CN112980424A - Preparation method of fast photochromic holographic storage material under low-power writing - Google Patents
Preparation method of fast photochromic holographic storage material under low-power writing Download PDFInfo
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- CN112980424A CN112980424A CN202110153779.0A CN202110153779A CN112980424A CN 112980424 A CN112980424 A CN 112980424A CN 202110153779 A CN202110153779 A CN 202110153779A CN 112980424 A CN112980424 A CN 112980424A
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- titanium dioxide
- silver
- dioxide film
- potassium chloride
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- 239000011232 storage material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 216
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 108
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 102
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229910001923 silver oxide Inorganic materials 0.000 claims abstract description 71
- 239000001103 potassium chloride Substances 0.000 claims abstract description 55
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 54
- 239000001263 FEMA 3042 Substances 0.000 claims abstract description 45
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims abstract description 44
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims abstract description 44
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 44
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims abstract description 44
- 229940033123 tannic acid Drugs 0.000 claims abstract description 44
- 235000015523 tannic acid Nutrition 0.000 claims abstract description 44
- 229920002258 tannic acid Polymers 0.000 claims abstract description 44
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 22
- 230000009471 action Effects 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000002791 soaking Methods 0.000 claims abstract description 8
- 239000010408 film Substances 0.000 claims description 121
- 239000000243 solution Substances 0.000 claims description 47
- 238000000034 method Methods 0.000 claims description 26
- 230000008569 process Effects 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 6
- 230000001678 irradiating effect Effects 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000010409 thin film Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000003618 dip coating Methods 0.000 claims 2
- 238000003860 storage Methods 0.000 abstract description 26
- 230000004044 response Effects 0.000 abstract description 9
- 239000002114 nanocomposite Substances 0.000 abstract description 7
- 230000003287 optical effect Effects 0.000 abstract description 5
- 229910021649 silver-doped titanium dioxide Inorganic materials 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 238000006552 photochemical reaction Methods 0.000 abstract description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 58
- 238000010521 absorption reaction Methods 0.000 description 19
- 238000011065 in-situ storage Methods 0.000 description 13
- -1 potassium chloride modified silver Chemical class 0.000 description 9
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 8
- 238000012360 testing method Methods 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 5
- 238000000862 absorption spectrum Methods 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000008213 purified water Substances 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 241001025261 Neoraja caerulea Species 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229920001400 block copolymer Polymers 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
- G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
- G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
- G11B7/2403—Layers; Shape, structure or physical properties thereof
- G11B7/24035—Recording layers
- G11B7/24044—Recording layers for storing optical interference patterns, e.g. holograms; for storing data in three dimensions, e.g. volume storage
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
- G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
- G11B7/241—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material
- G11B7/242—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers
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- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
- G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
- G11B7/26—Apparatus or processes specially adapted for the manufacture of record carriers
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- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
- G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
- G11B2007/240025—Record carriers characterised by shape, structure or physical properties, or by the selection of the material for storing optical interference patterns, e.g. holograms
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Abstract
A preparation method of a fast photochromic holographic storage material under low-power writing relates to the technical field of optical information storage, and solves the problems of the existing Ag/TiO2The nano composite film has low response speed in holographic storage, and the preparation method comprises preparing the titanium dioxide film attached with tannic acid under the condition of keeping out of the sun; immersing the film in silver nitrate solution in a dark condition, and soaking the film in a water bath at 30 ℃ to obtain a silver/titanium dioxide film; then visible laser irradiation is carried out and the silver/titanium dioxide film is dipped in silver nitrate solution to obtain a silver/titanium dioxide film under the combined action of laser and tannic acid; final immersionAnd (3) in a potassium chloride solution, obtaining the silver/titanium dioxide film modified by the potassium chloride. The invention adopts potassium chloride for modification, creates a new photochemical reaction environment, further regulates and controls the photochromic speed, realizes the quick photochromic of low-power monochromatic light, obtains the holographic storage material with higher response speed, and is suitable for the quick and efficient holographic storage of blue light under low power.
