CN103663354A - Micro/nano array and application thereof in micro/nano material standard bending strain loading - Google Patents
Micro/nano array and application thereof in micro/nano material standard bending strain loading Download PDFInfo
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Abstract
The invention discloses a micro/nano array and application thereof in micro/nano material standard bending strain loading. The micro/nano support array is composed of a substrate and a plurality of column-shaped structures which are located vertically on the substrate and are distributed at intervals to serve as supporting points. A micro/nano supporting dot matrix pattern can be defined freely. The micro/nano array is used for standard bending strain loading of quasi-one-dimensional micro/nano materials with different lengths and thicknesses, and has great application prospects in development of microforce and displacement sensors, flexible micro-nano biology, photoelectric detection and many other aspects.
Description
Technical field
The present invention relates to a kind of micro-/ nano array and the application in the bending strain of micro/nano material standard loads thereof.
Background technology
The mechanical property of material is an importance of nominal material, and strain has tremendous influence for the physical property of material itself.As far back as 1932, strain just started to cause research widely to the impact of crystal electronics, utilizes afterwards strain improved semiconductor device, has become a kind of indispensable technology in semi-conductor industry.Especially recent, develop in swift and violent low-dimensional materials, as nanotube, nano wire, nano thin-film and single-layer graphene etc., mechanical property is more superior, and strain is simultaneously also more remarkable for the physical property impact of material itself.And show under many circumstances strong yardstick and rely on effect (P.W.Bridgman, The effect of homogeneous mechanical stress on the electrical resistance of crystals.Phys.Rev.42, 858-863 (1932) .A.Maiti, Carbon nanotubes:Bandgap engineering with strain.Nat.Mater.2, 440-442 (2003) .K.H.Hong, J.Kim, S.H.Lee & J.K.Shin, Strain-driven electronic band structure modulation of Si nanowires.Nano Lett.8, 1335-1340 (2008) .J.Zang, M.Huang & F.Liu, Mechanism for nanotube formation from self-bending nanofilms driven by atomic-scale surface-stress imbalance.Phys.Rev.Lett.98, 146102 (2007), N.Levy, et al.Strain-Induced Pseudo-Magnetic Fields Greater Than 300Tesla in Graphene Nanobubbles.Science 329 (5991), 544-547 (2010)).Mechanics Performance Testing and research strain (especially heterogeneous strain) for the accurate one dimension micro/nano material of micro-scale seems particularly important to the impact of its physical property thus, and caused that people study widely to it.And developed the method (Han Xiaodong of several widely used nano material strain loadings, Yue Yonghai, Zheng Kun, Zhang Yuefei, open pool. the stress test grid of nano material used for transmission electron microscopy (patent No.: 200810056836) .X.Han, et al.Electronic and mechanical coupling in bent ZnO nanowires.Adv Mater 21, 4937-4941 (2009) .H.Xue, et al.Probing the strain effect near band edge emission of a curved ZnO nanowire via spatially resolved cathodoluminescence.Nanotechnology 21, 215701 (2010) .C.Dietrich, et al.Strain distribution in bent ZnO microwires.Appl Phys Lett 98, 031105 (2011) .Q.Fu, et al.Linear strain-gradient effect on the energy bandgap in bent CdS nanowires.Nano Res 4, 308-314 (2011)).But more than aiming at one dimension micro/nano material carries out in method, all failing in bending strain loading real realization and aims at one dimension micro/nano material and realize effective standard bending strain and load.
Summary of the invention
The object of this invention is to provide a kind of micro-/ nano array and the application in the bending strain of micro/nano material standard loads thereof.
Micro-/ nano provided by the invention supports array, substrate, consists of with vertical several column constructions as the strong point that are intervally arranged that are positioned on described substrate;
In above-mentioned array, described substrate is N-shaped monocrystalline substrate;
The shape of cross section of described column construction can be determined according to actual needs, as can be circular or square or triangle; The shape of cross section of this column construction and size can be set by mask plate depending on requirement of experiment, and more specifically, the diameter of described column construction is 14 μ m, cross section be shaped as circle;
The number of described column construction is at least 3.
The arrangement mode of described column construction (being also the pattern of micro-/ nano array) can freely define, can be freely size and the distance of the strong point in three of design standard and four-point bending strain loading as requested, for the one dimension micro/nano material of different length and thickness, carry out better standard bending strain loading.Size, interval and the arrangement mode of column construction in array (being also the strong point) can load for the accurate one dimension micro/nano material standard bending strain of different size and require arbitrarily design.Only require the array processing to have enough intensity to bear the stress that the deformation of accurate one dimension micro/nano structure produces.
