CN105911311A - In-situ test system and method for mechanical properties of nano material - Google Patents
In-situ test system and method for mechanical properties of nano material Download PDFInfo
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- CN105911311A CN105911311A CN201610523453.1A CN201610523453A CN105911311A CN 105911311 A CN105911311 A CN 105911311A CN 201610523453 A CN201610523453 A CN 201610523453A CN 105911311 A CN105911311 A CN 105911311A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/02—Non-SPM analysing devices, e.g. SEM [Scanning Electron Microscope], spectrometer or optical microscope
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/04—Display or data processing devices
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Abstract
The invention provides an in-situ test system for mechanical properties of a nano material. The in-situ test system comprises a scanning electronic microscope, a scanning probe test unit, a control unit and a computer; the scanning probe test unit comprises a base, an adjusting table arranged at one side of the upper surface of the base, and a measuring mechanism arranged at the other side of the upper surface of the base; the scanning electronic microscope comprises an electron microscope pole shoe, and the adjusting table is provided with a sample table, an X-axis adjusting apparatus, a Y-axis adjusting apparatus and a Z-axis adjusting apparatus; the measuring mechanism comprises a laser light path adjusting apparatus, a probe foundation support arranged on the base, and a probe arranged on the probe foundation support, the probe is positioned below the electron microscope pole shoe, and the laser light path adjusting apparatus is used for collimating and focusing laser. By adopting the in-situ test system and the in-situ test method, an acting process of the scanning probe and a sample and an evolution process of a sample microstructure under a physical mechanical function of an external field in the test process can be actually observed in site, and micro images of a series event and mechanical property test data are transmitted to a computer.
Description
Technical field
The present invention relates to microstructure performance detection apparatus technical field, particularly relate to a kind of nano material force
Learn performance in-situ test system and method.
Background technology
During the progress and development of nanoscale science and technology, two class scientific instrument have played important promotion
Effect, a class is the ultramicroscope using electron beam as probe, representative have transmission electron microscope
And scanning electron microscope (SEM) (TEM)；Another kind of is that the scanning using solid needle point as probe is visited
Pin microscope (SPM), representational have PSTM (STM) and atomic force microscope (AFM).
But be as micro-nano device fast development and on yardstick approaching to the nanometer limit, how
Characterize micro-nano-scale material, structure and device outfield (electric field in such as device operation, thermal field and
Induction stress field) effect under character, performance and variation tendency become grinding of nanoscale science and technology field
Study carefully forward position and focus, to seek the further breakthrough in terms of new material, new technique, new technology.
Realize physical property under outer field action of nano material, structure and device and microstructure phase
The measurement of closing property and sign, need to realize simultaneously reliable fixing, apply outer field action and microexamination
Trinitarian measurement.
Current PSTM, atomic force microscope, scanning electron microscope, transmission electron microscopy
The micro analysiss such as mirror and test instrunment are in structure, pattern, composition and mechanics, electricity etc. the property of nano material
Aspect can be tested and played important function, become current people and probe into the main of the various physical property of nano material
Method.But, these instruments are only capable of carrying out nano material the measurement of single aspect, it is impossible to enough satisfied to sample
Product are handled simultaneously and measure, and the function in situ, dynamically observed, it is difficult to realize reliably fixing, executing
Add outer field action and the Trinitarian measurement of microexamination.
Summary of the invention
It is an object of the invention to provide one and be capable of reliable fixing, applying External Force Acting and microexamination
The in-situ test system of Trinitarian measurement nanometer dynamic performance and method.The present invention combines scanning electron and shows
Micro mirror and scanning probe microscopy development fresh approach and technology, devise and can be arranged on scanning electron
Scanning probe test unit in microscope example room, develops based on sweeping in scanning electron microscope sample room
Retouch the nano material mechanics performance in-situ test method of probe test function.
For achieving the above object, the invention provides a kind of nano material mechanics performance in-situ test system, bag
Include scanning electron microscope, be located at the scanning probe test list within the sample room of described scanning electron microscope
Unit, the control unit being connected with described scanning electron microscope and described scanning probe test unit, and
The computer being connected with described control unit；Described scanning probe test unit includes base, is located at the described end
The regulating platform of seat upper surface side, is located at the measuring mechanism of described base upper surface opposite side；Described scanning electricity
Sub-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
Joint platform length direction move X-axis adjusting means, can make described sample stage along be perpendicular to described regulation director
Spend direction and be perpendicular to the Y-axis adjusting means that the direction of described base upper surface is moved, and sample can be made
Platform is along being perpendicular to the length direction of described regulating platform and being parallel to the Z that the direction of described bottom surface upper surface is moved
Axis adjustment device；X-axis is parallel to described regulating platform length direction and is parallel to described base upper surface, Y-axis
Being perpendicular to described regulating platform length direction and be perpendicular to the upper surface of described base, Z axis is perpendicular to regulate director
Spending direction and be parallel to described base upper surface, described sample stage surface is positioned at described X-axis and described Y-axis
In the plane constituted；Described measuring mechanism includes laser optical path adjusting means, the probe base being located on base,
And it is located at the probe on described probe base, described probe is positioned at below described Electronic Speculum pole shoe, described laser
Light path regulating device is used 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,
Being located at the X-axis upper rail on described X-axis lower guideway, described X-axis upper rail is provided with X-axis linear electric motors,
One end of described X-axis linear electric motors is connected with described X-axis lower guideway, described X-axis linear electric motors and institute
State control unit to be connected.
