CN108153112B - Graphene oxide doped photopolymer holographic recording material and preparation method thereof - Google Patents
Graphene oxide doped photopolymer holographic recording material and preparation method thereof Download PDFInfo
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- CN108153112B CN108153112B CN201711146415.XA CN201711146415A CN108153112B CN 108153112 B CN108153112 B CN 108153112B CN 201711146415 A CN201711146415 A CN 201711146415A CN 108153112 B CN108153112 B CN 108153112B
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/027—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds
- G03F7/028—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds with photosensitivity-increasing substances, e.g. photoinitiators
- G03F7/031—Organic compounds not covered by group G03F7/029
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
Abstract
The invention provides a photopolymer holographic recording material doped with graphene oxide and a preparation method thereof. The preparation process comprises the steps of respectively adding a monomer solution and a graphene oxide solution into a polyvinyl alcohol solution, uniformly stirring, adding a photosensitizer solution, removing bubbles by an ultrasonic method to obtain a photopolymer sol, uniformly coating the photopolymer sol on a clean substrate, and fully volatilizing moisture to obtain the photopolymer holographic recording material. The material prepared by the invention has excellent holographic performance and dimensional stability, and is suitable for holographic three-dimensional display and volume holographic storage.
Description
Technical Field
The invention relates to the field of optical recording materials, in particular to a graphene oxide doped photopolymer film photosensitive material for holographic recording and a preparation method thereof.
Background
Optical storage technology is gradually replacing the traditional magnetic storage technology and occupies the mainstream of information storage. The optical storage technology widely used at present is two-dimensional optical disc storage, and the binary data reading of 0 or 1 is mainly realized by whether laser is reflected on a local point on the surface of the optical disc or not. However, with the advent of the age of storing big data information, the limitations of optical disc storage become more and more obvious, which mainly manifests as: firstly, under the influence of system diffraction limitation and the like, the storage density approaches to the theoretical limit; the second is that the "serial" way of storing and reading out bits limits the data transmission rate.
Holographic storage is considered to be the most likely next-generation optical storage technology to be implemented, which records and reproduces information in a holographic manner and has the characteristics of high storage density, high transmission rate, high redundancy, and the like. Among them, volume holographic storage is a representative holographic storage technology. The volume holographic storage technology with ultra-high storage density and ultra-fast transmission rate puts a series of strict requirements on the performance of a recording material, such as the requirement of simultaneously having holographic storage performances of large dynamic range, high sensitivity, good dimensional stability, high optical quality, proper thickness and the like. Although the traditional photopolymer recording material has the characteristics of better holographic performance, no need of post-humidification treatment and the like, the water-soluble material also generally has the problems of large contractibility, unstable holographic performance, poor long-term storage performance and the like.
Disclosure of Invention
The invention aims to solve the problems and provides a photopolymer holographic recording material doped with graphene oxide and a preparation method thereof, which can inhibit shrinkage of the material, improve dimensional stability and improve holographic performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
the photopolymer holographic recording material doped with graphene oxide comprises polyvinyl alcohol, acrylamide, methylene bisacrylamide, triethanolamine, a photosensitizer and graphene oxide. The weight percentage (wt%) of the components is as follows: 40-60% of polyvinyl alcohol, 10-30% of acrylamide, 0-10% of methylene bisacrylamide, 20-40% of triethanolamine, 0.05-0.3% of photosensitizer and 0.1-10% of graphene oxide. Wherein the alcoholysis degree of the polyvinyl alcohol is 80-99%. The photosensitizer is selected from one or more of the following: eosin Y, erythrosin B, methylene blue, acridine orange.
The preparation method of the photopolymer holographic recording material doped with graphene oxide comprises the following steps:
cleaning a substrate: cutting the optical glass sheet into proper sizes, firstly cleaning the optical glass sheet in an ultrasonic cleaner by using absolute ethyl alcohol, then washing the optical glass sheet by using deionized water, and finally drying the optical glass sheet in a drying oven for later use;
preparing a polyvinyl alcohol solution, a monomer solution, a graphene oxide solution and a photosensitizer solution respectively;
respectively adding the monomer solution and the graphene oxide solution into the polyvinyl alcohol solution for mixing, adding the photosensitizer solution after uniformly stirring, and finally removing bubbles by using an ultrasonic method to prepare the photopolymer sol;
and fourthly, uniformly coating the photopolymer sol on a clean substrate, standing for 36-48 h for natural airing, and obtaining the photopolymer holographic recording material after moisture is fully volatilized.
And the step two-four is carried out in a darkroom environment at the temperature of 20-25 ℃ and the relative humidity of 40-60%.
The preparation method of the polyvinyl alcohol solution comprises the following steps: adding polyvinyl alcohol into deionized water, stirring at normal temperature for 10min, after full swelling, heating in a water bath to gradually increase the temperature to 60-90 ℃, stirring while heating, simultaneously limiting the temperature rise speed to be not more than 150 ℃/h, and the stirring speed to be 60-100 r/min, and dissolving for 4h to obtain a polyvinyl alcohol solution.