Description
Technical Field
The invention relates to the technical field of optical information storage, in particular to a preparation method of a fast photochromic holographic storage material under low-power writing.
Background
The society enters the information age, the data volume is increased rapidly, and the mass data puts more rigorous requirements on storage. Among several major storage technologies, optical storage is likely to become an important industry of storage technology due to its characteristics of long storage life, low energy consumption, and the like. Among them, the high-density holographic storage can effectively meet the requirement of storing mass data, the holographic recording medium is a core unit of storage, and the further development of the high-density optical storage can be promoted by optimizing the performance of the recording medium. Improving the speed and efficiency of holographic storage has been a hot spot in applications. After the metal nano particles and the semiconductor are compounded, the electron transfer of the interface of the metal nano particles and the semiconductor can be realized under the illumination. An Ag/TiO film holographic material and its preparing process and application are disclosed in the Chinese patent with application number CN201710981715.32Nano composite film, Ag/TiO2The nano composite film can be used for optical information storage due to the photochromic property, but the spectral hole burning rate of the nano composite film can influence Ag/TiO2The storage speed of the film is high, the size of Ag NPs is an important factor influencing the spectrum hole burning rate, the holographic storage speed can be improved by reducing the size of silver nanoparticles, the particle concentration and the exposure sensitivity of the storage medium under low-power writing light are improved to a very limited extent, and therefore, the Ag/TiO2The nano composite film holographic memory has development bottleneck on the problem of response speed improvement under low-power writing.
Disclosure of Invention
To solve the problem of Ag/TiO2The invention provides a preparation method of a fast photochromic holographic storage material under low-power writing.
The technical scheme adopted by the invention for solving the technical problem is as follows:
the preparation method of the fast photochromic holographic storage material under low-power writing comprises the following steps:
s1, soaking the titanium dioxide film in a tannic acid solution under the dark condition to obtain the titanium dioxide film attached with tannic acid;
s2, immersing the titanium dioxide film attached with the tannic acid obtained in the step S1 in a silver nitrate solution under the condition of keeping out of the sun, and soaking in a water bath at the temperature of 30 ℃ for 10min to obtain a silver/titanium dioxide film;
s3, irradiating the silver/titanium dioxide film immersed in the silver nitrate solution by using visible laser to obtain a silver/titanium dioxide film under the combined action of the laser and the tannic acid;
s4, immersing the silver/titanium dioxide film which is obtained by the combined action of the laser and the tannic acid and is obtained in the S3 into a potassium chloride solution, and obtaining the silver/titanium dioxide film modified by the potassium chloride.
According to the preparation method of the quick photochromic holographic storage material under low-power writing, the silver/titanium dioxide film modified by the potassium chloride is applied to blue-ray holographic storage.
The invention has the beneficial effects that:
the invention provides a preparation method of a fast photochromic holographic storage material under low-power writing, and provides a potassium chloride modified silver/titanium dioxide nano composite film material, which obtains high-efficiency narrow-band silver nano particle absorption under the combined action of visible laser and tannic acid, further adopts potassium chloride for modification, creates a new photochemical reaction environment, realizes the effect of further regulating and controlling photochromic speed, realizes fast photochromic of low-power monochromatic light, obtains a holographic storage material with faster response speed, and is suitable for fast and efficient holographic storage of blue light under low power.
Drawings
FIG. 1 is a flow chart of the preparation method of the fast photochromic holographic storage material under low power writing of the present invention.
FIG. 2a is a scanning electron micrograph of a laser co-acting silver/titanium dioxide film with tannic acid.
FIG. 2b is a scanning electron micrograph of a potassium chloride modified silver/titanium dioxide film.
FIG. 3 is an in-situ absorption spectrum obtained from the in-situ absorption test of a silver/titanium dioxide film under the combined action of laser and tannic acid under the irradiation of 473nm laser with different powers.
FIG. 4 is an in-situ absorption spectrum obtained by in-situ absorption test of a silver/titanium dioxide film modified by potassium chloride under 473nm laser irradiation with different powers.
