CN107589104A - The experimental provision and method of array micro nano structure in Raman enhancing substrate are prepared based on power modulation miniature carving stroke/micro-indentations process - Google Patents
The experimental provision and method of array micro nano structure in Raman enhancing substrate are prepared based on power modulation miniature carving stroke/micro-indentations process Download PDFInfo
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Abstract
The invention discloses a kind of experimental provision and method that array micro nano structure in Raman enhancing substrate is prepared based on power modulation miniature carving stroke/micro-indentations process, the experimental provision includes XY and drives the motion for carrying out Z-direction by force snesor by nano-precision workbench to accurate mobile controller, Z-direction precision translation stages controller, nano-precision workbench, force snesor, diamond probe, sample, grand dynamic precision stage, the diamond probe；Force signal between diamond probe and sample moves up and down control by Z-direction precision translation stages controller；Sample drives by grand dynamic precision stage from XY to accurate mobile controller and does two dimensional motion in X Y planes.Process middle probe of the present invention is carried out continuously miniature carving stroke, Indentation Process, while drives the workbench of exemplar to make two-dimensional translation, realizes the processing of efficient, large-scale cyclic array micro-nano structure；The vertical load of process middle probe changes in real time, realizes the processing of the micro-nano structure of complexity.
Description
Technical field
The invention belongs to micro-nano structure processing technique field, is related to a kind of processing unit (plant) of power modulation miniature carving stroke/micro-indentations
And method, more particularly to one kind modulates miniature carving stroke by power, micro-indentations process realizes that metal surface array micro-nano structure manufactures, and
The experimental provision and method of Raman enhancing substrate can be used as.
Background technology
Life science has come into unimolecule, single stage, and there is an urgent need to from macromolecular level by researchers
Phenomena such as interaction of generation Yu the development, medicine and body of the rule, disease of upper research vital movement.Raman spectrum conduct
The Fingerprint of molecular vibration energy level is characterized, has been widely used in field of biology.Possess the metal of micro nano structure
（Such as gold, silver, copper）, can produce Raman enhancing scattering effect, increase substantially the substrate of Raman measuring accuracy by scholars
Referred to as Raman enhancing substrate.Therefore, the focus that high-precision Raman enhancing substrate has become domestic and foreign scholars research how is prepared
And difficulties.At present, chemical synthesis process mainly prepares the micro-nano in Raman enhancing substrate with nanoprocessing two ways
Rice corpuscles/structure.Yet with nano-particle/structure disperses of chemical synthesis process preparation, poor repeatability, the substrate of preparation not
Preserved beneficial to long-term；Conventional nano processing method process equipment is expensive, manufacturing process flow is complicated, environmental Kuznets Curves requirement is strict,
Nanostructured distribution is small etc., domestic and foreign scholars is being pursued new low cost, high efficiency, high accuracy and can be with always
It is accurately positioned, the processing method for the array micro nano structure that physical dimension, distribution density are controllable.
Inexpensive, the high-precision advantage and structure chi that tradition machinery processing is combined with micro-indentations technology are drawn in miniature carving
Very little, position etc. can accurately control.This technology, which is expected to turn into, meets array micro nano structure manufacture in Raman enhancing substrate
A kind of processing method of demand.However, this technology mainly uses commercialized impression instrument at present.This instrument and equipment be towards
The mechanical property of test sample material micro-nano metrical scale and develop, in order to ensure test high accuracy and stability, its test
Speed can not be set very high, and the test for single-point is typically much deeper than 1 second.Meanwhile the test scope within 100 microns is
Through meeting for testing requirement in most cases.Therefore, its processing efficiency is relatively low, processes yardstick is limited.In addition use
This technology is only capable of realizing at present the processing of the micro-nano structures such as simple groove, pit, and structure type is single, causes using its detection
The species of biomolecule be limited.
The content of the invention
Prepare Raman enhancing substrate based on power modulation miniature carving stroke/micro-indentations process it is an object of the invention to provide one kind and go into battle
The experimental provision and method of row micro nano structure, it can not only realize that size, density etc. are controllable, repeat good across yardstick micro-nano
The highly-efficient processing of array structure, and can change probe shape, forms complicated micro-nano structure, and the structure easily positions, can be with
It is permanent to preserve, it disclosure satisfy that the demand of the Raman enhancing substrate of detection biomolecule.
