CN104045054A - Method for preparing high-adhesion micro-nano array structure film through wet etching and reverse transfer printing - Google Patents
Method for preparing high-adhesion micro-nano array structure film through wet etching and reverse transfer printing Download PDFInfo
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- CN104045054A CN104045054A CN201410207015.5A CN201410207015A CN104045054A CN 104045054 A CN104045054 A CN 104045054A CN 201410207015 A CN201410207015 A CN 201410207015A CN 104045054 A CN104045054 A CN 104045054A
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Abstract
The invention discloses a method for preparing a high-adhesion micro-nano array structure film through wet etching and reverse transfer printing. The method comprises the following steps: with a silver nitrate/hydrofluoric acid solution as a silver deposition solution, depositing a layer of porous silver film on a silicon chip so as to obtain an etching catalytic metal and etching a desired micro-nano array structure in a hydrofluoric acid/hydrogen peroxide solution or potassium hydroxide/isopropanol solution; carrying out soaking with concentrated nitric acid so as to remove the silver film, carrying out air drying and using the treated silicon chip as a template silicon chip; uniformly coating the template silicon chip with organic matter colloid and standing the template silicon chip for a period of time; and placing the template silicon chip on a heating plate after precipitation and uniform distribution of bubbles, heating the template silicon chip at a certain temperature for a period of time, stripping off a colloid film when the colloid completely solidifies and printing a reversed structure of the prepared micro-nano array structure on the colloid film through transfer printing so as to realize preparation of the high-adhesion micro-nano array structure film. The method is simple to operate, has low cost, is not restricted by a preparation area and can be extensively applied to the field of bionic adhesion.
Description
Technical field
the present invention relates to a kind of wet etching method and reversion seal legal system utilized for the method for the micro-nano array structure thin film of high-adhesiveness, belong to technical field of nano material.
Background technology
Object has adhering reason and has: suction that atmospheric pressure causes, frictional force, micro-connection function (micro-connection function is present in adhesive and rough body surface conventionally), electrostatic attraction, viscose glue effect (liquid that refers generally to animal glandular secretion has certain viscosity), capillary force etc.The adhesion principles of micro-nano adhesion Array structure prepared by this method is micro-, (Van der Waals for is neutral molecule mutual distance when very near, the faint electromagnetic attraction of one of generation) that the Van der Waals for accumulation that produces between the projection of rank and body surface molecule received forms on polyurethane film surface.
The method of the micro-nano adhesion Array structure of current preparation generally has following several: utilize inclination array structure that photoetching technique obtains photoresist as template, and then obtain polyurethane inclination array with template duplicating, but because some photoresist pliability is poor and be combined not firmly with substrate, therefore its use is restricted.Utilize deep etching technology on silicon chip, to manufacture silicon chip hole as template, then injection of polymer, demoulding can be made into a micron adhesion arrangement array, utilize the adhesion arrangement array that the method obtains to there is very strong adhesion, but the precompression needing while use is too large, and template can not be reused, and cost is larger.Utilize nanometer embossing that traditional template replica application of principle is manufactured to field to microcosmic, this method has the features such as high-resolution, high efficiency, low cost and technical process are simple, but its process of preparing template often need to adopt photoetching technique, and the clean type in moulding process between thermal expansivity and the compactness contacting, template and the substrate of template and substrate has very large restriction to fidelity of repair, template is also difficult to recycling.In addition, also prepare the adhesion arrangement array being formed by high-density carbon nano-tube array and utilize dip coating technology to prepare the method for anisotropic dryness adhesion material by employing chemical vapour deposition (CVD) at present.But above method is prepared expensive ion etching and harsh processing environment or the complicated technological process of needs of optical exposure equipment needs of technology needs in preparation process of micro-nano adhesion arrangement array, and has the shortcomings such as instrument maintenance.In document, there is no at present the report of preparing high-adhesiveness array structure thin film that adopts wet etching legal system to combine for template silicon chip and micro-nano structure transfer technique.Therefore, we have invented new method prepared by a kind of adhesion arrangement.
Summary of the invention
The object of the present invention is to provide a kind of low cost, utilize wet etching method and reversion to print the method for legal system for the micro-nano array structure thin film of high-adhesiveness simply, efficiently.The method does not need expensive experimental facilities, only need on silicon chip, prepare suitable micro-nano structure, be used in conjunction with suitable organic matter and select suitable film-forming temperature, the micro-nano array structure reversion that just can realize Large-Area-Uniform prints on organic matter, the adhesion property that improves material itself with this, preparation has the film of the micro-nano array structure of high-adhesiveness.