The preparation method of the monomer solution comprises the following steps: adding acrylamide and methylene bisacrylamide into deionized water, heating in a constant-temperature water bath at 30-50 ℃, uniformly stirring, adding a photoinitiator triethanolamine, and continuously uniformly stirring to obtain a monomer solution.
The preparation method of the graphene oxide solution comprises the following steps: adding graphene oxide into deionized water, heating in a constant-temperature water bath at 30-50 ℃, and uniformly stirring to obtain a graphene oxide solution.
The preparation method of the photosensitizer solution comprises the following steps: adding a photosensitizer into deionized water, heating in a constant-temperature water bath at 30-50 ℃, and uniformly stirring to obtain a photosensitizer solution.
The working mechanism of the photopolymer holographic recording material doped with graphene oxide is based on the double diffusion effect under coherent light irradiation to form a holographic grating. Due to the large refractive index modulation and excellent mechanical and optical properties of the graphene oxide, the prepared holographic recording material has the following advantages: after the holographic recording is finished, the recorded information of the material is stable, the weather resistance is strong, and the storage life is long; high diffraction efficiency, resolution and sensitivity, and is suitable for large-capacity holographic storage and three-dimensional display.
Detailed Description
The invention is further illustrated by the following specific examples.
Example 1
The photopolymer holographic recording material doped with graphene oxide comprises the following components in percentage by mass: 45.5% of polyvinyl alcohol, 12.2% of acrylamide, 2.8% of methylene bisacrylamide, 36.45% of triethanolamine, 0.05% of methylene blue and 3% of graphene oxide. Wherein, the polyvinyl alcohol is 1788 type with alcoholysis degree of 88%. The preparation method comprises the following steps:
firstly, cleaning a substrate, cutting an optical glass sheet into sizes of 60mm multiplied by 0.5mm, firstly cleaning the optical glass sheet in an ultrasonic cleaner by using absolute ethyl alcohol, then washing the optical glass sheet by using deionized water, and finally drying the optical glass sheet in a drying oven for later use;
adding 45.5g of polyvinyl alcohol into deionized water, stirring at normal temperature for 10min, after full swelling, heating in a water bath to gradually increase the temperature to 75 ℃, stirring while heating, and simultaneously limiting the temperature increase speed to 150 ℃/h and the stirring speed to 80r/min, and dissolving for 4h to obtain a polyvinyl alcohol solution;
thirdly, adding 12.2g of acrylamide and 2.8g of methylene bisacrylamide into deionized water, heating and uniformly stirring in a constant-temperature water bath at 40 ℃, then adding 36.45g of photoinitiator triethanolamine into the mixture, and continuously and uniformly stirring to obtain a monomer solution;
adding 3g of graphene oxide into deionized water, heating in a constant-temperature water bath at 40 ℃, and uniformly stirring to obtain a graphene oxide solution;
adding 0.05g of photosensitizer methylene blue into deionized water, heating in a constant-temperature water bath at 40 ℃, and uniformly stirring to obtain a photosensitizer solution;
sixthly, respectively adding the monomer solution and the graphene oxide solution into the polyvinyl alcohol solution for mixing, adding the photosensitizer solution after uniformly stirring, and finally removing bubbles by using an ultrasonic method to obtain the photopolymer sol;
seventhly, uniformly coating a proper amount of the photopolymer sol on a clean substrate, standing for 42h for naturally drying, and fully volatilizing moisture to obtain the photopolymer holographic recording material.
And (c) carrying out the step (c) under the conditions of a dark room environment, a temperature of 22 ℃ and a relative humidity of 50%.
Example 2
The photopolymer holographic recording material doped with graphene oxide comprises the following components in percentage by mass: 60% of polyvinyl alcohol, 10% of acrylamide, 5% of methylene bisacrylamide, 20% of triethanolamine, 0.05% of eosin Y + methylene blue and 4.95% of graphene oxide. Wherein, the polyvinyl alcohol is 1780 type with alcoholysis degree of 80%. The preparation method comprises the following steps:
firstly, cleaning a substrate, cutting an optical glass sheet into sizes of 60mm multiplied by 0.5mm, firstly cleaning the optical glass sheet in an ultrasonic cleaner by using absolute ethyl alcohol, then washing the optical glass sheet by using deionized water, and finally drying the optical glass sheet in a drying oven for later use;
adding 60g of polyvinyl alcohol into deionized water, stirring at normal temperature for 10min, after full swelling, heating in water bath to gradually increase the temperature to 60 ℃, stirring while heating, simultaneously limiting the temperature increase speed to 130 ℃/h, and the stirring speed to 60r/min, and dissolving for 4h to obtain a polyvinyl alcohol solution;
thirdly, adding 10g of acrylamide and 5g of methylene bisacrylamide into deionized water, heating and uniformly stirring in a constant-temperature water bath at 30 ℃, then adding 20g of photoinitiator triethanolamine into the mixture, and continuously and uniformly stirring to obtain a monomer solution;
adding 4.95g of graphene oxide into deionized water, heating in a constant-temperature water bath at 30 ℃, and uniformly stirring to obtain a graphene oxide solution;
adding 0.05g of photosensitizer eosin Y + methylene blue into deionized water, heating in a constant-temperature water bath at 30 ℃, and uniformly stirring to obtain a photosensitizer solution;
sixthly, respectively adding the monomer solution and the graphene oxide solution into the polyvinyl alcohol solution for mixing, adding the photosensitizer solution after uniformly stirring, and finally removing bubbles by using an ultrasonic method to obtain the photopolymer sol;
seventhly, uniformly coating a proper amount of the photopolymer sol on a clean substrate, standing for 36h for naturally drying, and fully volatilizing moisture to obtain the photopolymer holographic recording material.
