CN203534987U - In-situ biaxial tilting nanoindentor used for transmission electron microscope (TEM) - Google Patents
In-situ biaxial tilting nanoindentor used for transmission electron microscope (TEM) Download PDFInfo
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- CN203534987U CN203534987U CN201320574347.8U CN201320574347U CN203534987U CN 203534987 U CN203534987 U CN 203534987U CN 201320574347 U CN201320574347 U CN 201320574347U CN 203534987 U CN203534987 U CN 203534987U
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Abstract
The utility model provides an in-situ biaxial tilting nanoindentor used for a transmission electron microscope (TEM), belonging to the field of in-situ testing for nano-materials. One end of a thermal bimetallic strip is fixed on a metal ring, the other end of the thermal bimetallic strip is a free end; a cantilever needle tip is fixed at the free end and on one side with a low thermal expansion coefficient, a needle tip on the cantilever needle tip is placed back to the thermal bimetallic strip, a sample is fixed at one end of a sample supporting platform, the other end of the sample supporting platform is fixed on the metal ring to enable the sample to be placed just opposite to the cantilever needle tip, and a gap between the sample and the needle tip is 2-50 microns; and the thermal bimetallic strip and the cantilever needle, as well as the sample and the sample supporting platform are respectively fixed together by using a conductive material, the thermal bimetallic strip and the sample supporting platform are respectively fixed with the metal ring in an insulating manner, and electrodes are respectively welded on the thermal bimetallic strip and the sample supporting platform, and connected with an external testing circuit. The in-situ biaxial tilting nanoindentor provided by the utility model maintains X-axis and Y-axis two degrees of freedom simultaneously, and can be used for real-time in-situ atom-scale observation for the structure of the nano-materials while compression is carried out.
Description
Technical field
The utility model relates to a kind of transmission electron microscope situ double shaft tilting nano impress instrument apparatus.This device is fixed on a dynamometry semi-girder on thrermostatic bimetal-plate, this thrermostatic bimetal-plate is fixed on used in transmission electron microscope copper ring, by the crease operation to nano material to the method cantilever tip of thrermostatic bimetal-plate heating.The deformation that in-situ image register system records semi-girder obtains mechanical signal, keeping X, two degree of freedom of Y-axis simultaneously, in compression, utilize transmission electron microscope the structure of nano material to be carried out to the observation of real-time in-situ atomic scale, belong to nano material in-situ method of testing field.
Background technology
Along with the development of microelectric technique and micro-system, many smile structures have obtained actual application.Meanwhile, the mechanical property of material under miniature scale also becomes the object that people pay close attention to gradually, and the Micro Mechanical Properties research of material is also carried out thereupon.Under the effect of stress and load, these micro-members usually can show with macroscopic conditions under difference characteristic, thereby arouse great concern.At present, this field has become science frontier and study hotspot.But for the research of the mechanical property of low-dimension nano material but in relatively backward state.Effort through decades, people have been developed multiple nano material mechanics Performance Test System, Nanoindentation wherein, due to the day by day maturation of its technical method, can realize the mechanical test test of the materials such as nano wire, nano particle, nano thin-film and make Nanoindentation become a kind of popular in-situ testing technique to the accurate Characterization of the fundamental physical quantities such as material modulus, hardness.But, because Nanoindentation can not provide the information of original position atomic scale, so in a lot of situations, all needing to infer the deformation mechanism under material strain state by the observation of rear position, this has caused obstacle just to people's correct understanding material deformation mechanism.After transmission electron microscope development, become gradually the characterization method and the method that disclose material atomicscale structure information, but due to the restriction in its narrow and small space, sample chamber, in so narrow and small space, sample chamber, realize the announcement of structural information under realizing material deformation process situ, atomic scale when material stress is applied and just seem very difficult.Therefore, the difficult problem of pendulum in face of researchist is how in transmission electron microscope, to realize the operations such as original position impression distortion of material at present.
