CN103471905B - For single-axis bidirectional micro mechanics measurement mechanism and the measuring method of scanning microscopy environment - Google Patents
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Abstract
The invention belongs to micro nanometer mechanics and precision optical machinery field, particularly a kind of single-axis bidirectional micro mechanics measurement mechanism and measuring method for scanning microscopy environment. This device is installed the three-dimensional mobile precision surface plate of fine tuning and the sample platform of the three-dimensional coarse adjustment translation stage of symmetrical co-ordinate-type, symmetry on body supports unit, by control system and actuation unit control operation, can complete the detection of micro-nano characteristic dimension material and structural mechanical property, realize unidirectional centering stretching, compression, bending and vibration measurement, and the distortion of micro-nano-scale specimen surface and Microstructure Evolution detection; Device can repeatedly use, and can realize in conjunction with digital picture/speckle correlation technique, image processing techniques or micro-labelling technique original position distortion and the mechanical property detection of the sample under high-space resolution scanning microscopy environment.
Description
Technical field
The invention belongs to micro nanometer mechanics and precision optical machinery field, particularly a kind of for scanning microscopy environmentSingle-axis bidirectional micro mechanics measurement mechanism and measuring method.
Background technology
Micro nanometer mechanics is tested as the important part of micro-nano scientific domain, at micro/nano-scale material, knotIn the mechanical property detection of structure and device and checking, play important and irreplaceable effect. Its initial demand is comeCome from the Research Requirements to small dimensional material mechanical property, derive from MEMS and other minute yardstick devicePrediction and the analysis of energy and reliability, derive from meticulous, the many chis to describing labyrinth material behaviorThe checking of degree model. Especially due to material and feature size reduce cause new mechanics, physics, addThe change of the performances such as work, can, at micron to nanometer, under even less yardstick, directly carry out the inspection of mechanical propertySurvey and characterize, so obtain when material or structure after its external dimensions and internal microstructure feature sharply reduce itsThe variation of mechanical property. Since the eighties in last century, mechanics in the thin sight of material and structure, microcosmic andReceive theory and the calculating aspect of seeing yardstick performance and behavior and obtained important progress, aspect experiment, althoughThrough the effort of two more than ten years of researcher, compare micro-nano-scale Experiments of Machanics with numerical computations with theory analysisProgress want difficulty many because the experiment under this yardstick is complete at needs, detect clearly principle and methodTime, also need to be by basic experimental technique and checkout equipment, and this is to have challenge under small scaleProblem. Therefore, experiment detection field, be in today, the characteristic dimension of detected object sub-micron withUnder experiment remain extremely difficult.
Obviously, be no matter size, in function, or clamping, loading and manipulation aspect, to so smallResearch object, macroscopic view checkout equipment can not adapt to this new demand. Yardstick that research object has is little,Performance complexity, there is the features such as strong coupling interaction with detection system and environmental energy, make micro-nano realityTest mechanics and face numerous challenges.
In the face of the demand of basic research and high-tech application, producer has been studied according to numerous users' demand on the one handFor example, at the general formula small-scale experiment machine relatively lagging behind aspect function and performance two: be applicable to optical microscope systemWith the Britain Gatan mechanics module of SEM environmental chamber, be applicable to the U.S. Tytron250 of fiber and small scale sampleMicro-power the static and dynamic experiment machine and be mainly used in the American MTS NanoBionix experimental machine of biological medicine materialDeng. Although these experimental machine are compared with macroscopical experimental machine in the past, at aspects such as load, displacement range and resolution ratioAll draw close to minute yardstick, but mainly still apply traditional material testing machine principle, test specimen yardstick centimetre arrives substantiallyMillimeter magnitude, load and displacement are much larger than the desired scope of micro Nano material, and instrument is expensive. AnotherAspect, in view of the difficulty of commercial experimental machine, researcher both domestic and external, according to the demand of oneself, has carried out again voluntarilyThe more advanced micro Nano material mechanical property experiment device of some functions and performance (why be called device, be because ofFor these measuring systems are not also complete material experiment-machines, major part is the system of temporarily building, and only may completeThe unit that Some Mechanical Properties is measured). This class is by the material mechanical performance detection dress of early exploitation in period of researcherPut or system, price is comparatively cheap, and the mechanical property that is applicable to some special material or structure detects, but large portionSeparating device only can be worked under optical microphotograph platform, and the mechanics that can not meet material and structure under micro-nano-scale is learnedPerformance Detection, more can not realize under micro-nano-scale testing conditions, to the requirement such as clamping and manipulation of micro-structural.