FIG. 5 is a graph showing the differential absorption spectra of a silver/titanium dioxide film with a laser and tannic acid coacting under irradiation of a 473nm laser at different powers.
FIG. 6 is a differential absorption spectrum of a silver/titanium dioxide film modified with potassium chloride under 473nm laser irradiation at different powers.
FIG. 7 is a graph of a fitted differential absorption hole burning rate of a silver/titanium dioxide film co-acted by a laser and tannic acid under irradiation of 473nm laser at different powers.
FIG. 8 is a graph of a fit of differential absorption hole burning rates of potassium chloride modified silver/titanium dioxide films under 473nm laser irradiation at different powers.
FIG. 9 is a graph comparing the holographic kinetic curves of a laser co-acted silver/titanium dioxide film with tannic acid and a potassium chloride modified silver/titanium dioxide film.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation method of the fast photochromic holographic storage material under low-power writing, as shown in figure 1, comprises the following steps:
s1, soaking the titanium dioxide film in a tannic acid solution under the dark condition to obtain the titanium dioxide film attached with tannic acid;
s2, immersing the titanium dioxide film attached with the tannic acid obtained in the step S1 in a silver nitrate solution under the condition of keeping out of the sun, and soaking in a water bath at the temperature of 30 ℃ for 10min to obtain a silver/titanium dioxide film;
immersing the silver/titanium dioxide film obtained in S3 and S2 in silver nitrate solution, and irradiating the silver/titanium dioxide film immersed in the silver nitrate solution by using visible laser to obtain the silver/titanium dioxide film under the combined action of laser and tannic acid;
and S4, immersing the silver/titanium dioxide film which is obtained by the combined action of the laser and the tannic acid and obtained in the S3 in a potassium chloride solution to obtain the silver/titanium dioxide film modified by potassium chloride, namely the quick photochromic holographic storage material under the low-power writing.
The preparation method comprises the following specific processes:
s1.1, preparing a titanium dioxide film
Taking the volume ratio of 1: 2 TiO 22And putting the sol and the purified water into a beaker, and magnetically stirring until the sol and the purified water are uniformly mixed to prepare the titanium dioxide solution. Get P123(PEO20-PPO70-PEO20) Placing the block copolymer gel in another beaker, adding purified water, and magnetically stirring for a long time (about 2h) until the block copolymer gel is uniformly dissolved into a liquid state, thereby obtaining the pore-forming agent solution. Mixing a titanium dioxide solution and a pore-forming agent solution, stirring for 1h by magnetic force until the mixture is uniformly mixed, and then adding ethanol to ensure that the volume ratio of the titanium dioxide solution to the pore-forming agent solution is 3: 2, the product is obtained. The TiO obtained above is mixed2/P123The mixed solution was placed in a beaker, and a film was drawn on a glass substrate using a film drawing machine. Irradiating, baking and annealing the film by an infrared lamp in sequence after the film is extracted, specifically irradiating the film by the infrared lamp for 2-3 min immediately after the film is extracted, then putting the film into a 120 ℃ oven for baking for 5min, repeating the film extraction and baking for 3 times, and then putting the film into an electric furnace for heating and annealing, wherein the annealing temperature is 450-500 ℃. And after annealing treatment, taking out the titanium dioxide film, placing the titanium dioxide film in a room, and cooling the titanium dioxide film to room temperature to finally obtain the stable, colorless, transparent, loose and porous titanium dioxide film.
S1.2, preparing a tannic acid solution with the pH value of 8.5
Respectively preparing 0.002mol/L tannic acid solution and 0.009mol/L potassium carbonate solution at room temperature, and magnetically stirring to prepare a mixed solution of the tannic acid solution and the potassium carbonate solution; and measuring the pH value of the mixed solution by a pH meter, adjusting the pH value to 8.5, changing the solution into dark green, completing the preparation of the tannic acid solution, and storing the prepared tannic acid solution in a dark place. Preferably, the molar concentration of tannic acid is 0.002mol/L to 0.004 mol/L.
