CN108535106A - A kind of method that low error accurately measures single nano material Young's modulus - Google Patents
A kind of method that low error accurately measures single nano material Young's modulus Download PDFInfo
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- CN108535106A CN108535106A CN201810258770.4A CN201810258770A CN108535106A CN 108535106 A CN108535106 A CN 108535106A CN 201810258770 A CN201810258770 A CN 201810258770A CN 108535106 A CN108535106 A CN 108535106A
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 24
- 230000005540 biological transmission Effects 0.000 claims abstract description 14
- 238000005259 measurement Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 27
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims description 16
- 238000009413 insulation Methods 0.000 claims description 15
- 238000005286 illumination Methods 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 5
- 230000009514 concussion Effects 0.000 claims description 2
- 230000002452 interceptive effect Effects 0.000 claims 1
- 238000000926 separation method Methods 0.000 claims 1
- 230000008859 change Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 2
- 230000009897 systematic effect Effects 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 4
- 238000000691 measurement method Methods 0.000 description 3
- 239000002070 nanowire Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 241000219000 Populus Species 0.000 description 2
- 239000002134 carbon nanofiber Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000407 epitaxy Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 230000009471 action Effects 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000006243 chemical reaction Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000009666 routine test Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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Abstract
The invention discloses a kind of methods that low error accurately measures single nano material Young's modulus, and the characteristic size of single linear nano material sample to be measured is measured by transmission electron microscope；Single linear nano material sample to be measured is fixed in sample academic title's device on an electrode in two discharge electrodes being oppositely arranged；Applying alternate electrical signal to two discharge electrodes on sample clamping device makes sample generate vibration, change the frequency of alternate electrical signal, the vibrational state of single linear nano material sample to be measured is monitored using transmission electron microscope simultaneously, the frequency of acted on alternate electrical signal when there is peak swing by finding it, that is resonant frequency, to determine the intrinsic intrinsic frequency of the sample；It finally utilizes known function to calculate and obtains Young's modulus Y；The systematic error and human error in measurement process are sterilized as far as possible, improve the precision actually measured.
Description
Technical field
The present invention relates to Young's modulus field of measuring technique, specially a kind of low error accurately measures single nano material poplar
The method of family name's modulus.
Background technology
Prior art generally use drawing process is Young according to material stress-strain stress relation formula △ σ=Y/delta ε, wherein Y
Modulus, Δ σ are stress, and Δ ε is that strain obtains the Young's modulus Y of material by measuring Δ σ and Δ ε.Due to this stretching side
Method is only used for measuring macroscopic view or the Young's modulus of magnanimity sample, and the Young's modulus of single linear nano material is then needed
Find other measurement methods.
And in existing technical solution, it is microcosmic on measurement be also by manually being observed, in this way processing processing
Error is larger, is difficult to ensure for finally obtaining precision.
Invention content
In order to overcome the shortcomings of that prior art, a kind of low error of present invention offer accurately measure single nano material poplar
The method of family name's modulus can effectively solve the problem that the problem of background technology proposes.
The technical solution adopted by the present invention to solve the technical problems is：
A kind of method that low error accurately measures single nano material Young's modulus, includes the following steps：
Step 100, the characteristic size that single linear nano material sample to be measured is measured using transmission electron microscope；
Single linear nano material sample to be measured is fixed on sample clamping device, the sample clamping device by step 200
There are two the discharge electrode being oppositely arranged, single linear nano material samples to be measured to be actively installed between two discharge electrodes for tool；
Step 300, the alternate electrical signal that two discharge electrodes on sample clamping device are applied with different voltages, and by
It is as low as big to change the frequency of alternate electrical signal, while being existed to single linear nano material sample to be measured by transmission electron microscope
Vibrational state under alternate electrical signal effect is detected, and gradually obtains resonant frequency f, and converse intrinsic frequency f0；
Step 400, by the characteristic size of the single linear nano material sample to be measured measured and its corresponding intrinsic frequency
Substitute into known function f0In=F (Y, S, ρ), wherein f0For the intrinsic frequency of material, S represents the characteristic size of material, and ρ is material
Density, to obtain single linear nano material sample Young's modulus Y to be measured.