Summary of the invention
The object of the invention is the height based on SEM (SEM) or light microscope (OM)Space micro-imaging environment, provides a kind of single-axis bidirectional micro mechanics measurement mechanism for scanning microscopy environment,Can be for studying the test specimens such as micro-nano characteristic dimension film, silk, line at bars such as uniaxial tension, compression, bendingsMechanical property under part.
The technical solution used in the present invention is:
Integrated support cellular installation is on SEM sample stage pedestal, and its upper surface center arranges circular hole, in holeThe stretchable SEM sample stage of interior installation, bilateral symmetry position arranges respectively three-dimensional coordinate translation stage and integrated supportUnit connection substrate;
Each three-dimensional coordinate translation stage and integrated support unit connection substrate are installed respectively by directions X translation piezoelectricityThe three-dimensional coarse adjustment translation stage of co-ordinate-type of guide rail, Y-direction translation piezoelectricity guide rail, Z direction translation piezoelectricity guide rail composition;Upper end and the coarse adjustment platform linking arm of Z direction translation piezoelectricity guide rail are affixed, and coarse adjustment platform linking arm is by piezoelectricity coverPipe is connected with the three-dimensional mobile platform of fine tuning piezoelectric ceramics; The front end of the three-dimensional mobile platform of fine tuning piezoelectric ceramics is by passingSensor is connected with sensor with fine tuning translation stage joint sleeve, and front end and the sample platform of sensor are affixed.
Between described integrated support unit and SEM sample stage pedestal, fix by 3 internal threads, two alignment pinsConnect.
Described directions X translation piezoelectricity guide rail, Y-direction translation piezoelectricity guide rail, Z direction translation piezoelectricity guide rail are divided equallyDo not formed by an one dimension piezoelectric motor and a guide rail.
Described sample platform is the symmetrical loading end of plane, V-type loading end or sonde-type loading end, and phaseThe configuration of answering is fixed structure.
Based on described device, the present invention also provides a kind of measuring method, carries out as follows:
(a) adjust sample platform centering, flat according to sample characteristics size Selection at optics or SEM imaging circumstancesDirectly, the consistent rear locking of axis; Adjust sample platform and reach suitable initial loading spacing; At light microscope orIn SEM cavity, complete sample holder and installation, when installation, ensure long axis and the SEM sample stage tensile axis of sampleLine overlaps;
(b) adjust the detection platform position, multiplication factor, imaging and the image capturing system that scan microscopic systemAnd make it be in detected state, then drive unit carries out the micro-stretching experiment of single-axis bidirectional to test specimen, and simultaneously logicalCross the sequence deformation pattern that SEM scan image records sample surveyed area;
(c) the sequence deformation pattern of gained is carried out respectively to Digital Image Processing, micro-labeled analysis, obtain examinationSurveyed area surface micro-structure deformation evolution situation in single-axis bidirectional drawing process when sample stretches; Meanwhile knotClose Micro-force sensor and obtain corresponding load information, can obtain power-displacement or the stress-strain song of test samplesLine, and other mechanical property parameter, and knowing in conjunction with the microstructure about expanded material, micromorphology aspectKnowledge and theory are analyzed.
In described step (a), sample is large scale sample and while sample being installed under optical microphotograph environment, makesSample two ends are bonded in symmetrical sample platform and are solidified with glue, and then whole measurement mechanism is put into SEMEnvironmental chamber completes subsequent operation and measurement.
In described step (a), when sample is micro-nano sample, by sample platform adjusted centering and straightDevice is put into SEM environmental chamber, by SEM imaging, and the micro-nano that utilizes assisted control equipment to detectRice sample is attached in sample platform, and it is fixing to weld (EBID) by electron beam deposition.
