CN106276775B - A kind of micro-nano array structure, preparation method and application - Google Patents
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- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 32
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002086 nanomaterial Substances 0.000 claims abstract description 30
- 239000000758 substrate Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000010521 absorption reaction Methods 0.000 claims description 18
- 229920002120 photoresistant polymer Polymers 0.000 claims description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 10
- 238000001020 plasma etching Methods 0.000 claims description 8
- 238000005566 electron beam evaporation Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000004528 spin coating Methods 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000003763 carbonization Methods 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
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- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
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Abstract
The present invention relates to micro-nano processing technique fields, more particularly to a kind of micro-nano array structure, preparation method and application, the structure includes silicon carbide substrate, the micron cylinder in the silicon carbide substrate and the nanostructure in the silicon carbide substrate and the micron damaged surface.Micron cylinder of the invention is not limited by shape, and nanostructure is not limited by shape；It realizes 10-13 μm of middle infrared broad spectrum to absorb, absorptance is almost 1；Material of the present invention is simple, and operating procedure is single, and nanostructure is easy to process, using equipment such as ultraviolet photolithographics, reduces costs, it can be achieved that large area rapid processing, lays a good foundation for practical application.
Description
Technical field
It polarizes processing technique field the present invention relates to micro-nano surface, and in particular to a kind of micro-nano array structure, preparation
Method and application.
Background technique
Infrared absorption, infrared stealth and infra-red radiation cooling technology obtain more and more extensive in terms of civilian and military project
Wide spectrum is realized in concern, and high-intensitive infrared absorption is an important directions of development in science and technology.Traditional infrared absorption process is difficult
Accomplish not only to be able to achieve wide spectrum, high-intensitive infrared absorption characteristic, but also can work under extreme environment, and silicon carbide device
It can then be worked with its superior mechanics, calorifics and mechanical performance and widely be favored in extreme circumstances.
Surface phonon-polaritons (Surface Phonon Polariton, SPhP), which refer to, is present in Polar Crystal Surfaces
Lattice vibration and electromagnetic wave phase interaction generate along Polar Crystal Surfaces propagate phonon.Its main feature is that local is in polarity crystalline substance
Body surface face is presented electromagnetic field exponential damping along crystal normal direction, therefore can only tangentially propagate along crystal, swashs similar to surface plasma
Member.By change metallic surface structures, the property of SPhP and its with the available effective tune of the property of electromagnetic wave phase interaction
Section, to realize that the infrared broad spectrum absorption of silicon carbide high intensity provides possibility.
General silicon carbide infrared absorption technology is by the array nanostructure in silicon carbide processing rule come real
Existing, but the nano-structure array of this rule can only realize the absorption of some wavelength, can not achieve wide spectrum absorption.And
And these processing will generally use expensive manufacturing process, such as electron beam exposure, focused-ion-beam lithography technology, be difficult reality
Existing large area rapid processing, brings obstruction to practical application.
Summary of the invention
The object of the present invention is to provide a kind of micro-nano array structure, preparation method and application, to realize wide spectrum, high-strength
The infrared absorption of degree.
To achieve this purpose, the present invention adopts the following technical scheme:
On the one hand, the present invention provides a kind of micro-nano array structure, the structure includes silicon carbide substrate, in the carbon
Micron cylinder in SiClx substrate and the nanostructure in the silicon carbide substrate and the micron damaged surface.
In the present invention, the infrared absorption of micro nano structure is the interaction by surface phonon-polaritons and electromagnetic wave
Come what is realized, by preparing micron cylinder in silicon carbide-based bottom surface, then by preparing nanostructure on micron cylinder, to make
The array nanostructure of silicon carbide substrate and micron damaged surface formation rule is obtained, to realize that infrared broad spectrum absorbs.
Preferably, the silicon carbide substrate is the carborundum crystals there are Surface polaritons.
In the present invention, the carborundum crystals exist in infrared band with optical phonon.
Preferably, the micron cylinder is any one in cylinder, tetragonal prism or polygonal column structure.
Preferably, the nanostructure is any one in nano particle, nanometer pinpoint or nanocone.
Preferably, the nanostructure and substrate are same material.