As a kind of preferred technical solution of the present invention, in step 200, on single linear nano material sample to be measured
It is provided with locking lantern ring, the locking lantern ring is fixedly connected with discharge electrode, and the locking lantern ring is in single linear nanometer to be measured
It is moved with equidistant Δ x on material sample, carries out measurement gradually, and by mobile distance x and measured resonant frequency
Corresponding record.
As a kind of preferred technical solution of the present invention, in step S300, the specific scaling step of intrinsic frequency is：
Step 301, using the position x of fixed point as abscissa, and relationship is made as ordinate using corresponding resonant frequency
Curve；
Step 302, the resonance for asking the frequency corresponding to curve minimum point to be single linear nano material sample to be measured frequency
Rate；
Step 303, according to reduction formula, resonant frequency is scaled to the intrinsic frequency of single linear nano material sample to be measured
Rate, reduction formula are：
Wherein, Q is the mechanical quality factor of sample.
As a kind of preferred technical solution of the present invention, in step 300, the specific acquisition method of resonant frequency is：
Sample clamping device both sides are installed with interference light emitting devices respectively and photosensitive reception resistance, the single linear to be measured are received
Rice material sample is located between interference light emitting devices and photosensitive reception resistance, wherein single linear nano material sample to be measured
Shake the curve that direction is vertical with plane where interference light, and the photosensitive reception resistance passes through display display intensity of illumination
Figure, and then determine as resonant frequency when intensity of illumination is most weak.
As a kind of preferred technical solution of the present invention, the sample clamping device is equipped with and the transmission electron microscopy
The insulation fixed pedestal that sample stage assembling structure on mirror matches, two discharge electrodes are located at and insulation fixed pedestal phase
On strut even.
As a kind of preferred technical solution of the present invention, it is provided on the insulation fixed pedestal for adjusting two electric discharges
The fine tuning regulating device of electrode gap, the fine tuning regulating device include differential head, are adjusted axially bar and sliding guide, the cunning
Dynamic guide rod is fixedly connected with insulation fixed pedestal, and is oriented to the axial stretching for being adjusted axially bar, wherein one
The discharge electrode is fixed on the end for being adjusted axially bar, and another discharge electrode is fixedly connected with the sliding guide,
The insulating lead-through terminal of connection discharge electrode is provided on the insulation fixed pedestal.
Compared with prior art, the beneficial effects of the invention are as follows：
The physical property of nano material is directly mapped with its microstructure and is measured using transmission electron microscope by the present invention
The characteristic size of sample obtains the intrinsic intrinsic frequency of sample by way of applying alternate electrical signal to sample, then utilizes
Known function obtains the Young's modulus of sample, solves the problems, such as to measure single linear nanometerial Young's modulus；Base of the present invention
Make forced vibration under the action of adding driving force outside in material, when the intrinsic frequency of the frequency domain material of driving force is identical, just
Covibration occurs, the intrinsic frequency of material is due to Young's modulus and the characteristic size decision of itself, i.e. existence function relationship
Formula：f0=F (Y, S, ρ), wherein f0For the intrinsic frequency of material, S represents the characteristic size of material, and ρ is the density of material, is
Known quantity, by measuring f0With S so that it is determined that Young's modulus Y.
Description of the drawings
Fig. 1 is flow diagram of the present invention；
Fig. 2 is inventive samples clamping device structural schematic diagram；
Fig. 3 is inventive samples clamping device end structure schematic diagram；
Fig. 4 is discharge electrode structure schematic diagram of the present invention；
Figure label：1- single linear nano material samples to be measured；2- locks lantern ring；3- discharge electrodes；4- sample clampings
Device；5- interferes light emitting devices；The photosensitive reception resistance of 6-；7- insulation fixed pedestals；8- finely tunes regulating device；9- differential heads；
10- is adjusted axially bar；11- sliding guides；12- insulating lead-through terminals.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
As shown in Figures 1 to 4, the present invention provides the sides that a kind of low error accurately measures single nano material Young's modulus
Method before measuring single linear nanometerial Young's modulus to be measured, will be fixed with single linear nano material sample to be measured first
Sample clamping device is inserted into transmission electron microscope, then exports alternate electrical signal generating means (not shown) signal
End is connected with connecting terminal.