At present, many commercial companies and laboratory are dropped into a large amount of human and material resources and are developed in-situ mechanical test products and obtained gratifying economic benefit, as 654 uniclinal stretching specimen holders of U.S. Gatan company production, can realize transmission electron microscope situ stretched operation, realize the research of structural evolution information under material strain state, but owing to having lost the Y-axis degree of freedom of verting, for crystalline material, cannot realize the differentiation information of microstructure under original position atomic scale; In addition, the STM-TEM sample stage that Nanofactory company produces can be realized the deformation operation of material, but, owing to having lost equally Y-axis degree of freedom, therefore the deformation operation that realizes original position atomic scale is also more difficult, for the crystal prototype that need to observe, just seem unable to do what one wishes under the positive tape spool of low index, also therefore limited its range of application.The PI-95 sample for use in transmitted electron microscope bar that U.S. Hysitron company produces can carry out quantitative nano impression and the test of nanometer cut easily, but only has equally the X-axis degree of freedom of verting, the vert range of application that has limited to a certain extent this specimen holder that is lost in of degree of freedom of Y-axis.
It needs to be noted, these methods can realize the Mechanics Performance Testing under the strain regime of material above, utilize said method, researcher has obtained extraordinary result of study, but owing to cannot realizing verting of Y-axis, thereby the probability of atomic scale observation material microstructure structural change under the positive tape spool of low index is reduced greatly, be unfavorable for the announcement of atomicscale structure evolution mechanism, this has just brought huge challenge to people's correct understanding material strain physics.In addition,, because the design cost of this type of sample stage is very high, be also unfavorable for the penetration and promotion of this series products.Therefore, design a kind of simple and convenient, with low cost, do not lose the vert used in transmission electron microscope original position double shaft tilting nano-hardness tester of degree of freedom of Y-axis, the mechanical property of the materials such as systematic study nano wire, nano particle, nano thin-film is a very challenging and very important job simultaneously.
Utility model content
The problem existing for prior art, the purpose of this utility model is to provide a kind of used in transmission electron microscope original position double shaft tilting nano-hardness tester based on thrermostatic bimetal-plate and dynamometry cantilever tip, it will be used in transmission electron microscope and realize nano material in-situ crease operation deformation experiment, utilize the mechanical signal that is applied to nano material that records that this used in transmission electron microscope original position double shaft tilting nano-hardness tester can be quantitative simultaneously, realize atomic scale microstructure change information corresponding with mechanical signal, investigate the mechanical property of nano material.
This used in transmission electron microscope original position double shaft tilting nano-hardness tester is suitable with transmission electron microscope carrier net size now used, being fixed on existing pair inclines on transmission electron microscope warm table, be not subject to the restriction of sample driving element size, put into transmission electron microscope and can realize wide-angle vert (the two warm tables that incline of at present commercialization can reach ± 30 °/± 60 °), sample can easily be tilted under the positive tape spool of low index of crystal prototype, realize the original position deformation operation that realizes nano material when atom level is differentiated, simultaneously, utilize on it size that is applied to the power in nano material of measuring that the cantilever tip that is equipped with can be quantitative, by image recording system real time record semi-girder deformation process, provide the Mechanical loading signal in material deformation process.
The basic structure of this used in transmission electron microscope original position double shaft tilting nano-hardness tester is one end of the thrermostatic bimetal-plate of a temperature-sensitive deformation to be fixed on to a side of common transmission electron microscope copper ring, the other end is unsettled, and fix one with the needle point of semi-girder at this section, after the sample that will study is fixed on sample support beam, the sample on brace summer is faced to needle point and the distance of sample and needle point is adjusted to 2-50 micron under the microscope.This impression instrument is arranged on and in business-like two transmission electron microscope warm table that inclines, puts into transmission electron microscope and heat, thrermostatic bimetal-plate on impression instrument is occured bending and deformation, drive cantilever tip on it to a lateral movement that has sample, realize impression distortion and the cut of sample are tested.Meanwhile, record the size that is applied to the power on sample by cantilever deflection of beam, the object information of the impression deformation process Atom yardstick of recording with image recording system is corresponding, discloses the deformation mechanism of material atomic scale.Utilize this impression instrument, Micro Zone Mechanical Properties and micromechanism directly can be mapped, from atom level, disclose mechanical property and the deformation mechanism of nano wire or film.
