CN106185792A - A kind of population parameter controllable method for preparing of super-hydrophobic micro-nano compound structure - Google Patents
A kind of population parameter controllable method for preparing of super-hydrophobic micro-nano compound structure Download PDFInfo
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Abstract
The invention discloses the population parameter controllable method for preparing of a kind of super-hydrophobic micro-nano compound structure, belong to micro-nano structure preparing technical field.The method is to prepare micrometer structure and nanostructured to combine, prepared by layering, i.e. realize micrometer structure by photoetching to prepare, realizing nanostructured by colloid Soft lithograph and body silicon etching to prepare, compound being combined with micrometer structure array by Nano microsphere mask of micron and nanostructured is realized.The method is the scientific research of micro-nano structure super hydrophobic surface and engineering practice provides Research foundation, effectively the macroscopic appearance of material surface is connected with microstructure, provides the foundation for exploring the physicochemical properties of super hydrophobic surface quantitatively, qualitatively.The method is to be combined with body silicon etching by colloid Soft lithograph, and process controllability is strong, simple to operate, with low cost, and machining accuracy is high.
Description
Technical field
The invention belongs to micro-nano structure preparing technical field, relate to the full ginseng of a kind of super-hydrophobic micro-nano compound structure
Number controllable method for preparing.
Background technology
Super-hydrophobic is the special wetting state of one of material surface, and it has widely in scientific research and commercial production
Application.Super hydrophobic surface refers to the surface of static contact angle θ >=150 ° of water droplet, the thing that this water droplet is mutually exclusive with surface
Rationality matter, result in the contact area minimizing of water droplet and surface, and water droplet is in a kind of suspended state on surface.Due to super-hydrophobic table
This advantageous characteristic in face, therefore at the aspect such as antifog, anti-icing, snow defence, automatically cleaning, drag reduction, desorption, corrosion-resistant and antioxidation all
Playing an important role, potential using value is the highest.
Surface wetting characteristic is mainly determined by surface free energy and surface microscopic topographic.Y T Cheng
(Nanotechnology, 17 (5), 1359-1362) finds that when studying lotus leaf surface super-hydrophobicity lotus leaf surface is a kind of double
The micro-nano compound structure of stratum, its surface distributed many diameters in 5~9 μm, the micron projection of highly 1~20 μm and average straight
Footpath is at the nanometer raised structures of 200nm, and surface is made up of the waxiness of one layer of basal surface energy
[Chem.Soc.Rev.2010.39,3240], and research prove micro-nano compound structure binary cooperative effect be have super-hydrophobic
The crucial factor of performance.Therefore it is treated as preparing a kind of approach of super hydrophobic surface by structure micro-nano structure and surface.
At present, the preparation method of super hydrophobic surface has chemical gaseous phase deposition, electrochemistry, template, sol-gal process, hydro-thermal
Method, photoengraving, femtosecond laser etc., these methods are to construct micro-nano structure in different base, and modify low-surface-energy thing on surface
Matter, it is achieved super-hydrophobicity.But it is mixed and disorderly that electrochemistry, collosol and gel, hydro-thermal method all utilize chemical reaction to be formed in substrate
Micro-nano compound structure, it is impossible to realize the controlled preparation of population parameter of micro-nano structure;Chemical gaseous phase deposition is by preparing in substrate
The fluorination class thin film with low-energy surface realizes super-hydrophobic, this past only by constructing super hydrophobic surface prepared by low-energy surface
Short toward poor stability, life-span, low with substrate caking power, it is easy to be destroyed;For femtosecond laser is processed, essence can be realized
The controlled preparation of close size, but due to heat effect, thawing, burr and crackle and it needs to expensive process equipment etc. so that fly
Second Laser Processing is restricted.Photoetching is to realize a kind of common method prepared by micro structure, but, current photo etched mask can only
Realize submicron and be prepared by micron-sized structure, therefore, limited the nanostructured essence of size adjustable on a large scale by photo etched mask
True preparation, still needs to explore.
