CN109835869B - Micro-nano through hole template and preparation method and application thereof - Google Patents
Micro-nano through hole template and preparation method and application thereof Download PDFInfo
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- CN109835869B CN109835869B CN201910092159.3A CN201910092159A CN109835869B CN 109835869 B CN109835869 B CN 109835869B CN 201910092159 A CN201910092159 A CN 201910092159A CN 109835869 B CN109835869 B CN 109835869B
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Abstract
The invention discloses a micro-nano through hole template and a preparation method and application thereof, wherein the preparation method of the micro-nano through hole template comprises the following steps: s1, depositing a hydrophilic film on a blade; s2, uniformly mixing PDMS with a curing agent, and pouring the mixture on a hydrophilic film to obtain a PDMS template; s3, stripping the blade to obtain an inverse structure template of the micro-nano structure on the surface of the blade; and S4, thinning the reverse structure template in the step S3 to obtain a micro-nano through hole template. According to the invention, a hydrophilic film is deposited on a blade, an inverse structure template is prepared by utilizing a micro-nano structure on the surface of the blade, and the micro-nano through hole template is obtained by thinning the inverse structure template. The preparation method provided by the invention has the advantages of simple process, low cost, no need of complex equipment and low environmental pollution degree, and solves the problems of complex preparation process and high cost of the hole template.
Description
Technical Field
The invention relates to the technical field of micro-nano device preparation and application, in particular to a micro-nano through hole template and a preparation method and application thereof.
Background
Since Gleiter in germany successfully prepares nano bulk metal crystal iron, copper and the like in 1984, research on nano materials gradually becomes a hotspot in the field of materials, and the nano materials have wide application prospects in the aspects of catalysis, medicine, water treatment, light absorption and the like due to the structural characteristics of the nano materials, so that how to prepare ideal nano materials also becomes a hotspot in research. In the preparation research of the nano material, the control of the composition, structure, morphology, arrangement and the like of the material can influence the expected special physical properties of the nano material. Therefore, the template method for preparing the nano material draws wide attention, and different from the common method, the reaction is always carried out in an effectively controlled range area, the template method for preparing the nano material has better flexibility, the size and the structure of the nano material can be better controlled, and the agglomeration phenomenon of the nano material can be prevented.
The pore template is used as the core of the template method for preparing the nano material, is the key for preparing the ideal nano material, and has the problems of higher cost, complex process and the like on the preparation method of the pore template. For example, in the process of preparing an anodic aluminum oxide template (AAO template), the process steps of high-temperature annealing, electrochemical polishing, anodic oxidation, hole expansion and the like are involved, the hole template not only has the problem of complex preparation process, but also causes certain pollution to the environment by the used acidic electrolyte. Therefore, how to realize low cost, cleanness and simplicity in the preparation process of the pore template is a serious challenge in the field of preparing nano materials by the template method.
Therefore, a preparation method of the micro-nano through hole template with simple process and low cost needs to be researched.
Disclosure of Invention
The invention provides a method for preparing a micro-nano through hole template, aiming at overcoming the defects of complex preparation process and high cost of the hole template in the prior art.
The invention also aims to provide the micro-nano through hole template prepared by the preparation method.
The invention also aims to provide application of the micro-nano through hole template in preparation of nano materials or micro-nano devices.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of a micro-nano through hole template comprises the following steps:
s1, depositing a hydrophilic film on the leaf;
s2, uniformly mixing PDMS with a curing agent, and pouring the mixture on a hydrophilic film to obtain a PDMS template;
s3, stripping the blade to obtain an inverse structure template of the micro-nano structure on the surface of the blade;
and S4, thinning the reverse structure template in the step S3 to obtain a micro-nano through hole template.
The invention provides a preparation method of a micro-nano through hole template, which is characterized in that a hydrophilic film is deposited on a blade, an inverse structure template is prepared by utilizing a micro-nano structure on the surface of the blade, and the micro-nano through hole template is obtained by thinning the inverse structure template. The hydrophilic film is beneficial to the separation of the blade and the PDMS template in the subsequent steps, so that the PDMS template can more completely copy the micro-nano structure on the surface of the blade. The preparation method has the advantages of simple process, low cost, no need of complex equipment and low environmental pollution. The invention solves the problems of complex preparation process and higher cost of the hole template.
Preferably, the hydrophilic film in step S1 is an aluminum oxide film, a titanium oxide film, or a hafnium oxide film. More preferably, the hydrophilic film in step S1 is a titanium oxide film.
The hydrophilic film can increase the contact area between the reverse mold solution and the blade, so that the micro-nano structure on the surface of the blade can be more completely copied by the PDMS template, and the hydrophilic film is favorable for stripping the PDMS template from the blade in the subsequent steps.
Preferably, the thickness of the hydrophilic film in the step S1 is 2nm to 20 nm. More preferably, the thickness of the hydrophilic film in step S1 is 10 nm.
Preferably, in step S1, the leaves are lotus leaves, rice leaves, rose petals.
More preferably, the leaf is a lotus leaf in step S1.
Preferably, the lotus leaves are ripe fresh lotus leaves. The leaves are trimmed to the desired shape.