S1.3, preparing the titanium dioxide film attached with the tannic acid
Immersing the titanium dioxide film obtained in the step S1.1 in the tannic acid solution prepared in the step S1.2 at room temperature, wherein the immersion conditions are as follows: the temperature is 20-28 ℃, and the dipping time is 1-5 h; in the embodiment, the titanium dioxide film is dipped for 2 hours, the dipping process is carried out under the condition of keeping out of the sun, after the dipping is finished, the titanium dioxide film is taken out, and the titanium dioxide film is dried by adopting compressed air to obtain the titanium dioxide film attached with the tannic acid, wherein the titanium dioxide film is a light yellow transparent film.
S2.1, preparing silver nitrate solution
The solvent of the silver nitrate solution is a mixed solution of water and ethanol, and the volume ratio of the ethanol to the water is 1: (1-100), wherein the molar concentration of silver nitrate in the silver nitrate solution is 0.1-0.5 mol/L. The molar concentration of silver nitrate in the silver nitrate solution prepared in the present embodiment is 0.1 mol/L.
S2.2, obtaining the silver/titanium dioxide film by a water bath heating method
Immersing the titanium dioxide film attached with the tannic acid obtained in the step S1.3 in the silver nitrate solution prepared in the step S2.1, and soaking in a constant-temperature water bath at the temperature of 30 ℃ for 10min to change the titanium dioxide film from light yellow transparent to light brown silver/titanium dioxide film, so as to obtain the titanium dioxide film attached with the tannic acid.
S3 efficient narrow-band silver/titanium dioxide film by visible laser reduction method
Irradiating the light brown silver/titanium dioxide film in the silver nitrate solution by using visible laser with the laser wavelength of 400-700 nm and the power of 10-50 mW for 1-30 min, wherein the visible laser is irradiated for 5min by using 30mW visible laser in the embodiment, taking the film out of the silver nitrate solution while stopping irradiation, rinsing the film taken out of the silver nitrate solution by using ultrapure water, and drying by using compressed air to obtain the brown silver/titanium dioxide film, namely the silver/titanium dioxide film under the combined action of the laser and the tannic acid.
S4.1, preparing a potassium chloride solution
The molar concentration of the potassium chloride solution is 0.08mol/L to 0.12mol/L, and in the present embodiment, a potassium chloride solution having a molar concentration of 0.1mol/L is prepared.
S4.2, preparing the silver/titanium dioxide film modified by potassium chloride
And (2) under visible light and at room temperature, without light shielding and laser irradiation, immersing the silver/titanium dioxide film which is obtained in the step (S3) and has the combined action of the laser and the tannic acid in the potassium chloride solution prepared in the step (S4.1), immediately taking out the silver/titanium dioxide film, wherein the immersion time is less than 1min, rinsing the taken-out film by using ultrapure water, and drying by using compressed air to obtain the silver/titanium dioxide film modified by the potassium chloride. The silver/titanium dioxide film modified by potassium chloride is stored away from light for later use, the inner layer of the double-layer package is wrapped by lens wiping paper, and the outer layer of the double-layer package is wrapped by tinfoil.
The silver/titanium dioxide film obtained by the combined action of the laser and the tannic acid obtained in the method S3 and the silver/titanium dioxide film obtained by the method S4 and modified by the potassium chloride are subjected to a scanning electron microscope, an in-situ absorption spectrum test and a holographic storage test, and the obtained results are explained below.
(1) The scanning electron micrograph of the film obtained in S3 is shown in FIG. 2a by using the scanning electron micrograph; the scanning electron micrograph of the film obtained in S4 is shown in FIG. 2 b. As can be seen from fig. 2a and 2b, the number of silver nanoparticles in the silver/titanium dioxide thin film modified with potassium chloride according to the present invention is smaller than that of the existing silver/titanium dioxide thin film, and the particles are more dispersed.