The purpose of the present invention is achieved through the following technical solutions：
A kind of experiment dress that array micro nano structure in Raman enhancing substrate is prepared based on power modulation miniature carving stroke/micro-indentations process
Put, including XY is to accurate mobile controller, Z-direction precision translation stages controller, nano-precision workbench, force snesor, diamond
Probe, sample, grand dynamic precision stage, wherein：
The diamond probe is driven the motion for carrying out Z-direction by nano-precision workbench by force snesor；
Force signal between the diamond probe and sample moves up and down control by Z-direction precision translation stages controller；
The sample drives by grand dynamic precision stage from XY to accurate mobile controller and two dimensional motion is done in X-Y plane.
A kind of method that array micro nano structure in Raman enhancing substrate is prepared using above-mentioned experimental provision, including following step
Suddenly：
First, power modulation micro-indentations processing
（1）After diamond probe is pressed into sample surfaces with an initial perpendicular load, while start vertical load cyclically-varying
Micro-indentations process, grand dynamic precision stage drives sample with VySpeed make at the uniform velocity feed motion, adjust the modulated signal of power
Cycle and VyMatching relationship, so as to processing a line lattice structure on sample surfaces；
（2）After a line dot matrix process finishing, sample is driven along X to doing stepping feeding from grand dynamic precision stage；
（3）Repeat step（1）With（2）, realize by the processing for the two-dimensional array micro-nano structure that two-dimensional lattice is overlapping and is formed.
2nd, process is drawn in power modulation miniature carving
（1）Cyclic force signal value using L1, L2 as two adjacent trenches；
（2）After diamond probe press-in sample surfaces, the cyclic force signal value using L1 as groove, grand dynamic precision stage drives
Sample is along the Y direction with speed VyThe delineation of groove, after being worked into the length of requirement, Y-direction workbench are carried out on sample surfaces
Stop motion, obtain first very low power；
（3）Grand dynamic precision stage drives sample, and stepping is fed along the X direction, then the cyclic force signal value using L2 as groove,
Process Article 2 very low power；
（4）With step（2）With（3）For a period of change, by changing vertical load, the spacing of groove realizes the superposition of groove,
The processing of execution cycle property structure.
The present invention is clearly distinguishable from traditional miniature carving and drawn and micro-indentations method：Process middle probe is carried out continuously miniature carving
Draw, Indentation Process, while drive the workbench of exemplar to make two-dimensional translation, realize efficient, large-scale cyclic array micro-nano knot
The processing of structure；The vertical load of process middle probe changes in real time, realizes the processing of the micro-nano structure of complexity.
Brief description of the drawings
Fig. 1 is the principle that impression and scoring process formation array micro nano structure are carried out using probe；
Fig. 2 is to prepare Raman based on power modulation miniature carving stroke/micro-indentations process to strengthen the experiment dress of array micro nano structure in substrate
The structural representation put；
Fig. 3 is the process of the nano impress based on power modulation；
Fig. 4 is the process of the nanometer delineation based on power modulation；
Fig. 5 is the triangular pyramid probe that impression processing is carried out in experiment；
Fig. 6 is the AFM shape appearance figures that Cu (110) crystal face processes micro- side hole；
Fig. 7 is that concentration is 10-5The Raman signal of mol R6G surface micro-structures when Cu (110) crystal face processes the different amount of feeding；
The AFM schematic diagrames of triangular pyramid impression dot matrix when Fig. 8 is X, Y-direction difference feed speed；
It with detectable concentration on structured single crystal Cu Cu (110) surface is 10 that Fig. 9, which is,-6The Raman spectrum of mol R6G molecules.
Embodiment
Technical scheme is further described below in conjunction with the accompanying drawings, but is not limited thereto, it is every to this
Inventive technique scheme is modified or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, all should cover
In protection scope of the present invention.
Array micro-nano in Raman enhancing substrate is prepared based on power modulation miniature carving stroke/micro-indentations process the invention provides one kind
The system and method for rice structure, the process principle and implementation process of the power modulation miniature carving stroke/micro-indentations are as follows：
First, the process principle of power modulation micro-indentations
The present invention can use different types of diamond probe in impression processing is carried out, with diamond triangular pyramid probe
（cube corner tip）Exemplified by, the drift angle of its needle point is 90 °, and the arc radius of needle point is less than 200nm, as shown in Figure 5.