Microscopic appearance determines macroscopic appearance, it is achieved the controlled preparation of micro-nano structure population parameter, carry out quantitatively for macroscopic appearance,
Qualitative analysis provides the foundation.In material surface wetting theory is studied, the change of microscopic dimensions parameter, to material surface pattern
The impact of dutycycle, the impact on the size of the air pocket between micro structure and water droplet, its micro-nano compound structure two grades is worked in coordination with
The impact etc. of effect, is required for carrying out quantitatively, scientific research qualitatively, but, it is controlled that present stage lacks micro-nano structure population parameter
The method of preparation, causes and cannot explore its mechanism;In engineer applied, micro-nano structure super hydrophobic surface is utilized to prevent
In the engineering practice of ice, explore the change of micro-nano structure parameter, to super-cooling waterdrop at substrate surface adhesion, heat transfer and forming core
Impact, the most critically important;In micronano optical research field, the change of micro-nano structure dimensional parameters, to light at micro-nano structure surface
Electromagnetic enhancement effect, Raman effect have significant impact.
In sum, the preparation method of existing micro-nano structure has multiple, but these methods all cannot realize micro-nano and be combined
The controlled preparation of structure population parameter, particularly controlled on the micrometer structure nanostructured preparing size adjustable.But, it is achieved
Scientific research and engineer applied are all made great sense by the controlled preparation of micro-nano structure population parameter.Therefore, development one is needed badly
Simply, the method facilitating controlled preparation.
We are from micro electronmechanical (MEMS) photoetching technique, the method for association colloid Soft lithograph, and first passing through self assembly will receive
Meter Wei Qiu is assembled into monolayer compact nanometer mask.Then by monolayer compact nanometer mask and the silica-based bear building-up with micrometer structure
Close, by RIE (oxygen plasma etching), nanometer bead is carried out Soft lithograph, regulation Nano microsphere diameter and spacing, then passes through body
Silicon etching silicon base, removes Nano microsphere and has just prepared micro-nano compound structure, modifies with silicon fluoride the most again, obtains having excellent
The more super hydrophobic surface of performance.
Summary of the invention
A kind of method that present invention aim at providing silica-based super-hydrophobic controlled preparation of micro-nano structure population parameter.Pass through the party
Method can reach and accurately control micrometer structure, nanostructured and micro-nano to be combined second order population parameter modulated standby.
The key point of the present invention is that nanometer mask is compound with micrometer structure array and nanostructured population parameter is controlled
Preparation.Micrometer structure can realize the controlled preparation of population parameter in length and array gap by traditional photoetching technique.But
Nanostructured is compound on micrometer structure, it is necessary to nanometer mask is combined with micrometer structure array, the most again should
The controlled preparation of nanostructured population parameter is realized with colloid Soft lithograph and body silicon etching.
Technical scheme is as follows:
A kind of silica-based super-hydrophobic controlled preparation of micro-nano structure population parameter, is to prepare micrometer structure and nanostructured to combine
Come, prepared by layering, i.e. realize micrometer structure by photoetching and prepare, realize nano junction by colloid Soft lithograph and body silicon etching
Body plan is standby, and compound being combined with micrometer structure array by Nano microsphere mask of micron and nanostructured is realized.
A kind of method of silica-based super-hydrophobic controlled preparation of micro-nano structure population parameter, it is characterised in that comprise the steps:
Step one: the preparation of silica-based micrometre array structure: utilize ripe photoetching technique, prepared by mask respectively, be coated with
Glue, exposing, develop, ICP etching just can be prepared the micrometer structure array of pre-set dimension and show.Micrometer structure is square microtrabeculae, its
Square column length of side a=5~20 μm, highly h=10~60 μm, spacing b=10~120 μm;
Step 2: the preparation of nanometer mask;This process includes following four sub-steps:
Sub-step one: the Nano microsphere suspension of configuration monodisperse system;
Sub-step two: by another hydrophobic substrate of oxygen plasma treatment so that it is surface hydrophilic, revolves Nano microsphere suspension
It is applied in this substrate, forms venation shape monolayer Nano microsphere thin film on the substrate;
Sub-step three: peel off venation shape monolayer Nano microsphere thin film: first stand the venation shape in sub-step two there being spin coating
The substrate of monolayer Nano microsphere thin film so that it is be recovered to hydrophobicity;Then venation shape monolayer Nano microsphere thin film spin coating being had