Optionally, under described Y-axis adjusting means includes being fixed on the Y-axis of described X-axis upper rail upper surface
Guide rail, is located at the Y-axis upper rail on described Y-axis lower guideway, and described Y-axis upper rail is provided with Y-axis straight line
Motor, one end of described Y-axis linear electric motors is connected with described Y-axis lower guideway, described Y-axis linear electric motors
It is connected with described control unit.
Optionally, under described Z axis adjusting means includes being fixed on the Z axis of described Y-axis upper rail upper surface
Guide rail, is located at the Z axis upper rail on described Z axis lower guideway, and described Z axis lower guideway is provided with Z axis straight line
Motor, one end of described Z axis linear electric motors is connected with described Z axis upper rail, described Z axis linear electric motors
It is connected with control unit.
Optionally, X-axis piezoelectric ceramics, Y-axis piezoelectric ceramics and Z it are provided with between described regulating platform and sample stage
Axial compression electroceramics, described X-axis piezoelectric ceramics is finely tuned along the displacement of X axis for described sample stage, described
Y-axis piezoelectric ceramics is finely tuned along the displacement of Y-axis for described sample stage, and described Z axis piezoelectric ceramics is used for
Described sample stage is finely tuned along the displacement of Z-axis direction, described X-axis piezoelectric ceramics, Y-axis piezoelectric ceramics and Z axis
Piezoelectric ceramics is connected with described control unit respectively.
Optionally, described laser optical path adjusting means includes laser sight, reflecting mirror group, four-quadrant photoelectricity
Detector, and regulate the first laser modulation device of described laser sight deflection, regulation reflecting mirror group rotation
Second laser modulation device of angle and the 3rd laser modulation device, regulate what described four-quadrant photo detector moved
4th laser modulation device；Described laser sight is oppositely arranged with described four-quadrant photo detector, described instead
Penetrate mirror to be mounted between described laser sight and described four-quadrant photo detector, and be located at described sample stage
Table top is just to position, and described four-quadrant photo detector is connected with described control unit, described laser aiming
Device is connected with generating laser by optical fiber.
Optionally, described sample room is provided with hatch door, and described hatch door is provided with Function Extension signal and connects hole, signal
Line interface, ground wire connect hole and optical fiber connects hole.
Optionally, the axis direction of the electron beam that described Electronic Speculum pole shoe is launched and the folder of described sample stage table top
Angle is 20～30 °, and the tip of described electron beam is irradiated to the tip of described probe.
Present invention also offers one and utilize nano material mechanics performance in-situ test system test nano material
The method of mechanical property, described nano material mechanics performance in-situ test system includes scanning electron microscopy
Mirror, is located at the scanning probe test unit within the sample room of described scanning electron microscope, with described scanning
The control unit that ultramicroscope is connected with described scanning probe test unit, and with described control unit
The computer connected；Described scanning probe test unit includes base, is located at described base upper surface side
Regulating platform, is located at the measuring mechanism of described base upper surface opposite side；Described scanning electron microscope includes electricity
Mirror pole shoe, described regulating platform is provided with sample stage, and described sample stage can be made to move along described regulating platform length direction
Dynamic X-axis adjusting means, described sample stage can be made along being perpendicular to described regulating platform length direction and being perpendicular to
The Y-axis adjusting means that the direction of described base upper surface is moved, and sample stage can be made described along being perpendicular to
The length direction of regulating platform and be parallel to the Z axis adjusting means that the direction of described bottom surface upper surface is moved；X-axis
Being parallel to described regulating platform length direction and be parallel to described base upper surface, Y-axis is perpendicular to described regulating platform
Length direction and be perpendicular to the upper surface of described base, Z axis is perpendicular to regulating platform length direction and is parallel to institute
Stating base upper surface, described sample stage surface is positioned at the plane that described X-axis is constituted with described Y-axis；Institute
State measuring mechanism and include laser optical path adjusting means, the probe base being located on base, and it is located at described spy
Probe on pin pedestal, described probe is positioned at below described Electronic Speculum pole shoe, and described laser optical path adjusting means is used
In collimation and focusing 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,
The sample on sample stage is made to be 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 and sample
Product contact；
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, at the beginning of controlling Z axis piezoelectric ceramics stop motion and returning to
Beginning state；
Control computer recording and export photosignal and the piezoelectricity of four-quadrant photo detector in loading procedure
Pottery displacement relation curve.
Optionally, sample is fixed on described sample stage, shuts the hatch door of scanning electron microscope, evacuation
After, the electron gun high voltage of scanning electron microscope, then open electron beam, adjust scanning electron microscope
Duty, observes scanning probe microscopy under different enlargement ratios and nano material is carried out mechanical property survey
The microprocess of examination.