First, probe is with certain initial perpendicular load（10mN-100mN）It is applied to sample surfaces, such as Fig. 1（a）It is shown.Power
The process principle based on Indentation Process is as follows under modulating action：
1st, power modulation micro-indentations process principle
Such as Fig. 1（a）It is shown, continuous Indentation Process is done with certain vertical load F on the surface, changes the spacing of adjacent indentationsf,
Due tofChange, can make bump be overlapped mutually extruding form controllable array structure, such as Fig. 1（c）It is shown.
2nd, process principle is drawn in power modulation miniature carving
Such as Fig. 1（b）It is shown, depict a length of L very low power on the surface with certain vertical load F1, vertically and groove
Direction steppingf, then Article 2 groove depicted with vertical load F2 on the surface.F1 can be identical with F2, or different.This
Afterwards, as a period of change, continuous delineation.By control room away fromfAnd the amplitude of vertical load, processing array can be controlled
The shape of structure, such as Fig. 1（d）It is shown.
2nd, the experimental provision and process of power modulation micro-indentations
Based on above-mentioned principle, drawn the invention provides the modulation miniature carving of a set of power of realization, the experimental provision of micro-indentations process, such as
Shown in Fig. 2, its from PC1, controller 2, XY to accurate mobile controller 3, Z-direction precision translation stages controller 4, amplifying circuit 5, receive
Rice precision stage 6, force snesor 7, diamond probe 8, sample 9, grand dynamic precision stage 10 are formed.PC 1 and controller 2
Communicated by router, amplifying circuit 5 and force snesor 7（LSB200 series range 50g, FUTEK companies, the U.S.）Carry out
Connection.Diamond probe 8 is by nano-precision workbench 6（XP-63X, core company's tomorrow, China）By force snesor 7 drive into
The motion of row Z-direction.Force signal between force snesor sensitivity diamond probe 8 and sample 9, by Z-direction precision translation stages controller 4
Move up and down, ensure variable signal of the active force between diamond probe 8 and sample 9 for setting.Sample 9 is moved from XY to precision
Movement controller 3（P-517, PI Corp., the U.S.）Driven by grand dynamic precision stage 10 and two dimensional motion is done in X-Y plane, used
To change the spacing between adjacent structuref, so as to form array structure.
1st, power modulation micro-indentations process
As shown in figure 3, amplitude is in figureA, the cycle befPeriodic signal be applied to power on sample for the diamond probe of setting
Signal, signal frequency range：5-10Hz, it is greater than the frequency for being conventionally used to the press-in of test and lifting；Signal type
Can be triangular wave, sine wave etc..Power modulation micro-indentations process is as follows：
（1）After diamond probe is pressed into sample surfaces with an initial perpendicular load, while start vertical load cyclically-varying
Micro-indentations process, while grand dynamic precision stage drives sample with VySpeed make at the uniform velocity feed motion, adjust the modulation of power
Signal period and VyMatching relationship, you can superposition degree between points is adjusted, so as to realize efficiently in sample surfaces
On process a line lattice structure.In addition, lattice structure processing yardstick from grand dynamic precision stage X-Y to moving range
Determine, reach mm-scale.
（2）After a line dot matrix process finishing, sample is driven along X to doing stepping feeding from grand dynamic precision stage；
（3）Repeat step（1）With（2）, realize by the processing for the two-dimensional array micro-nano structure that two-dimensional lattice is overlapping and is formed.
2nd, process is drawn in power modulation miniature carving
As shown in figure 4, the cyclic force signal value of corresponding two adjacent trenches of L1, L2, corresponding grand dynamic precision stage drives sample
Product are along the Y direction with speed VyCarry out the delineation of groove, after being worked into the length of requirement, Y-direction workbench stop motion；Then it is grand
Dynamic precision stage drives sample, and stepping is fed along the X direction, processes Article 2 groove；By changing vertical load, groove
Spacing etc. realizes the superposition of groove, the processing of execution cycle property structure.
Processing method provided by the invention is adapted to the material of processing to be metal material, polymeric material, glass, semiconductor
Material etc..