(2) And testing the in-situ absorption of the film obtained in the step S3 and the film obtained in the step S4 after irradiation of laser light with different powers of 473nm by using an ultraviolet-visible absorption spectrometer, wherein the irradiation time is 0min, 0.5min, 1min, 3min, 5min, 10min, 20min and 30min, the in-situ absorption spectrograms are shown in the graph in the figure 3 and the graph in the figure 4, further carrying out differential processing on the in-situ absorption, the differential absorption spectrograms are shown in the figure 5 and the figure 6, and the fitting result of the differential absorption hole burning rate is shown in the figure 7 and the figure 8. Wherein the laser power corresponding to fig. 3(a) (b) (c), fig. 4(a) (b) (c), fig. 5(a) (b) (c) and fig. 6(a) (b) (c) are respectively 0.5mW, 2.5mW and 5mW, and 12 small graphs in fig. 3 to 6 are provided, each small graph has 8 curves corresponding to the irradiation time, the irradiation time of the 8 curves corresponding to the abscissa 420nm is gradually lengthened from top to bottom, and the irradiation time of the 8 curves corresponding to the abscissa 650nm is gradually shortened from top to bottom. By observing a differential absorption curve and a differential absorption hole burning rate fitting curve, the silver/titanium dioxide film modified by potassium chloride prepared by the invention can be verified to have faster photochromic property. Further details are provided below:
an in-situ absorption test of blue light (473nm laser) irradiation is carried out, and compared with an in-situ absorption spectrogram of the existing silver/titanium dioxide film, the absorbance of the in-situ absorption of the potassium chloride modified silver/titanium dioxide film material prepared by the method disclosed by the invention near the resonant light wavelength is reduced more quickly; the in-situ absorption is differentially processed to respectively obtain the differential absorption of the existing silver/titanium dioxide film (namely, no potassium chloride modification) and the silver/titanium dioxide film modified by potassium chloride, and the spectrum hole burning of the silver/titanium dioxide film material modified by potassium chloride prepared by the method is more obvious along with the change of time and power. According to the results of spectrum hole burning and in-situ absorption, the fast spectrum hole burning of the silver/titanium dioxide film modified by potassium chloride is analyzed, firstly, the silver nano particles are dispersed more uniformly and are dissolved by light under 473nm laser irradiation, secondly, potassium ions and chloride ions in a potassium chloride solution exist in the form of ions, and the silver nano particles are dissolved into silver ions under 473nm laser irradiation, so that electrons separated based on plasmon charges of the silver nano particles can be captured by oxygen in the air, and the dissolved silver ions are combined with the chloride ions. In the field of photocatalysis, under the irradiation of visible light, the common explanation is that electrons separated from plasmon charges of silver nanoparticles can be captured by oxygen in the air, and the rest holes can react with chloride ions to generate chlorine, so that the silver nanoparticle light dissolution speed of the reaction participation is much higher than that of the traditional light dissolution speed, and the silver/titanium dioxide film modified by potassium chloride prepared by the invention has faster photochromic property.
Further rate fitting was performed on the change in maximum hole burning depth over time using the following equation:
A1(t)=A11e(-t/τ)+A1∞ (1)
wherein in the formula (1), A1(t) the absorbance of the silver/titanium dioxide film at the maximum burning hole depth of the laser and tannic acid combined action at different times; a. the11Denotes e(-t/τ)The weight coefficient of (a), is related to the depth and efficiency of the hole burning; t is the laser irradiation time of the silver/titanium dioxide film under the combined action of the laser and the tannic acid; tau is a time attenuation factor of the maximum hole burning depth changing with the laser irradiation time; a. the1∞The silver/titanium dioxide film which is acted by the laser and the tannic acid is exposed to the exciting light for infinite time, and the maximum hole burning depth is the absorbance. Thus, according to the fitting result, when the laser power is 0.5mW, the time attenuation factor is 6.04min, A110.05224; the time attenuation factor obtained when the laser power is 2.5mW is 8.64min, A110.09902; the time attenuation factor of the laser power is 9.72min at 5mW, A11Is 0.20555. The fitting result shows that the photochromic rate is faster under the irradiation of the laser power of 0.5 mW. But the burning hole depth is relatively small under low power, and the photochromic efficiency is low. Wherein the formula (2), A2(t1,t2) The absorbance of the silver/titanium dioxide film modified by potassium chloride at the maximum burning hole depth at different