CN113497361B - Patterned SiC microstructure and application thereof - Google Patents
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- CN113497361B CN113497361B CN202110768585.1A CN202110768585A CN113497361B CN 113497361 B CN113497361 B CN 113497361B CN 202110768585 A CN202110768585 A CN 202110768585A CN 113497361 B CN113497361 B CN 113497361B
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- 239000011358 absorbing material Substances 0.000 claims abstract description 28
- 239000010931 gold Substances 0.000 claims abstract description 27
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052737 gold Inorganic materials 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 229920002396 Polyurea Polymers 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 4
- 239000002070 nanowire Substances 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 3
- 230000000737 periodic effect Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 235000012431 wafers Nutrition 0.000 description 14
- 238000000862 absorption spectrum Methods 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 9
- 230000010287 polarization Effects 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000000197 pyrolysis Methods 0.000 description 5
- 239000006096 absorbing agent Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 3
- 238000003491 array Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000004088 simulation Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
- H01Q17/008—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems with a particular shape
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/28—Investigating the spectrum
- G01J3/42—Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry
Abstract
The invention relates to a patterned SiC microstructure and application thereof. The patterned SiC micro-structure is an SiC nanoneedle array grown on a patterned gold film on a 6H-SiC wafer substrate, the nanoneedles being perpendicular to the surface of the gold film, with a tapered bamboo-like geometry and sharp tips. The length of the nanoneedle is 0.1-100 μm, the diameter of the root is about 180nm, and the diameter of the tip is about 10nm. The patterned SiC microstructure is used as a terahertz wave absorbing material. The terahertz wave absorbing material with the patterned SiC microstructure has enhanced wave absorbing performance and is insensitive to an incident angle.
Description
Technical Field
The invention relates to a SiC terahertz wave absorbing material and application thereof, in particular to a patterned SiC microstructure and application thereof.
Background
Terahertz technology has rapid development and application in nondestructive testing, security, communication and induction. The application not only needs a high-efficiency terahertz source and a high-sensitivity filtering detector, but also needs a broadband terahertz wave absorbing material with high absorption efficiency and smaller size. In recent years, as an artificial structure, a metamaterial absorber has the advantages of high absorption efficiency, thickness of a sub-wavelength scale, adjustable electromagnetic resonance response and the like, and becomes a research hot spot. At present, most metamaterial wave absorbers commonly adopt a metal-medium-metal microstructure array, and although the metamaterial wave absorbers have perfect absorption, the absorption bandwidth is generally narrow, so that the wave absorbing application of the metamaterial wave absorbers is greatly limited.
In order to realize a broadband wave-absorbing metamaterial device, one method is to introduce a plurality of resonance units in a plane so as to realize a plurality of resonance peaks. However, the number of resonant cells that can be integrated in a plane is limited, and thus this approach often does not significantly extend the operating bandwidth. The other method is that a plurality of resonance units with gradually changed sizes are vertically overlapped into a pyramid-shaped, step-shaped or conical metal-medium multilayer film stacking structure, so that the number of the integrated resonance units is broken through, and the expansion of the working bandwidth is realized. However, such materials significantly increase the difficulty of practical preparation due to the large number of required membrane structures and the complex structure.
Disclosure of Invention
Aiming at the problems existing in the background technology, the invention aims to provide a patterned SiC microstructure with simple preparation characteristics and broadband terahertz wave absorbing performance.
The aim of the invention can be achieved by the following technical scheme: a patterned SiC micro-structure is a SiC nanoneedle array vertically grown on the surface of a patterned gold film on a 6H-SiC wafer substrate. The length of the nano needle in the SiC nano needle array is 0.1-100 mu m, the diameter of the root is about 200nm, and the diameter of the tip is about 10nm.
The SiC nanoneedle with the SiC microstructure has tapered bamboo-like geometric shape and tip, and is obviously different from nanobelts, nanowires and the like in morphology. Among these features, the tapered bamboo-like or bamboo-shaped nanoneedle structure is more advantageous for improving the terahertz wave absorbing performance.
In the SiC microstructure, the patterned gold film is a geometric pattern of n×n periodic arrangement, and the geometric pattern is consistent with the hollowed-out portion of the mask.