The present invention also provides a kind of method that described micro-/ nano supports array of preparing, and comprises the steps: on substrate, to prepare described column construction, obtains described micro-/ nano and supports array.
The described method of preparing column construction can be photoetching process, electron beam exposure method, dry etching method, wet etching method or focused-ion-beam lithography method.
Wherein, described photoetching process comprises the steps: to prepare after photoresist layer on described substrate, then optical graving, for described column construction, obtains described micro-/ nano and supports array on described photoresist layer.
This photolithographic principle is, by ultraviolet light, the strand of photoresist (as SU-8 photoresist) is carried out to modification, then by developing, the photoresist without overexposure (as SU-8 photoresist) is removed.Arranging of experiment parameter can be with reference to the experiment parameter of rotine exposure, as exposure dose can be 13mW/cm
2, the time for exposure can be 12s.Developing fixing, without special requirement, can carry out with reference to the parameter of conventional uv-exposure.
This photoresist also photoresist of available other types replaces, but will guarantee the adhesive force stronger with substrate and enough strong hardness.Substrate also can other type surfacing substrate replace, depend primarily on the experiment test requirement that will carry out, as whether insulate etc.
The thickness of described photoresist layer is adjustable, is specially 15 microns;
In the method, the described method of preparing photoresist layer is included in front baking, uv-exposure and rear baking after spin coating photoresist on described substrate;
Described spin coating step is first spin coating 10 seconds under the rotating speed of 500rpm, then spin coating 60 seconds under the rotating speed of 3000rpm, is specially first under the rotating speed of 500rpm spin coating 10 seconds, then spin coating 60 seconds under the rotating speed of 3000rpm;
Described front baking step keeps 3 minutes for being first warming up to 95 ℃ with the heating rate of 2 ℃/s at 65 ℃ after keeping 1 minute;
In described uv-exposure step, exposure dose is 13mW/cm
2, the time for exposure is 12s;
Described rear baking step keeps 3 minutes for being first warming up to 95 ℃ with the heating rate of 2 ℃/s at 65 ℃ after keeping 1 minute.
The thickness of gluing depends on the concentration of SU-8 glue and the speed of spin coating simultaneously, specifically can be with reference to the whirl coating curve of SU-8 glue production firm.When SU-8 glue thickness is not enough to meet actual requirement, can obtains thicker SU-8 glue by gluing repeatedly, or obtain thinner SU-8 glue by dilution SU-8 colloidal solution.
Little heating rate can reduce the possibility of SU-8 glue cracking.
The present invention also provides a kind of described micro-/ nano to support the application of array in the bending strain of one dimension micro/nano material loads.
Wherein, described bending strain loads and is specially standard bending strain loading; During described micro/nano material bending strain loads, adding load mode is standard three-point bending or standard four-point bending;
Described micro/nano material is selected from least one in semi-conducting material, metal material, organic material, dielectric material, ceramic material, alloy material and magnetic material.
In described micro/nano material bending strain load step, loading tool used is needle point.Concrete, the material that forms described needle point is selected from least one in glass, metal and pottery.This load step is specially: utilize loading tool to handle single micro/nano material, described single micro/nano material is stuck between three or four column constructions vacantly, thereby complete the loading of standard bending strain.
Various micro/nano materials are all applicable, as the ZnO micro-/ nano line of length hundreds of micron.
In order to depart from the impact of substrate completely, realize standard bending, in crooked process, will make crooked target sample not touch substrate at crooked position with careful control of glass needle point.
Provided by the invention to 3 of the standards of any accurate one dimension micro/nano material of micro-scale or the loading method of four-point bending strain, the strain regime of the standard bending of material has obtained enough confirmations by the cathode-luminescence spectrum analysis of (5.5K) high spatial resolution (10nm) under low temperature and high spectral resolution (0.5nm) on ZnO material.
The present invention has broken through dimensional constraints and direct numerous defects that crooked accurate one dimension micro/nano material is subject to complicated substrate active force on substrate that traditional standard mechanics of bending is measured, has realized first and has aimed at the loading that one dimension micro/nano material carries out standard bending strain.With respect to the bending strain loading method of former bibliographical information, outstanding contributions of the present invention are:
1) realized first the standard bending strain loading of aiming at one dimension micro/nano material
Traditional standard crooked experiment tester can only carry out mechanics of bending experiment test to macroscopical body material, and the frictional force that directly bending of accurate one dimension micro/nano material is relied on substrate to substrate keeps the method for case of bending, complexity due to substrate frictional force, sample is in a kind of off-gauge bending strain state, and the strain regime of sample interior is very complicated.By contrast, our method has just increased together simple optical graving for micro-/ nano array operation, has realized first 3 of standards and the four-point bending strain loading of aiming at one dimension micro/nano material.The strain regime of target sample is very simply clear.