When measurement, opens transmission electron microscope and the characteristic size of single linear nano material sample to be measured is surveyed
Amount applies alternate electrical signal to two discharge electrodes, exists to single linear nano material sample to be measured under transmission electron microscope
Judgement is observed and measured to vibrational state under alternate electrical signal effect, changes the frequency of alternate electrical signal, until making to be measured
Resonance state occurs for single linear nano material sample, with the resonant frequency of determination single linear nano material sample to be measured, most
The intrinsic frequency after the characteristic size of the single linear nano material sample to be measured measured and its conversion is substituted into accordingly afterwards
Know function f0In=F (Y, S, ρ), wherein f0For the intrinsic frequency of material, S represents the characteristic size of material, and ρ is the density of material,
The Young's modulus of the sample is calculated.
Specifically comprise the following steps：
Step 100, the characteristic size that single linear nano material sample to be measured is measured using transmission electron microscope.
Single linear nano material sample to be measured is fixed on sample clamping device, the sample clamping device by step 200
There are two the discharge electrode being oppositely arranged, single linear nano material samples to be measured to be actively installed between two discharge electrodes for tool.
In step 200, locking lantern ring 2, the locking lantern ring are provided on single linear nano material sample 1 to be measured
2 are fixedly connected with discharge electrode 3, and the locking lantern ring 2 is moved on single linear nano material sample 1 to be measured with equidistant Δ x
It is dynamic, carry out measurement gradually, and by mobile distance x and measured resonant frequency corresponding record.
It, can be to two in order to make single linear nano material sample to be measured generate corresponding vibration under alternate electrical signal effect
The spacing of discharge electrode is adjusted, so as to have between single linear nano material swatched end to be measured and another discharge electrode
Gap appropriate.
Step 300, the alternate electrical signal that two discharge electrodes on sample clamping device are applied with different voltages, and by
It is as low as big to change the frequency of alternate electrical signal, while being existed to single linear nano material sample to be measured by transmission electron microscope
Vibrational state under alternate electrical signal effect is detected, and gradually obtains resonant frequency f, and converse intrinsic frequency f0。
Substantially it is the resonance frequency of single linear nano material sample to be measured what is calculated according to the method described above
Rate, and resonant frequency and intrinsic frequency are different, intrinsic frequency is only determined by the property of system itself, on routine test,
Intrinsic frequency and resonant frequency are directly used as identical concept generally, but finely measured, it is necessary into
Row correction, and in fine measure, due to different measurement methods, deviation difference between resonant frequency and intrinsic frequency compared with
Greatly.
In step S300, the specific scaling step of intrinsic frequency is：
Step 301, using the position x of fixed point as abscissa, and relationship is made as ordinate using corresponding resonant frequency
Curve；
Step 302, the resonance for asking the frequency corresponding to curve minimum point to be single linear nano material sample to be measured frequency
Rate；
Step 303, according to reduction formula, resonant frequency is scaled to the intrinsic frequency of single linear nano material sample to be measured
Rate, reduction formula are：
Wherein, Q is the mechanical quality factor of sample.
In the present embodiment, Q values characterize the energy that piezoelectrics are consumed in resonance because overcoming interior friction, can pass through
Specific measurement method obtains its specific parameter value.
When above-mentioned resonance valve measures the resonant frequency of sample, freely shake since reality is unlikely to be undamped
Dynamic, the intrinsic frequency of the thin stick of metal cannot be measured directly, it is generally the case that so that sample is done permanent forced oscillation using excitation energy converter
It is dynamic, measure resonant frequency when forced vibration.According to experimental principle, it is desirable that detect to resonate under the conditions of sample both ends are free
Frequency, but node does not vibrate, therefore fixed point must deviate node when testing, resonant frequency by with the difference of fixed point position and
Variation, fixed point deviation node is remoter, and detectable signal is stronger, but thus generation system error is also bigger.In order to eliminate this
Error, can be used interpolation method or epitaxy deduces the resonant frequency of sample when assuming to be fixed on node.
In above-mentioned chart, using the position x of fixed point as abscissa, and make by ordinate of corresponding resonant frequency
Go out relation curve, the both direction reduced along frequency approaches, and can obtain the resonant frequency at node.Experiments have shown that:Using interior
The method of inserting or epitaxy processing experimental data can improve the accuracy of measurement result, eliminate systematic error, intrinsic to improve
The measurement accuracy of frequency.