The present invention compared with prior art, has the following advantages:
(1) conventionally because high power microscan region is very limited, its small visual field yardstick makes detection zoneTerritory runs off visual field very soon and cannot realize the continuous detecting in whole loading procedure. The present invention has by designEnsure the mechanical structure, two of adjusting of two objective table axis three-dimensional coordinate formula consistent and in same levelMobile platform single-axis bidirectional drive system realizes bi-directional symmetrical and loads, and is suitable for high spatial resolution microscopic systemSmall field of view feature, ensure interested film scanning region in whole drawing process all the time in micro-systemIn system visual field, thereby can complete the continuous detecting of test samples surface micro-structure Character evolution in micro-surveyed area.
(2) by applying piezoelectric motor and two kinds of drive units of piezoelectric ceramic tube, can realize mould in thick, thin twoFormula loads, and this is that detected object characteristic dimension is from hundreds of microns to the material of tens nanometer or the mechanical meaurement of structureProvide and loaded and location guarantee.
(3) in order to realize effective and the accurate mechanical meaurement of micro-nano-scale sample, clamping and manipulation, establishCounted the objective table of two types, a kind of is platform-type, and another kind is probe-type, can be applicable to respectively film,Measurement, clamping, loading and the manipulation of the micro-nano-scale samples such as silk, line, pipe and post. Meanwhile, in order to adapt toThe installation of small scale sample and the adjustment of device, this apparatus system has also comprised auxiliary micro-test sample clamping and has handledUnit, sample objective table neutralization is adjusted to benchmark jig etc., the installation, the loading that have effectively solved micro-test samplePlatform regulates and the sample axis calibration problem consistent with objective table axis in horizontal plane.
And existing chip type film test piece under scanning electron beam microscope system, the clamping knot of being applied to (4)The integrated micro-tensile loading device of structure is compared, and this checkout gear can repeatedly use, and can be applicable to the not same sexThe minute yardstick material of matter, size and the detection of structure, expanded the range of application of installing greatly. In conjunction with digitized mapThe correlation techniques such as picture processing can realize minute yardstick specimen surface micro-structural distortion under high spatial resolution microscopy environmentWith the detection of developing, equally also can be adapted to the continuous detecting of large deformation, complex topography feature etc.
Brief description of the drawings
Fig. 1 is co-ordinate-type single-axis bidirectional stretching device overall structure schematic diagram;
Number in the figure:
1-X direction translation piezoelectricity guide rail; 2-Y direction translation piezoelectricity guide rail; 3-Z direction translation piezoelectricity guide rail; 4-Coarse adjustment platform linking arm; 5-piezoelectricity sleeve pipe; The three-dimensional mobile platform of 6-fine tuning piezoelectric ceramics; 7-sensor and fine tuningTranslation stage joint sleeve; 8-sensor; 9-sample platform; 10-sample; 11-three-dimensional coordinate translation stage and entiretySupport unit connection substrate; 12-M4-20 hexagon socket head cap screw; 13-integrated support unit; 14-SEM sample stagePedestal; 15-SEM sample stage; 16-alignment pin.
Detailed description of the invention
The invention provides a kind of single-axis bidirectional micro mechanics measurement mechanism and measurement side for scanning microscopy environmentMethod, stretches and detects as example taking single-axis bidirectional under SEM microscopic system below, by reference to the accompanying drawings to principle of the present invention,Concrete structure, stretching detection method are described further.