2) target material is applied widely
This technology can range the bending strain weighted platform in mechaanical property of materials test, and target material is not had to what restriction.Accurate one dimension micro/nano material that can be to any micro-scale, comprises semi-conducting material, metal material, and organic material, dielectric material, ceramic material, alloy material, magnetic materials etc., carry out 3 of standards in various degree and the loading of four-point bending strain.
3) cost is low, simple to operate, and micro-/ nano supports array and can freely define
The method mode of operation is easy, and equipment is not had to too high request.Only need the equipment such as sol evenning machine, litho machine, light microscope and micro OS, be easy to realize the production application of scale.The photoetching technique that this technology is prepared micro-/ nano support dot matrix employing required in bending in substrate can freely define micro-/ nano array pattern, can be freely size and the distance of the strong point in three of design standard and four-point bending strain loading as requested, for the accurate one dimension micro/nano material of different length and thickness, carry out better standard bending strain loading.
4) micro-/ nano array substrate is reusable, compatible strong
The repeatability of the method operation is strong, can repeat the accurate one dimension target of a plurality of differences micro/nano material to carry out standard bending strain loading, thereby reduce application cost for the micro-/ nano array substrate designing.As in conjunction with existing micro-nano process technology, middle bent support cylinder design is become to mobilizable piston type strong point, and the power of using with existing mechanical meaurement and displacement transducer and measurement of correlation software combine, can be developed to the standard platform that aligning one dimension micro/nano material that a set of practicality is stronger carries out the performance test of standard mechanics of bending, realizing to various accurate one dimension micro/nano materials the power under standard bending strain, heat, light, the characteristic research such as electricity and micro-power, displacement, huge effect can be brought into play in the aspects such as flexible micro-/ nano biology and photodetector.
Accompanying drawing explanation
Fig. 1 is 3 of standards and four-point bending ZnO micro wire pattern.
Fig. 2 is the same ZnO micro wire pattern of standard four-point bending strain loading in various degree.
Fig. 3 is that the line of standard three-point bending ZnO micro wire pattern and varying cross-section is swept CL spectrum.
Fig. 4 is that the line of standard four-point bending ZnO micro wire pattern and varying cross-section is swept CL spectrum.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Described method is conventional method if no special instructions.Described raw material all can obtain from open commercial sources if no special instructions.Following embodiment SU-8 negative photoresist used is purchased from U.S. MicroChem company.Substrate used is N-shaped monocrystalline substrate (100MM/CZ/1-0-0/PHOS/N Type/Resis 0.0500-0.2000), buys Microelectronic Institute in Peking University.
In following embodiment, the feature image of accurate one dimension micro/nano material ZnO under 3 of standards and four-point bending strain regime, is to obtain by scan electronic microscopic method.For the checking of its bending strain state, be to realize by the cathode-luminescence spectrum of (5.5K) high spatial resolution (10nm) under low temperature and high spectral resolution (0.5nm).
Embodiment 1, prepare micro-/ nano and support array
1) first spin coating SU-8 photoresist 10 seconds under the rotating speed of 500rpm on substrate, spin coating after 60 seconds under the rotating speed of 3000rpm again, at 65 ℃, with the heating rate of 2 ℃/s, be warming up to 95 ℃ of maintenances after keeping 1 minute again and under condition, carry out front baking in 3 minutes, obtain the photoresist layer that thickness is 15 μ m.
2) mask blank with pre-designed pattern carries out mask, and utilizing ultraviolet light is 13mW/cm to step 1) gained photoresist layer (as SU-8 photoresist) at exposure dose
2, expose under the time for exposure condition that is 12s, then use the special-purpose developer solution of SU-8 photoresist (PGMEA-U.S. MicroChem company) to develop after 4 minutes, after the SU-8 photoresist without overexposure is removed, obtain micro-/ nano and support array.
This embodiment gained micro-/ nano supports array and is comprised of with vertical several column constructions as the strong point that are intervally arranged that are positioned on described substrate substrate; Column construction is all perpendicular to substrate, and the diameter of described column construction is 14 μ m, cross section be shaped as circle.
