CN114351236B - Full-color domain structural color encryption module and preparation method thereof - Google Patents
Full-color domain structural color encryption module and preparation method thereof Download PDFInfo
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- CN114351236B CN114351236B CN202111623154.2A CN202111623154A CN114351236B CN 114351236 B CN114351236 B CN 114351236B CN 202111623154 A CN202111623154 A CN 202111623154A CN 114351236 B CN114351236 B CN 114351236B
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Abstract
The invention provides a full-color domain structural color encryption module and a preparation method thereof, wherein the module is of a three-layer film structure, and an aluminum substrate is used as a reflecting layer and is positioned at the bottommost layer of the structural color module; the alumina film is used as a medium layer and is positioned in the middle of the structural color module; the noble metal layer is used as a decryption layer and is positioned at the uppermost layer of the structural color module; through adjusting the color difference between the thickness control information of the medium layer and the background, the color information is presented and hidden through the deposition and erasure of the noble metal layer, the short-range ordered nano structure of the AAO is beneficial to reducing the angle dependence of the color, and the characteristics of hardness and corrosion resistance of the AAO can improve the service life of the structural color module and realize the repeated use of the encryption module. The anodic aluminum oxide material adopted by the structural color module has higher hardness, corrosion resistance and wear resistance, can prolong the service life of the module to a limited extent, and can be reused after the sample repeatedly shows and erases information.
Description
Technical Field
The invention belongs to the technical field of nano photonics, and particularly relates to an encryptable full-color domain structural color module and a preparation method thereof. The preparation method of the encryption module is simple and convenient, and not only can realize the encryption of naked eyes images and characters, but also is difficult to crack even under a high-precision nanoscale characterization method. Decryption and information display can be realized by simple vapor deposition of noble metal materials. The nanostructure and the preparation material of the encryption module enable the encryption module to have encryption property and low angle dependence characteristic of color.
Background
The information encryption technology is a technology for protecting the transmission and storage processes of information by using mathematical or physical means so as to prevent information leakage. In an optical encryption system, light waves are limited by diffraction during transmission, diffraction is necessarily accompanied, parameters such as wavelength, amplitude, phase, polarization state, space frequency and the like can be provided, the parameters can be used as encryption keys of the system, the encryption images and characters are processed according to optical operation and optical transformation by means of the action of the keys, and ciphertext can be restored to plaintext information only by obtaining the keys. Encryption is realized based on an optical or nano-photonics method, and two modes exist, namely, information conversion is performed, and information hiding is performed. Currently, the optical transformation encryption method mainly includes three types: a dual random phase code encryption technique, a fractional fourier transform based encryption technique and a joint transform correlator based optical encryption system. The technical thresholds of the systems are high, and the decryption time length depends on the computing power of the equipment. The optical hiding encryption method is to fine tune the optical signal based on the micro-nano functional sequence structure, and realize information hiding by utilizing holographic technology or phase regulation. The method has higher requirements on micro-nano functional sequence, expensive focusing ion beam equipment or electron beam etching equipment is needed in the processing process, and meanwhile, the sample area of the micro-nano structure is limited and the processing time is longer. Therefore, a convenient and efficient information encryption method is needed to be developed, and the display and encryption of images or characters can be directly realized.
The structural color is also called physical color, and is characterized in that light waves are refracted, diffusely reflected, diffracted or interfered by an artificially constructed sub-wavelength structure, so that the enhancement or inhibition of specific wavelength is realized, and various colors are generated. Specific principles relate to photonic crystals, localized Surface Plasmon Resonances (LSPRs), mie resonances, fabry-Perot interferometry, rayleigh-Wood diffraction anomalies from two-dimensional periodic lattices, and the like. The advantages of high stability, adjustability, functional compatibility and the like of the artificial structural color excite the application of the artificial structural color in the fields of full-color filters, polaroids, macroscopic color holograms, electrochromic devices, color printing and the like, generate considerable benefits in the aspects of basic science and application technology, and have important promotion potential for the next-generation color printing technology. Based on the closely related characteristics of the artificial structure color and the micro-nano structure, the encryption of the artificial structure color can be realized through the regulation and control of the micro-nano structure.