To achieve these goals, the utility model is realized by the following technical solutions:
This used in transmission electron microscope original position double shaft tilting nano-hardness tester comprises support section, drive part, described support section is becket 1, described drive part is a thrermostatic bimetal-plate being comprised of different linear expansion coefficients 2, thrermostatic bimetal-plate one end be fixed on becket above, the other end is free end; At free end and the low side of thermal expansivity, fix a cantilever tip 3, needle point in cantilever tip 3 is placed back to thrermostatic bimetal-plate 2, sample 4 is fixed on one end of sample holder 5, the other end of sample holder 5 is fixed on becket 1 and will allows sample 4 place over against cantilever tip 3, and the gap between sample 4 and cantilever tip 3 is between 2-50 micron; Thrermostatic bimetal-plate 2 and cantilever tip 3 use conductive materials are fixed together, sample 4 and sample holder 5 use conductive materials are fixed together, thrermostatic bimetal-plate 2, sample holder 5 are fixing with becket 1 insulation respectively, difference welding electrode in thrermostatic bimetal-plate 2, sample holder 5, electrode is connected with external test circuitry.
Electrode is connected the measurement of the nano material electrical properties that can realize under impression state with external test circuitry.
In the time of on the transmission electron microscope warm table that this impression instrument is fixed on to prior art, put into transmission electron microscope, rising along with warm table temperature, thrermostatic bimetal-plate is because thermal expansivity difference will occur bending and deformation to the low side of thermal expansivity, drive is fixed on the cantilever tip of this side to sample one lateral movement, along with the rising of temperature, cantilever tip will realize the crease operation to sample.Compression distance can regulate by adjusting outside temperature control original paper.By the deformation process of transmission electron microscope imaging system original position recording materials, and the deflection that occurs of semi-girder, from atom level, disclose the deformation mechanism of nano material, simultaneously, according to cantilever, deflection of beam obtains being applied to the size of the power in nano material, provides corresponding mechanical parameter.
Described support section is that electrical and thermal conductivity is good, the copper ring of easily processing, nickel ring, Jin Huan, the beckets such as molybdenum ring, in order to guarantee that this impression is to be fixed on sample for use in transmitted electron microscope bar, it is 3mm that the external diameter of becket carries net consistent with prior art, in order to guarantee that electron beam sees through, sample is carried out to structure analysis, center drilling, the thickness of becket is between 0.01mm-0.1mm.
Described drive part is the relatively very large sheet metal thrermostatic bimetal-plate that combines of difference of linear expansion, and when temperature variation, two kinds of different materials difference of linear expansions are very large and produce different expansions and contraction, cause bimetallic strip to produce flexural deformation.
Described drive part also can utilize the materials such as twin crystal piezoelectric ceramic piece, memorial alloy to replace, and forms intelligentized nano impress device.
Described cantilever tip can adopt the cantilever tip of commodity production, also can experimentally need to make cantilever tip by oneself, meanwhile, needle point can adopt traditional traditional AFM tip needle point, also can need to adopt the needle point etc. of tack or other shapes according to experiment.
Described sample type can comprise the zero-dimension nano materials such as nanosphere, nano particle; The monodimension nanometer material such as nano wire, nanometer rods; The two-dimensional nano materials such as nano thin-film; Three-dimensional block materials etc.
Utilize this used in transmission electron microscope original position double shaft tilting nano-hardness tester can realize the indentation test research of the original position atomic scale from zero dimension to the full material system of three-dimensional dimension all standing.
The utility model has the following advantages:
1, the utility model has carried out new structural design to transmission electron microscope carrier net, realization in transmission electron microscope nano material or even block materials be the nano impress operation of atomic scale originally, a kind of new material in situ mechanical measuring and calculation method is provided, there is dependable performance, easy for installation, feature simple in structure, has greatly expanded the function of transmission electron microscope.
2, in the utility model carry net physical dimension and prior art carry net basically identical, can pack into easily in high-resolution-ration transmission electric-lens, realize X, Y both direction wide-angle is verted, from best zone axis, realize high-resolution imaging when impression deformation operation in position, obtain the structural information of atomic scale.
