CN114293237A - 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 PDFInfo
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Abstract
The invention discloses a preparation method of a one-dimensional topological photonic crystal based on porous alumina, which is characterized in that a group of layered symmetrical photonic crystal structures are prepared by periodically changing anodic oxidation voltage, and excitation of a topological state of the one-dimensional photonic crystal is realized. 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 avoids a series of defects of using a large amount of toxic reagents, complicated regulation and control steps, overlong time required by regulation and control 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
Technical Field
The invention relates to the fields of topological photonics, condensed state physics and photonic crystals.
Background
Topological states, such as topological insulators, topological semi-metals, etc., are very popular research directions in condensed state physics, and possess many excellent properties, including unidirectional transport, chiral anomalies, etc. In recent years, the concept of topology has been introduced into photonic systems, resulting in many new optical phenomena, such as topological phase transitions, optical quantum hall effects, and the like. The photon topological structure has good application prospect in the aspects of sensing, lasers and filters. The method for constructing the topological photonic mode comprises an optical waveguide, a plasma nano particle, a one-dimensional photonic crystal, a two-dimensional photonic crystal, a three-dimensional photonic crystal and the like. Among them, the photonic crystal has great advantages in the control of light due to its unique photonic band gap and photonic local characteristics.
Photonic crystals are novel materials that use photons as information carriers. The concept of photonic crystals has been proposed and has been receiving wide attention from researchers at home and abroad. Photonic crystals are a promising area and a large number of photonic crystal optical devices have been proposed and applied successively to date. Photonic crystals exhibit unique advantages in optical communications, optical waveguides, integrated photonic devices, and the like. With the rapid development of photonic crystals and nanotechnology, the structural requirements for nanomaterials are also higher and higher, and not only in the morphology of the structure, but also the optical performance and 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 the current research. The method for preparing the one-dimensional photonic crystal comprises a deposition method, a spin coating method, a photoetching method, an electrochemical anode oxidation method 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 all be used to make photonic crystals. Among them, the Anodic Aluminum Oxide (AAO) is the most widely used of all porous anodic oxidation structures, and is also the most studied structure at home and abroad.
Disclosure of Invention
The invention aims to provide a novel anodic oxidation method for preparing a one-dimensional aluminum oxide photonic crystal with a topological state.
The invention is realized by the following technical scheme:
a preparation method of one-dimensional topological photonic crystals based on porous alumina is characterized by comprising the following steps: preparing porous alumina one-dimensional photonic crystals by adopting a variable voltage anodic oxidation method, and exciting a topological state at an interface by constructing a layered symmetrical photonic crystal structure; firstly, carrying out primary oxidation on an annealed aluminum sheet, then carrying out secondary oxidation, wherein the periodic voltage waveform of the secondary oxidation is designed to be t1 、t2 、t3 、t4；t1 、t2 、t3 To lower blood pressure, t4Boosting the pressure; and at t of the Nth period of the first stage of the secondary oxidation2Stopping when the section is finished, immediately starting a first period of a second stage of secondary oxidation, and then normally oxidizing each period of the rest second stage;
the preparation method of the one-dimensional topological photonic crystal based on porous alumina is characterized by comprising the following steps: the method comprises the following specific steps: the waveform diagram of one complete cycle of the periodic voltage of the secondary oxidation is as follows: t is t1=90s, the voltage drops linearly from 50V to 35.5V; t is t2=60s, the voltage drops linearly from 35.5V to 30V; t is t3The voltage of the time period is kept unchanged at 30V; t is t4=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 t3The 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: the method comprises the following specific steps:
(1) carrying out primary oxidation on the annealed aluminum sheet by using constant voltage;
(2) after the sample subjected to the primary oxidation in the step (1) is subjected to acid washing by using chromic acid phosphate, secondary oxidation is carried out by using a designed periodic voltage waveform, and t in the first period2Stopping when the section is finished, immediately starting the next period, and then normally oxidizing the rest periods;
(3) using CuCl2Removing the residual aluminum substrate on the back surface of the sample after the secondary oxidation in the step (2) by using the solution;
(4) and (4) measuring the transmission spectrum of the porous alumina template subjected to aluminum removal in the step (3) by using an ultraviolet spectrophotometer.
The primary oxidation voltage is 40V, and the oxidation time is 12 h.
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 primary oxidation is as follows: putting the annealed high-purity aluminum sheet into a container with 0.3 mol.L-1In the anodic oxidation electrolytic cell of oxalic acid solution, 40V direct current voltage is applied, and continuous oxidation is carried out for 12h 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 CuCl2The solution was 15% CuCl2And (3) solution.