Preferably, the micron cylinder is periodic array, and the period of micron cylinder is too small, has exceeded the processing of ultraviolet photolithographic
The limit；If the period is excessive, the effect of cylinder cannot be played, and influence infrared absorption effect, so the period is 2-20 μm, such as can
Be 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, 11 μm, 12 μm, 13 μm, 14 μm, 15 μm, 16 μm, 17 μm,
18 μm, 19 μm or 20 μm, preferably 5-15 μm.
Preferably, the micron cylinder sizes are too small, are more than ultraviolet photolithographic manufacturing limit；It is oversized, it also can be more than purple
The manufacturing limit of outer photoetching, while the infrared absorption effect of micron cylinder cannot be played, the cross-sectional area of the micron cylinder is
3-30μm2, such as can be 3 μm2、4μm2、5μm2、6μm2、7μm2、8μm2、10μm2、11μm2、12μm2、13μm2、15μm2、16μ
m2、17μm2、18μm2、20μm2、22μm2、25μm2、26μm2、27μm2、28μm2、29μm2Or 30 μm2。
Preferably, the height of the micron cylinder is 0-30 μm, such as can be 0.1 μm, 1 μm, 2 μm, 3 μm, 4 μm, 5 μ
M, 6 μm, 8 μm, 10 μm, 12 μm, 15 μm, 16 μm, 18 μm, 20 μm, 22 μm, 25 μm, 26 μm, 28 μm or 30 μm.
Preferably, the floor space of nanostructure is too small in process, in view of ICP processing characteristic, while also resulting in and receiving
Rice structure height is smaller, lowers the infrared absorption effect of nanostructure；Nanostructure floor space is excessive, then will affect nanostructure
Size and density, also will affect infrared absorption effect, the bottom surface cross-sectional area of the nanostructure is 0.01-4 μm2, such as
It can be 0.01 μm2、0.02μm2、0.05μm2、0.06μm2、0.08μm2、0.1μm2、0.2μm2、0.3μm2、0.5μm2、0.6μ
m2、0.8μm2、1μm2、2μm2、3μm2Or 4 μm2。
Preferably, the too small SPhP of the height of the nanostructure cannot be excited effectively, then will affect infrared absorption effect, from
And seriously affect the use of the structure；The height of nanostructure is excessive, and plated film and etch period lengthen, and quicklys increase cost, institute
The height for stating nanostructure is 1-10 μm, such as can be 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm or 10 μm.
Second aspect, the present invention also provides a kind of method for preparing micro-nano array structure as described in relation to the first aspect,
Include the following steps:
(1) the spin coating ultraviolet photoresist in silicon carbide substrate toasts after spin coating, after reusing the exposure of ultraviolet photolithographic machine,
Develop in developer solution；
(2) it removes photoresist after the copper facing of deposited by electron beam evaporation plated film instrument, preferably removes photoresist in acetone；
(3) reactive ion etching is used, columnar arrays structure is transferred in silicon carbide substrate；
(4) deposited by electron beam evaporation plated film instrument copper facing, then with reactive ion etching, obtain carbonization silicon micro-nano array structure.
Preferably, silicon carbide substrate described in step (1) with a thickness of 100-400 μm, such as can be 100 μm, 150 μ
m、200μm、220μm、230μm、250μm、260μm、270μm、280μm、290μm、300μm、310μm、320μm、330μm、340
μm, 350 μm, 360 μm, 370 μm, 380 μm, 390 μm or 400 μm, preferably 200-350 μm.
Preferably, ultraviolet photoresist described in step (1) is with a thickness of 0.2-5 μm, such as can be 0.2 μm, 0.4 μm, 0.6
μm, 0.8 μm, 1 μm, 2 μm, 3 μm, 4 μm or 5 μm, preferably 2 μm.
Preferably, the time of step (1) described baking be 1-8min, such as can be 1min, 2min, 3min, 4min,
5min, 6min, 7min or 8min.
Preferably, the time for exposure described in step (1) be 20-50s, such as can be 20s, 21s, 22s, 23s, 24s, 25s,
26s, 27s, 28s, 29s, 30s, 31s, 32s, 33s, 35s, 36s, 38s, 40s, 42s, 45s, 46s, 48s or 50s, preferably 30-45s.