In the above-described SiC microstructure, the phase component of the nanoneedle is 3c—sic.
In the SiC microstructure described above, the nanoneedle has a single crystal structure.
The preparation method of the patterned SiC microstructure comprises the following steps: : (1) Depositing a 6H-SiC wafer substrate in vacuum by using a mask to obtain a patterned Au film with the thickness of 50-200 nm, wherein the Au film is used as a catalyst for growing a SiC nanowire array; (2) The SiC wafer covered with gold film was placed on polyurea silazane powder and placed in a vacuum oven at 10 -4 Heating the furnace to 1400-1500 ℃ at a speed of 20-40 ℃/min under the vacuum of Pa magnitude for pyrolysis, and then cooling the furnace to the ambient temperature along with the furnace to obtain the patterned SiC microstructure.
In the SiC microstructure described above, the polyurea silazane powder may be other organic precursors containing Si and C elements, and polyurea silazane is most preferable.
Another object of the invention is to provide the use of a patterned SiC microstructure as a terahertz wave-absorbing material.
In the application of the patterned SiC microstructure, the patterned SiC microstructure on the multi-resonance unit terahertz wave absorbing unit formed by the patterned gold film and the 6H-SiC wafer substrate can effectively broaden the working bandwidth of terahertz wave absorbing and is insensitive to the incident angle.
Compared with the prior art, the invention has the following advantages:
1. the preparation method of the terahertz wave absorbing material with the patterned SiC microstructure is realized.
2. The terahertz wave absorbing material with the patterned SiC microstructure prepared by the invention can effectively broaden the working bandwidth of a simple terahertz wave absorbing unit with multiple resonance units, and meanwhile, the preparation method is simple and convenient.
3. The terahertz wave absorbing material with the patterned SiC microstructure prepared by the invention is insensitive to the incidence angle of terahertz waves.
Drawings
FIG. 1 is a top view of a low-power Scanning Electron Microscope (SEM) of a patterned SiC microstructured terahertz wave absorbing material of the present invention;
fig. 2 is a schematic diagram showing a unit structure of the patterned SiC microstructure terahertz wave absorbing material of the present invention;
FIG. 3 is a high power electron microscope image of a nanoneedle of the patterned SiC microstructure terahertz wave absorbing material of the invention; wherein (A) is a typical TEM image of a single SiC nanoneedle, (B) is an A-area TEM image in (A), the SiC nanoneedle is displayed to be in a tapered bamboo joint structure, (C) is a typical TEM image of the tip of the SiC nanoneedle, and (D) is a typical SEM image of the SiC nanoneedle array;
fig. 4 is a terahertz wave absorption spectrum of the present invention in different structures under normal incidence; the solid line represents the actual measurement terahertz absorption spectrum of the whole structure, and the dotted line represents the simulation terahertz wave absorption spectrum of the structure without the SiC nanoneedle;
FIG. 5 is a graph showing the actual measurement absorption spectrum of terahertz wave by the change of the incident angle of a terahertz source with TE polarization oblique incidence;
FIG. 6 is a graph showing the actual measurement absorption spectrum of the terahertz wave by the change of the incident angle of the terahertz source with the TM polarization oblique incidence;
in the figure: 1. SiC nanoneedle array, 2, patterned gold film, 3, 6H-SiC wafer substrate.
Detailed Description
The following are specific embodiments of the present invention, and the technical solutions of the present invention will be further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
Example 1
The embodiment provides a patterned SiC micro-structure, wherein the SiC micro-structure is a SiC nano-needle array 1 vertically grown on the surface of a patterned gold film 2, nano-needles in the SiC nano-needle array have tapered bamboo-like geometric shapes and tips, the length of the nano-needles is 0.1-100 mu m, the diameter of the nano-needles is 10-200nm, the diameter of the tips is 10nm, the SiC micro-structure is of a single crystal structure, the phase components are 3C-SiC, the top ends of the SiC micro-structure are not provided with catalyst particles, and the top ends of the SiC micro-needles are not provided with (gold) catalyst particles, so that terahertz wave absorption is facilitated; the patterned gold film 2 is in n×n periodic geometrical patterns, and the geometrical patterns are consistent with the hollowed-out parts of the mask.
