CN107986224B - Large area multilevel surface folding structure and its preparation - Google Patents
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- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B1/00—Devices without movable or flexible elements, e.g. microcapillary devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00214—Processes for the simultaneaous manufacturing of a network or an array of similar microstructural devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B2203/00—Basic microelectromechanical structures
- B81B2203/03—Static structures
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Abstract
The present invention provides a kind of large area multilevel surface folding structure, is the multilevel pleated structure with binary cycle, and wherein the period of minor cycle fold is 100-200nm, and the period of large period fold is 3-4 μm.The present invention also proposes the preparation method of the large area multilevel surface folding structure.The pleated structure for the multilevel bi-period structure that the present invention is prepared, two sets of folds formation multilevel structure nested against one another, the area of isotropism, multilevel structure can accomplish 200mm or more, have good industrial applicibility.
Description
Technical field
The invention belongs to multilevel structure material fields, and in particular to a kind of multistage knot of organic polymer and metal composite
Structure.
Background technique
Wrinkle is considered as the mark of material failure as a kind of common natural phenomena for a long time.However in recent years,
Many research discovery folds also have in terms of flexible electronic, special surface structure manufacture, thin film mechanical performance to be permitted
Mostly positive application.In nature, either in the upper of organism, or on the surface of man-made structures, all there is very much
Complicated multilevel surface micro-nano structure.These multiple level structures have many unique surface naturies, such as wetability, adhesiveness
With photoelectric properties etc., therefore in solar battery, LED, activated adoption, self-cleaning surface, surface catalysis etc. has extensive
Application, have stimulated the methods that researcher constantly explored and developed various novel preparation surface multilevel structures.
Typically, pleated structure can be simply by the bilayer membrane body as composed by soft substrate and rigid surface layer
System applies compression strain to generate.Pleated structure have eigenperiod, the eigenperiod by materials at two layers thickness and springform
Amount determines.Although the pleated structure with binary cycle is also prepared in some researchs, the most complicated difficult of these preparation methods is with reality
With.
One layer of metal layer is plated on PDMS after hardening or forms one layer on surface by the methods of UVO (UV ozone)
Oxide layer, then release strain can generate fold pattern (N.Bowden et al, Nature, 1998,393:146-149).
If straining by first release part, then one layer of new surface layer film is plated, then discharges residual strain again, can realize two sets of periods
Nested multilevel pleated structure (K.Efimenko et al, Nat.Mater.2005,4,293-297).Such methods lack
Point is that step is complex, and technique is cumbersome.Also studies have found that, directly pass through FIB (focused ion beam) direct write on the surface PDMS,
The region of inscription can generate multilevel fold (M.Moon et al, PNAS, 2007,104 (4): 1130-1133).However it is more
Level fold can only be generated in the local tiny area of inscription, it is difficult to realize that large area is uniformly prepared.In conclusion at present also
There is no a kind of simple one step forming method, large area uniformly multiple grade binary cycle surface folding structure can be prepared.
Summary of the invention
Place in view of the shortcomings of the prior art, the purpose of the present invention is to propose to a kind of large area multilevel surface foldings
Structure.
Second object of the present invention is to propose the preparation method of the multilevel surface folding structure.
Realize the technical solution of above-mentioned purpose of the present invention are as follows:
A kind of large area multilevel surface folding structure is the multilevel pleated structure with binary cycle, wherein the minor cycle
The period of fold is 100~200nm, and the period of large period fold is 3~4 μm.
Further, the folded structure is made of metal film on surface and polymeric substrates, the metal film on surface covering
In polymeric substrate surface, the metal for constituting metal film on surface is one of Au, Ag, Cu, Pt or a variety of, the polymer matrix
Bottom is by one of dimethyl silicone polymer, thermoplastic polyurethane TPU, thermoplastic polyester elastomer TPEE or a variety of constitutes.
The polymeric base material of this method preferably is PDMS, the english abbreviation of dimethyl silicone polymer.It is with light
Learn it is transparent, and under normal circumstances, it is considered to be inertia, it is nontoxic, it is nonflammable.Because its is at low cost, using simple, between silicon wafer
With good adhesiveness, and have the characteristics that good chemical inertness, becomes one kind and be widely used in micro-fluidic Deng fields
Polymer material.In addition, PDMS is also that artificial fold prepares common polymeric base material.
Wherein, the area of the folded structure is 1-1000mm2。
Wherein, the metal film on surface with a thickness of 10-50nm.
Preferably, it is 300-350mm that the polymeric substrates, which are areas,2Regular shape, with a thickness of 1 ± 0.2mm, surface
Thickness of metal film is 25-35nm.So-called regular shape is one of rectangle, square, circle, ellipse, triangle.
The preparation method of large area multilevel surface folding structure of the present invention, comprising the following steps:
Step 1): by being poured and solidification prepares polymer elasticity substrate；
Step 2): metallic film is prepared in the resulting polymeric substrates of step 1) at high temperature with magnetron sputtering；
Step 3): the sample to sputter in step 2) is cooled to room temperature to be taken out from sputtering chamber.