Preferably, developing time described in step (1) be 20-50s, such as can be 20s, 21s, 22s, 23s, 24s, 25s,
26s, 27s, 28s, 29s, 30s, 31s, 32s, 33s, 35s, 36s, 38s, 40s, 42s, 45s, 46s, 48s or 50s, preferably 30-45s.
Preferably, copper facing described in step (2) is with a thickness of 330-480nm, for example, can be 330nm, 340nm, 350nm,
360nm, 380nm, 390nm, 400nm, 420nm, 430nm, 440nm, 450nm, 460nm or 480nm.
Preferably, copper facing described in step (4) is with a thickness of 220-400nm, for example, can be 220nm, 230nm, 240nm,
250nm, 260nm, 280nm, 290nm, 300nm, 310nm, 320nm, 330nm, 340nm, 350nm, 360nm, 380nm or 400nm.
Preferably, etch period described in step (4) be 20-50min, such as can be 20min, 21min, 22min,
23min、24min、25min、26min、27min、28min、29min、30min、31min、32min、33min、35min、
36min, 38min, 40min, 42min, 45min, 46min, 48min or 50min, preferably 30-45min.
The third aspect, the present invention also provides a kind of applications of micro-nano array structure as described in relation to the first aspect, use
Infrared incident light irradiation carbonization silicon micro-nano array structure surface, realizes the absorption of infrared broad spectrum.
Preferably, there are the wave bands of optical phonon for the infrared incident light covering silicon carbide substrate.
Preferably, the irradiating angle of the infrared incident light be 0-90 °, such as can be 0 °, 1 °, 2 °, 3 °, 5 °, 6 °,
8°、10°、12°、14°、15°、16°、18°、20°、23°、25°、26°、28°、30°、35°、40°、45°、50°、55°、60°、
65 °, 70 °, 75 °, 80 °, 85 ° or 90 °.
In the present invention, 0 ° of expression vertical incidence of irradiating angle of infrared incident light, infrared incident light shines micro-nano array
Body structure surface has excited SPhP, realizes that 10-13 μm of wide spectrum fully absorbs.
Compared with prior art, the invention has the following beneficial effects:
(1) the micro-nano array structure of the present invention, micron cylinder and nanostructure are not limited by shape, pass through the two
Synergistic effect realizes surface phonon-polaritons and electromagnetic wave phase mutual coupling, to realize infrared broad spectrum absorption；
(2) the middle infrared broad spectrum that the present invention realizes 10-13 μm absorbs, and absorptance is almost 1；
(3) substrate of the present invention is single silicon carbide substrate, and material is simple, and operating procedure is single, and micro nano structure
Easy to process, price is relatively cheap, using equipment such as ultraviolet photolithographics, avoids using electron beam lithography and focused-ion-beam lithography,
It reduces costs, it can be achieved that large area rapid processing, has paved road for practical application.
Detailed description of the invention
Fig. 1 is the micro-nano array structure schematic diagram of the invention processed on silicon carbide structure.
Fig. 2 is the micro-nano array structure scanning electron microscope (SEM) photograph of the embodiment of the present invention 1, wherein the line of box composition is described
The FDTD software simulation gained infrared absorption spectrum of structure, solid line is infrared absorption spectrum obtained by the experiment of the structure.
Fig. 3 is the micro-nano array structure schematic diagram of the embodiment of the present invention 2, wherein solid black lines are the structures
FDTD software simulation gained infrared absorption spectrum.
Fig. 4 is the micro-nano array structure schematic diagram of the embodiment of the present invention 3, wherein solid black lines are the structures
FDTD software simulation gained infrared absorption spectrum.
Fig. 5 is the micro-nano array structure schematic diagram of the embodiment of the present invention 4, wherein solid black lines are the structures
FDTD software simulation gained infrared absorption spectrum.
Specific embodiment
Further to illustrate technological means and its effect adopted by the present invention, below in conjunction with attached drawing and by specific real
Mode to further illustrate the technical scheme of the present invention is applied, but the present invention is not limited in scope of embodiments.