Referring to fig. 2, a schematic perspective view of a unit structure of the prepared patterned SiC microstructure terahertz wave absorbing material is shown.
The embodiment provides a method for preparing a patterned SiC microstructure, which comprises the following steps:
(1) Depositing a 6H-SiC wafer substrate 3 in vacuum by using a mask to obtain a patterned Au film with the thickness of 50-200 and nm, wherein the Au film is used as a catalyst for growing a SiC nanowire array;
(2) The SiC wafer covered with gold film was placed on polyurea silazane powder and placed in a vacuum oven at 10 -4 Heating the furnace to 1400-1500 ℃ at a speed of 20-40 ℃/min under the vacuum of Pa magnitude, and then cooling to the ambient temperature along with the furnace to obtain the patterned SiC microstructure.
The thickness of the 6H-SiC wafer substrate 3 is 3-50 μm.
The present embodiment provides the application of a patterned SiC microstructure as a terahertz wave-absorbing material. The patterned SiC microstructure terahertz wave absorbing material can effectively broaden the working bandwidth of a simple multi-resonance unit terahertz wave absorbing unit, and is insensitive to the incidence angle of terahertz waves.
Example 2
This example provides a patterned SiC microstructure fabrication method,
(1) Depositing a 5 mu m 6H-SiC wafer substrate in vacuum by using a mask to obtain a 50 nm-thick patterned Au film, wherein the Au film pattern is a circle which is uniformly and orthogonally distributed along a 45-degree axis symmetry on the 6H-SiC wafer substrate with a period of 60 mu m, and the diameters of the circles are 28 mu m and 20 mu m respectively;
(2) In a high purity alumina crucible, a gold film-covered SiC wafer was placed on polyurea silazane powder and covered with graphite paper, the crucible was placed in a vacuum furnace, at 10 -4 And heating the furnace to 1500 ℃ at a speed of 30 ℃/min under vacuum of Pa magnitude for pyrolysis, and then cooling the furnace to the ambient temperature along with the furnace to obtain the patterned SiC microstructure terahertz wave absorbing material.
The patterned SiC microstructure terahertz wave absorbing material prepared in example 2 is placed on a metal substrate for testing the absorbing performance, and the test results are shown in the figure.
Fig. 1 is a top view of a low-power Scanning Electron Microscope (SEM) of the patterned SiC microstructure terahertz wave absorbing material prepared in example 1. The SiC nanoneedle is fully distributed on the surface of the patterned Au film and has higher arrangement density.
Fig. 3 is a Transmission Electron Microscope (TEM) image of a nanoneedle of the patterned SiC microstructure terahertz wave absorbing material prepared in example 1. The prepared SiC nano needle structure is 10-60 mu m long, presents a novel tapered bamboo-like geometry and a sharp clean tip, the diameter of the root of the nano needle is about 180nm, and the diameter of the tip of the needle is about 10nm.
The terahertz wave absorbing material with the patterned SiC microstructure prepared in the embodiment 2 is measured on a terahertz time-domain spectrometer, and compared with a simulated wave absorbing spectrum of a structure with the SiC nanoneedle removed, the terahertz wave absorbing material with the patterned SiC microstructure has excellent terahertz broadband absorbing performance. Referring to fig. 4, terahertz wave absorption spectra of different structures under normal incidence; the solid line represents the actual measurement terahertz absorption spectrum of the whole structure, and the dotted line represents the simulation terahertz wave absorption spectrum of the structure without the SiC nanoneedle;
the patterned SiC microstructure terahertz wave absorbing material prepared in example 2 is used for measuring the absorption spectra of different polarizations and incidence angles on a terahertz time-domain spectrometer, which shows that the material is insensitive to the polarizations and incidence angles. Referring to fig. 5-6, the influence of the incident angle change of the terahertz source with TE polarization oblique incidence and TM polarization oblique incidence on the actual measurement absorption spectrum of the terahertz wave is shown.
In the embodiment of preparing the patterned SiC microstructure terahertz wave absorbing material and the alternative solution thereof, the pattern of the Au film may also be a top metal layer of other multi-resonant metal-dielectric-metal microstructure arrays, for example, other wafers with different sizes, other square pieces with different sizes, other cross pieces with different sizes, and the like.