The specific embodiment provided according to the present invention, the invention discloses techniques below effect:
In scanning probe test unit in the nano material mechanics performance in-situ test system that the present invention provides
X-axis adjusting means, Y-axis adjusting means and Z axis adjusting means can regulate sample stage, it is also possible to fixing sample
Sample platform, it is achieved sample stable fixing；And owing to sample stage can also pass through X-axis adjusting means, Y
Axis adjustment device and Z axis adjusting means change position and angle of inclination, also therefore are able to realize applying sample
The effect in outfield；Owing to the test system of the present invention also includes scanning electron microscope, it is possible to by scanning electricity
Sub-microscope Real Time Observation micro-image.Therefore, the test system that the present invention provides is capable of nanometer material
Reliable fixing, the applying outer field action of material and the Trinitarian measurement of microexamination.
The present invention also has a beneficial effect:
1, the overall structure of the scanning probe test unit in the present invention is according to scanning electron microscope sample room
Inner space is designed, and volume is little, compact conformation, conveniently installs and dismantles, easy and simple to handle, surveys
Examination degree of accuracy 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 the real-time monitored of manipulation process, it is to avoid to be blocked by other structures and affect in real time
The problem of observation, further increases measuring accuracy.
2, the scanning electron microscope sample room in the present invention devises some wiring holes, can not only realize
The connection of scanning probe test unit and external control unit outside, and can also attachment force field, electric field, thermal field,
The multiple additional physical field such as magnetic field, it is achieved the expansion of Joint Systems Test function.
3, scanning electron microscope is combined by the present invention with scanning probe test unit, electricity
Son bundle scanning imagery is handled can carry out simultaneously with scanning probe micro-nano, does not interfere with each other, it is achieved truly
Original position outfield quantitative measurement function.
4, the scanning probe scanning probe test unit in the present invention can be carried out easily according to experiment demand
Change, it is achieved material nanometer material under different loads, different method of testing and different probe pressure head effect
Material Mechanics Performance Testing function.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to enforcement
In example, the required accompanying drawing used is briefly described, it should be apparent that, the accompanying drawing in describing below is only
Some embodiments of the present invention, for those of ordinary skill in the art, are not paying creative work
On the premise of, it is also possible to other accompanying drawing is obtained according to these accompanying drawings.
Fig. 1 is the scanning probe test unit three-dimensional structural representation in the present invention；
Fig. 2 is the scanning probe test unit plan structure schematic diagram in the present invention；
Fig. 3 is that the needle point scanning probe in the scanning probe test unit in the present invention contacts local with sample
Enlarged drawing；
Fig. 4 is the scanning probe test unit middle probe needle point in the present invention, sample and scanning electron microscope electron bundle
Angle schematic diagram；
Fig. 5 is the scanning electron microscope sample room structural representation in the present invention；
Fig. 6 is the three-dimensional appearance image that the present invention scans probe test in-situ test groove structure；
Fig. 7 is that the scanning probe in the present invention 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 that the photosignal output of the four-quadrant photo detector of nano material in-situ test is made pottery with piezoelectricity
Porcelain displacement relation curve chart；
Figure 11 is the force-displacement curve of nano silver wire of the present invention three-point bend test in situ and output.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clearly
Chu, be fully described by, it is clear that described embodiment be only a part of embodiment of the present invention rather than
Whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creation
The every other embodiment obtained under property work premise, broadly falls into the scope of protection of the invention.
As Figure 1-5, the invention provides a kind of nano material mechanics performance in-situ test system, including
Scanning electron microscope 1, is located at the scanning probe test within sample room 11 of scanning electron microscope 1
Unit 2, the control unit being connected with scanning electron microscope 1 and scanning probe test unit 2, and
The computer being connected with control unit；Scanning probe test unit 2 includes base 21, is located on base 21
The regulating platform 22 of side, surface, is located at the measuring mechanism of base 21 upper surface opposite side；Scanning electron microscopy
Mirror 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 regulating platform
X-axis adjusting means 24 that 22 length directions move, sample stage 23 can be made along being perpendicular to regulating platform 22 length
Direction and be perpendicular to the Y-axis adjusting means 25 that the direction of base 21 upper surface is moved, and sample stage can be made
23 along being perpendicular to the length direction of regulating platform 22 and being parallel to the Z axis that the direction of base 21 upper surface is moved
Adjusting means 26；X-axis is parallel to regulating platform 22 length direction and is parallel to base 21 upper surface, Y-axis
Being perpendicular to regulating platform 22 length direction and be perpendicular to the upper surface of base 21, Z axis is perpendicular to regulating platform 22
Length direction and be parallel to base 21 upper surface, it is flat with what Y-axis was constituted that sample stage 23 surface is positioned at X-axis
In face；Measuring mechanism includes laser optical path adjusting means 27, the probe base 28 being located on base 21, with
And the probe 281 being located on probe base 28, probe 281 is positioned at below Electronic Speculum pole shoe 12, laser optical path
Adjusting means 27 is used for collimating and focusing on laser.