Experimental material:
Ultraviolet photoresist S1813 type
Experiment equipment:
Ultraviolet photolithographic machine MA6
Electron beam evaporation deposition instrument OHMIKER-50B
Reactive ion etching SENTECH PTSA ICP-RIE ETCHER SI 500
Embodiment 1
Micro-nano array structure is prepared, is included the following steps:
(1) in the silicon carbide substrate of 330 μ m-thicks 2 μ m-thick of spin coating ultraviolet photoresist, toast 5min after spin coating, reuse
After ultraviolet photolithographic machine exposes 40s, develop 40s in developer solution；
(2) it after deposited by electron beam evaporation plated film instrument plating 400nm copper, puts and removes photoresist in acetone；
(3) reactive ion etching is utilized, columnar arrays structure is transferred in silicon carbide substrate, it is accurate to control micron cylinder
Structure height；
(4) deposited by electron beam evaporation plated film instrument plates 300nm copper again, recycles reactive ion etching 40min, obtains micro-nano knot
Structure.
The micro-nano array structure being prepared is as shown in Fig. 2, micron cylinder is cylinder, and the period is 8 μm, and diameter is 6 μm,
Height is 8.75 μm；Carbonization silicon micro-nano array structure is nanocone, and bottom surface cross-sectional area is 0.01-4 μm2, it is highly 1-7 μ
m.Experiment and analog result meet preferably, in 10-13 μm or so wave band absorptance close to 100%.
Embodiment 2
The preparation method is the same as that of Example 1, and the micro-nano array structure being prepared is as shown in figure 3, micron cylinder is square column, week
Phase is 6 μm, and it is highly 14 μm that side length, which is 4 μm,；Nanostructure is nanocone, and bottom surface cross-sectional area is 0.04-4 μm2, highly it is
2-8μm.It is greater than 80% in 10-13 μm or so wave band absorptance.
Embodiment 3
The preparation method is the same as that of Example 1, and the micro-nano array structure being prepared is as shown in figure 4, micron cylinder is octagon
Column, period are 6 μm, and cross section column is made of two cuboid intersections, and a length of 4 μm of each cuboid, width is 1.657 μm, height
It is 8.5 μm；Nanostructure is nanocone, and bottom surface cross-sectional area is 0.04-4 μm2, it is highly 2-8 μm.In 10-13 μm or so wave
Section absorptance is greater than 85%.
Embodiment 4
The preparation method is the same as that of Example 1, and the micro-nano array structure being prepared is as shown in figure 4, micron cylinder is decagon
Column, period are 6 μm, and cross section column is made of two cuboid intersections, and a length of 4 μm of each cuboid, width is 1.657 μm, height
It is 8.5 μm；Nanostructure is nanocone, and bottom surface cross-sectional area is 0.04-4 μm2, it is highly 2-8 μm.In 10-13 μm or so wave
Section absorptance is greater than 85%.
Integrated embodiment 1-4, micron cylinder of the invention are not limited by shape, can be cylinder, square column, polygon column
Body；Nanostructure is not limited by shape, can be nano particle, nanometer pinpoint and nanometer centrum；The present invention realizes 10-13 μm
Middle infrared broad spectrum absorb, absorptance is almost 1；Substrate of the present invention is single silicon carbide substrate, and material is simple, operation step
It is rapid single, and nanostructure is easy to process, and price is relatively easy, using equipment such as ultraviolet photolithographics, avoids using electron beam light
Quarter and focused-ion-beam lithography reduce costs, it can be achieved that large area rapid processing, has paved road for practical application.
The Applicant declares that the present invention is explained by the above embodiments method detailed of the invention, but the present invention not office
Be limited to above-mentioned method detailed, that is, do not mean that the invention must rely on the above detailed methods to implement.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., all of which fall within the scope of protection and disclosure of the present invention.
Claims (22)
1. a kind of micro-nano array structure, which is characterized in that the structure includes silicon carbide substrate, in the silicon carbide substrate
Micron cylinder and nanostructure in the silicon carbide substrate and micron cylinder upper surface, the silicon carbide substrate be
There are the silicon carbide of Surface polaritons；
Wherein, the cross-sectional area of the micron cylinder is 4-30 μm2, the height of the micron cylinder is 0-30 μm, the nano junction
The bottom surface cross-sectional area of structure is 0.01-4 μm2, the height of the nanostructure is 1-10 μm, and the micron cylinder is period battle array
Column, period are 5-15 μm.