For achieving the above object, the present invention adopts technical scheme as follows:
Utilize wet etching method and reversion to print the method for legal system for the micro-nano array structure thin film of high-adhesiveness, comprise the following steps:
(1) cleaning of silicon chip: use successively the mixed solution ultrasonic cleaning monocrystalline silicon piece 20-30 minute of alcohol, acetone, hydrogen peroxide and ammoniacal liquor, then soak 5-10 hour with the mixed solution of hydrogen peroxide and the concentrated sulfuric acid;
(2) on silicon chip, deposit porous silverskin: using the mixed aqueous solution of silver nitrate/hydrofluoric acid as heavy silvering solution, get the silicon chip cleaning in step (1) and put into wherein, the standing certain hour that deposits at 25 DEG C of room temperatures, obtaining superficial growth has the silicon chip of porous silverskin;
(3) " growth " required micro nano structure array: the porous silverskin making using step (2) is as etching catalytic metal on silicon chip, put into and at 25 DEG C of hydrofluoric acid/hydrogen peroxide solution room temperatures, leave standstill etching certain hour, or the silicon chip after step (1) cleaning is put into potassium hydroxide/aqueous isopropanol, 80 DEG C of processing certain hours of water-bath, obtain the template silicon chip of surface with micro-nano array structure;
(4) remove silverskin: red fuming nitric acid (RFNA) is put into the template silicon chip of micro-nano array structure in the surface preparing in step (3), soak 1-2min, remove silverskin, in deionized water, clean up, naturally dry;
(5) preparation of the micro-nano array structure thin film of high-adhesiveness: the organic matter colloid mixing is according to a certain ratio coated on template silicon chip uniformly, at 25 DEG C of room temperatures, leave standstill certain hour, until Bubble and after being evenly distributed, silicon chip is put on heating plate, with uniform temperature heating certain hour, after glue solidifies completely, take colloid film off, the antistructure of the micro-nano array structure of preparing on silicon chip can be transferred on colloid film, realize the preparation of the micro-nano array structure thin film of high-adhesiveness.
Described micro-nano array structure can be nano wire, nano-pillar, nano-pore, micro-/ nano pyramid, nanometer grid or nm wall etc.
On described template silicon chip, the parameter of micro-nano array structure can be by heavy silver time and hydrofluoric acid/hydrogen peroxide in the mixed aqueous solution of silver nitrate/hydrofluoric acid) etching period in solution or potassium hydroxide/aqueous isopropanol carries out accuracy controlling, can realize the regulation and control to antistructure parameter on organic matter colloid film, and then realize the viscosity control to micro-nano adhesion Array structure.
Described template silicon chip can reuse.
Described organic matter colloid can be organic matter colloid or PDMS colloid.
Beneficial effect of the present invention:
1, the method for preparing template of the present invention is wet chemical etching method, and solution ratio is simple, be easy to preparation, can synthesize large-area reproducible micro-nano structure.
2, the adhesion material that the present invention selects is polyurethane or PDMS, and its elastic modelling quantity adjustability is strong, and viscoplasticity is good, and adhesion is moderate; The process of transfer printing is without solution participation with without cull processing procedure, simple to operate and quick, has high efficiency-cost ratio.
3, the micro-nano array structure thin film of high-adhesiveness that the present invention prepares have not can to template surface cause damage, self-cleaning, can Reusability etc. advantage, be applicable to being very much applied to the adhesion climbing mechanism of Micro-Robot, the field such as development, bionic science of novel adhesive tape.
Brief description of the drawings
Fig. 1 is the preparation of template silicon chip and the preparation process schematic diagram of the micro-nano array structure thin film of high-adhesiveness; Wherein, (a) cleaning silicon wafer; (b) the porous silverskin depositing on silicon chip; (c) prepare the silicon nanowire array structure of Len req; (d) removal of silverskin; (e) on template silicon chip, apply one deck polyurethane gel; (f) after solidifying, the polyurethane film of taking off, the antistructure of the micro-nano structure on template silicon chip is successfully transferred on polyurethane film.
Fig. 2 increases with silicon nanowires etching period, the variation of dimension nanometer construction differentiation and cut/normal adhesion force on polyurethane, wherein, (a) on polyurethane, micro nano structure develops, I, II, III, IV, V, VI, the template nano wire etching period of VII figure is respectively 0,30,60,180,480,780,1200,2100s; (b) variation of cut/normal adhesion force, the I in 1,2,3, No. 4 sample corresponding diagram (a), II, III, IV sample.
Fig. 3 is the micro-nano structure scanning electron microscope diagram sheet after various transfer printings on polyurethane film; Wherein, (a) the nanometer convex pack arrangement of random distribution (template is short silicon nanowire array structure on silicon chip); (b) the micro-nano convex closure structure of random distribution (template is cluster silicon nanowire array structure on silicon chip); (c) the micron convex closure structure of random distribution (being micron pit array structure on silicon chip in template); (d) random micron pit array structure (template is random silicon nanowire array structure); (e) regular nanometer pit array structure (template is the polystyrene microsphere array structure of silicon chip surface solid matter); (f) inverted pyramid pit array structure (template is the pyramid array structure of silicon chip surface random distribution).
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be described in detail.