This substrate immerse the most from top to bottom in liquid, described liquid is preferably deionized water;Described venation shape monolayer Nano microsphere
Thin film is peeled off from this substrate and is suspended in liquid level;
Sub-step four: dripping surfactant at liquid level, the crowded venation shape monolayer Nano microsphere thin film that pushes away is assembled into fine and close single
Layer film, completes liquid-vapor interface secondary and assembles;
Step 3: nanometer mask and micrometre array structure composite: on the basis of the sub-step four of step 2, reduces liquid level,
Described fine and close single thin film is transferred on the silica-based micrometre array body structure surface described in step one;
Step 4: colloid Soft lithograph, regulation nanometer mask spacing and radius;
By step 2, three achieve the compound of compact nanometer microsphere mask and micrometer structure array.Due to nanopillars
Array pitch is to be determined by Nano microsphere original diameter dimensions, and the diameter of nanopillars is determined by nanometer diameter after etching,
Therefore, we pass through colloid Soft lithograph, etch compact arranged Nano microsphere diameter, regulate nano array structure chi with this
Very little, this step can realize nanometer mask diameter d=200~800nm, highly h1=3 μm~200nm range;
Step 5: the controlled preparation of silicon-based nano structure population parameter;This step uses metal auxiliary etch method etching silicon base,
It is divided into two sub-steps;
Sub-step one: silicon substrate surface evaporation silver, after step 4, monolayer pycnomorphous Nano microsphere diameter diminishes,
Gap occurs between Nano microsphere, then by evaporation silver, between Nano microsphere, fills silver layer, utilize galvanic principles to silica-based
Perform etching, it is however noted that, evaporation silver thickness must not exceed the radius of Nano microsphere after Soft lithograph;
Sub-step two: metal auxiliary etch solution is prepared, and has been deposited with one layer between Nano microsphere by sub-step one
Silver, is placed on HF and H by the silicon base handled well2O2Mixed solution performs etching;
Sub-step three: obtained for step 4 silicon base be placed in drying baker and carry out heat treatment, increases nanometer bead and silicon
The adhesion of substrate;It is then placed in the joined solution of sub-step two, reacts.By controlling the response time, can control to receive
The degree of depth of meter Wei Zhu;
Sub-step four: the silicon base after etching is placed in oxolane immersion and removes Nano microsphere;
Step 6: silicon fluoride modifies silica-based micro-nano compound structure, prepares and has ultra-hydrophobicity surface.
Beneficial effects of the present invention:
Present invention firstly provides a kind of micro-nano compound structure population parameter controllable method for preparing, especially on micrometer structure
The compound full-scale controlled preparation of nanostructured, the method is the scientific research of micro-nano structure super hydrophobic surface and engineering practice carries
Supply Research foundation, effectively the macroscopic appearance of material surface has been connected with microstructure, super for exploring quantitatively, qualitatively
The physicochemical properties of hydrophobic surface provide the foundation.The method is to be combined with body silicon etching by colloid Soft lithograph, technique
Controllability is strong, simple to operate, with low cost, and machining accuracy is high.
Accompanying drawing explanation
Fig. 1 shows silica-based micrometer structure array schematic diagram;
Fig. 2 shows monolayer compact nanometer mask entirety optical microscope;
Fig. 3 shows monolayer compact nanometer microsphere partial sweep Electronic Speculum figure;
Fig. 4 shows nanometer mask and micrometer structure array complex optics microscope photograph;
Fig. 5 shows that Nano microsphere mask diameter reduces microgram after colloid Soft lithograph;
Fig. 6 shows micro-nano compound structure electron scanning micrograph;
Fig. 7 shows the scanning electron microscope microgram of single micro-nano compound structure;
Fig. 8 shows silica-based micro-nano super hydrophobic surface Static Contact angular measurement.
Detailed description of the invention
Below by way of instantiation, the present invention is described in more detail.
Embodiment 1
Super-hydrophobic micro-nano compound structure in the implementation case is: a kind of silica-based super-hydrophobic micro-nano compound structure, silica-based table
There is micron-sized square column array in face, has nanopillars array on square column top and silica-based bottom.Micron square column structure length of side a=10
μm, highly h1=20 μm, adjacent two micrometer structure spacing are b=20 μm;Composite nanostructure size on micrometer structure: diameter
D=600nm, highly h2=1.5 μm spacing L=900nm.
The controlled super-hydrophobic micro-nano compound structure preparing pre-designed size of the implementation case comprises the steps:
Step one: the preparation of silica-based micrometre array structure: first design photo etched mask makes array micrometer structure dimensional parameters
For a=10 μm, spacing b=20 μm.Then, by photoetching, figure is transferred on photoresist, then by inductive etc.