2. micro-nano array structure according to claim 1, which is characterized in that the micron cylinder is cylinder or polygon
Any one in shape column structure.
3. micro-nano array structure according to claim 1, which is characterized in that the nanostructure is nano particle or receives
Rice cone in any one.
4. micro-nano array structure according to claim 1, which is characterized in that the nanostructure is material of the same race with substrate
Material.
5. a kind of prepare the method such as micro-nano array structure of any of claims 1-4, which is characterized in that including
Following steps:
(1) the spin coating ultraviolet photoresist in silicon carbide substrate toasts after spin coating, after reusing the exposure of ultraviolet photolithographic machine, is developing
Develop in liquid；
(2) it removes photoresist after the copper facing of deposited by electron beam evaporation plated film instrument；
(3) reactive ion etching is used, columnar arrays structure is transferred in silicon carbide substrate；
(4) deposited by electron beam evaporation plated film instrument copper facing, then with reactive ion etching, obtain carbonization silicon micro-nano array structure.
6. according to the method described in claim 5, it is characterized in that, described remove photoresist of step (1) carries out in acetone.
7. according to the method described in claim 5, it is characterized in that, silicon carbide substrate described in step (1) with a thickness of 100-
400μm。
8. the method according to the description of claim 7 is characterized in that silicon carbide substrate described in step (1) with a thickness of 200-
350μm。
9. according to the method described in claim 5, it is characterized in that, ultraviolet photoresist described in step (1) is with a thickness of 0.2-5 μ
m。
10. according to the method described in claim 9, it is characterized in that, ultraviolet photoresist described in step (1) is with a thickness of 2 μm.
11. according to the method described in claim 5, it is characterized in that, the time of step (1) described baking is 1-8min.
12. according to the method described in claim 5, it is characterized in that, the time for exposure described in step (1) is 20-50s.
13. according to the method for claim 12, which is characterized in that the time for exposure described in step (1) is 30-45s.
14. according to the method described in claim 5, it is characterized in that, developing time described in step (1) is 20-50s.
15. according to the method for claim 14, which is characterized in that developing time described in step (1) is 30-45s.
16. according to the method described in claim 5, it is characterized in that, copper facing described in step (2) is with a thickness of 330-480nm.
17. according to the method described in claim 5, it is characterized in that, copper facing described in step (4) is with a thickness of 220-400nm.
18. according to the method described in claim 5, it is characterized in that, etch period described in step (4) is 20-50min.
19. according to the method for claim 18, which is characterized in that etch period described in step (4) is 30-45min.
20. a kind of application of such as micro-nano array structure of any of claims 1-4, which is characterized in that using red
Outer incident light irradiation carbonization silicon micro-nano array structure surface, realizes the absorption of infrared broad spectrum.
21. application according to claim 20, which is characterized in that there are light for the infrared incident light covering silicon carbide substrate
Learn the wave band of phonon.
22. application according to claim 20, which is characterized in that the irradiating angle of the infrared incident light is 0-90 °.
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| CN108535967A (en) * | 2018-03-26 | 2018-09-14 | 太原理工大学 | A kind of preparation method of polymer nanocomposite column array |
| CN110007381A (en) * | 2019-01-22 | 2019-07-12 | 西北工业大学 | A kind of visible light broadband absorption device and preparation method thereof |
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| US20130298977A1 (en) * | 2010-11-01 | 2013-11-14 | Yi Chen | Method of forming an array of nanostructures |
| CN103086319A (en) * | 2013-01-16 | 2013-05-08 | 西安交通大学 | Induction preparation process for electric field with dry adhesion type two-level structure |
| CN103199004A (en) * | 2013-02-22 | 2013-07-10 | 国家纳米科学中心 | Manufacturing method of III-group nitride nano-structure |
| CN104022186A (en) * | 2014-06-19 | 2014-09-03 | 电子科技大学 | Method for manufacturing black silicon material for enhancing infrared absorption |
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