The standard bending strain of embodiment 2, micro/nano material loads
Utilize the micro OS under light microscope, accurate one dimension target micro/nano material ZnO micro-/ nano line is transferred to embodiment 1 to be prepared on gained micro-/ nano support array, (diameter is 0.2 ~ 5.0 μ m to make single ZnO micro-/ nano line, length is 300 ~ 800 μ m) be stuck in vacantly between three or four column constructions, the standard bending strain that completes single ZnO micro-/ nano line loads;
Two glass needle points that micro-control system used is controlled by long confocal optical microscope (BX51M, OLYMPUS) and three axle hydraulic systems (MMO-202ND, OLYMPUS) form.By Real Time Observation under the microscope, can easily ZnO micro-/ nano line be transferred on the substrate that is prepared with micro-/ nano array from growth substrates.
The example cross section of standard bending is carried out to low temperature CL spectral characterization, and check strain regime wherein, is specially:
Strain regime in conjunction with the crooked ZnO micro-/ nano of cathode-luminescence spectrum (Gatan monocle 3+) the Analysis deterrmination standard of the high spatial resolution (10nm) under low temperature (5.5K) and high spectral resolution (0.5nm) line.Substrate with crooked sample is fixed on the liquid helium low temperature platform of cathode-luminescence spectrometer, pass into circulation liquid helium temperature is reduced to 5.5K, in order to obtain good spectral signal-noise ratio, accelerating potential is elected 10KV(pot size 4 as), select CCD to adopt spectral model (300-450nm, spectral resolution is 0.5nm), along the crooked position difference of sample, carry out the CL spectrum that line is swept (step-length 70-100nm) collection difference in cross section very much.The identical spectrum of crooked position varying cross-section between two of centres pillar in four-point bending proves that this part is pure bending, is the four-point bending of standard.The three-point bending that three-point bending is standard simultaneously.
Acquired results as shown in Figures 1 to 4.
Fig. 1, the typical SEM pattern of 3 of standards and four-point bending ZnO micro wire.(a) the SEM shape appearance figure of 0 ° of inclination of standard three-point bending ZnO micro wire, the diameter of this ZnO micro wire is 2.2 μ m.(b) the SEM shape appearance figure of 45 ° of inclinations of standard four-point bending ZnO micro wire, the diameter of this ZnO micro wire is 2.7 μ m.The SEM shape appearance figure of 45 ° of inclinations from (b) can be clear that, the crooked position of ZnO micro wire is not in contact with one another with substrate, in vacant state, its bending strain state is not subject to the impact of substrate effect, and the crooked position between middle two SU-8 pillars is pure bending strain regime.
Fig. 2, same ZnO micro wire be SEM shape appearance figure during standard four-point bending strain loading in various degree, and the diameter of this ZnO micro wire is 1.7 μ m.(a) the SEM shape appearance figure of 30 ° of inclinations when ZnO micro wire does not carry out bending.(b) ZnO micro wire carries out the SEM shape appearance figure of 30 ° of inclinations after standard four-point bending for the first time, and the radius of curvature of pure bending position bending is 175.4 μ m.(c) ZnO micro wire carries out the SEM shape appearance figure of 30 ° of inclinations after standard four-point bending for the second time, and the radius of curvature of pure bending position bending is 86.2 μ m.Identical in figure (b) and size scale (c) and figure (a).In the time of can being clear that differently curved degree, the crooked position of ZnO micro wire is not all in contact with one another with substrate.
Fig. 3, under standard three-point bending ZnO micro wire pattern and 5.5K, the line of varying cross-section is swept CL spectrum.(a) the SEM shape appearance figure of 0 ° of inclination of standard three-point bending ZnO micro wire, the diameter of this ZnO micro wire is 2.2 μ m.The direction that the varying cross-section position of pink arrow indication collection CL spectrum and line are swept is from the end that stretches to compression end.(b) line of the indicated varying cross-section of arrow at 5.5K temperature swept CL spectrum in corresponding figure (a).When in figure, peach dotted line represents there is no bending strain, ZnO micro wire is in the position of 5.5K temperature glow peak, and the redness of spectrum (figure bottom glow peak) represents elongation strain end, and blue (figure top glow peak) represents compression strain end.I does not have the line of bending strain cross section to sweep CL spectrum, can see and only have to be positioned at the very sharp-pointed bound exciton (D in 3.3598eV position
0x
a) glow peak.At crooked position II ~ V, along with the increase of bending strain degree, D
0x
awhole red shift amount increase gradually, and go out a plurality of sub-glow peaks in the high-energy tail splitting of compression end spectrum, this is the result that causes ZnO electronic band structure to change by heterogeneous strain.Visible ZnO micro wire is in standard three-point bending strain regime.