The present invention anodizes a sample using a periodically varying oxidation voltage waveform. When the voltage value drops from the highest point to 1/√ 2 times the maximum value, the resulting cell channel will diverge. As the oxidation proceeds, a periodic layered structure of the straight-hole layer (a) -branched-hole layer (B) -straight-hole layer-branched-hole layer appears. If starting from a certain period, the structural arrangement changes from A-B-A-B to B-A-B-A, i.e. a structure symmetrical to the photonic crystal structure in the first half, having the same energy band but opposite topological properties, as shown in FIG. 1. A topological state can be excited at the interface between them. Preparation pairThe method of weighing the structure is to run to t in a period when the oxidation is performed to a half of the total period2When the process is finished, the current period is stopped and the voltage of the next period is started immediately, and then the second half part is finished by normal oxidation, as shown in figure 3, so that the symmetrical structure of A-B-B-A can be prepared. By adjusting parameters in the voltage waveform, the proportion of the bifurcation layer and the straight hole layer and the proportion of air in the photonic crystal can be changed, so that the effective refractive index of the photonic crystal is changed.
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 periodic layered structure is prepared by the periodically changed oxidation voltage to excite the topological state. The method is efficient, environment-friendly, pollution-free, low in cost and simple in process. The method has wide application in the fields of photonic devices, sensing and the like.
Drawings
FIG. 1 is a schematic diagram of a periodic straight-branched pore (A-B-B-A) structure of porous alumina;
FIG. 2 is a waveform of the periodic oxidation voltage for one full cycle in the present invention: t is t1=90s, the voltage drops linearly from 50V to 35.5V; t is t2=60s, the voltage drops linearly from 35.5V to 30V; t is t3The voltage of the time period is kept unchanged at 30V; t is t4=30s, the voltage rises sinusoidally from 30V to 50V;
FIG. 3 shows the operation of the present invention at voltage up to a certain period t2Stopping the current cycle at the end of the segment and immediately beginning to run the voltage waveform diagram for the next cycle, where T represents one cycle in fig. 2;
FIG. 4 is a scanning electron micrograph of a topological photonic crystal sample 1;
FIG. 5 is a transmitted light spectrum of the topological photonic crystal sample 1;
fig. 6 is a transmission spectrum of the topological photonic crystal sample 2.
Detailed Description
The technical solution of the present invention is further described below with reference to the specific embodiments. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available on the market.
The embodiment uses t3=60s, total oxidation period is 200, and operation is carried out from 101 th period to t2The sample which stops when the section is finished and immediately starts the next period is taken as an example, and through testing, the transmission spectrum of the sample has a more obvious transmission peak at a wavelength of 742nm, the half-peak width is 15nm, and the product description is met.
Waveform diagram of one complete cycle of the periodic voltage of the secondary oxidation: t is t1=90s, the voltage drops linearly from 50V to 35.5V; t is t2=60s, the voltage drops linearly from 35.5V to 30V; t is t3The voltage of the time period is kept unchanged at 30V; t is t4=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) ultrasonic cleaning 99.999% high-purity aluminum sheet in acetone, absolute ethyl alcohol and deionized water for 5 minutes respectively for degreasing, and annealing to eliminate internal mechanical stress;
(2) putting the high-purity aluminum sheet annealed in the step (1) into a container with 0.3 mol.L-1Applying 40V direct current voltage in an anodic oxidation electrolytic cell of oxalic acid solution, and continuously oxidizing for 12h under the condition of keeping constant temperature of 11 ℃;
(3) the sample in step (2) is subjected to acid washing with a phosphoric acid and then to secondary oxidation by using a periodic voltage shown in the attached figure 2, t3 For a time of 60s, the oxidation proceeds to t of the 101 th cycle2The end of the segment is stopped and the next cycle is started immediately, followed by the normal oxidation 100 cycles. Preparing a porous alumina template by a two-step anodic oxidation method;
(4) 15% of CuCl was used2Removing the residual aluminum substrate on the back surface 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 spectrophotometer;
through testing, the anodic aluminum oxide topological photonic crystal sample has 1-total oxidation period of 200, t3=60s, 101 th cycle t2End of segment stop-transmission peak 742nm, transmittance 60.4%, half-peak width 15 nm.
Anodic aluminum oxide rubbingPurphotonic crystal sample 2-Total Oxidation 200 period, t3=120s, 101 th cycle t2End of segment stop-transmission peak 674nm, transmission 61.8%, half-peak width 12 nm.