As shown in Figure 1, integrated support unit 13 is rectangle flat aluminium alloy plate (175mm × 95mm × 7mm),Surface is sprayed with argentine paint, and integrated support unit 13 is arranged on SEM sample stage pedestal 14, both itBetween connect by 16,3 M4-20 hexagon socket head cap screws 12 of two alignment pins. Integrated support unit 13Upper surface center arranges the circular hole that diameter is 48mm, and SEM sample stage 15 is through integrated support unit 13Center hole can be used as the objective table of stretching device. Establish respectively the bilateral symmetry position of integrated support unit 13Put three-dimensional coordinate translation stage and integrated support unit connection substrate 11; Each three-dimensional coordinate translation stage and integrated supportUnit connection substrate 11 is installed respectively by directions X translation piezoelectricity guide rail 1, Y-direction translation piezoelectricity guide rail 2, ZThe three-dimensional coarse adjustment translation stage of co-ordinate-type that direction translation piezoelectricity guide rail 3 forms. Z direction translation piezoelectricity guide rail 3 upperEnd is affixed with coarse adjustment platform linking arm 4, can realize large stroke and load; Coarse adjustment platform linking arm 4 passes through piezoelectricitySleeve pipe 5 is connected with the three-dimensional mobile platform 6 of fine tuning piezoelectric ceramics, realizes three-dimensional accurate displacement; Fine tuning piezoelectricity potteryThe front end of the three-dimensional mobile platform 6 of porcelain is connected with sensor 8 with fine tuning translation stage joint sleeve 7 by sensor,The front end of sensor 8 and sample platform 9 are affixed.
Directions X translation piezoelectricity guide rail 1, Y-direction translation piezoelectricity guide rail 2, Z direction translation piezoelectricity guide rail 3 are divided equallyDo not formed by an one dimension piezoelectric motor and a guide rail. Each piezoelectric motor is respectively by power supply and holding wireBe connected with drive system, under the effect of drive system, make platform that guide rail drives respectively along X, Y,Z direction co-ordinate-type moves (single step or continuous), and its stroke in X, Y, Z direction is respectively 12mm,200nm is differentiated in displacement.
The three-dimensional mobile platform 6 of fine tuning piezoelectric ceramics is connected with drive system by power supply, holding wire respectively,Can be respectively in X, Y and the meticulous movement of Z direction under the driving of drive system, its stroke is 6 μ m, positionMove and differentiate 1nm.
In order to realize the connection of dissimilar sensor, sensor 8 and sample platform 9 adopt screw thread and solidRationed marketing connects. Sample platform 9 has two types, and one is the symmetrical loading end of plane or V-type loading end,For measurements such as the drawing of film and silk class sample, pressures, another kind of is sonde-type loading end, be tungsten filament orGlass probe formula, for the measurement such as bending, vibration of film or silk class, micro-nano rice noodles, post etc. SamplePlatform 9 can configure and be fixed accordingly structure. Sample 10 and sample platform 9 according to sample yardstick withMaterial, optionally sticks with glue, any mode such as electron beam irradiation welding and V-type bayonet socket is connected. In displacementLoad while not needing sensor 8, sensor and fine tuning translation stage joint sleeve 7 and sample platform 9 can be directBe connected with alignment pin by sleeve pipe.
Two M4 screws are also set on integrated support unit 13, for connecting other manipulation or auxiliary establishingStandby.
In the whole process of device, adopt higher machining accuracy requirement, a symmetrical structure left side,Right three-dimensional mobile platform, then left and right sample platform feeding cuts apart shape in same block materials Integratively processingBecome, thus the symmetry of the machining accuracy of assurance device and structure.
The operation principle of this device is as follows: first the device of adjusting is put in the sample platform of SEM cavity(supporting Electronic Speculum: the Quanta450FEG of FEI Co.), by 16 and 3 M4-20 of alignment pin sixAngle screw 12 is connected the integrated support unit 13 of device with SEM sample platform base 14. In order to ensure deviceSteady operation, be fastenedly connected screw. Then the power supply of device and holding wire are passed through to supporting ring flange and chamberExternal manipulation control module is connected with drive system. About the communication of SEM cavity with control by the structure of ring flange andRequirement, makes or buys according to the requirement of Electronic Speculum used. After all signals of telecommunication connect, can be byElectronic Speculum chamber door is closed, and carries out platform and device operation after vacuumizing. Before mechanics detects, first device is passed throughSEM three-dimensional platform is adjusted to field of view center, and by selecting the suitably multiplication factor of size, observes sample flatPlatform 9 and sample 10. About the adjustment of sample platform in checkout gear and the installation of sample, can divide two kinds of situations,For tens microns of above test specimens of characteristic dimension, can be by light microscope, sample platform outside SEM cavity9 chucking device is adjusted, and then by gluing or V-type draw-in groove, test specimen is installed; For light microscope withoutFirst the sample that method is differentiated, adjust jig by sample and adjust both sides sample platform 9 under light microscopeCentering and straight, be then arranged on as described above in SEM cavity, after vacuumizing, by SEM againStraight and the centering of sample platform 9 is adjusted in inferior imaging, and adjusts by thick, the thin mobile platform of device,After completing, the sample platform of both sides symmetry 9 is adjusted to suitable distance, then by assisted control equipment, asMicro-nano manipulator will detect micro-nano rice noodles, micro-nano mitron or post and be attached in sample platform 9, and by electricitySon bundle is welded and fixed, and completes the installation of micro-nano sample.