Embodiment
To prepare high-adhesiveness nanowire array structure film as example
(1) cleaning of silicon chip: use successively alcohol, acetone, hydrogen peroxide (mass fraction 30%): ammoniacal liquor (mass fraction 25%-28%): deionized water=1:1:5(volume ratio) ultrasonic cleaning monocrystalline silicon piece 20 minutes, then use hydrogen peroxide (mass fraction 30%): the concentrated sulfuric acid (mass fraction 98%): deionized water=3:1(volume ratio) soak 8 hours;
(2) on silicon chip, deposit porous silverskin: use deionized water 0.5mmol(0.085g) silver nitrate (AgNO
3) and 0.46mol(20ml) hydrofluoric acid (HF, mass fraction is 40%) be diluted to 100ml, after stirring, get the silicon chip cleaning in step (1) and put into wherein, the standing silverskin 2min that deposits at 25 DEG C of room temperatures, obtaining superficial growth has the silicon chip of porous silverskin;
(3) on silicon chip " growth " silicon nanowire array structure of Len req: by deionized water 40mmol(4.1ml) hydrogen peroxide (H2O2, mass fraction 30%) and 0.46mol(20ml) hydrofluoric acid (HF, mass fraction is 40%) dilution be mixed with the etching solution of 100ml.Sample in step 2 is put into etching solution, at 25 DEG C of room temperatures, leave standstill etching 3min, obtain surface with the template silicon chip of silicon nanowire array structure (nanowire length can by change time accuracy controlling);
(4) remove silverskin: red fuming nitric acid (RFNA) (HNO is put into the template silicon chip of silicon nanowire array structure in the surface preparing in step (3)
3, mass fraction is 65%-68%) in, soak 1min, remove silverskin.In deionized water, clean, naturally dry;
(5) preparation of high-adhesiveness nanowire array structure film: get the sample in step (4), drip on its surface and be coated with standing 2h under 25 DEG C of conditions of one deck polyurethane adhesive (adhesiveness is adjustable) room temperature, until Bubble and after being evenly distributed, place 65 DEG C of heating 24h on heating plate, after gelling is solid, peeled, the antistructure of the nanowire array structure of preparing on silicon chip can be transferred on polyurethane film, realized the preparation of high-adhesiveness nanowire array structure film.
Claims (5)
1. utilize wet etching method and reversion to print the method for legal system for the micro-nano array structure thin film of high-adhesiveness, it is characterized in that comprising the following steps:
(1) cleaning of silicon chip: use successively the mixed solution ultrasonic cleaning monocrystalline silicon piece 20-30 minute of alcohol, acetone, hydrogen peroxide and ammoniacal liquor, then soak 5-10 hour with the mixed solution of hydrogen peroxide and the concentrated sulfuric acid;
(2) on silicon chip, deposit porous silverskin: using the mixed aqueous solution of silver nitrate/hydrofluoric acid as heavy silvering solution, get the silicon chip cleaning in step (1) and put into wherein, the standing certain hour that deposits at 25 DEG C of room temperatures, obtaining superficial growth has the silicon chip of porous silverskin;
(3) " growth " required micro nano structure array: the porous silverskin making using step (2) is as etching catalytic metal on silicon chip, put into hydrofluoric acid/hydrogen peroxide solution or potassium hydroxide/aqueous isopropanol, at 25 DEG C of room temperatures, leave standstill etching certain hour, or the silicon chip after step (1) cleaning is put into potassium hydroxide/aqueous isopropanol, 80 DEG C of certain hours of water-bath, obtain the template silicon chip of surface with micro-nano array structure;
(4) remove silverskin: red fuming nitric acid (RFNA) is put into the template silicon chip of micro-nano array structure in the surface preparing in step (3), soak 1-2min, remove silverskin, in deionized water, clean up, naturally dry;
(5) preparation of the micro-nano array structure thin film of high-adhesiveness: the organic matter colloid mixing is according to a certain ratio coated on template silicon chip uniformly, at 25 DEG C of room temperatures, leave standstill certain hour, until Bubble and after being evenly distributed, silicon chip is put on heating plate, with uniform temperature heating certain hour, after glue solidifies completely, take colloid film off, the antistructure of the micro-nano array structure of preparing on silicon chip can be transferred on colloid film, realize the preparation of the micro-nano array structure thin film of high-adhesiveness.
2. wet etching method and the method for reversion seal legal system for the micro-nano array structure thin film of high-adhesiveness utilized according to claim 1, it is characterized in that, described micro-nano array structure can be nano wire, nano-pillar, nano-pore, micro-/ nano pyramid, nanometer grid or nm wall etc.
3. utilize wet etching method and reversion to print the method for legal system for the micro-nano array structure thin film of high-adhesiveness according to claimed in claim 1, it is characterized in that, on described template silicon chip, the parameter of micro-nano array structure can be carried out accuracy controlling by the etching period in heavy silver time and hydrofluoric acid/hydrogen peroxide solution or potassium hydroxide/aqueous isopropanol in the mixed aqueous solution of silver nitrate/hydrofluoric acid, can realize the regulation and control to antistructure parameter on organic matter colloid film, and then realize the viscosity control to micro-nano adhesion Array structure.
4. utilize wet etching method and reversion to print the method for legal system for the micro-nano array structure thin film of high-adhesiveness according to claimed in claim 1, it is characterized in that, described template silicon chip can reuse.
5. utilize wet etching method and reversion to print the method for legal system for the micro-nano array structure thin film of high-adhesiveness according to claimed in claim 1, it is characterized in that, described organic matter colloid can be organic matter colloid or PDMS colloid.
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