Z axis piezoelectric ceramics 233 is scanning probe
The bending value of cantilever beam and the bending value sum of nano wire, so nano wire bending displacement should be Z axis piezoelectric ceramics 233 displacement
Amount deducts the value of the amount of bow gained of scanning micro cantilever probe, such " power-displacement " curve being only nano wire obtained.Connect
Get off, can by " power-displacement " curve and combine the mechanical property formula of the material in table 1 and obtain the mechanics parameter of respective material,
dmax/ r represents the ratio of maximum compression distance and nano wire radius, according to dmaxThe difference of/r value uses different computation models,
Concrete as shown in table 1.
Table 1
In table, dmaxFor maximum compression distance, r is the radius of nano wire, and F is the power applied, and E is the springform of nano wire
Amount, L is nano wire length on groove, σyFor the yield strength of nano wire, FyFor the pressure during surrender of nano wire, dyFor
The displacement during surrender of nano wire, f (α), g (α) are the correction function of bending-stretch model.
This utility model can be applied in the various test needing microcosmic to test and research, and part this practicality is set forth below
Novel application in correlational study.
Example one: the application in combined test system of the present utility model three-dimensional appearance imaging in position
Utilizing this combined test system to carry out three-dimensional appearance imaging, its principle is identical with commercial AFM image-forming principle.Experiment
Middle probe 281 selects the NSC11 type probe of μm asch company, and its elastic constant is 3.0N/m.Sample selection standard AFM grating sample
Product, it is dimensioned as periodic width 2 μm, calibrated altitude 200nm, selects this standard sample can realize three-dimensional appearance imaging merit
Can, the displacement accuracy calibration of test system can be carried out again.Sample is installed with step 1.3 according to step 1.2 respectively with probe 281
Good, gained standard specimen shape appearance figure is as shown in Figure 6.Experimental studies have found that, the periodic width measured by master grating Sample Scan picture
Being 2.1 ± 0.1 μm, grid height is 190 ± 5nm, less with being dimensioned error, the displacement accuracy of this test system is described relatively
High.
Example two: the application in combined test system of the present utility model nano material manipulation process in position
Different from AFM scan imaging pattern, the manipulation of scanning probe test unit 2 and test function are by closing Z axis
Piezoelectric ceramics 233 feedback realizes.Under imaging pattern, probe 281 contacts with each other with sample, by the regulation in real time of signal feedback
Z axis piezoelectric ceramics 233 stroke, certain relative altitude is to maintain certain and needle point sample to make probe 281 and sample remain
The physical quantity that product spacing is relevant is constant.Handle and test pattern is then the feedback closing Z axis piezoelectric ceramics 233 displacement, so
When needle point moves just can with direct collision sample thus produce interaction force.
As a example by the planar movement of nanometer rods arranges, now rely on the side force of needle point to overcome the matrix adhesion to material
Effect, it is achieved the operation such as nanometer rods slip planar and rolling.Ultrasonic wavelength-division after nanometer rods ethanol being diluted before experiment
Dissipate, then dripped on silicon chip with dropper.Nano-manipulation selects the PL2NCL10 type tack scanning of NanoSensors company to visit
Pin, probe tip diameter is 1.8 ± 0.5 μm.The original position manipulation process of nanometer rods is as it is shown in fig. 7, in figure, utilize tack scanning to visit
Arrange with No. 2 two nanometer rods for No. 1, by the most mobile, make distance between the two more and more less, finally
Arrive on same horizontal line.Additionally by the probe 281 Vertical loading to nanometer rods, additionally it is possible to realize its machining functions.
Example three: the combined test system of the present utility model application in nano silver wire in situ three-point bend test
By even thickness and be typical quintic system structure nano silver wire alcoholic solution dilution after ultrasonic wave concussion,
It is allowed to dispersed, is then dripped on the silicon chip with etching microflute with dropper, treat alcoholic solution volatilization rear section nanometer
Line suspended span is combined as shown in Figure 4 by adhesion in the two ends of etching groove, contact portion.Three-point bend test choosing in situ
Probe 281 be commercial μm asch probe, elastic constant is respectively 3.5N/m (NSC18), and the radius of curvature of needle point is 10nm.