Further, the specific acquisition method of resonant frequency is：It is installed with respectively in 4 both sides of sample clamping device dry
Light emitting devices 5 and photosensitive reception resistance 6 are related to, the single linear nano material sample 1 to be measured is located at interference light emitting devices 5
Between photosensitive reception resistance 6, wherein the concussion direction of single linear nano material sample 1 to be measured and plane where interference light
Vertically, it is described it is photosensitive receive resistance 6 by display show intensity of illumination curve graph, and then determine intensity of illumination it is most weak when
For resonant frequency.
The acquisition of resonant frequency being carried out in the above manner, main advantage is that, single linear to be measured can be received
The resonance of rice material sample 1 is amplified, consequently facilitating its specific vibration captures, and is carried out by way of photo resistance
Acquisition, can effectively avoid the artificial capture method on conventional meaning, pass through the intensity of illumination curve of generation and the frequency of alternating signal
Rate corresponds to, you can accurately obtains the resonant frequency of single linear nano material sample to be measured.
Step 400, by the characteristic size of the single linear nano material sample to be measured measured and its corresponding intrinsic frequency
Substitute into known function f0In=F (Y, S, ρ), wherein f0For the intrinsic frequency of material, S represents the characteristic size of material, and ρ is material
Density, to obtain single linear nano material sample Young's modulus Y to be measured.
In the present invention, the sample clamping device 4 is equipped with assembles with the sample stage on the transmission electron microscope
The insulation fixed pedestal 7 that structure matches, two discharge electrodes 3 are located on the strut being connected with insulation fixed pedestal 7.
Preferably, the fine tuning being provided on the insulation fixed pedestal 7 for adjusting two 3 gaps of discharge electrode is adjusted
Device 8, the fine tuning regulating device 8 include differential head 9, are adjusted axially bar 10 and sliding guide 11, the sliding guide 11 with
Insulation fixed pedestal 7 is fixedly connected, and is oriented to the axial stretching for being adjusted axially bar 10, wherein being put described in one
Electrode 3 is fixed on the end for being adjusted axially bar 10, and another discharge electrode 3 is fixedly connected with the sliding guide 11,
The insulating lead-through terminal 12 of connection discharge electrode 3 is provided on the insulation fixed pedestal 7.
In addition, in the present invention, it is also necessary to which further explanation is：
The section configuration of single linear nano material sample to be measured is different, expresses the known function of its Young's modulus also not
Together, the characteristic size of material involved in corresponding known function is different.
Such as when section is solid circles nano wire, the function for expressing its Young's modulus is：
Wherein L is nanowire length to be measured, and D is nanowire diameter to be measured, and ρ is density of material；
When the nanobelt that section is rectangle, the function for expressing its Young's modulus is：
Wherein L is nanometer strip length to be measured, and T is nanometer tape thickness to be measured, and ρ is density of material；
When the nanotube that section is annular, the function for expressing its Young's modulus is：
Wherein L is nanotube length to be measured, D1For nanometer bore to be measured, D2For nanometer pipe outside diameter to be measured, ρ is that material is close
Degree.
In actually detected, which is carbon nano-fiber, and characteristic size is：Length
L=6.5 μm, diameter D=45nm, the resonant frequency measured is：F=717kHz, and the mechanical quality factor Q minimum values of sample are
50, intrinsic frequency f0=0.005%f, i.e., f in this example0=f=717kHz, density：ρ=2.26 × 103kg/m3, will be upper
It states parameter and substitutes into function：
Obtain the Young's modulus of the carbon nano-fiber：Y=52Gpa.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
Claims (6)
1. a kind of method that low error accurately measures single nano material Young's modulus, which is characterized in that include the following steps：
Step 100, the characteristic size S that single linear nano material sample to be measured is measured using transmission electron microscope；
Single linear nano material sample to be measured is fixed on sample clamping device by step 200, which has
Two discharge electrodes being oppositely arranged, single linear nano material sample to be measured are actively installed between two discharge electrodes；
Step 300, the alternate electrical signal that two discharge electrodes on sample clamping device are applied with different voltages, and by as low as
The big frequency for changing alternate electrical signal, at the same by transmission electron microscope to single linear nano material sample to be measured in alternation
Vibrational state under electric signal effect is detected, and gradually obtains resonant frequency f, and converse intrinsic frequency f0；
Step 400, by the characteristic size of the single linear nano material sample to be measured measured and its corresponding intrinsic frequency f0It substitutes into
Known function f0In=F (Y, S, ρ), wherein f0For the intrinsic frequency of material, S represents the characteristic size of material, and ρ is the close of material
Degree, to obtain single linear nano material sample Young's modulus Y to be measured.