Fig. 4, under standard four-point bending ZnO micro wire pattern and 5.5K, the line of varying cross-section is swept CL spectrum.(a) the SEM shape appearance figure of 0 ° of inclination of standard four-point bending ZnO micro wire, the diameter of this ZnO micro wire is 1.4 μ m.The direction that the varying cross-section position of pink arrow indication collection CL spectrum and line are swept is from the end that stretches to compression end.(b) line of the indicated varying cross-section of arrow at 5.5K temperature swept CL spectrum in corresponding figure (a).The position of ZnO micro wire glow peak at 5.5K temperature when peach dotted line represents there is no bending strain in figure, the redness of spectrum (figure bottom glow peak) represents elongation strain end, blue (figure top glow peak) represents compression strain end.I does not have the line of bending strain cross section to sweep CL spectrum, can see and only have to be positioned at the very sharp-pointed bound exciton (D in 3.3598eV position
0x
a) glow peak.At the line of three cross section II ~ IV positions of crooked position, sweep CL spectrum identical, D
0x
aglow peak is whole there is red shift, in the high-energy tail splitting of compression end spectrum, goes out a very weak sub-glow peak, and this is the result that causes ZnO electronic band structure to change by heterogeneous strain.The crooked position that the spectrum proof that varying cross-section is identical mediates between two SU-8 pillars is pure bending state, and whole ZnO micro wire is in standard four-point bending strain regime.
Claims (10)
1. micro-/ nano supports an array, substrate, consists of with vertical several column constructions as the strong point that are intervally arranged that are positioned on described substrate.
2. array according to claim 1, is characterized in that: described substrate is N-shaped monocrystalline substrate;
The shape of cross section of described column construction is circular or square or triangle;
The number of described column construction is at least 3.
3. prepare the method that micro-/ nano described in claim 1 or 2 supports array, comprise the steps: on substrate, to prepare described column construction, obtain described micro-/ nano and support array.
4. method according to claim 3, is characterized in that: the described method of preparing column construction is photoetching process, electron beam exposure method, dry etching method, wet etching method or focused-ion-beam lithography method.
5. method according to claim 4, is characterized in that: described photoetching process comprises the steps: to prepare after photoresist layer on described substrate, then optical graving, for described column construction, obtains described micro-/ nano and supports array on described photoresist layer.
6. method according to claim 5, is characterized in that: the described method of preparing photoresist layer is included in front baking, uv-exposure and rear baking after spin coating photoresist on described substrate;
Described spin coating step is first spin coating 10 seconds under the rotating speed of 500rpm, then spin coating 60 seconds under the rotating speed of 3000rpm, is specially first under the rotating speed of 500rpm spin coating 10 seconds, then spin coating 60 seconds under the rotating speed of 3000rpm;
Described front baking step keeps 3 minutes for being first warming up to 95 ℃ with the heating rate of 2 ℃/s at 65 ℃ after keeping 1 minute;
In described uv-exposure step, exposure dose is 13mW/cm
2, the time for exposure is 12s;
Described rear baking step keeps 3 minutes for being first warming up to 95 ℃ with the heating rate of 2 ℃/s at 65 ℃ after keeping 1 minute.
7. the arbitrary described micro-/ nano of claim 1 or 2 supports the application of array in the bending strain of one dimension micro/nano material or accurate one dimension micro/nano material loads.
8. application according to claim 7, is characterized in that: described bending strain loads and is specially standard bending strain loading;
Described standard bending strain adds load mode and is specially standard three-point bending or standard four-point bending in loading;
Described one dimension micro/nano material or accurate one dimension micro/nano material are selected from least one in semi-conducting material, metal material, organic material, dielectric material, ceramic material, alloy material and magnetic material.
9. according to the application described in claim 7 or 8, it is characterized in that: in the bending strain load step of described one dimension micro/nano material or accurate one dimension micro/nano material, loading tool used is needle point.
10. according to the arbitrary described application of claim 7-9, it is characterized in that: the material that forms described needle point is selected from least one in glass, metal and pottery.
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| CN107990918B (en) * | 2017-10-20 | 2020-04-17 | 苏州大学 | Method for manufacturing high-sensitivity piezoresistive sensor through multi-level structural design |
| CN112379129A (en) * | 2020-11-16 | 2021-02-19 | 付学文 | High-space-time resolution multi-mode carrier dynamics measurement system and measurement method |
| CN112379129B (en) * | 2020-11-16 | 2022-08-23 | 付学文 | High-space-time-resolution multi-mode carrier dynamics measurement system and measurement method |
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