The present invention is by being integrated into scanning electron microscope 1 by the scanning probe microscopy unit of compact conformation
In sample room 11, it is utilized respectively function and scanning probe that sample microcosmic is tested by scanning electron microscope 1
Microscope carries out the function of the test such as micro-scale mechanics, electricity, constituent material original position, online microcosmic to sample
Structure and morphology feature tests system with physical property integrated analysis.The present invention is by scanning electron microscope 1
Combine with scanning probe test unit 2, electron beam scanning imaging and scanning probe micro-nano behaviour
Indulge and can carry out simultaneously, do not interfere with each other, it is achieved original position outfield quantitative measurement function truly.
The overall structure of scanning probe test unit 2 is entered according to inner space, scanning electron microscope 1 sample room 11
Row design, volume is little, compact conformation, conveniently installs and dismantles, easy and simple to handle, and testing precision is high.
The probe 281 scanning probe test unit 2 in the present invention can be replaced easily according to experiment demand,
Realize material quantitative measurement merit under different loads, different method of testing and different physical field effect
Energy.This system structure is compact, easy and simple to handle, organically combines scanning electron microscope 1 and scanning probe
Microscopical test function, can be widely applied to bar-shaped, filamentary material, the thin-film material of micro-nano-scale,
The microstructure of the materials such as micro-nano granules, the integrated in site measurement of the performance such as mechanics, electricity.
As the optional embodiment of one, X-axis adjusting means 24 includes being fixed on regulating platform 22 upper surface
X-axis lower guideway 241, the X-axis upper rail 242 being located on X-axis lower guideway 241, X-axis upper rail
242 are provided with X-axis linear electric motors 243, and one end of X-axis linear electric motors 243 is connected with X-axis lower guideway 241,
X-axis linear electric motors 243 are connected with control unit.Control unit controls X-axis linear electric motors 243 and moves,
Owing to one end of X-axis linear electric motors 243 is connected with X-axis lower guideway 241, therefore X-axis linear electric motors 243
Athletic meeting drive X-axis upper rail 242 to translate, then also will drive sample by X-axis upper rail 242
Sample platform 23 translates along X-axis, 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 being fixed on X-axis upper rail 242
The Y-axis lower guideway 251 of upper surface, 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, leads under the other end of Y-axis linear electric motors 253 and Y-axis
Rail 251 connects, and Y-axis linear electric motors 253 are connected with control unit.Control unit controls Y-axis straight line
Motor 253 moves, owing to the other end of Y-axis linear electric motors 253 is connected with Y-axis lower guideway 251, because of
The athletic meeting of these Y-axis linear electric motors 253 drives Y-axis upper rail 252 to translate, then also will pass through Y
Axle upper rail 252 drives sample stage 23 to 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 being fixed on Y-axis upper rail 252
The Z axis lower guideway 261 of upper surface, the Z axis upper rail 262 being located on Z axis lower guideway 261, under Z axis
Guide rail 261 is provided with Z axis linear electric motors 263, the other end of Z axis linear electric motors 263 and Z axis upper rail 262
Connecting, Z axis linear electric motors 263 are connected with control unit.Control unit controls Z axis linear electric motors 263
Motion, 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 pass through Z axis upper rail
262 drive sample stage 23 to 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 piezoelectricity pottery
Porcelain 231, Y-axis piezoelectric ceramics 232 and Z axis piezoelectric ceramics 233, X-axis piezoelectric ceramics 231 is for sample
Platform 23 is finely tuned along the displacement of X axis, and Y-axis piezoelectric ceramics 232 is used for the sample stage 23 position along Y-axis
Moving fine setting, Z axis piezoelectric ceramics 233 is finely tuned along the displacement of Z-axis direction for sample stage 23, and X-axis piezoelectricity is made pottery
Porcelain 231, Y-axis piezoelectric ceramics 232 are connected with control unit respectively with Z axis piezoelectric ceramics 233.Pass through
Control unit controls X-axis piezoelectric ceramics 231 and realizes X with Y-axis piezoelectric ceramics 232, and Y-direction displacement is micro-
Adjusting, Z axis piezoelectric ceramics 233 realizes Z-direction displacement fine setting.See under scanning electron microscope image formation state
Examining probe 281 and sample carries out the performance tests such as microcell mechanics, calorifics, real time record sample is at outer field action
Under structural information and performance change, by information processing system, four-quadrant photo detector is received simultaneously
Voltage signal carry out Treatment Analysis, i.e. can get the performances such as the microcell mechanics of sample, calorifics, it is thus achieved that knot
Structure is 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 of regulation laser sight 271 deflection
Actuator 273, the second laser modulation device 274 and the 3rd laser modulation device of the regulation reflecting mirror group anglec of rotation
275, the 4th laser modulation device 276 that regulation four-quadrant photo detector 272 moves；Laser sight 271
Being oppositely arranged with four-quadrant photo detector 272, reflecting mirror is mounted on laser sight 271 and four-quadrant light
Between electric explorer 272, and it is located at sample stage 23 table top just to position, four-quadrant photo detector 272
Being connected with control unit, laser sight 271 is connected with generating laser 29 by optical fiber.Laser
The laser optical path of scanning probe test unit 2 it is irradiated into by laser sight 271, and through reflecting mirror group
In the first reflecting mirror 277, probe 281, the multiple reflections of the second reflecting mirror 278 in reflecting mirror group shine
It is mapped to the photosensitive area of four-quadrant photo detector 272.Regulate the second laser modulation device the 274, the 3rd successively to swash
It is anti-that light regulator the 275, first laser modulation device 273 and the 4th laser modulation device 276 adjust first respectively
Penetrate the anglec of rotation of 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
Signal connects hole 13, signal wire interface 14, ground wire connects hole 15 and optical fiber connects hole 16 in extension.Scanning electron
Sample room 11 hatch door 17 of microscope 1 has some wiring holes, it is simple to scanning probe test unit 2 is with outer
The connection of portion's control unit and functions expanding.Wherein Function Extension signal connects hole 13 and can connect the field of force, electricity
The outfields such as field, thermal field, magnetic field, it is achieved the expansion of Joint Systems Test function；Signal wire interface 14 uses
Self-feeding type connector binding post, connects internal SPM test cell and external control unit outside, controls SPM and surveys
The operation of examination unit；Ground wire connects hole 15 for discharging unnecessary electric charge, reduces Electronic Speculum imaging interference, improves
Image quality；Optical fiber connects hole 16 and outside laser is imported sample room 11 inner scanning probe test unit 2
Light path part.