2. the method that a kind of low error according to claim 1 accurately measures single nano material Young's modulus, feature
It is, in step 200, locking lantern ring (2), the locking set is provided on single linear nano material sample (1) to be measured
Ring (2) is fixedly connected with discharge electrode (3), the locking lantern ring (2) on single linear nano material sample (1) to be measured with etc.
Separation delta x movement, carries out measurement gradually, and by mobile distance x and measured resonant frequency corresponding record.
3. the method that a kind of low error according to claim 1 accurately measures single nano material Young's modulus, feature
It is, in step S300, the specific scaling step of intrinsic frequency is：
Step 301, using the position x of fixed point as abscissa, and relation curve is made as ordinate using corresponding resonant frequency；
Step 302 asks the frequency corresponding to curve minimum point to be the resonant frequency f of single linear nano material sample to be measured；
Step 303, according to reduction formula, resonant frequency is scaled to the intrinsic frequency of single linear nano material sample to be measured,
Reduction formula is：
Wherein, Q is the mechanical quality factor of sample.
4. the method that a kind of low error according to claim 1 accurately measures single nano material Young's modulus, feature
It is, in step 300, the specific acquisition method of resonant frequency is：It is installed with respectively in sample clamping device (4) both sides
Interference light emitting devices (5) and photosensitive reception resistance (6), the single linear nano material sample (1) to be measured are located at interference light
Between emitter (5) and photosensitive reception resistance (6), wherein the concussion direction of single linear nano material sample to be measured (1) with
Plane where interfering light is vertical, the photosensitive curve graph for receiving resistance (6) and showing intensity of illumination by display, and then really
Determine intensity of illumination it is most weak when as resonant frequency.
5. the method that a kind of low error according to claim 1 accurately measures single nano material Young's modulus, feature
It is, the sample clamping device (4), which is equipped with, to be matched with the sample stage assembling structure on the transmission electron microscope
Insulate fixed pedestal (7), and two discharge electrodes (3) are located on the strut being connected with insulation fixed pedestal (7).
6. the method that a kind of low error according to claim 5 accurately measures single nano material Young's modulus, feature
It is, the fine tuning regulating device (8) for adjusting two discharge electrode (3) gaps is provided on the insulation fixed pedestal (7),
The fine tuning regulating device (8) includes differential head (9), is adjusted axially bar (10) and sliding guide (11), the sliding guide
(11) it is fixedly connected with insulation fixed pedestal (7), and the axial stretching for being adjusted axially bar (10) is oriented to, wherein
A piece discharge electrode (3) is fixed on the end for being adjusted axially bar (10), another discharge electrode (3) and the sliding
Guide rod (11) is fixedly connected, and the insulating lead-through terminal of connection discharge electrode (3) is provided on the insulation fixed pedestal (7)
(12)。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110286140A (en) * | 2019-06-28 | 2019-09-27 | 中国人民解放军陆军工程大学 | Method for detecting vibration characteristics of resonator of nano-electromechanical system |
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| CN1410775A (en) * | 2002-11-14 | 2003-04-16 | 上海交通大学 | Method of measuring nano grade crystal whisker material Young modulus |
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| CN110286140A (en) * | 2019-06-28 | 2019-09-27 | 中国人民解放军陆军工程大学 | Method for detecting vibration characteristics of resonator of nano-electromechanical system |
| CN110286140B (en) * | 2019-06-28 | 2022-01-25 | 中国人民解放军陆军工程大学 | Method for detecting vibration characteristics of resonator of nano-electromechanical system |
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| CN108535106B (en) | 2021-05-07 |
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Inventor after: Zhang Xiaolong Inventor before: Xu Zhi Inventor before: Zhang Xiaolong Inventor before: Bai Xuedong |