Preferably, the shape is circular.
Preferably, the mastoid height of the leaf is 6 to 13 μm in step S1.
Preferably, the deposition in step S1 is Atomic Layer Deposition (ALD), Molecular Layer Deposition (MLD), or electron cyclotron resonance plasma-assisted pulsed laser deposition (ECR-PLD). More preferably, the deposition in step S1 is Atomic Layer Deposition (ALD).
In the invention, the PDMS is polydimethylsiloxane.
Preferably, the curing agent is a crosslinking agent of tin dibutylcinnamate dilaurate.
Preferably, the mass ratio of the PDMS to the curing agent in the step S2 is 5-30: 1. More preferably, the mass ratio of the PDMS to the curing agent in the step S2 is 10: 1.
Preferably, the thickness of the PDMS template in the step S2 is 15 μm to 100 μm. More preferably, the thickness of the PDMS template in step S2 is 15 μm.
Preferably, the method for preparing the PDMS template further includes a step of baking and curing.
Preferably, the peeling in step S3 is performed by a micro-robot.
Preferably, the thinning in step S4 employs an ion thinning technique.
Preferably, the micro-nano through hole template in step S4 is a micro-nano through hole template or a nano through hole template.
Preferably, the thickness of the micron through-hole template is 4-12 μm. More preferably, the thickness of the micro through-hole template is 11 μm.
Preferably, the aperture of the micron through hole template is 3-10 μm. More preferably, the pore size of the micro via template is 5 μm.
Preferably, the thickness of the nano through hole template is 5-13 μm. More preferably, the thickness of the nano-via template is 12 μm.
Preferably, the aperture of the nano through hole template is 5-100 nm. More preferably, the pore size of the nano-via template is 20 nm.
The invention also protects the micro-nano through hole template prepared by the preparation method.
The invention also protects the application of the micro-nano through hole template in the preparation of nano materials or micro-nano devices.
The invention also protects the application of the micro-nano through hole template in quantum dots.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, a hydrophilic film is deposited on a blade, an inverse structure template is prepared by utilizing a micro-nano structure on the surface of the blade, and the micro-nano through hole template is obtained by thinning the inverse structure template. The preparation method provided by the invention has the advantages of simple process, low cost, no need of complex equipment and low environmental pollution degree, and solves the problems of complex preparation process and high cost of the hole template.
Drawings
Fig. 1 is a process flow diagram of a method for preparing a micro-nano through hole template in embodiment 1.
Fig. 2 is a schematic view of the surface structure of lotus leaves.
Fig. 3 is a schematic structural diagram of the micro-nano through hole template preparation method in example 1, presented in step S1.
Fig. 4 is a schematic structural diagram of the micro-nano through hole template preparation method in example 1, presented in step S2.
Fig. 5 is a schematic structural diagram of the micro-nano through hole template preparation method in example 1, presented in step S3.
Fig. 6 is an axial cross-sectional view of the micro-nano through hole structure appearing in step S4 of the micro-nano through hole template preparation method of embodiment 1.
Fig. 7 is an axial cross-sectional view of the micro-nano through hole structure appearing in step S4 of the micro-nano through hole template preparation method of embodiment 2.
The template comprises 1, lotus leaves in a required shape, 2, a hydrophilic film, 3, a PDMS template, 30, a micron through hole template, 31 and a nanometer through hole template.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the embodiments of the present invention are not limited thereto. The raw materials in the examples are all commercially available; reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Please refer to fig. 1 to 6. It should be noted that the drawings provided in the present embodiment are only for illustrating the basic idea of the present invention, and the components related to the present invention are only shown in the drawings rather than drawn according to the number, shape and size of the components in actual implementation, and the type, quantity and proportion of the components in actual implementation may be changed freely, and the layout of the components may be more complicated.
Example 1
A preparation method of a micro-nano through hole template comprises the following steps:
s1, cutting the ripe fresh lotus leaves into required shapes, and depositing a layer of titanium oxide film with the thickness of 10 nm on the round lotus leaves by adopting an atomic layer deposition method;
s2, uniformly mixing PDMS and a crosslinking agent curing agent of tin dilauryl dibutyl cinnamate according to the mass ratio of 10: 1, pouring the mixture on a titanium oxide film, and drying and curing to obtain a PDMS template with the thickness of 15 micrometers;
s3, stripping the blade to obtain an inverse structure template of the micro-nano structure on the surface of the blade;
and S4, thinning the reverse structure template in the step S3 by using an ion thinning technology to obtain a micron through hole template with the thickness of 11 microns and the aperture of 5 microns.
Example 2
A preparation method of a micro-nano through hole template comprises the following steps:
s1, cutting mature fresh rice leaves into required shapes, and depositing a layer of 2nm alumina film on the round lotus leaves by adopting an atomic layer deposition method;
s2, uniformly mixing PDMS and a crosslinking agent curing agent of tin dilauryl dibutyl cinnamate according to the mass ratio of 5: 1, pouring the mixture on an alumina film, and drying and curing to obtain a PDMS template with the thickness of 15 micrometers;
s3, stripping the blade to obtain an inverse structure template of the micro-nano structure on the surface of the blade;
and S4, thinning the reverse structure template in the step S3 by using an ion thinning technology to obtain a micron through hole template with the thickness of 11 microns and the aperture of 4 microns.