The sample prepared is installed with step 1.3 according to step 1.2 respectively with probe 281, and carries out three-point bending survey in situ
Examination.
Research find, pair radius nano silver wire in the range of 45～160nm, its elastic modelling quantity be 81.40～
149.8GPa, meansigma methods is 112.1 ± 20GPa, slightly above silver block materials (82.7GPa), and without dimensional effect, and its surrender is strong
Angle value progressively increases to 2.40GPa along with the reduction of radius from 1.07, shows obvious dimensional effect, and nano silver wire
Yield strength is far above block silver (55MPa), and its maximum is more than 40 times of block silver yield strength, calculates close to simulation
Theoretical value.
By three above example, this scanning electron microscope 1 is with scanning probe microscopy combined test system not
Only retain the imaging function of scanning probe microscopy, but also the original position being capable of minute yardstick micro Nano material handle processing with
And the test of the performance such as sample microcell mechanics, electricity, calorifics, this mechanical property being better understood from nano material for us has
The highest scientific value.
In this specification, each embodiment uses the mode gone forward one by one to describe, and what each embodiment stressed is and other
The difference of embodiment, between each embodiment, identical similar portion sees mutually.
Principle of the present utility model and embodiment are set forth by specific case used herein, above example
Explanation be only intended to help to understand method of the present utility model and core concept thereof；General technology simultaneously for this area
Personnel, according to thought of the present utility model, the most all will change.To sum up, this theory
Bright book content should not be construed as restriction of the present utility model.
Claims (8)
1. a nano material mechanics performance in-situ test system, it is characterised in that include scanning electron microscope, is located at described
Scanning probe test unit within the sample room of scanning electron microscope, visits with described scanning electron microscope and described scanning
The control unit that pin test cell is connected, and the computer being connected with described control unit；Described scanning probe test list
Unit includes base, is located at the regulating platform of described base upper surface side, is located at the measuring mechanism of described base upper surface opposite side；
Described scanning electron microscope includes that Electronic Speculum pole shoe, described regulating platform are provided with sample stage, and described sample stage can be made along described tune
X-axis adjusting means that joint platform length direction moves, described sample stage can be made along being perpendicular to described regulating platform length direction and vertical
The Y-axis adjusting means moved in the direction of described base upper surface, and sample stage can be made along the length being perpendicular to described regulating platform
Spend direction and be parallel to the Z axis adjusting means that the direction of described base upper surface is moved；X-axis is parallel to described regulating platform length side
To and be parallel to described base upper surface, Y-axis is perpendicular to described regulating platform length direction and is perpendicular to the upper surface of described base,
Z axis is perpendicular to regulating platform length direction and is parallel to described base upper surface, and described sample stage surface is positioned at described X-axis with described
In the plane that Y-axis is constituted；Described measuring mechanism includes laser optical path adjusting means, the probe base being located on base, Yi Jishe
Probe on described probe base, described probe is positioned at below described Electronic Speculum pole shoe, and described laser optical path adjusting means is used for
Collimation and focusing laser.
A kind of nano material mechanics performance in-situ test system the most according to claim 1, it is characterised in that described X-axis
Adjusting means includes the X-axis lower guideway being fixed on described regulating platform upper surface, is located at the X-axis upper rail on described X-axis lower guideway,
Described X-axis upper rail 242 is provided with X-axis linear electric motors, and one end of described X-axis linear electric motors is connected with described X-axis lower guideway, institute
State X-axis linear electric motors to be connected with described control unit.
A kind of nano material mechanics performance in-situ test system the most according to claim 2, it is characterised in that described Y-axis
Adjusting means includes the Y-axis lower guideway being fixed on described X-axis upper rail upper surface, is located in the Y-axis on described Y-axis lower guideway and leads
Rail, described Y-axis upper rail is provided with Y-axis linear electric motors, and one end of described Y-axis linear electric motors is connected with described Y-axis lower guideway, described
Y-axis linear electric motors are connected with described control unit.