In the field of artificial structural colors, indexes for measuring the color rendering quality mainly comprise saturation, brightness and color gamut size. Although the existing research results show good performance in resolution, color quality, color gamut and the like, the research results are still limited by conditions of complicated angle, polarization, expensive preparation process and the like. In addition, artificial structural color devices are difficult to compromise in terms of sample size, resolution, and cost. The electron beam lithography and the laser direct writing technology are emerging, and the customizable and ultra-high resolution (breaking through diffraction limit) structural color patterns are prepared, but the sample still has the problem of limited size. To enhance commercialization of structural color technology, mass production techniques such as nanoimprinting, injection molding, embossing, and large-area chemical/physical vapor deposition have been developed. These methods reproduce template structures to give high resolution patterns suitable for producing large area structural color patterns, but require further development to improve color reproducibility. Therefore, there is still a great progress space for optimizing the artificial structural color device, and a more accurate regulation and control method is also needed in the aspects of information and text encryption application, so that effective hiding of the information under the non-key condition is finally realized, and the correct information can be conveniently obtained under the key condition.
Object of the Invention
The invention relates to a full-color domain structural color encryption module, which aims to solve the problem of complex preparation of an optical encryption module, realize encrypted information which is difficult to distinguish under the nanoscale, and realize encryption of artificial structural colors on the basis of high-quality color development.
The purpose of the invention is realized in the following way:
the structural color module is a three-layer film structure, as shown in figure 1 a. The aluminum substrate is used as a reflecting layer and is positioned at the bottommost layer of the structural color module; the alumina film is used as a medium layer and is positioned in the middle of the structural color module; noble metal layers (gold, silver, etc.) are used as decryption layers and are positioned at the uppermost layer of the structural color module. The color information is presented and hidden by adjusting the color difference between the thickness control information of the medium layer and the background and by depositing and erasing the noble metal layer. The short-range ordered nano structure of the AAO is beneficial to reducing the angle dependence of the color, and the AAO is hard and corrosion-resistant, so that the service life of the structural color module can be prolonged, and the repeated use of the encryption module can be realized.
In order to achieve the above purpose, the technical scheme adopted by the invention is to realize the basic color development structure of the module in an electrochemical anodic oxidation mode, and the specific steps are as follows:
(1) Cutting high-purity aluminum foil into required size, and respectively ultrasonic treating with water and ethanol for 7-10 min. And (3) carrying out electrochemical polishing on the aluminum foil in an ice water bath (0 ℃) environment, wherein the electrolyte adopts a mixed solution of perchloric acid and absolute ethyl alcohol, and the volume ratio of the perchloric acid to the absolute ethyl alcohol is 1:7. The voltage is 20-30V, the current is 2-4A, and the polishing time is 3-5 minutes. And (3) attaching an electrostatic adhesive tape to the surface of the polished aluminum foil, and carrying out patterning treatment on the electrostatic adhesive tape on the surface by using laser according to the required encrypted information so as to expose the position corresponding to the information.
(2) And carrying out electrochemical anodic oxidation on the polished aluminum foil to form an aluminum oxide film. The primary oxidation environment temperature is 2-4 ℃, oxalic acid electrolyte is adopted, the constant voltage is 40V, and the oxidation time is 10-12 hours. AAO was immersed in a mixture of 0.9g chromic acid and 50ml of 6wt% phosphoric acid for 12 hours at room temperature to remove the primary oxide layer, leaving a series of circular dimples on the aluminum surface.
(3) The secondary oxidation environment temperature is 2-4 ℃, oxalic acid electrolyte is adopted, the constant voltage is 40V, the oxidation time is adjusted according to the color difference between the information and the background, and the color regulation and control within the full color range can be realized in 3-10 minutes. If the background portion does not need to develop color, the oxidation ends. If the background part needs to develop color, the electrostatic adhesive tape is removed and then oxidized for a proper time.