Gas ions reactive ion etching (ICP) etching silicon base, etching depth h1=20 μm;Its etch process parameters used is: radio frequency merit
Rate RF=100w, pressure is 20pa;SF6, gas flow 100sccm/min, etch period 12s;C4F6, gas flow 80sccm/
Min, passivation time 9s;Etching/passivation cycle number of times 16 times;Photoresist, deionized water rinsing, nitrogen is removed with acetone after etching
Dry up, just obtain the micrometer structure array with pre-set dimension, as shown in Figure 1.
Step 2: the preparation of nanometer mask;This process includes following four sub-steps:
Sub-step one: the Nano microsphere suspension of configuration monodisperse system;The present embodiment uses a diameter of 900nm's
Pipe/polyhenylethylene nano bead.
Sub-step two: by another hydrophobic substrate of oxygen plasma treatment so that it is surface hydrophilic, revolves Nano microsphere suspension
It is applied in this substrate, forms venation shape monolayer Nano microsphere thin film on the substrate;
Sub-step three: peel off venation shape monolayer Nano microsphere thin film: first stand the venation shape in sub-step two there being spin coating
The substrate of monolayer Nano microsphere thin film so that it is be recovered to hydrophobicity;Then venation shape monolayer Nano microsphere thin film spin coating being had
This substrate immerse the most from top to bottom in liquid, described liquid is deionized water;Described venation shape monolayer Nano microsphere thin film
Peel off from this substrate and be suspended in liquid level;
Sub-step four: dripping surfactant at liquid level, the crowded venation shape monolayer Nano microsphere thin film that pushes away is assembled into fine and close single
Layer film, completes liquid-vapor interface secondary and assembles, and this monolayer compact nanometer microsphere Film Optics macroscopic view observation figure is as in figure 2 it is shown, sweep
Face electron microscopic microgram is as shown in Figure 3
Step 3: nanometer mask and micrometre array structure composite: on the basis of the sub-step four of step 2, reduces liquid level,
Described fine and close single thin film is transferred on the silica-based micrometre array body structure surface described in step one, nanometer mask as shown in Figure 4
With micrometer structure array complex optics microscope photograph.
Step 4: colloid Soft lithograph, regulation nanometer mask spacing and radius;
By step 2, three achieve the compound of compact nanometer microsphere mask and micrometer structure array.Due to nanopillars
Array pitch is to be determined by Nano microsphere original diameter dimensions, and the diameter of nanopillars is determined by nanometer diameter after etching,
Therefore, we pass through colloid Soft lithograph, etch compact arranged Nano microsphere diameter, regulate nano array structure chi with this
Very little, this step can realize nanometer mask diameter d=200~800nm, highly h1=3 μm~200nm range.
In the present embodiment, it is as follows that application oxygen plasma etching (RIE) carries out Soft lithograph concrete technology parameter to Nano microsphere:
O2Gas flow 100sccm/min, CF4 gas flow is that 9.0sccm/min indoor pressure is: 26pa, and gas radio frequency merit is
100w, etch period is 30s~120s, and primary working gas is O2, etch period determines the final diameter of Nano microsphere, as
Shown in Fig. 5, pycnomorphous Nano microsphere diameter diminishes, and occurs in that gap between Nano microsphere, it is achieved that nanometer mask size
Regulation and control.
Step 5: the controlled preparation of silicon-based nano structure population parameter;This step uses metal auxiliary etch method etching silicon base,
It is divided into two sub-steps.
Sub-step one: silicon substrate surface evaporation silver, after step 4, monolayer pycnomorphous Nano microsphere diameter diminishes,
Gap occurs between Nano microsphere, then by evaporation silver, between Nano microsphere, fills silver layer, utilize galvanic principles to silica-based
Perform etching, in the present embodiment, silver thickness h3=40nm.
As follows at the concrete technology of silicon substrate surface evaporation silver: vacuum is 1.5 × 10-4Pa, the temperature of evaporation source is 1100
DEG C, target is silver target.
Sub-step two: metal auxiliary etch solution is prepared, and has been deposited with one layer between Nano microsphere by sub-step one
Silver, is placed on HF and H by the silicon base handled well2O2Performing etching in mixed solution, concrete etching solution preparation parameter is: treating excess syndrome
Test with HF (mass fraction is 39%) solution 18ml, take H2O2(mass fraction is 60%) solution 5ml, deionized water 77ml, uniformly
Mixing.