According to the embodiment of the invention, the preparation of the anodic aluminum oxide topological photonic crystal is realized through 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 parameter. The sample transmission peak wavelength range is between 650-750 nm. The prepared sample has a narrower transmission peak, and the half-peak width can reach 12nm at most.
Claims (7)
1. A preparation method of one-dimensional topological photonic crystals based on porous alumina is characterized by comprising the following steps: preparing porous alumina one-dimensional photonic crystals by adopting a variable voltage anodic oxidation method, and exciting a topological state at an interface by constructing a layered symmetrical photonic crystal structure; firstly, carrying out primary oxidation on an annealed aluminum sheet, then carrying out secondary oxidation, wherein the periodic voltage waveform of the secondary oxidation is designed to be t1 、t2 、t3 、t4；t1 、t2 、t3 To lower blood pressure, t4Boosting the pressure; and at t of the Nth period of the first stage of the secondary oxidation2Stopping at the end of the segment, then immediately starting the first cycle of the second stage of the secondary oxidation, and then normally oxidizing the rest of the second stage of each cycle.
2. The method for preparing one-dimensional topological photonic crystals based on porous alumina according to claim 1, characterized in that: the method comprises the following specific steps: the waveform diagram of one complete cycle of the periodic voltage of the secondary oxidation is as follows: t is t1=90s, the voltage drops linearly from 50V to 35.5V; t is t2=60s, the voltage drops linearly from 35.5V to 30V; t is t3The voltage of the time period is kept unchanged at 30V; t is t4=30s, the voltage rises sinusoidally from 30V to 50V.
3. The method of claim 2, wherein the one-dimensional anode is prepared by an anodic oxidation methodThe method for preparing the aluminum oxide topological photonic crystal is characterized by comprising the following steps: adjusting t3The time lengths are respectively 60s and 120s, and topological photonic crystal structures with different effective refractive indexes are prepared.
4. The method for preparing one-dimensional topological photonic crystals based on porous alumina according to claim 1, characterized in that: the method comprises the following specific steps:
(1) carrying out primary oxidation on the annealed aluminum sheet by using constant voltage;
(2) after the sample subjected to the primary oxidation in the step (1) is subjected to acid washing by using chromic acid phosphate, secondary oxidation is carried out by using a designed periodic voltage waveform, and t in the first period2Stopping when the section is finished, immediately starting the next period, and then normally oxidizing the rest periods;
(3) using CuCl2Removing the residual aluminum substrate on the back surface of the sample after the secondary oxidation in the step (2) by using the solution;
(4) and (4) measuring the transmission spectrum of the porous alumina template subjected to aluminum removal in the step (3) by using an ultraviolet spectrophotometer.
5. The method for preparing the one-dimensional anodic aluminum oxide topological photonic crystal based on the anodic oxidation method according to claim 4, characterized in that: in the step (1), the primary oxidation voltage is 40V, and the oxidation time is 12 h.
6. The method for preparing the one-dimensional anodic aluminum oxide topological photonic crystal based on the anodic oxidation method according to claim 1, which is characterized in that: the primary oxidation is as follows: putting the annealed high-purity aluminum sheet into a container with 0.3 mol.L-1In the anodic oxidation electrolytic cell of oxalic acid solution, 40V direct current voltage is applied, and continuous oxidation is carried out for 12h under the condition of keeping the constant temperature of 11 ℃.
7. The method for preparing the one-dimensional anodic aluminum oxide topological photonic crystal based on the anodic oxidation method according to claim 1, which is characterized in that: the CuCl2The solution was 15% CuCl2And (3) solution.
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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 |
| CN106226865A (en) * | 2016-09-06 | 2016-12-14 | 江苏大学 | Nanometer straight hole cyclic array preparation method in a kind of photonic crystal |
| CN109031519A (en) * | 2018-07-28 | 2018-12-18 | 中国地质大学（北京） | A kind of narrow-band optical filter and all-optical diode |
| CN109989086A (en) * | 2019-04-19 | 2019-07-09 | 河北工业大学 | A kind of preparation method of the porous aluminas photon crystal film with high saturation schemochrome |
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Patent Citations (8)
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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 |
| WO2003034113A2 (en) * | 2001-10-19 | 2003-04-24 | Nkt Research & Innovation A/S | Integrated photonic crystal structure and method of producing same |
| CN1752296A (en) * | 2005-06-08 | 2006-03-29 | 武汉大学 | Method for preparing aluminium oxide nano-form photon crystal |
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