(4) Depositing 5-10nm silver on the AAO film by a physical vapor deposition device. The color difference between the information and the background causes the information to appear as shown in fig. 1 b. When information hiding is needed, the surface of the sample is quickly wiped by adopting a mixed solution of 3.4g of copper chloride, 100mL of hydrochloric acid and 100mL of water, and the ultrasonic treatment is carried out for 5-7 minutes by using water, alcohol and water respectively (shown in figure 1 c). And (5) silver with the wavelength of 5-10nm is deposited again to realize information redisplay.
The invention is characterized in that the full-color-gamut encryptable structural color module is prepared. Because the structural parameters of the alumina template adopted in the module are flexible to regulate and control, the color with low angle dependence of the full color gamut can be realized, the AAO film has higher hardness, and the service life of the structural color module can be effectively prolonged. Carrying out patterning treatment on the surface of the module according to the required encryption information; by regulating oxidation time and oxidation current, encryption information is conveniently input; by regulating the noble metal layer, the encryption and display of information are realized.
Compared with the prior art, the invention has the beneficial effects that:
1. in view of the high hardness, corrosion resistance and wear resistance of the anodic aluminum oxide material adopted by the structural color module, the service life of the module can be prolonged to a limited extent, and according to the embodiment 1, the sample can be reused after repeatedly displaying and erasing information;
2. encryption information can be input by regulating and controlling AAO structure parameters, and color of information display is regulated and controlled, so that full-color domain encryption is realized;
3. color encryption is realized through the silver layer, and the color encryption is a difference which is difficult to distinguish under a micro-nano level microscope;
4. the pattern processing is convenient, the precision is high, the large-area preparation can be realized, the artificial structural color can truly go out of a laboratory, and the practical application is oriented;
5. based on the short-range ordered structure of the anodic aluminum oxide film, the structural color module can realize low-angle dependence of color, and can keep uniformity of color within an angle range of 45 degrees.
Drawings
Fig. 1: a schematic cross-sectional view of the structural color encryption module;
the names of the parts are as follows: aluminum base 1, aluminum oxide dielectric layer 2, silver layer 3, information position 4, background position 5;
fig. 2: an optical photograph of the structural color trichromatic module prepared in example 1;
fig. 3: schematic diagrams of interactions between light waves and interfaces of the structural color module;
fig. 4: reflectance spectra before and after sample encryption;
fig. 5: the optical photograph of the encrypted structural color module prepared in example 1 and the corresponding scanning electron microscope photograph;
fig. 6: electromagnetic field distribution diagrams before and after silver plating are steamed by the structural color module.
Detailed Description
The invention is described in further detail below with reference to the drawings and the detailed description.
Example 1: a preparation method of a full-color domain encryption structural color module comprises the following steps:
(1) Cutting high-purity aluminum foil into required size, and respectively performing ultrasonic treatment with water and ethanol for 8 minutes. And (3) carrying out electrochemical polishing on the aluminum foil in an ice water bath (0 ℃) environment, wherein the electrolyte adopts a mixed solution of perchloric acid and absolute ethyl alcohol, and the volume ratio of the perchloric acid to the absolute ethyl alcohol is 1:7. The voltage was 30V, the current was 4A, and the polishing time was 3 minutes. And (3) attaching an electrostatic adhesive tape to the surface of the polished aluminum foil, and carrying out patterning treatment on the electrostatic adhesive tape on the surface by using laser according to the required encrypted information so as to expose the position corresponding to the information.
(2) And performing electrochemical anodic oxidation on the polished aluminum foil by adopting a two-step method to form an aluminum oxide film. The primary oxidation environment temperature is 2 ℃, oxalic acid electrolyte is adopted, the constant voltage is 40V, and the oxidation time is 10 hours. AAO was immersed in a mixture of 0.9g chromic acid and 50ml of 6wt% phosphoric acid for 12 hours at room temperature to remove the primary oxide layer, leaving a series of circular dimples on the aluminum surface.
(3) The secondary oxidation environment temperature is 2 ℃, oxalic acid electrolyte is adopted, the constant voltage is 40V, and the oxidation time is adjusted according to the difference between the information and the background color. If the background part does not need to develop color, the oxidation is finished. If the background part needs to develop color, the electrostatic adhesive tape is removed and then oxidized for a proper time.