Completion system starts drive unit, sensor, SEM image capturing system, after installing, adjustingThe mechanical property that can realize micro-nano sample under micro-condition detects.
The micro-stretching measuring method of micro-nano-scale sample single-axis bidirectional under scanning microscopy environment:
Micro-nano-scale sample measurement device under scanning microscopy environment has been applied to the micro-stretching of single-axis bidirectionalWhen measurement, first place it on the article carrying platform of microscopic system (optics or SEM), utilize microscopic systemSurface texture to test samples and deformation pattern are observed and acquisition and recording. Its concrete measuring method is by as followsStep is carried out:
1) as mentioned before, flat at optics or SEM imaging circumstances adjustment sample according to sample characteristics size SelectionPlatform centering, straight, locking after axis is consistent; Adjust sample platform and reach suitable initial loading spacing; ClampingWith installation test specimen, in light microscope or SEM cavity, complete sample and install. When installation, ensure the major axis of sampleLine and objective table stretching dead in line. While sample being installed under large scale sample and optical microphotograph environment, can useGlue is bonded in sample two ends in the symmetrical sample platform of device and solidifies, and then device is put into SEM environmental chamberComplete subsequent operation and measurement; In the time of micro-nano sample, by the device of adjusted centering and straight sample platformPut into SEM environmental chamber, by utilizing SEM imaging, and it is micro-nano to utilize assisted control equipment to detectSample is attached in sample platform, and fixes by electron beam welding.
2) detection platform position, multiplication factor, imaging and the image capturing system of adjustment scanning microscopic system are alsoMake it be in detected state, then drive unit carries out the micro-stretching experiment of single-axis bidirectional to micro-nano test specimen, and withTime record the sequence deformation pattern of sample surveyed area by SEM scan image;
3) the sequence deformation pattern of gained is carried out respectively to Digital Image Processing, micro-labeled analysis, obtain sampleSurveyed area surface micro-structure deformation evolution situation in single-axis bidirectional drawing process when stretching; Meanwhile combinationMicro-force sensor obtains corresponding load information, can obtain power-displacement or the stress-strain song of test samplesLine, and other mechanical property parameter, as Young's modulus, yield stress, break limit, and draw in conjunction with relevantStretch the microstructure of thin-film material, the knowledge and theory of micromorphology aspect is analyzed, and finds out its Microstructure EvolutionWith experience result or the rule of mechanical property.
4) the corresponding surface of image and the sub-surface second electron emission intensity of scanning microscopic system, it has disclosed inspectionThe information such as test specimens micro-structural, micromorphology, and show in the mode of gray level image; When specimen surface distortionOr motion is hour, the surface micro-structure spy that these images that represent with gray scale can Complete Characterization material film micro areaThe motion and deformation of levying, so the problem of the feature distortion of specimen surface micro-structural, evolution just converts to obtainingThe gray level image problem of carrying out respective image processing, and these problems can be correlated with by image digitization (DIC)Or micro-gauge point tracking technique obtains.
Other metering system, as the measurement of compression, bending, vibration etc., similar and above-mentioned measuring method, only existsDifference to some extent on sample platform type and drive pattern.