As the optional embodiment of one, electron beam 121 and the sample stage 23 that Electronic Speculum pole shoe 12 is launched
The angle of table top is 20～30 °, and the tip of electron beam 121 is irradiated to the tip of probe 281.In order to ensure
Test system can be observed in situ, and probe 281 is positioned at the underface of Electronic Speculum pole shoe 12, and scanning
The sample stage 23 of probe test unit 2 is 20～30 ° of angles with the axis direction of electron beam 121, makes electricity
Son bundle 121 can shine directly into the end of probe 281 needle point.When test, keep needle point static, electricity
Son bundle 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.
Present invention also offers one and utilize scanning electron microscope 1 and scanning probe microscopy joint test
The method of system test nano ZnO, scanning electron microscope 1 and scanning probe microscopy joint test
System includes scanning electron microscope 1, is located within the sample room 11 of scanning electron microscope 1
Scanning probe test unit 2, the control being connected with scanning electron microscope 1 and scanning probe test unit 2
Unit processed, and the computer being connected with control unit；Scanning probe test unit 2 includes base 21,
It is located at the regulating platform 22 of base 21 upper surface side, is located at the measuring mechanism of base 21 upper surface opposite side；
Scanning electron microscope 1 includes that Electronic Speculum pole shoe 12, regulating platform 22 are provided with sample stage 23, can make sample stage
The 23 X-axis adjusting meanss 24 moved along regulating platform 22 length direction, can make sample stage 23 along be perpendicular to adjust
Save platform 22 length direction and be perpendicular to the Y-axis adjusting means 25 that the direction of base 21 upper surface is moved, with
And sample stage 23 can be made along being perpendicular to the length direction of regulating platform 22 and being parallel to the direction shifting of bottom surface upper surface
Dynamic Z axis adjusting means 26；X-axis is parallel to regulating platform 22 length direction and is parallel to table on base 21
Face, Y-axis is perpendicular to regulating platform 22 length direction and is perpendicular to the upper surface of base 21, and Z axis is perpendicular to adjust
Saving platform 22 length direction and be parallel to base 21 upper surface, sample stage 23 surface is positioned at X-axis and Y-axis structure
In the plane become；Measuring mechanism includes laser optical path adjusting means 27, is located at the probe base on base 21
28, and the probe 281 being located on probe base 28, probe 281 is positioned at below Electronic Speculum pole shoe 12, swashs
Light light path regulating device 27 is used for collimating and focusing on laser；The method of test nano ZnO includes following
Step:
S1: regulation laser optical path adjusting means 27, makes laser focusing to four-quadrant photo detector 272
Center；
S2: control X-axis adjusting means 24, Y-axis adjusting means 25 and Z axis adjusting means 26 and regulate sample
The position of sample platform 23, makes the sample on sample stage 23 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,
Probe 281 tip is made to 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 and stop fortune
Move and return to original state；
S8: control computer recording and export photosignal and the pressure of four-quadrant photo detector in loading procedure
Electroceramics displacement relation curve.
The scanning electron microscope 1 that utilizes provided the following detailed description of the present invention joins with scanning probe microscopy
The concrete steps of the method for conjunction test system and 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 scan probe test unit 2
Base 21 links together with original sample stage in electron microscope sample room 11, and passes through electron microscopic
In mirror sample room 11, scanning probe test unit 2 is fixed by the spinfunction of original sample stage, prevents from surveying
Unstable vibration during examination.Then by scanning probe test unit 2 in self-locking aggregating cable connectors with
Signal wire interface on hatch door connects, and connects external control unit outside by wire.
1.2 samples and sample stage 23 are installed: after sample prepares, with conductive tape, sample is fixed on sample
On platform 23.Then sample stage 23 is fixed on the sample above Z axis piezoelectric ceramics 233 by trip bolt
In platform 23 mounting seat, and adjust the position of sample.