Sub-step three: obtained for step 4 silicon base be placed in drying baker and carry out heat treatment, increases nanometer bead and silicon
The adhesion of substrate, concrete operations: step 4 60 DEG C is processed 1h.It is then placed in the joined solution of sub-step two, reacts.
Silver-plated silicon base is placed in the present embodiment in metal auxiliary etch liquid reaction 8min, and can obtain is highly that the nanometer of 1.5 μm is micro-
Post array.
Sub-step four: the silicon base after etching is placed in oxolane immersion 1h, removes Nano microsphere, can be such as Fig. 6
Shown micro-nano compound structure.
Step 6: silicon fluoride modifies silica-based micro-nano compound structure, prepares and has superior ultra-hydrophobicity surface: by made
Standby silica-based micro-nano compound structure is put in vacuum tank, evacuation 5~15min, is passed through nitrogen, after stable gas pressure, opens true
Empty van, drips 2~3ml silicon fluorides, closes the lid, again evacuation, very in the culture dish near silica-based micro-nano compound structure
After reciprocal of duty cycle is stable, stands 2~4h, i.e. obtain the silica-based micro-nano compound structure with ultra-hydrophobicity needed for the present embodiment, warp
Test this micro-nano compound structure surface static contact angle and be more than 150 °, present excellent super-hydrophobicity as shown in Figure 8.
Claims (2)
1. the method for the silica-based super-hydrophobic controlled preparation of micro-nano structure population parameter, it is characterised in that comprise the steps:
Step one: the preparation of silica-based micrometre array structure, described micrometer structure is square microtrabeculae, its square column length of side a=5~20 μ
M, highly h=10~60 μm, spacing b=10~120 μm;
Step 2: the preparation of nanometer mask;This process includes following four sub-steps:
Sub-step one: the Nano microsphere suspension of configuration monodisperse system;
Sub-step two: by another hydrophobic substrate of oxygen plasma treatment so that it is surface hydrophilic, Nano microsphere suspension is spun on
In this substrate, form venation shape monolayer Nano microsphere thin film on the substrate;
Sub-step three: peel off venation shape monolayer Nano microsphere thin film: first stand the venation shape monolayer in sub-step two there being spin coating
The substrate of Nano microsphere thin film so that it is be recovered to hydrophobicity;Then being somebody's turn to do of venation shape monolayer Nano microsphere thin film spin coating being had
Substrate is immersed in liquid the most from top to bottom;Described venation shape monolayer Nano microsphere thin film is peeled off from this substrate and is suspended in liquid
Face;
Sub-step four: drip surfactant at liquid level, the crowded venation shape monolayer Nano microsphere thin film that pushes away is assembled into fine and close single thin layer
Film, completes liquid-vapor interface secondary and assembles;
Step 3: nanometer mask and micrometre array structure composite: on the basis of the sub-step four of step 2, reduces liquid level, by institute
State fine and close single thin film to transfer on the silica-based micrometre array body structure surface described in step one;
Step 4: colloid Soft lithograph, regulation nanometer mask spacing and radius, it is achieved nanometer mask diameter d=200~800nm are high
Degree h1=3 μm~200nm range;
Step 5: the controlled preparation of silicon-based nano structure population parameter, this step uses metal auxiliary etch method etching silicon base, is divided into
Two sub-steps;
Sub-step one: silicon substrate surface evaporation silver, described evaporation silver thickness is less than the radius of Nano microsphere after Soft lithograph;
Sub-step two: the silicon base handled well is placed on HF and H2O2Mixed solution performs etching;
Sub-step three: obtained for step 4 silicon base be placed in drying baker and carry out heat treatment, is then placed in sub-step two and is joined
In solution, react, control the degree of depth of nanopillars by controlling the response time;
Sub-step four: the silicon base after etching is placed in oxolane immersion and removes Nano microsphere;
Step 6: silicon fluoride modifies silica-based micro-nano compound structure, prepares ultra-hydrophobicity surface.
2. the method for the silica-based super-hydrophobic controlled preparation of micro-nano structure population parameter as claimed in claim 1, it is characterised in that
In the sub-step three of described step 2, the venation shape monolayer Nano microsphere film substrate liquid slowly that described immersion spin coating has is
Deionized water.
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