Wherein, in the step 1), the mass ratio of polymer body and curing agent is 5:1-40:1, and solidification temperature is
50-90 DEG C, the operation of step 2) is carried out when polymer is not fully cured.
Preferably, in the step 1), the mass ratio of polymer body and curing agent is 8:1-12:1, polymer body
It is stirred 1-10 minutes with after curing agent mixing, vacuumizes to remove the bubble generated in whipping process, pour into plastic containers, it is right
In pouring into the mixing object amount that height is 0.5-3mm, the operation of step 2) is carried out after solidifying 0.5-2 hours.
Wherein, the step 2) sputtering process carries out at 200-300 DEG C of temperature.
Sputtering uses higher temperature, this is because PDMS meeting expanded by heating, to generate strain, strain is the shape of fold
At necessary condition.
Wherein, in the step 2), polymeric substrates is sticked on substrate and are put into sputtering chamber, first heated the substrate and be allowed to rise
Temperature then passes to argon gas, and pressure when control sputters is 4-6mTorr, sputtering power 100-200W, sputtering time 200-
400s。
The beneficial effects of the present invention are:
The present invention proposes a kind of simple one step forming method, has multilevel binary cycle knot to prepare large area uniformly
The pleated structure surface of structure.Metal film on surface is plated using magnetically controlled sputter method, preferably with gold.The metals such as platinum, silver, bucket, property
Stablize, is not oxidizable, and ductility is preferable, crack is not likely to produce during corrugated.
The pleated structure for the multilevel bi-period structure that the present invention is prepared, two sets of folds formation multilevel nested against one another
The area of structure, isotropism, multilevel structure can accomplish 200mm or more, have good industrial applicibility.
Detailed description of the invention
Fig. 1: the photo of the sample with large area multilevel pleated structure surface.Size: 16 × 16 × 1mm.
Fig. 2: the AFM shape appearance figure on multilevel pleated structure surface.
Fig. 3: the SEM surface topography map on multilevel pleated structure surface.
Specific embodiment
Illustrate the performance of material preparation of the present invention and its separation aspect below by way of specific embodiment.Those skilled in the art
Member it will be clearly understood that it is described examples are only for helping to understand the present invention, should not be regarded as a specific limitation of the invention.
Raw material used in embodiment is commercially available.Means as used in the following examples unless otherwise specified, are
Techniques known in the art means.
Experimental example
PDMS (polydimethylsiloxane, dimethyl silicone polymer) ontology with curing agent be it is commercially available, ontology and
Curing agent is coordinates.The operation of conventional PDMS is the PDMS ontology and curing agent of (10:1) mixing by a certain percentage, in room
Middle benefit gas places two to three days, can be fully cured.Or by that in 80 DEG C or so 4 hours of heating, can also be rapidly achieved completely
Solidification.
By PDMS ontology and curing agent that 10:1 mass ratio mixes, places two days at room temperature or heat four at 80 DEG C
Hour, the PDMS that can be all fully cured.The PDMS elasticity modulus being fully cured is larger, deposits Au on this surface, only meeting
Since the thermal dilation difference of PDMS and Au generates the single cycle pleated structure of micro-meter scale.
By thinking and comparing, it is proposed that a kind of simple one step forming method, uniformly has to prepare large area
There is the pleated structure surface of multilevel bi-period structure.And PDMS prepared in the present invention is different from a bit of other work
It is that PDMS is not fully cured.
Embodiment 1
In this preferred embodiment of the invention, the cure parameter used is 60 DEG C of 1 hour of heating, and PDMS is not at this time
It is fully cured, this is conducive to the generation of binary cycle fold.Specific experimental method are as follows: a certain amount of PDMS is toppled over into plastic cup
Ontology, then instills curing agent in the ratio of quality 10:1, and stirring is allowed to substantially uniformity fusion for 5 minutes.Drying box is subsequently placed into,
It vacuumizes to remove the bubble generated in whipping process.It takes out after about 10 minutes, pours into a certain amount of ontology and curing agent
Mixing liquid in plastic petri dishes, is stood for a moment, the height poured into is about 1mm.Then it puts it into baking oven, 60 DEG C of heating
It is taken out after 1 hour.
It waits for using in next step with the fritter that blade cuts 16 × 16mm square.The size is conducive to binary cycle multilevel fold
Formation.It is needing it is noted that PDMS take out after i.e. at once carry out next step operation, if waiting time it is too long
Words, curing degree can also change.
Second step is the metal-coated membrane in the PDMS substrate prepared.It used here as Au, is not easy because Au property is stablized
Oxidation, and ductility is preferable, and crack is not likely to produce during corrugated.It plates Au and uses magnetron sputtering, and sputtering process is 250
It is carried out at DEG C.Specific sputtering process and parameter are as follows: the PDMS substrate that will be prepared, which is sticked on substrate, to be put into sputtering chamber, first
It heats the substrate and is allowed to be warming up to 250 DEG C, then pass to argon gas, so that pressure when sputtering is remained 5mTorr, then begin to sputter
Process, sputtering power 100W, sputtering time 300s.The Au film thickness sputtered under this parameter is about 30nm.It has been sputtered that, sample
Product are in intracavitary natural cooling.