3rd, the preparation of micro-nano structure Raman enhancing substrate
For the micro-nano array structure of above-mentioned processing method processing, there are following two methods to may be used as Raman enhancing substrate：
（1）Micro-nano structure can directly be processed on metallic copper, gold, silver exemplar using the above method.Because above-mentioned metal has
There is plasma enhancement effect, therefore, the exemplar directly can be used as Raman enhancing substrate to use（The wave-length coverage of test：
532nm-633nm）.
（2）, can not be direct if processing micro-nano structure on metallic aluminium or its alloy surface using the above method
It is used for testing conventional biomolecule or cell etc. as Raman enhancing substrate, then needs to be transferred, the work such as gold-plated or silverskin
Sequence, prepared in conventional Raman enhancing substrate.
4th, Raman enhancing substrate enhancement effect detection example
Micro- scoring process is modulated using power and prepares Raman enhancing substrate.Fig. 6 is the reciprocating motion speed that normal force is 5mN, x direction
To process on single crystal Cu Cu (110) crystal face the shape appearance figure in micro- side hole, its machining sketch chart when 100 μm/s and the different amount of feeding
As shown in Figure 6.The amount of feeding selected in process is respectively 1600nm, 1000nm and 800nm, such as Fig. 6 (a)-(c).Pass through
Other side cheats the contrast of upper and lower both sides pattern, and when processing single crystal Cu Cu (110) crystal face, the removing method of material is mainly with material
More material stackings can be generated based on accumulation and with the reduction of the amount of feeding.
Using R6G as mark molecule, Raman enhancing test is carried out, using the drawing of Renishaw companies of Britain production in experiment
The means that graceful spectroscopy equipment (Invia) is detected as surface enhanced Raman substrate (SERS).The equipment is equipped with dual wavelength 532nm
From spot diameter it is 1 μm in detection process, the energy of incident light is 6.4mW, wavelength is 633nm's with 633nm laser
Laser and 50 times of object lens.Sample is immersed in rhodamine R6G first before detection（Probe molecule）In solution, then with one
Individual Si substrates are calibrated as the sample of standard to Raman signal to ensure that no special peak value generates and to sample
Scanning range area is 20 × 20 μm2.As shown in fig. 7, rhodamine R6G absorption is cheated on single crystal Cu Cu (110) surfaces and micro- side
Raman peak values on surface, the concentration of R6G solution used is 10 in experiment-5mol.As shown in fig. 7, with side hole structure
It is respectively 771cm that the Raman signal of R6G molecules and the characteristic peak of R6G molecules are detected on surface−1, 1183cm−1,
1311cm−1, 1360cm−1, 1504cm−1And 1603cm−1。
The AFM schematic diagrames of triangular pyramid impression dot matrix when Fig. 8 is X, Y-direction difference feed speed.The cycle of triangular wave is
1Hz, the area for processing lattice structure are 30 × 30 μm2, the feed speed scope of X-direction and Y-direction is respectively vx=10 μm/s and
vy=10μm/s、vx=5 μm/s and vy=1μm/s、vx=2 μm/s and vy=2μm/s.From figure 8 (a) can be drawn, when X, Y-direction
Feed speed it is larger (>5 μm/s) when, adjacent impression separates with impression.And when the feed speed of X, Y-direction is less than 5 μm/s,
Carried out between adjacent impression and impression overlapping as shown in Fig. 8 (b) -8 (c).Because in this way with feed speed vy
The adjacent impression of being gradually reduced carry out overlapping and extrude and then produce more nanostructureds.In addition, the projected area of impression
With feed speed vyReduction and be gradually reduced.Feed speed vyScope when being 1 μm/s-2 μm/s, the impression knot of triangle
Structure is divided into two parts and forms structure similar to fish scale shape, such as Fig. 8 (b) -8 (c).
Detectable concentration is 10 on structured single crystal Cu Cu (110) surface when Fig. 9 show different machining parameters- 6The Raman spectrum of mol R6G molecules.It can significantly observe that the amount of feeding has obvious influence to Raman enhancing from figure.Institute
There is curve (1) in the characteristic peak such as Fig. 9 of Raman to have most weak enhancing effect, this is also satisfied with Fig. 8 (a).When this is due to processing
The amount of feeding of selection is big, and its adjacent impression distance is greatly without producing overlapping effect, as shown in Fig. 8 (a).The 1362 of R6G
cm−1The intensity of peak value increases with the reduction of the Y-direction amount of feeding, as shown in curve (2)-(6) in Fig. 9 (a).Work as Y-direction
The amount of feeding be 1 μm when, its Raman enhancing effect is most strong.In addition, adjacent triangular pyramid impression is using different processing speed
Degree forms different nanostructureds by overlapping and extruding.Using process velocity vx=5 μm/s and vyThe nanometer that=1 μm/s is formed
The depth as shallow of other machined parameters generating structures of the depth ratio of structure.