A kind of nano material mechanics performance in-situ test system the most according to claim 3, it is characterised in that described Z axis
Adjusting means includes the Z axis lower guideway being fixed on described Y-axis upper rail upper surface, is located on the Z axis on described Z axis lower guideway
Guide rail, described Z axis lower guideway is provided with Z axis linear electric motors, and one end of described Z axis linear electric motors is connected with described Z axis upper rail, institute
State Z axis linear electric motors to be connected with control unit.
A kind of nano material mechanics performance in-situ test system the most according to claim 1, it is characterised in that described regulation
Being provided with X-axis piezoelectric ceramics, Y-axis piezoelectric ceramics and Z axis piezoelectric ceramics between platform and described sample stage, described X-axis piezoelectric ceramics is used
Finely tuning along the displacement of X axis in described sample stage, described Y-axis piezoelectric ceramics is finely tuned along the displacement of Y-axis for described sample stage,
Described Z axis piezoelectric ceramics is finely tuned along the displacement of Z-axis direction for described sample stage, and described X-axis piezoelectric ceramics, described Y-axis piezoelectricity are made pottery
Porcelain is connected with control unit respectively with described Z axis piezoelectric ceramics.
A kind of nano material mechanics performance in-situ test system the most according to claim 1, it is characterised in that described laser
Light path regulating device includes laser sight, reflecting mirror group, four-quadrant photo detector, and it is inclined to regulate described laser sight
The first laser modulation device, the second laser modulation device of the regulation reflecting mirror group anglec of rotation and the 3rd laser modulation device, the regulation turned
The 4th laser modulation device that described four-quadrant photo detector moves；Described laser sight and described four-quadrant photo detector
Being oppositely arranged, described reflecting mirror is mounted between described laser sight and described four-quadrant photo detector, and is located at described
Sample stage table top is just to position, and described four-quadrant photo detector is connected with described control unit, and described laser sight leads to
Cross optical fiber to be connected with generating laser.
A kind of nano material mechanics performance in-situ test system the most according to claim 1, it is characterised in that described sample
Room is provided with hatch door, and described hatch door is provided with that Function Extension signal connects hole, signal wire interface, ground wire connects hole and optical fiber connects hole.
A kind of nano material mechanics performance in-situ test system the most according to claim 1, it is characterised in that described Electronic Speculum
The axis direction of the electron beam that pole shoe is launched is 20～30 ° with the angle of described sample stage table top, the tip of described electron beam
It is irradiated to the tip of described probe.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105911311A (en) * | 2016-07-05 | 2016-08-31 | 北京工业大学 | In-situ test system and method for mechanical properties of nano material |
| CN110487628A (en) * | 2019-08-23 | 2019-11-22 | 杭州源位科技有限公司 | A kind of miniature mechanical test platform in original position |
| CN112014237A (en) * | 2020-09-07 | 2020-12-01 | 山东大学 | Device and method for preparing cement stone microscopic sample and testing bending tensile strength |
-
2016
- 2016-07-05 CN CN201620700597.5U patent/CN205749569U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105911311A (en) * | 2016-07-05 | 2016-08-31 | 北京工业大学 | In-situ test system and method for mechanical properties of nano material |
| CN110487628A (en) * | 2019-08-23 | 2019-11-22 | 杭州源位科技有限公司 | A kind of miniature mechanical test platform in original position |
| CN112014237A (en) * | 2020-09-07 | 2020-12-01 | 山东大学 | Device and method for preparing cement stone microscopic sample and testing bending tensile strength |
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Effective date of registration: 20231108 Address after: Factory Building No. 4, 487 Chengdongxing Road, Tonglu County, Hangzhou City, Zhejiang Province, 311599 Patentee after: Zhejiang Qiyue Technology Co.,Ltd. Address before: 100 000 Pingle Garden Village, Chaoyang District, Beijing Patentee before: Beijing University of Technology |
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