times is shown; a. the21To representA weight coefficient; a. the22To representThe weight coefficient of (a); t is t1And t2The time of laser irradiation of the silver/titanium dioxide film modified by potassium chloride in the fast process and the slow process respectively; tau is1And τ2Fast and slow process time decay factors, respectively, of the change in maximum hole burning depth over time; a. the2∞Silver/titanium dioxide films modified with potassium chloride were exposed to excitation light for an infinite period of absorbance. According to the fitting result, the time attenuation factor tau is obtained when the laser power is 0.5mW1And τ2Respectively 1.07min and 11.34min, A21And A220.35515 and 0.11131, respectively; time attenuation factor tau obtained at a power of 2.5mW1And τ2Respectively at 1.40min and 10.85min, A21And A220.33021 and 0.23835, respectively; attenuation factor tau at a power of 5mW1And τ2Respectively 0.35min and 11.97min, A21And A220.97557 and 0.18597,. And a weight coefficient A derived from the data result21Greater than A22Namely, the silver/titanium dioxide film modified by potassium chloride is mainly fast in process, the time attenuation factor of the fast process is far smaller than that of the silver/titanium dioxide film under the combined action of laser and tannic acid, and the weight coefficient of the sample modified by introducing the potassium chloride is obviously increased, which shows that the silver/titanium dioxide film modified by the potassium chloride prepared by the invention has faster and more efficient photochromic capability. Meanwhile, the fast process and the slow process of photochromism are influenced by the laser power.
(3) The silver/titanium dioxide film modified by the potassium chloride obtained in the step S4 can be used as a holographic storage material, can be used for holographic storage, and can particularly be used for holographic storage of blue light. The grating growth kinetic curve graph of the blue-ray holographic storage of the silver/titanium dioxide film modified based on potassium chloride and the silver/titanium dioxide film prepared by the existing method is compared, the kinetic curve is further fitted by adopting index fitting, and the two comparisons of the writing laser (473nm) with the power of 0.5mW and 2.5mW are carried out in total, and the result is shown in the graph9, wherein STA+laserSilver/titanium dioxide film, S, showing the interaction of laser and tannic acidKClThe silver/titanium dioxide films modified with potassium chloride are shown. When the power is 2.5mW, the grating response time of the KCl modified silver/titanium dioxide film prepared by the invention and the grating response time of the silver/titanium dioxide film prepared by the existing method are respectively 56s and 209 s; when the power is 0.5mW, the response time of the two is 335s and 520s respectively. The silver/titanium dioxide film modified by potassium chloride prepared by the invention has shorter holographic storage response time and is more suitable for fast and efficient holographic storage of blue light under low power.
The invention provides a preparation method of a fast photochromic holographic storage material under low-power writing, which is characterized in that the material provided by the invention is a potassium chloride modified silver/titanium dioxide nano composite film, the silver nano particles with high efficiency and narrow band can be absorbed under the combined action of visible laser and tannic acid, the silver nano particles are further modified by potassium chloride, a new plasmon photochromic photochemical reaction environment is created, the effect of further regulating and controlling the photochromic speed is realized, the fast photochromic of low-power monochromatic light is realized, the holographic storage material with higher response speed is obtained, and the fast photochromic holographic storage material is suitable for fast and efficient holographic storage of blue light under low power.
Claims (8)
1. The preparation method of the fast photochromic holographic storage material under low-power writing is characterized by comprising the following steps:
s1, soaking the titanium dioxide film in a tannic acid solution under the dark condition to obtain the titanium dioxide film attached with tannic acid;
s2, immersing the titanium dioxide film attached with the tannic acid obtained in the step S1 in a silver nitrate solution under the condition of keeping out of the sun, and soaking in a water bath at the temperature of 30 ℃ for 10min to obtain a silver/titanium dioxide film;
s3, irradiating the silver/titanium dioxide film immersed in the silver nitrate solution by using visible laser to obtain a silver/titanium dioxide film under the combined action of the laser and the tannic acid;
s4, immersing the silver/titanium dioxide film which is obtained by the combined action of the laser and the tannic acid and is obtained in the S3 into a potassium chloride solution, and obtaining the silver/titanium dioxide film modified by the potassium chloride.