1.3 probes 281 and probe base 28 are installed: select suitable probe 281 according to testing requirement and incite somebody to action
It is fixed on probe base 28, then utilizes screw that probe base 28 is arranged on the side of pedestal, as
Shown in Fig. 1 and 2.
1.4 connect laser: taken aim at laser by optical fiber interface reserved in scanning electron microscope 1 sample room 11
Quasi-device 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 meter
Calculation machine controls software, proceeds by the debugging of scanning probe test unit 2.
2.1 optical path adjustings: laser is irradiated into swashing of scanning probe test unit 2 by laser sight 271
In light light path, and the first reflecting mirror 277 in reflecting mirror group, probe 281, reflecting mirror group second
The multiple reflections of reflecting mirror 278 is irradiated to the photosensitive area of four-quadrant photo detector 272.Regulate second successively
Laser modulation device the 274, the 3rd laser modulation device the 275, first laser modulation device 273 and the regulation of the 4th laser
Device 276 adjusts the anglec of rotation of first reflecting mirror the 277, second reflecting mirror 278, laser sight respectively
The incoming position of 271, four limits as the displacement of detector, make laser focusing to optimum state and be in four limits as
Photosensitive area the most central.
2.2 sample displacement coarse adjustment: utilize control unit to control X-axis adjusting means 24, Y-axis regulation dress respectively
Put 25 and Z axis adjusting means 26, drive the motion of each axle drive rod to realize the coarse adjustment of sample displacement.Repeatedly adjust
The displacement of whole each axle, makes sample gradually approach probe 281 and be positioned at the underface of probe 281, and distance is more
Closely, the speed approached is the least.When the two distance reaches preset 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
" Pump " button on computer control software, evacuation, then add high pressure, open electron beam 121,
It is focused on the basis of probe 281 needle point tip, under the real-time monitored of electron beam 121, carries out following behaviour
Make:
2.3 sample displacement fine settings: utilize electron beam 121 to find target sample, pass through control unit after determining
Control X-axis piezoelectric ceramics 231, Y-axis piezoelectric ceramics 232 realizes sample displacement fine setting, is progressively moved by sample
Move the underface of probe 281.
3, test process: preset less " Setpoint " value, slowly drives three Z axis to drive horse
Reach, make probe 281 slowly approach with sample and contact with each other.Then target setting " Setpoint " value (mesh
Scale value), and set in control software each parameter in " force curve " module, click on " Start ", Z axis pressure
Electroceramics 233 starts elongation, and probe 281 is to target sample imposed load.Load reaches " Setpoint "
Z axis piezoelectric ceramics 233 stop motion return to original state after value, simultaneous computer record also exports loading
During photosignal curve of output.The least " Setpoint " value and target " Setpoint " value
For force value.
After this test process completes, the fine setting of repeat the above steps 2.3 sample displacement and step 3 test process are just
Can realize multiple samples are tested.In test process, electron beam 121 is utilized to carry out former to target sample
Position real-time monitored, and obtain scanning electron microscope 1 picture during this.
4, process is exited: after all having tested, according to the step of inverted order successively by this each unit of test system
Part returns to original state, takes out scanning probe test unit 2, closes generating laser 29, control unit
And computer control software.
5, data conversion, calculating process: first will press the PSD four-quadrant photodetection that hard substrate obtains
The T-B magnitude of voltage that device 272 receives is converted into Z axis piezoelectric ceramics 233 voltage value signal relation curve
The force-displacement curve of three-point bending, method particularly includes: according to piezoelectric ceramics characteristic, voltage signal is converted into
Displacement signal, due to scanning probe 281 needle point pressure hard base, compression distance is relative to cantilever beam 241
Amount of bow is the least, displacement can be regarded as the amount of bow of scanning micro cantilever probe, obtain under this active force
The amount of bow of cantilever beam, is obtained scanning the size of the power of micro cantilever probe, i.e. can be scanned by Hooke's law
The corresponding force-displacement curve during hard substrate pressed by probe 24.
The T-B the most again the PSD four-quadrant photo detector 272 that nano wire three-point bending obtains received
Magnitude of voltage and Z axis piezoelectric ceramics 233 voltage value signal relation curve be converted into nano wire three-point bending " power-
Displacement " curve, method particularly includes: according to piezoelectric ceramics characteristic, voltage signal is converted into displacement signal, visits
When pin pressure hard substrate and pressure nano wire carry out three-point bending, at identical T-B, represent scanning probe cantilever
Deflection of beam degree is the same, the relation between both can calculate the size of corresponding power, and then obtain
To " power-displacement " curve.Owing to the displacement of Z axis piezoelectric ceramics 233 is the bending value of scanning micro cantilever probe
With the bending value sum of nano wire, so nano wire bending displacement should be Z axis piezoelectric ceramics 233 displacement
Deduct the value of the amount of bow gained of scanning micro cantilever probe, such " power-position being only nano wire obtained
Move " curve.It follows that can be by " power-displacement " curve and combine the mechanical property formula of the material in table 1 and ask
Go out the mechanics parameter of respective material, dmax/ r represents the ratio of maximum compression distance and nano wire radius, according to
d maxThe difference of/r value uses different computation models, the most 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 for receiving
The elastic modelling quantity of rice noodle, L is nano wire length on groove, σyFor the yield strength of nano wire, Fy
For the pressure during surrender of nano wire, dyFor the displacement during surrender of nano wire, f (α), g (α) are for bending-drawing
Stretch the correction function of model.