Third step is taken out after sample is cooled to room temperature, and the sample after taking-up is shown in Fig. 1.As can be seen from the figure surface is simultaneously
It is equally smoothless like mirror surface, but similar frosted glass, illustrate to show to have had pleated structure generation.Pass through further AFM (Fig. 2)
It is observed with SEM (Fig. 3, right figure are left figure partial enlargements), it can be found that the surface PDMS has the multilevel pleated structure of binary cycle to produce
It is raw.Wherein biggish a set of fold is micro-meter scale, and the period is about 3~4 μm；And lesser a set of fold is nanoscale
, the period is about 100~200nm.Two sets of folds formation multilevel structure nested against one another, and be it is isotropic, take at random
To.
The compacting mechanism of binary cycle multilevel pleated structure is as described below.The machine that the pleated structure of two sets of different cycles is formed
Reason is different.Nanoscale fold be ion due to being sputtered in magnetron sputtering process for the modifying function on the surface PDMS and
It generates.The period of nanoscale fold is unrelated with Au film thickness, therefore should not adjust, therefore be fixed as 100~200nm.And
The fold of micro-meter scale is then as caused by the mismatch of the thermal expansion coefficient of PDMS and Au.Particularly, PDMS substrate is heated
Expansion, plates layer of Au above at this time, cooling to sample, and PDMS shrinks back original size, and Au coefficient of expansion ratio PDMS
It is much smaller, it can not be restored to size same as PDMS, therefore the Au film on surface layer will receive compression, then generate buckling and formed
Fold.The period of the pleated structure is related with the elasticity modulus of the thickness of Au and PDMS.It is worth noting that control PDMS base
The size at bottom is 16 × 16mm, with a thickness of 1mm, is provided to generate strain convenient for its expanded by heating.If area is too small or thick
If degree is too thick, all it is unfavorable for the generation of fold.More importantly in the present invention, the micro-meter scale of suitable period in order to obtain
Fold, it is 30nm that we, which control Au film thickness, and does not allow PDMS to be fully cured, and the elasticity modulus for controlling PDMS is in a phase
To lesser value.In the case, the fold period obtained is larger.The fold Cycle accurate control of micro-meter scale in this patent
It is being 3~4 μm.The purpose for controlling the period in this way is in order to allow the periodic inequality of two sets of folds away from an order of magnitude or so, in this way
It can significantly observe that the fold in two sets of periods is nested against one another, the pleated structure surface of multilevel is collectively formed.
Embodiment 2
In the present embodiment, the cured operation of polymeric substrates is the same as embodiment 1.
The size of the PDMS substrate of cutting is 8 × 8mm, and with a thickness of 1mm, sputtering golden film is 7nm, and the pleated structure of generation is only
It is observed that a cycle, is 100-200nm.The fold of the nanoscale is the ion pair due to sputtering in magnetron sputtering process
In the surface PDMS modifying function and generate.In this case, the mismatch of the thermal expansion coefficient of PDMS and Au still remains, but
Since golden film is too thin, and PDMS size is too small, can not generate the fold of micro-meter scale.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (3)
1. a kind of preparation method of large area multilevel surface folding structure, which comprises the following steps:
Step 1): by being poured and solidifying preparation polymeric substrates, wherein the mass ratio of polymer body and curing agent is 5:
1-40:1, solidification temperature are 50-90 DEG C, and the operation of step 2) is carried out when polymer is not fully cured；
Step 2): metallic film is prepared in the resulting polymeric substrates of step 1) at 200-300 DEG C of temperature with magnetron sputtering；
Step 3): the sample to sputter in step 2) is cooled to room temperature to be taken out from sputtering chamber.
2. preparation method according to claim 1, which is characterized in that in the step 1), polymer body and curing agent
Mass ratio be 8:1-12:1, polymer body and curing agent mixing after stir 1-10 minutes, vacuumize stirred to remove
The bubble generated in journey, is poured into plastic containers, for pouring into the mixing object amount that height is 0.5-3mm, after solidification 0.5-2 hours
Carry out the operation of step 2).
3. preparation method according to claim 1 or 2, which is characterized in that in the step 2), polymeric substrates are sticked to
It is put into sputtering chamber on substrate, first heats the substrate and be allowed to heat up, then pass to argon gas, pressure when control sputters is 4-
6mTorr, sputtering power 100-200W, sputtering time 200-400s.
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| CN111766000A (en) * | 2019-04-01 | 2020-10-13 | 天津大学 | Gold thin film flexible crack sensor based on micro-scale wrinkles |
| CN110903508B (en) * | 2019-12-08 | 2022-05-24 | 香港中文大学（深圳） | Stimulus-responsive polymer grafted wrinkled intelligent surface and preparation method and application thereof |
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