Claims (9)
- A kind of 1. experiment dress that array micro nano structure in Raman enhancing substrate is prepared based on power modulation miniature carving stroke/micro-indentations process Put, it is characterised in that the experimental provision includes XY to accurate mobile controller, Z-direction precision translation stages controller, nano-precision Workbench, force snesor, diamond probe, sample, grand dynamic precision stage, wherein：The diamond probe is driven the motion for carrying out Z-direction by nano-precision workbench by force snesor；Force signal between the diamond probe and sample moves up and down control by Z-direction precision translation stages controller；The sample drives by grand dynamic precision stage from XY to accurate mobile controller and two dimensional motion is done in X-Y plane.
- 2. a kind of method that array micro nano structure in Raman enhancing substrate is prepared based on power modulation micro-indentations process, its feature are existed It is as follows in methods described step：（1）After diamond probe is pressed into sample surfaces with an initial perpendicular load, while start vertical load cyclically-varying Micro-indentations process, grand dynamic precision stage drives sample with VySpeed make at the uniform velocity feed motion, adjust the modulated signal of power Cycle and VyMatching relationship, so as to processing a line lattice structure on sample surfaces；（2）After a line dot matrix process finishing, sample is driven along X to doing stepping feeding from grand dynamic precision stage；（3）Repeat step（1）With（2）, realize by the processing for the two-dimensional array micro-nano structure that two-dimensional lattice is overlapping and is formed.
- 3. according to claim 2 prepare array micro nano structure in Raman enhancing substrate based on power modulation micro-indentations process Method, it is characterised in that in the step 1, using amplitude asA, the cycle befPeriodic signal for setting diamond probe apply The signal for the power being added on sample, signal frequency range 5-10Hz.
- 4. according to claim 2 prepare array micro nano structure in Raman enhancing substrate based on power modulation micro-indentations process Method, it is characterised in that the signal type is triangular wave or sine wave.
- 5. according to claim 2 prepare array micro nano structure in Raman enhancing substrate based on power modulation micro-indentations process Method, it is characterised in that the material of the sample is metal material, polymeric material, glass or semi-conducting material.
- 6. a kind of method that array micro nano structure in Raman enhancing substrate is prepared based on the micro- scoring process of power modulation, its feature are existed It is as follows in methods described step：（1）Cyclic force signal value using L1, L2 as two adjacent trenches；（2）After diamond probe press-in sample surfaces, the cyclic force signal value using L1 as groove, grand dynamic precision stage drives Sample is along the Y direction with speed VyThe delineation of groove, after being worked into the length of requirement, Y-direction workbench are carried out on sample surfaces Stop motion, obtain first very low power；（3）Grand dynamic precision stage drives sample, and stepping is fed along the X direction, then the cyclic force signal value using L2 as groove, Process Article 2 very low power；（4）With step（2）With（3）For a period of change, by changing vertical load, the spacing of groove realizes the superposition of groove, The processing of execution cycle property structure.
- 7. according to claim 6 prepare array micro nano structure in Raman enhancing substrate based on the micro- scoring process of power modulation Method, it is characterised in that in the step 1, using amplitude asA, the cycle befPeriodic signal for setting diamond probe apply The signal for the power being added on sample, signal frequency range 5-10Hz.
- 8. according to claim 6 prepare array micro nano structure in Raman enhancing substrate based on the micro- scoring process of power modulation Method, it is characterised in that the signal type is triangular wave or sine wave.
- 9. according to claim 6 prepare array micro nano structure in Raman enhancing substrate based on the micro- scoring process of power modulation Method, it is characterised in that the material of the sample is metal material, polymeric material, glass or semi-conducting material.
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| CN112051254A (en) * | 2020-08-24 | 2020-12-08 | 长春理工大学 | Raman enhancement structure and preparation method and application thereof |
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