In the preparation embodiment and the alternative scheme of the patterned SiC microstructure terahertz wave absorbing material, the thickness of the 6H-SiC wafer substrate and the like can be other sizes ranging from 3 μm to 50 μm except 40 μm, and the patterned SiC microstructure terahertz wave absorbing material can be obtained by performing simulation optimization design on the resonance wave absorbing performance through patterns of an Au film.
In the preparation embodiment and the alternative scheme of the patterned SiC microstructure terahertz wave absorbing material, the pyrolysis temperature may also be 1400 ℃, 1410 ℃, 1420 ℃, 1430 ℃, 1440 ℃, 1460 ℃, 1470 ℃, 1480 ℃, 1490 ℃, 1500 ℃.
In the above-described preparation embodiment of the patterned SiC microstructure terahertz wave absorbing material and the alternative scheme thereof,
the heating rate of the pyrolysis can also be 20 ℃/min, 22 ℃/min, 23 ℃/min, 24 ℃/min, 25 ℃/min, 26 ℃/min, 27 ℃/min, 28 ℃/min, 29 ℃/min, 31 ℃/min, 32 ℃/min, 33 ℃/min, 34 ℃/min, 35 ℃/min, 36 ℃/min, 37 ℃/min, 38 ℃/min, 39 ℃/min, 40 ℃/min.
The micro-structures of the SiC nanoneedle arrays with different average lengths and arrangement densities are obtained through different pyrolysis temperatures and heating rates, the micro-structures have good impedance matching and loss performance on terahertz waves in corresponding frequency bands, and the micro-structures can be optimized and controlled through the micro-structures of the SiC nanoneedle arrays, such as the average lengths, and the like, when the micro-structures are compounded with multi-resonance terahertz narrow-band wave absorbing meta-materials composed of different patterned gold films and 6H-SiC wafer substrates, the terahertz broadband wave absorbing performance can be obtained.
In view of the numerous embodiments of the preparation scheme of the patterned SiC microstructure terahertz wave absorbing material, experimental data of each embodiment are huge and are not suitable for one-by-one listing and explanation here, but the content of verification needed by each embodiment and the obtained final conclusion are close, so that the verification content of each embodiment is not described one-by-one here, and only the embodiment 1 is taken as a representative for explaining the excellent point of the application of the invention.
The present examples are not exhaustive of the values of the points in the technical scope of the present invention, and are also within the scope of the present invention.
The specific embodiments described herein are offered by way of example only to illustrate the spirit of the invention. Various modifications or additions to the described embodiments may be made by those skilled in the art to which the invention pertains or may be substituted in a similar manner without departing from the spirit of the invention or beyond the scope of the appended claims.
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
Claims (6)
1. The patterned SiC micro-structure is characterized by being a SiC nano needle array vertically grown on the surface of a patterned gold film, wherein nano needles in the SiC nano needle array have tapered bamboo-like geometric shapes and tips, the length of each nano needle is 0.1-100 mu m, the diameter is 10-200nm, and the diameter of each tip is 10nm.
2. A patterned SiC microstructure according to claim 1, in which the SiC microstructure is a single crystal structure and the phase composition is 3C-SiC.
3. The patterned SiC microstructure of claim 1, in which the patterned gold film is a geometric pattern of periodic n x n arrangement, the geometric pattern being consistent with the mask hollowed-out portion.
4. A method of making a patterned SiC microstructure according to any one of claims 1 to 3, comprising the steps of:
(1) Depositing a 6H-SiC wafer substrate in vacuum by using a mask to obtain a patterned Au film with the thickness of 50-200 nm, wherein the Au film is used as a catalyst for growing a SiC nanowire array;
(2) The SiC wafer covered with gold film was placed on polyurea silazane powder and placed in a vacuum oven at 10 -4 Heating the furnace to 1400-1500 ℃ at a speed of 20-40 ℃/min under the vacuum of Pa magnitude, and then cooling to the ambient temperature along with the furnace to obtain the patterned SiC microstructure.
5. The method of producing a patterned SiC microstructure according to claim 4, wherein the thickness of the 6H-SiC wafer substrate is 3 to 50 μm.
6. Use of a patterned SiC microstructure according to any of claims 1 to 3 as a terahertz wave-absorbing material.
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