Example 3
A preparation method of a micro-nano through hole template comprises the following steps:
s1, cutting the ripe fresh sweet potato leaves into a required shape, and depositing a layer of 20nm hafnium oxide film on the round lotus leaves by adopting an atomic layer deposition method;
s2, uniformly mixing PDMS and a crosslinking agent curing agent of tin dilauryl dibutyl cinnamate according to the mass ratio of 30: 1, pouring the mixture on a hafnium oxide film, and drying and curing to obtain a PDMS template with the thickness of 15 micrometers;
s3, stripping the blade to obtain an inverse structure template of the micro-nano structure on the surface of the blade;
and S4, thinning the reverse structure template in the step S3 by using an ion thinning technology to obtain a micron through hole template with the thickness of 11 microns and the aperture of 9 microns.
Example 4
The difference between this example and example 1 is that the hydrophilic film of this example is an alumina film, and a micron through-hole template with a thickness of 11 μm and a pore size of 4 μm is obtained;
the other raw material steps and operating conditions were the same as in example 1.
Example 5
The difference between this example and example 1 is that the hydrophilic film of this example is a hafnium oxide film, and a micron through-hole template with a thickness of 11 μm and a pore diameter of 3 μm is obtained;
the other raw material steps and operating conditions were the same as in example 1.
Example 6
The difference between the present embodiment and embodiment 1 is that the present embodiment obtains a nano through-hole template with a thickness of 12 μm by ion thinning technology, and the aperture is 20 nm;
the other raw material steps and operating conditions were the same as in example 1.
Comparative example 1
A preparation method of a through hole template comprises the following steps:
s1, cutting the ripe fresh lotus leaves into required shapes;
s2, uniformly mixing PDMS and a crosslinking agent curing agent of tin dilauryl dibutyl cinnamate according to the mass ratio of 10: 1, pouring the mixture on lotus leaves, drying and curing to obtain a PDMS template with the thickness of 15 μm;
s3, stripping the blade to obtain an inverse structure template;
and S4, thinning the reverse structure template in the step S3 by using an ion thinning technology, wherein the micrometer through hole template cannot be obtained, and the nanometer through hole template cannot be obtained.
However, in the comparative example 1, since a hydrophilic film is not coated on the blade, the structure of the blade cannot be completely copied by the PDMS template, and thus the micro-via template cannot be obtained after the template is thinned by the ion thinning technique.
As can be seen by comparing examples 1 and 4 to 5, the effect of using the titanium oxide thin film is superior to that of the aluminum oxide thin film and the hafnium oxide thin film. Because the hydrophilic group of the titanium oxide is more than that of the aluminum oxide and the hafnium oxide, the titanium oxide has better hydrophilicity and can more completely copy the mastoid structure on the surface of the blade.
In conclusion, the micro-nano through hole template is prepared by utilizing the micro-nano structure on the surface of the blade, the preparation method is simple in process and low in cost, and complex equipment is not needed. The method for preparing the micro-nano through hole template based on the micro-nano structure on the surface of the blade takes the natural blade as a plant template to prepare the micro-nano through hole template, and has the characteristics of clean process and no pollution. The preparation process is clean and has low pollution degree to the environment. The method for preparing the micro-nano through hole template solves the problems of complex preparation process and high cost of the hole template.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (7)
1. A preparation method of a micro-nano through hole template is characterized by comprising the following steps:
s1, depositing a hydrophilic film on a blade;
s2, uniformly mixing PDMS with a curing agent, and pouring the mixture on a hydrophilic film to obtain a PDMS template;
s3, stripping the blade to obtain an inverse structure template of the micro-nano structure on the surface of the blade;
and S4, thinning the reverse structure template in the step S3 to obtain a micro-nano through hole template.
2. The production method according to claim 1, wherein the hydrophilic film in step S1 is a titanium oxide film, an aluminum oxide film, or a hafnium oxide film.
3. The production method according to claim 2, wherein the hydrophilic film in step S1 is a titanium oxide film.
4. The method according to any one of claims 1 to 3, wherein the thickness of the hydrophilic film in step S1 is 2nm to 20 nm.
5. The method according to claim 1, wherein the leaves in step S1 are lotus leaves, rice leaves, rose petals.
6. The method according to claim 1, wherein the mastoid height of the leaf is 6 to 13 μm in step S1.
7. The method according to claim 6, wherein the thickness of the PDMS mold in step S2 is 15 μm to 100 μm.
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| US7557051B2 (en) * | 2004-03-17 | 2009-07-07 | The Board Of Trustees Of The Leland Stanford Junior University | 3-D interconnected multi-layer microstructure of thermoplastic materials |
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| JP2007136790A (en) * | 2005-11-16 | 2007-06-07 | Ricoh Elemex Corp | Process for producing through hole structure by imprinting method, and through hole structure produced by that method |
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