CN114293237B - Preparation method of one-dimensional topological photonic crystal based on porous alumina - Google Patents

Preparation method of one-dimensional topological photonic crystal based on porous alumina Download PDF

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CN114293237B
CN114293237B CN202210002055.0A CN202210002055A CN114293237B CN 114293237 B CN114293237 B CN 114293237B CN 202210002055 A CN202210002055 A CN 202210002055A CN 114293237 B CN114293237 B CN 114293237B
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photonic crystal
oxidation
voltage
porous alumina
period
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CN114293237A (en
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张俊喜
王心宇
张维
胡志家
牛力捷
王晨
程锐
方峥
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Hefei University of Technology
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Hefei University of Technology
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Abstract

The invention discloses a preparation method of a one-dimensional topological photonic crystal based on porous alumina. The position of the transmission peak of the sample is regulated and controlled within a certain range by changing the parameter of the anodic oxidation voltage. The method provided by the invention avoids a series of defects of large use of toxic reagents, complex regulation and control steps, overlong regulation and control time and the like, and realizes the excitation of the topological state of the alumina one-dimensional photonic crystal in a green and efficient manner.

Description

Preparation method of one-dimensional topological photonic crystal based on porous alumina
Technical Field
The invention relates to the fields of topology photonics, condensed state physics and photonic crystal correlation.
Background
Topology, such as topology insulators, topology semi-metals, etc., are very popular research directions in the physics of coacervation, possessing many excellent properties including unidirectional transport, chiral anomalies, etc. In recent years, the concept of topology has been introduced into photonic systems, creating many new optical phenomena such as topological phase changes, optical quantum hall effects, etc. The photon topological structure has good application prospect in the aspects of sensing, lasers and filters. Methods of constructing topological photonic modes include optical waveguides, plasmonic nanoparticles, one-dimensional photonic crystals, two-dimensional photonic crystals, three-dimensional photonic crystals, and the like. Among them, photonic crystals have great advantages in light control due to their unique photonic band gap and photonic localization characteristics.
Photonic crystals are novel materials that use photons as information carriers. The concept of photonic crystals has been proposed and has been widely focused by researchers at home and abroad. Photonic crystals are a promising area, and a number of photonic crystal optical devices have been proposed and applied successively so far. Photonic crystals offer unique advantages in optical communications, optical waveguides, integrated photonic devices, and the like. With the rapid development of photonic crystals and nanotechnology, the requirements on the structure of the nano material are higher and higher, and not only the morphology of the structure, but also the optical performance and the controllability of the structure are more important.
The one-dimensional topological photonic crystal has a simple structure and is easy to prepare, and is the key point of current research. Methods for preparing the one-dimensional photonic crystal include deposition, spin coating, photolithography, electrochemical anodic oxidation, and the like. The anodic oxidation method has the advantages of simple process, low cost, strong controllability and the like. Anodic silicon oxide, aluminum and titanium can be used to prepare photonic crystals. Among them, anodic Aluminum Oxide (AAO) is the most widely used of all porous anodic oxidation structures, and is the most studied structure at home and abroad.
Disclosure of Invention
The invention aims to provide a method for preparing a one-dimensional alumina photonic crystal with a topological state by a novel anodic oxidation method.
The invention is realized by the following technical scheme:
a preparation method of a one-dimensional topological photonic crystal based on porous alumina is characterized by comprising the following steps: preparing a porous alumina one-dimensional photonic crystal by adopting a variable voltage anodic oxidation method, and exciting a topological state at an interface by constructing a layered symmetrical photonic crystal structure; specifically, firstly, oxidizing an annealed aluminum sheet once, then oxidizing the aluminum sheet twice, and designing a periodic voltage waveform of the secondary oxidation as t 1 、t 2 、t 3 、t 4 ;t 1 、t 2 、t 3 To reduce blood pressure, t 4 Boosting; and t of the N-th period in the first stage of the secondary oxidation 2 Stopping when the section is finished, immediately starting a first period of a second stage of secondary oxidation, and then finishing each period of the rest second stages of normal oxidation;
the preparation method of the one-dimensional topological photonic crystal based on porous alumina is characterized by comprising the following steps of: the method comprises the following specific steps: waveform diagram of a complete cycle of the secondary oxidized periodic voltage: t is t 1 =90 s, the voltage drops linearly from 50V to 35.5V; t is t 2 =60 s, the voltage drops linearly from 35.5V to 30V; t is t 3 The voltage is kept unchanged for 30V in the time period; t is t 4 =30s, the voltage rises sinusoidally from 30V to 50V.
The method for preparing the one-dimensional anodic aluminum oxide topological photonic crystal based on the anodic oxidation method is characterized by comprising the following steps of: adjusting t 3 The time lengths are respectively 60s and 120s, and topological photonic crystal structures with different effective refractive indexes are prepared.
The preparation method of the one-dimensional topological photonic crystal based on porous alumina is characterized by comprising the following steps of: the method comprises the following specific steps:
(1) Oxidizing the annealed aluminum sheet for the first time by using a constant voltage;
(2) Washing the sample subjected to the primary oxidation in the step (1) with phosphoric acid, performing secondary oxidation by using a designed periodic voltage waveform, and performing t in the first period 2 Stopping and immediately starting the next period when the segment is finished, and then finishing the rest periods normally;
(3) Using CuCl 2 Removing the residual aluminum substrate on the back of the sample subjected to the secondary oxidation in the step (2) by using the solution;
(4) And (3) measuring the transmission spectrum of the porous alumina template subjected to aluminum removal in the step (3) by using an ultraviolet spectrometer.
The primary oxidation voltage was 40V and the oxidation time was 12h.
The method for preparing the one-dimensional anodic aluminum oxide topological photonic crystal based on the anodic oxidation method is characterized by comprising the following steps of: the said processPrimary oxidation refers to: the annealed high-purity aluminum sheet was charged with 0.3 mol.L -1 In an anodic oxidation electrolytic tank of oxalic acid solution, a direct current voltage of 40V is applied, and continuous oxidation is carried out for 12 hours under the condition of keeping the constant temperature of 11 ℃.
The method for preparing the one-dimensional anodic aluminum oxide topological photonic crystal based on the anodic oxidation method is characterized by comprising the following steps of: the CuCl 2 15% CuCl solution 2 A solution.
The present invention uses a periodically varying oxidation voltage waveform to anodize a sample. When the voltage value drops from the highest point to 1/. V.2 times the maximum value, the formed cell will diverge. As oxidation proceeds, a periodic layered structure of the straight pore layer (a) -the branched pore layer (B) -the straight pore layer-the branched pore layer occurs. If starting from ase:Sub>A certain period, the structural arrangement changes from A-B-A-B to B-A-B-A, i.e. ase:Sub>A structure symmetrical to the first half of the photonic crystal structure, having the same energy band but opposite topological properties, as shown in FIG. 1. A topology can be excited at the interface between them. The symmetrical structure is prepared by, when oxidation proceeds to a period half of the total number of periods, running to t during this period 2 At the end, the current cycle is stopped and the voltage for the next cycle is immediately started, and then the second half of the normal oxidation is completed, as shown in fig. 3, so that the symmetrical structure of ase:Sub>A-B-ase:Sub>A can be prepared. By adjusting parameters in the voltage waveform, the ratio of the bifurcation layer to the straight hole layer and the air duty ratio in the photonic crystal can be changed, thereby changing the effective refractive index of the photonic crystal.