3, two other remarkable advantage of the present utility model is exactly the measurement that can be under obtaining nano material effect of stress obtains being applied to electrical signal in the size of the power in nano material and material impression deformation process in the high-resolution micro-image of microstructure change.
Accompanying drawing explanation
Fig. 1 adopts the used in transmission electron microscope double shaft tilting nano-hardness tester structural representation of tip needle point
Fig. 2 used in transmission electron microscope double shaft tilting nano-hardness tester fundamental diagram
The original position double shaft tilting nano-indentation experiment schematic diagram of nano wire under Fig. 3 a transmission electron microscope
Fig. 3 b is the enlarged drawing in Fig. 3 a dotted line frame
Fig. 4 a is the original position double shaft tilting nano-indentation experiment schematic diagram of nano particle under transmission electron microscope
Fig. 4 b is the enlarged drawing in Fig. 4 a dotted line frame
Drawing is described as follows
1 becket 2 thrermostatic bimetal-plate 3 cantilever tip 4 sample 5 sample holder 6 electrodes
Embodiment
This used in transmission electron microscope original position double shaft tilting nano-hardness tester comprises support section, drive part and mechanical test part, described support section is becket 1, described drive part is a thrermostatic bimetal-plate being comprised of different linear expansion coefficients 2, thrermostatic bimetal-plate one end be fixed on becket above, the other end is free end; At free end and the low side of thermal expansivity, fix a cantilever tip 3, needle point in cantilever tip 3 is placed back to thrermostatic bimetal-plate 2, sample 4 is fixed in sample holder 5, the other end of sample holder 5 is fixed on becket 1 and will allows sample 4 place over against cantilever tip 3, and under the microscope the gap between sample 4 and cantilever tip 3 is adjusted between 2-50 micron.Thrermostatic bimetal-plate 2, cantilever tip 3 and sample 4, sample holder 5 are fixed together with conductive material respectively, thrermostatic bimetal-plate 2, sample holder 5 are fixing with becket 1 insulation respectively, thrermostatic bimetal-plate 2, sample holder 5 with on welding electrode 6 respectively, electrode 6 is connected the measurement of the nano material electrical properties that can realize under impression state with external test circuitry.
Specific embodiment 1:
1, by thrermostatic bimetal-plate being made shown in Fig. 1 to width, be 0.2mm, thick is 0.08mm, and length is the bimetallic strip of 1.8mm.Simultaneously by one long be 0.45mm, wide 0.2mm, thick is 0.2mm, elasticity coefficient is that the Si cantilever tip of 0.2N/m is fixed on the side that thrermostatic bimetal-plate expansion coefficient is low, by on thrermostatic bimetal-plate not a side of cantilever mounted beam needle point be fixed in the middle of perforate, a side of the used in transmission electron microscope copper ring that external diameter is 3.0mm.
2, by unsettled through one section, the thin district of single crystalline Si sample of mechanical lapping, the two sprays of electrolysis, ion milling, the other end is fixed in sample holder, under optical microscope, sample holder is fixed on 3mm copper ring, and make sample over against the needle placement of semi-girder, the height of adjusting sample, makes itself and cantilever tip on a horizontal line.
3, this nano-hardness tester is fixed on commercial transmission electron microscope heated sample bar, puts into transmission electron microscope.Hot platform by two transmission electron microscopes that incline is tilted to sample the Si[011 the most easily observing] under positive tape spool, by outside temperature-controlling system, specimen holder is heated.
4, the rising thrermostatic bimetal-plate along with temperature drives cantilever tip to sample one lateral movement, when cantilever tip just will touch sample, adjusting temperature-controlling system stops the motion of thrermostatic bimetal-plate, utilize the image recording system of transmission electron microscope to record the pattern of indentation test front boom beam needle point, be the original state of cantilever tip.Continue to drive thrermostatic bimetal-plate to move, drive cantilever tip to realize the impression deformation operation to sample.
5, utilize the high-resolution atomic diagram of transmission electron microscope as real-time in-situ, to record the structural information variation of the atomic scale of single crystalline Si in impression deformation process.Utilize the in good time deformation process that records cantilever tip of low power imaging system original position.