2. The method for preparing a fast photochromic holographic memory material under low power writing as claimed in claim 1, wherein the specific process of S5 is as follows: and (3) immersing the silver/titanium dioxide film which is obtained by the combined action of the laser and the tannic acid and is obtained in the S3 in a potassium chloride solution, taking the silver/titanium dioxide film out of the potassium chloride solution, rinsing the film by using ultrapure water, and drying the film by using compressed air to obtain the silver/titanium dioxide film modified by the potassium chloride.
3. The method of claim 1 wherein the silver/titanium dioxide film is immersed in the potassium chloride solution for less than 1 min.
4. The method for preparing a fast photochromic holographic storage material under low power writing of claim 1, wherein the molar concentration of the potassium chloride solution is 0.08mol/L to 0.12 mol/L.
5. The method for preparing a fast photochromic holographic storage material under low power writing of claim 4, wherein the molar concentration of the potassium chloride solution is 0.1 mol/L.
6. The method for preparing a fast photochromic holographic memory material under low power writing of claim 1, wherein in the step S1, the dipping condition is: the temperature is 20-28 ℃, the time is 1-5 h, and after the dipping is finished, the titanium dioxide film attached with the tannic acid is dried by air; the solvent of the silver nitrate solution is a mixed solution of water and ethanol, and the volume ratio of the ethanol to the water is 1: (1-100), wherein the molar concentration of silver nitrate in the silver nitrate solution is 0.1-0.5 mol/L, and the conditions of visible laser irradiation are as follows: the laser wavelength is 400 nm-700 nm, the power is 10 mW-50 mW, and the irradiation time is 1 min-30 min.
7. The method for preparing a fast photochromic holographic storage material under low power writing according to claim 6, wherein the titanium dioxide thin film in S1 is prepared by a dip-coating method, the dip-coating speed is 2cm/S to 5cm/S, and the residence time is 5S to 10S; the steps of infrared lamp irradiation, baking and annealing are carried out in sequence after the extraction, and the annealing temperature is 450-500 ℃.
8. The method for preparing a fast photochromic holographic memory material under low power writing of any one of claims 1 to 7, wherein the silver/titanium dioxide thin film modified by potassium chloride is applied in blue light holographic memory.
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JP2000212553A (en) * | 1999-01-26 | 2000-08-02 | Asahi Glass Co Ltd | Production of photochromic article |
JP2004018549A (en) * | 2002-06-12 | 2004-01-22 | Foundation For The Promotion Of Industrial Science | Multicolored photochromic material, method for producing the same and method for using the same |
US20140120168A1 (en) * | 2012-10-26 | 2014-05-01 | Nanocomposix, Inc. | Metastable silver nanoparticle composites |
CN107779849A (en) * | 2017-10-20 | 2018-03-09 | 东北师范大学 | Narrow-band absorption silver/titanium dioxide thin film holographic material and preparation method and application |
CN110452403A (en) * | 2019-08-08 | 2019-11-15 | 东北师范大学 | A kind of flexible nano composite holographic memory films, method for manufacturing thin film and application |
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JP2000212553A (en) * | 1999-01-26 | 2000-08-02 | Asahi Glass Co Ltd | Production of photochromic article |
JP2004018549A (en) * | 2002-06-12 | 2004-01-22 | Foundation For The Promotion Of Industrial Science | Multicolored photochromic material, method for producing the same and method for using the same |
US20140120168A1 (en) * | 2012-10-26 | 2014-05-01 | Nanocomposix, Inc. | Metastable silver nanoparticle composites |
CN107779849A (en) * | 2017-10-20 | 2018-03-09 | 东北师范大学 | Narrow-band absorption silver/titanium dioxide thin film holographic material and preparation method and application |
CN110452403A (en) * | 2019-08-08 | 2019-11-15 | 东北师范大学 | A kind of flexible nano composite holographic memory films, method for manufacturing thin film and application |
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