Claims (7)
1. for the single-axis bidirectional micro mechanics measurement mechanism of scanning microscopy environment, it is characterized in that:
It is upper that integrated support unit (13) is arranged on SEM sample stage pedestal (14), in integrated support unit (13)Upper surface center circular hole is set, stretchable SEM sample stage (15) is installed in hole, SEM sample stage(15) bilateral symmetry position arranges respectively three-dimensional coordinate translation stage and integrated support unit connection substrate (11);
Each three-dimensional coordinate translation stage and integrated support unit connection substrate (11) are installed respectively by directions X translationThe coordinate of piezoelectricity guide rail (1), Y-direction translation piezoelectricity guide rail (2), Z direction translation piezoelectricity guide rail (3) compositionThe three-dimensional coarse adjustment translation stage of formula; The upper end of Z direction translation piezoelectricity guide rail (3) and coarse adjustment platform linking arm (4) are solidConnect, coarse adjustment platform linking arm (4) is by piezoelectricity sleeve pipe (5) and the three-dimensional mobile platform of fine tuning piezoelectric ceramics (6)Connect; The front end of the three-dimensional mobile platform of fine tuning piezoelectric ceramics (6) is by sensor and fine tuning translation stage adapter sleevePipe (7) is connected with sensor (8), and the front end of sensor (8) and sample platform (9) are affixed.
2. the single-axis bidirectional micro mechanics measurement mechanism for scanning microscopy environment according to claim 1,It is characterized in that: in passing through 3 between described integrated support unit (13) and SEM sample stage pedestal (14)Screw, two alignment pins (16) are fixedly connected with.
3. the single-axis bidirectional micro mechanics measurement mechanism for scanning microscopy environment according to claim 1,It is characterized in that: described directions X translation piezoelectricity guide rail (1), Y-direction translation piezoelectricity guide rail (2), Z directionTranslation piezoelectricity guide rail (3) is made up of an one dimension piezoelectric motor and a guide rail respectively.
4. the single-axis bidirectional micro mechanics measurement mechanism for scanning microscopy environment according to claim 1,It is characterized in that: described sample platform (9) is the symmetrical loading end of plane, V-type loading end or sonde-typeLoading end, and corresponding configuration is fixed structure.
Based on described in claim 1 device a measuring method, it is characterized in that, the method by asLower step is carried out:
(a) according to sample characteristics size Selection optics or SEM imaging circumstances adjust sample platform (9) centering,Straight, locking after axis is consistent; Adjust sample platform (9) and reach suitable initial loading spacing; At opticsIn microscope or SEM cavity, complete sample holder and installation, when installation, ensure long axis and the SEM sample of samplePlatform (15) stretching dead in line;
(b) adjust the detection platform position, multiplication factor, imaging and the image capturing system that scan microscopic systemAnd make it be in detected state, then drive unit carries out the micro-stretching experiment of single-axis bidirectional to test specimen, and simultaneously logicalCross the sequence deformation pattern that SEM scan image records sample surveyed area;
(c) the sequence deformation pattern of gained is carried out respectively to Digital Image Processing, micro-labeled analysis, obtain examinationSurveyed area surface micro-structure deformation evolution situation in single-axis bidirectional drawing process when sample stretches; Meanwhile knotClose Micro-force sensor and obtain corresponding load information, can obtain power-displacement or the stress-strain song of test samplesLine, and mechanical property parameter, comprising: Young's modulus, yield stress, break limit, and draw in conjunction with relevantStretch the microstructure of material, the knowledge and theory of micromorphology aspect is analyzed.
6. measuring method according to claim 5, is characterized in that, in described step (a), and sampleWhile sample being installed for large scale sample and under optical microphotograph environment, use glue that sample two ends are bonded in symmetricalSample platform (9) is upper solidifies, and then by whole measurement mechanism put into SEM environmental chamber complete subsequent operation andMeasure.
7. measuring method according to claim 5, is characterized in that, in described step (a), and sampleDuring for micro-nano sample, sample platform (9) adjusted centering and straight device are put into SEM environmental chamber,By SEM imaging, and utilize the micro-nano sample that assisted control equipment will detect to be attached to sample platform(9) upper, and be welded and fixed by electron beam deposition.
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