The invention has the advantages that: the invention provides a method for preparing an anodic aluminum oxide topological photonic crystal based on an anodic oxidation method. The topology is excited by preparing a periodic layered structure from a periodically varying oxidation voltage. The method is efficient, environment-friendly, pollution-free, low in cost and simple in process. The method has wide application in the fields of photon devices, sensing and the like.
Drawings
FIG. 1 is ase:Sub>A schematic diagram of ase:Sub>A periodic straight pore-forked pore (A-B-B-A) structure of porous aluminase:Sub>A;
FIG. 2 is a schematic illustration of the present inventionWaveform diagram of periodic oxidation voltage for one complete cycle: t is t 1 =90 s, the voltage drops linearly from 50V to 35.5V; t is t 2 =60 s, the voltage drops linearly from 35.5V to 30V; t is t 3 The voltage is kept unchanged for 30V in the time period; t is t 4 =30s, the voltage rises sinusoidally from 30V to 50V;
FIG. 3 shows the voltage during the period t 2 Stopping the current period and immediately starting to run the voltage waveform diagram of the next period when the segment is finished, wherein T represents one period in the diagram of FIG. 2;
FIG. 4 is a scanning electron microscope image of topological photonic crystal sample 1;
FIG. 5 is a transmission spectrum of topological photonic crystal sample 1;
fig. 6 is a transmission spectrum of topological photonic crystal sample 2.
Detailed Description
The technical scheme of the invention is further described below with reference to the specific embodiments. The reagents or apparatus used were conventional products available on the market without the manufacturer's attention.
The embodiment uses t 3 =60 s, total oxidation period 200, run to t in 101 th period 2 The sample of the next period is taken as an example when the section is stopped at the end and immediately started, and the transmission spectrum of the sample has a more obvious transmission peak at the wavelength of 742nm, and the half-peak width is 15nm, so that the sample meets the product description.
Waveform diagram of one complete cycle of the periodic voltage of the secondary oxidation: t is t 1 =90 s, the voltage drops linearly from 50V to 35.5V; t is t 2 =60 s, the voltage drops linearly from 35.5V to 30V; t is t 3 The voltage is kept unchanged for 30V in the time period; t is t 4 =30s, the voltage rises sinusoidally from 30V to 50V.
The preparation of the anodic aluminum oxide topological photonic crystal is realized according to the following steps:
(1) Ultrasonically cleaning 99.999% high-purity aluminum sheets in acetone, absolute ethyl alcohol and deionized water for 5 minutes respectively for degreasing, and annealing to eliminate internal mechanical stress;
(2) Placing the high-purity aluminum sheet annealed in the step (1) into a furnace with a concentration of 0.3 mol.L -1 Applying a direct current voltage of 40V in an anodic oxidation electrolytic tank of oxalic acid solution, and continuously oxidizing for 12 hours under the condition of keeping the constant temperature of 11 ℃;
(3) The sample from step (2) is subjected to a second oxidation after being subjected to a phosphoric acid pickling using the periodic voltage of FIG. 2, t 3 For 60s, oxidation proceeds to period t of 101 2 The segment ends, stops and immediately starts the next cycle, and then oxidizes normally for a further 100 cycles. Preparing a porous alumina template by a two-step anodic oxidation method;
(4) Using 15% CuCl 2 Removing the residual aluminum substrate on the back of the porous alumina template prepared in the step (3) by using the solution;
(5) Measuring the transmission spectrum of the porous alumina template subjected to aluminum removal in the step (4) by using an ultraviolet spectrometer;
through testing, an anodic aluminum oxide topological photonic crystal sample is subjected to 1-total oxidation for 200 cycles, t 3 =60 s, 101 st period t 2 Stop-transmission peak at end of segment 742nm, transmittance 60.4%, half-width 15nm.
Anodic aluminum oxide topological photonic crystal sample 2-total oxidation 200 period, t 3 =120s, 101 st period t 2 Stop-transmission peak at end of segment 674nm, transmittance 61.8%, half-width 12nm.
According to the method, the preparation of the anodic aluminum oxide topological photonic crystal is realized through the periodic voltage oxidation of different parameters and the introduction of a symmetrical structure, and the position of a transmission peak can be regulated and controlled within a certain range by changing the oxidation voltage parameters. The sample transmission peak wavelength ranges between 650-750 nm. The prepared sample has a narrower transmission peak, and the half-peak width can reach 12nm at the lowest.