The present invention can be applied to the various test needing microcosmic to test and research in, be set forth below part this
Bright application in correlational study.
Example one: the application in the three-dimensional appearance imaging in position of the combined test system of the present invention
This combined test system is utilized to carry out three-dimensional appearance imaging, its principle and commercial AFM image-forming principle phase
With.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, it is dimensioned as periodic width 2 μm, calibrated altitude 200nm,
Select this standard sample can realize three-dimensional appearance imaging function, the displacement accuracy school of test system can be carried out again
Accurate.Sample is installed with step 1.3 according to step 1.2 respectively with probe 281, gained standard specimen shape appearance figure
As shown in Figure 6.Experimental studies have found that, the periodic width measured by master grating Sample Scan picture is 2.1
± 0.1 μm, grid height is 190 ± 5nm, less with being dimensioned error, and this test system is described
Displacement accuracy is higher.
Example two: the application in the combined test system of present invention nano material manipulation process in position
Different from AFM scan imaging pattern, manipulation and the test function of scanning probe test unit 2 are logical
Cross and close what Z axis piezoelectric ceramics 233 feedback realized.Under imaging pattern, probe 281 and sample phase mutual connection
Touch, by signal feedback regulation Z axis piezoelectric ceramics 233 stroke in real time, make probe 281 and sample all the time
Keep certain relative altitude to maintain the physical quantity that certain is relevant to needle point sample interval constant.And handle and
Test pattern is then the feedback closing Z axis piezoelectric ceramics 233 displacement, so just can be straight when needle point moves
Connect 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 matrix to material
Adhesive attraction, it is achieved the operation such as nanometer rods slip planar and rolling.By nanometer rods wine before experiment
After essence dilution, ultrasound wave dispersion, is then dripped on silicon chip with dropper.Nano-manipulation selects NanoSensors
The PL2NCL10 type tack scanning probe of company, probe tip diameter is 1.8 ± 0.5 μm.Nanometer rods
Original position manipulation process as it is shown in fig. 7, in figure, utilize tack scanning probe to No. 1 with No. 2 two nanometers
Rod arranges, and by the most mobile, make distance between the two more and more less, finally arrives same
On bar 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 present invention 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
Ripple shakes, and is allowed to dispersed, then is dripped to, on the silicon chip with etching microflute, treat ethanol with dropper
The nano wire suspended span of solution evaporation rear section is combined by adhesion in the two ends of etching groove, contact portion
As shown in Figure 4.The probe 281 that three-point bend test is selected in situ is commercial μm asch probe, elastic normal
Number is respectively 3.5N/m (NSC18), and the radius of curvature of needle point is 10nm.By the sample prepared and probe
281 install with step 1.3 according to step 1.2 respectively, and carry out three-point bend test in situ.
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), without size
Effect, and its yield strength value progressively increases to 2.40GPa along with the reduction of radius from 1.07, shows
Significantly dimensional effect, and the yield strength of nano silver wire is far above block silver (55MPa), and it is maximum
Value is more than 40 times of block silver yield strength, the theoretical value calculated close to simulation.
By three above example, this scanning electron microscope 1 and scanning probe microscopy joint test
System not only retains the imaging function of scanning probe microscopy, but also is capable of minute yardstick micro Nano material
Original position handle processing and the test of the performances such as sample microcell mechanics, electricity, calorifics, this is more preferable for us
The mechanical property understanding nano material there is 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
With the difference of other embodiments, between each embodiment, identical similar portion sees mutually.
Principle and the embodiment of the present invention are set forth by specific case used herein, above enforcement
The explanation of example is only intended to help to understand method and the core concept thereof of the present invention；Simultaneously for this area
Those skilled in the art, according to the thought of the present invention, the most all can change
Part.To sum up, this specification content should not be construed as limitation of the present invention.
Claims (10)
1. a nano material mechanics performance in-situ test system, it is characterised in that include that scanning electron shows
Micro mirror, 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 with described scanning probe test unit, and control list with described
The computer that unit connects；Described scanning probe test unit includes base, is located at described base upper surface side
Regulating platform, be located at the measuring mechanism of described base upper surface opposite side；Described scanning electron microscope includes
Electronic Speculum pole shoe, described regulating platform is provided with sample stage, and described sample stage can be made along described regulating platform length direction
The X-axis adjusting means of movement, 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 being perpendicular to institute
State the length direction of regulating platform and be parallel to the Z axis adjusting means that the direction of described bottom surface upper surface is moved；X
Axle is parallel to described regulating platform length direction and is parallel to described base upper surface, and Y-axis is perpendicular to described regulation
Platform length direction and be 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 stage 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, the probe base being located on base, and is located at described
Probe on 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.