(4) 5nm silver was deposited on the AAO film by physical vapor deposition equipment, at which time information was displayed. When information is needed to be hidden, the surface of the sample is wiped by adopting a mixed solution of 3.4g of copper chloride, 100mL of hydrochloric acid and 100mL of water, and the ultrasonic treatment is carried out for 5 minutes by using water, alcohol and water respectively. The information redisplay can be realized by only depositing 5nm silver. The red corresponding oxidation time was 2 minutes, the green corresponding oxidation time was 2 minutes and 20 seconds, and the blue corresponding oxidation time was 3 minutes, and the photograph of the sample is shown in fig. 2.
The invention provides a full-color-domain encryptable structural color module. The invention is characterized in that: 1. the module adopts a thin film interference principle, a structural schematic diagram is shown in fig. 3, light rays are refracted and reflected through an interface I of a thin film, refracted light rays are reflected through an interface II, light rays reflected back to the interface I from the interface II are refracted, and reflected light 2 interferes with reflected light 1 to generate color. 2. The chip has simple preparation process and low cost, can meet the requirement of color presentation in full color range, and has great application potential. 3. The module encryption process can be repeated, and is an information encryption method which is difficult to distinguish in SEM. 4. The encryption module prepared by the scheme has a short-range ordered microstructure, and can realize low angle dependence of colors.
Example 2:
the structural color encryption module obtained in embodiment 1 was subjected to optical signal detection. Before and after encryption, the spectra of the samples exhibited significant differences. Before silver vapor deposition, the optical information of the sample is weaker, the peak-valley intensity difference in the spectrum is smaller, and the color cannot be displayed. After silver is steamed, the peak-to-valley ratio of the spectrum becomes large due to the plasmon property of silver, and the color display is obvious. As shown in fig. 4.
Example 3:
the structural color encryption module obtained in embodiment 1 was subjected to encryption test. The preparation pattern is the acronym HEU for english at the university of halbine engineering. According to the experimental procedure in example 1, the difference between the hole depth of the regulation information (HEU) and the background is used to obtain the basic model of the structural color encryption module, and the microscopic morphology of the sample is observed by using a scanning electron microscope, and the surface morphology and the corresponding optical photograph are shown in fig. 5 (a), and at this time, the information is not shown. The nanopore array is in a hexagonal close-packed structure with a short range order. Silver with a wavelength of 5nm is vapor-deposited on the surface of the substrate, so that information can be displayed as shown in FIG. 5 (b). The silver layer on the surface is in a continuous film shape and has certain roughness. After wiping the silver, the information was hidden and in fig. 5 (c), SEM pictures showed no damage to the sample surface. Because AAO has certain hardness and stable structure, repeated experiments can still realize good display and hiding of information, as shown in fig. 5 (d). The structural color encryption module has practical application value.
Example 4:
according to the structural color encryption module obtained in embodiment 1, electromagnetic field enhancement before and after information hiding is simulated by using a finite difference time domain method (FDTD). According to the micro-nano structure shown in fig. 1 and fig. 5b, model parameters established in FDTD are: the periodic spacing was 100nm and arranged in hexagonal close-packed arrangement, each periodic unit being a pore structure with a diameter of 30 nm. Incident light is incident from the front of the module to obtain an electromagnetic field distribution diagram (see fig. 6), wherein fig. 6 (a) is an electromagnetic field distribution diagram before silver evaporation, fig. 6 (b) is an electromagnetic field distribution diagram after silver evaporation, and the scale represents the enhancement degree of the electromagnetic field. It can be seen that the electromagnetic field before information display (before silver evaporation) is mainly concentrated in the AAO holes; the information is displayed (after silver evaporation) with stronger electromagnetic field enhancement and concentrated on the silver layer.
Example 5:
according to the structural color encryption module obtained in the embodiment 1, before silver film evaporation, the structural color encryption module is in an encryption state, text information cannot be observed by naked eyes, a scanning electron microscope is adopted to observe the microscopic morphology of a sample, and the information and the background part have no obvious difference, so that the structural color encryption module is difficult to crack under a high-precision nanoscale characterization method. And the difference of the hole depths of the two parts can be observed from the cross section observation of the information and the background part.