6,, by the comparative analysis to the Real-time High Resolution image of Si nano material microstructure change before and after distortion, can on atom level, disclose the heterogeneous microstructure change information of the reflection material mechanical performances such as the feature of nano material elastic-plastic deformation and the expansion of crackle.
7, simultaneously, by the deformation process of semi-girder that the imaging system of transmission electron microscope is recorded, analyze the signal that each stage is applied to the power on nano wire.Provide the microdeformation mechanism of nano material under effect of stress.
Claims (1)
1. used in transmission electron microscope original position double shaft tilting nano-hardness tester, it is characterized in that: comprise support section, drive part, described support section is becket, described drive part is a thrermostatic bimetal-plate being comprised of different linear expansion coefficients, thrermostatic bimetal-plate one end be fixed on becket above, the other end is free end; At free end and the low side of thermal expansivity, fix a cantilever tip, needle point in cantilever tip is placed back to thrermostatic bimetal-plate, sample is fixed on one end of sample holder, the other end of sample holder is fixed on becket and will allows sample place over against cantilever tip, and the gap between sample and cantilever tip is between 2-50 micron; Thrermostatic bimetal-plate and cantilever tip are fixed together with conductive material, sample and sample holder are fixed together with conductive material, thrermostatic bimetal-plate, sample holder are fixing with becket insulation respectively, difference welding electrode in thrermostatic bimetal-plate, sample holder, electrode is connected with external test circuitry.
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| CN201320574347.8U CN203534987U (en) | 2013-09-17 | 2013-09-17 | In-situ biaxial tilting nanoindentor used for transmission electron microscope (TEM) |
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| CN201320574347.8U CN203534987U (en) | 2013-09-17 | 2013-09-17 | In-situ biaxial tilting nanoindentor used for transmission electron microscope (TEM) |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103645199A (en) * | 2013-09-17 | 2014-03-19 | 北京工业大学 | In-situ double-axis tilting nanoindenter for transmission electron microscope |
| CN105223213A (en) * | 2015-09-28 | 2016-01-06 | 北京工业大学 | The two in-situ nano impression platform that inclines of a kind of transmission electron microscope |
| CN112649465A (en) * | 2020-11-20 | 2021-04-13 | 吉林大学 | Method for testing low-temperature thermal shrinkage coefficient of material by utilizing residual indentation morphology |
| CN113758949A (en) * | 2021-09-27 | 2021-12-07 | 南开大学 | Double-inclined TIP end applied to in-situ sample rod under transmission electron microscope for researching battery material |
-
2013
- 2013-09-17 CN CN201320574347.8U patent/CN203534987U/en not_active Withdrawn - After Issue
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103645199A (en) * | 2013-09-17 | 2014-03-19 | 北京工业大学 | In-situ double-axis tilting nanoindenter for transmission electron microscope |
| CN105223213A (en) * | 2015-09-28 | 2016-01-06 | 北京工业大学 | The two in-situ nano impression platform that inclines of a kind of transmission electron microscope |
| CN105223213B (en) * | 2015-09-28 | 2017-12-15 | 北京工业大学 | A kind of double in-situ nano impression platforms that incline of transmission electron microscope |
| US10410822B2 (en) | 2015-09-28 | 2019-09-10 | Beijing University Of Technology | Double-tilt in-situ nanoindentation platform for transmission electron microscope |
| CN112649465A (en) * | 2020-11-20 | 2021-04-13 | 吉林大学 | Method for testing low-temperature thermal shrinkage coefficient of material by utilizing residual indentation morphology |
| CN112649465B (en) * | 2020-11-20 | 2021-09-21 | 吉林大学 | Method for testing low-temperature thermal shrinkage coefficient of material by utilizing residual indentation morphology |
| CN113758949A (en) * | 2021-09-27 | 2021-12-07 | 南开大学 | Double-inclined TIP end applied to in-situ sample rod under transmission electron microscope for researching battery material |
| CN113758949B (en) * | 2021-09-27 | 2024-04-12 | 南开大学 | Double-tilting TIP (TIP) end applied to research of battery materials by in-situ sample rod under transmission electron microscope |
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| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20140409 Effective date of abandoning: 20151028 |
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| C25 | Abandonment of patent right or utility model to avoid double patenting |