A kind of nano material mechanics performance in-situ test system the most according to claim 1, its feature
Being, described X-axis adjusting means includes the X-axis lower guideway being fixed on described regulating platform upper surface, is located at
X-axis upper rail on described X-axis lower guideway, described X-axis upper rail 242 is provided with X-axis linear electric motors,
One end of described X-axis linear electric motors is connected with described X-axis lower guideway, described X-axis linear electric motors and institute
State control unit to be connected.
A kind of nano material mechanics performance in-situ test system the most according to claim 2, its feature
Being, described Y-axis adjusting means includes the Y-axis lower guideway being fixed on described X-axis upper rail upper surface,
Being located at the Y-axis upper rail on described 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 is connected with described Y-axis lower guideway, and described Y-axis linear electric motors are with described
Control unit is connected.
A kind of nano material mechanics performance in-situ test system the most according to claim 3, its feature
Being, described Z axis adjusting means includes the Z axis lower guideway being fixed on described Y-axis upper rail upper surface,
Being located at the Z axis upper rail on described 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 is connected with described Z axis upper rail, described Z axis linear electric motors and control
Unit is connected.
A kind of nano material mechanics performance in-situ test system the most according to claim 1, its feature
It is, between described regulating platform and described sample stage, is provided with X-axis piezoelectric ceramics, Y-axis piezoelectric ceramics and Z
Axial compression electroceramics, described X-axis piezoelectric ceramics is finely tuned along the displacement of X axis for described sample stage, described
Y-axis piezoelectric ceramics is finely tuned along the displacement of Y-axis for described sample stage, and described Z axis piezoelectric ceramics is used for
Described sample stage along Z-axis direction displacement finely tune, described X-axis piezoelectric ceramics, described Y-axis piezoelectric ceramics and
Described Z axis piezoelectric ceramics is connected with control unit respectively.
A kind of nano material mechanics performance in-situ test system the most according to claim 1, its feature
Being, described laser optical path adjusting means includes laser sight, reflecting mirror group, four-quadrant photo detector,
And regulate the first laser modulation device of described laser sight deflection, the of the regulation reflecting mirror group anglec of rotation
Dual-laser actuator and the 3rd laser modulation device, regulate the 4th laser that described four-quadrant photo detector moves
Actuator；Described laser sight is oppositely arranged with described four-quadrant photo detector, and described reflecting mirror group sets
Between described laser sight and described four-quadrant photo detector, and it is the most right to be located at described sample stage table top
Position, described four-quadrant photo detector is connected with described control unit, and described laser sight passes through light
Fibre is connected with generating laser.
A kind of nano material mechanics performance in-situ test system the most according to claim 1, its feature
Being, 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.
A kind of nano material mechanics performance in-situ test system the most according to claim 1, its feature
Being, the axis direction of the electron beam that described Electronic Speculum pole shoe is launched with the angle of described sample stage table top is
20～30 °, the tip of described electron beam is irradiated to the tip of described probe.
9. a method for nano material mechanics performance in-situ test system test nano material mechanics performance,
It is characterized in that, described nano material mechanics performance in-situ test system includes scanning electron microscope,
It is located at the scanning probe test unit within the sample room of described scanning electron microscope, with described scanning electron
The control unit that microscope is connected with described scanning probe test unit, and be connected with described control unit
Computer；Described scanning probe test unit includes base, is located at the regulation of described base upper surface side
Platform, is located at the measuring mechanism of described base upper surface opposite side；Described scanning electron microscope includes Electronic Speculum pole
Boots, described regulating platform is provided with sample stage, and described sample stage can be made to move along described regulating platform length direction
X-axis adjusting means, described sample stage can be made along being perpendicular to described regulating platform length direction and be perpendicular to the described end
The Y-axis adjusting means that the direction of seat upper surface is moved, and sample stage can be made along being perpendicular to described regulating platform
Length direction and be parallel to the Z axis adjusting means that the direction of described bottom surface upper surface is moved；X-axis is parallel to
Described regulating platform length direction and be parallel to described base upper surface, Y-axis is perpendicular to described regulating platform length side
To and be 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 stage surface is positioned at the plane that described X-axis is constituted with described Y-axis；Described measurement
Mechanism includes laser optical path adjusting means, the probe base being located on base, and is located at described probe base
On probe, described probe is positioned at below described Electronic Speculum pole shoe, and described laser optical path adjusting means is used for collimating
With focusing laser；The method of described test nano ZnO 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
Sample on sample stage 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 and sample
Contact；
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, at the beginning of controlling Z axis piezoelectric ceramics stop motion and returning to
Beginning state；
Control computer recording and export the photosignal of four-quadrant photo detector and piezoelectricity pottery in loading procedure
Porcelain displacement relation curve.
The most according to claim 9 nano material mechanics performance in-situ test system test is utilized to receive
The method of rice material mechanical performance, it is characterised in that sample is fixed on described sample stage, shuts scanning electricity
The microscopical hatch door of son, after evacuation, the electron gun high voltage of scanning electron microscope, then open electronics
Bundle, adjusts scanning electron microscope duty, observes scanning probe microscopy pair under different enlargement ratios
Nano material carries out the microprocess of Mechanics Performance Testing.
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