Claims (2)
1. The full-color domain structural color encryption module is characterized by being of a three-layer film structure, wherein an aluminum substrate is used as a reflecting layer and is positioned at the bottommost layer of the structural color module; the alumina film is used as a medium layer and is positioned in the middle of the structural color module; the noble metal layer is used as a decryption layer and is positioned at the uppermost layer of the structural color module; through adjusting the color difference between the thickness control information of the medium layer and the background, the color information is presented and hidden through the deposition and erasure of the noble metal layer, the short-range ordered nano structure of the AAO is beneficial to reducing the angle dependence of the color, and the characteristics of hardness and corrosion resistance of the AAO can improve the service life of the structural color module and realize the repeated use of the encryption module.
2. The preparation method of the full-color domain structural color encryption module is characterized by comprising the following steps of:
(1) Cutting high-purity aluminum foil into required sizes, carrying out ultrasonic treatment on the aluminum foil for 7-10 minutes by using water and ethanol respectively, carrying out electrochemical polishing on the aluminum foil in an ice-water bath environment at 0 ℃, adopting a mixed solution of perchloric acid and absolute ethanol as electrolyte, wherein the volume ratio of the perchloric acid to the absolute ethanol is 1:7, the voltage is 20-30V, the current is 2-4A, the polishing time is 3-5 minutes, attaching an electrostatic adhesive tape on the surface of the polished aluminum foil, and carrying out patterning treatment on the electrostatic adhesive tape on the surface by using laser according to required encryption information to expose the position corresponding to the information;
(2) Performing electrochemical anodic oxidation on the polished aluminum foil to form an aluminum oxide film, wherein the primary oxidation environment temperature is 2-4 ℃, oxalic acid electrolyte is adopted, the constant voltage is 40V, the oxidation time is 10-12 hours, and AAO is immersed into a mixed solution of 0.9g chromic acid and 50mL of 6wt% phosphoric acid for 12 hours at room temperature to remove the primary oxidation layer, so that a series of circular dents are reserved on the aluminum surface;
(3) The secondary oxidation environment temperature is 2-4 ℃, oxalic acid electrolyte is adopted, the constant voltage is 40V, the oxidation time is adjusted according to the color difference between information and the background, the color regulation and control in the full color range are realized in 3-10 minutes, if the background part does not need to be developed, the oxidation is finished, if the background part needs to be developed, the electrostatic adhesive tape is removed, and then the oxidation is carried out for a proper time;
(4) And depositing 5-10nm silver on the AAO film by using a physical vapor deposition device, wherein the color difference between information and a background is caused to enable the information to be displayed, when the information is needed to be hidden, the surface of a sample is quickly wiped by adopting a mixed solution of 3.4g of copper chloride, 100mL of hydrochloric acid and 100mL of water, the ultrasonic treatment is carried out for 5-7 minutes by using water, alcohol and water respectively, and the information can be redisplayed by depositing 5-10nm silver again.
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| US5167793A (en) * | 1991-05-07 | 1992-12-01 | Alcan International Limited | Process for producing anodic films exhibiting colored patterns and structures incorporating such films |
| CN102162115B (en) * | 2011-01-20 | 2012-05-02 | 浙江大学 | Color regulation and control method based on porous alumina and single atom deposition technology |
| 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 |
| CN104264202A (en) * | 2014-09-26 | 2015-01-07 | 山西师范大学 | Color-adjustable anodic aluminum oxide (AAO) film as well as preparation method and application thereof |
| CN105441949A (en) * | 2016-01-26 | 2016-03-30 | 苏州诺菲纳米科技有限公司 | Nano-silver etchant, method for preparing patterned nano-silver conducting film and touch sensor |
| CN106480484B (en) * | 2016-10-12 | 2018-06-26 | 中山大学 | A kind of preparation of reflective image device and application process |
| CN110341344B (en) * | 2019-07-03 | 2021-08-06 | 肇庆市华师大光电产业研究院 | Method for anti-counterfeiting by using structural color |
| CN111951662B (en) * | 2020-06-03 | 2022-06-10 | 中山大学 | Physical information hiding structure based on size difference of structural units and preparation method thereof |
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