Claims (6)

1. A preparation method of a one-dimensional topological photonic crystal based on porous alumina is characterized by comprising the following steps: preparing a porous alumina one-dimensional photonic crystal by adopting a variable voltage anodic oxidation method, and exciting a topological state at an interface by constructing a layered symmetrical photonic crystal structure; specifically, firstly, the annealed aluminum sheet is subjected to primary oxidation, then is subjected to secondary oxidation, and the secondary oxidation is carried outThe periodic voltage waveform is designed as t 1 、t 2 、t 3 、t 4 ;t 1 、t 2 、t 3 To reduce blood pressure, t 4 Boosting; and t of the N-th period in the first stage of the secondary oxidation 2 Stopping when the section is finished, immediately starting a first period of a second stage of secondary oxidation, and then finishing each period of the rest second stages of normal oxidation;
waveform diagram of a complete cycle of the secondary oxidized periodic voltage: t is t 1 =90 s, the voltage drops linearly from 50V to 35.5V; t is t 2 =60 s, the voltage drops linearly from 35.5V to 30V; t is t 3 The voltage is kept unchanged for 30V in the time period; t is t 4 =30s, the voltage rises sinusoidally from 30V to 50V.
2. The method for preparing the one-dimensional topological photonic crystal based on porous alumina according to claim 1, wherein the method comprises the following steps: adjusting t 3 The time lengths are respectively 60s and 120s, and topological photonic crystal structures with different effective refractive indexes are prepared.
3. The method for preparing the one-dimensional topological photonic crystal based on porous alumina according to claim 1, wherein the method comprises the following steps: the method comprises the following specific steps:
oxidizing the annealed aluminum sheet for the first time by using a constant voltage;
washing the sample subjected to the primary oxidation in the step (1) with phosphoric acid, performing secondary oxidation by using a designed periodic voltage waveform, and performing t in the first period 2 Stopping and immediately starting the next period when the segment is finished, and then finishing the rest periods normally;
using CuCl 2 Removing the residual aluminum substrate on the back of the sample subjected to the secondary oxidation in the step (2) by using the solution;
and (3) measuring the transmission spectrum of the porous alumina template subjected to aluminum removal in the step (3) by using an ultraviolet spectrometer.
4. A method for preparing a one-dimensional topological photonic crystal based on porous alumina according to claim 3, wherein the method comprises the following steps: the primary oxidation voltage in the step (1) is 40V, and the oxidation time is 12h.
5. The method for preparing the one-dimensional topological photonic crystal based on porous alumina according to claim 1, wherein the method comprises the following steps: the primary oxidation means: the annealed high-purity aluminum sheet was charged with 0.3 mol.L -1 In an anodic oxidation electrolytic tank of oxalic acid solution, a direct current voltage of 40V is applied, and continuous oxidation is carried out for 12 hours under the condition of keeping the constant temperature of 11 ℃.
6. A method for preparing a one-dimensional topological photonic crystal based on porous alumina according to claim 3, wherein the method comprises the following steps: the CuCl 2 15% CuCl solution 2 A solution.
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US5141603A (en) * 1988-03-28 1992-08-25 The United States Of America As Represented By The Secretary Of The Air Force Capacitor method for improved oxide dielectric
US7194174B2 (en) * 2001-10-19 2007-03-20 Ignis Technologies As Integrated photonic crystal structure and method of producing same
CN100381613C (en) * 2005-06-08 2008-04-16 武汉大学 Method for preparing aluminium oxide nano-form photon crystal
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CN103243368A (en) * 2013-03-28 2013-08-14 中国科学院化学研究所 Full-spectrum color-regulated two-dimensional photonic crystal structure design and porous alumina material-based preparation method
CN106226865B (en) * 2016-09-06 2019-02-05 江苏大学 Nanometer straight hole cyclic array preparation method in a kind of photonic crystal
CN109031519B (en) * 2018-07-28 2019-07-05 中国地质大学(北京) A kind of narrow-band optical filter and all-optical diode
CN109989086B (en) * 2019-04-19 2020-11-03 河北工业大学 Preparation method of porous alumina photonic crystal film with high-saturation structural color

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