And (c) carrying out the step (c) under the conditions of a dark room environment, the temperature of 20 ℃ and the relative humidity of 40%.
Example 3
The photopolymer holographic recording material doped with graphene oxide comprises the following components in percentage by mass: polyvinyl alcohol 40%, acrylamide 30%, triethanolamine 25.4%, eosin Y + acridine orange 0.1%, and graphene oxide 4.5%. Wherein, the polyvinyl alcohol is 1799 type with alcoholysis degree of 99%. The preparation method comprises the following steps:
firstly, cleaning a substrate, cutting an optical glass sheet into sizes of 60mm multiplied by 0.5mm, firstly cleaning the optical glass sheet in an ultrasonic cleaner by using absolute ethyl alcohol, then washing the optical glass sheet by using deionized water, and finally drying the optical glass sheet in a drying oven for later use;
adding 40g of polyvinyl alcohol into deionized water, stirring at normal temperature for 10min, after full swelling, heating in water bath to gradually increase the temperature to 90 ℃, stirring while heating, and simultaneously limiting the temperature increase speed to 130 ℃/h and the stirring speed to 100r/min, and dissolving for 4h to obtain a polyvinyl alcohol solution;
thirdly, adding 30g of acrylamide into deionized water, heating and uniformly stirring in a constant-temperature water bath at 50 ℃, then adding 25.4g of photoinitiator triethanolamine and continuously and uniformly stirring to prepare a monomer solution;
adding 4.5g of graphene oxide into deionized water, heating in a constant-temperature water bath at 50 ℃, and uniformly stirring to obtain a graphene oxide solution;
adding 0.1g of photosensitizer eosin Y + acridine orange into deionized water, heating in a constant-temperature water bath at 50 ℃, and uniformly stirring to obtain a photosensitizer solution;
sixthly, respectively adding the monomer solution and the graphene oxide solution into the polyvinyl alcohol solution for mixing, adding the photosensitizer solution after uniformly stirring, and finally removing bubbles by using an ultrasonic method to obtain the photopolymer sol;
seventhly, uniformly coating a proper amount of the photopolymer sol on a clean substrate, standing for 48h, naturally airing, and fully volatilizing moisture to obtain the photopolymer holographic recording material.
And (c) carrying out the step (c) under the conditions of a dark room environment, a temperature of 25 ℃ and a relative humidity of 60%.
Example 4
The photopolymer holographic recording material doped with graphene oxide comprises the following components in percentage by mass: 45% of polyvinyl alcohol, 12% of acrylamide, 10% of methylene bisacrylamide, 22.8% of triethanolamine, 0.2% of erythrosine B + acridine orange + methylene blue and 10% of graphene oxide. Wherein, the polyvinyl alcohol is 1785 type with alcoholysis degree of 85%. The preparation method comprises the following steps:
firstly, cleaning a substrate, cutting an optical glass sheet into sizes of 60mm multiplied by 0.5mm, firstly cleaning the optical glass sheet in an ultrasonic cleaner by using absolute ethyl alcohol, then washing the optical glass sheet by using deionized water, and finally drying the optical glass sheet in a drying oven for later use;
adding 45g of polyvinyl alcohol into deionized water, stirring at normal temperature for 10min, after full swelling, heating in water bath to gradually increase the temperature to 70 ℃, stirring while heating, and simultaneously limiting the temperature increase speed to 130 ℃/h and the stirring speed to 70r/min, and dissolving for 4h to obtain a polyvinyl alcohol solution;
thirdly, adding 12g of acrylamide and 10g of methylene bisacrylamide into deionized water, heating and uniformly stirring in a constant-temperature water bath at 35 ℃, then adding 22.8g of photoinitiator triethanolamine into the mixture, and continuously and uniformly stirring to obtain a monomer solution;
adding 10g of graphene oxide into deionized water, heating in a constant-temperature water bath at 35 ℃, and uniformly stirring to obtain a graphene oxide solution;
adding 0.2g of photosensitizer erythrosine B, acridine orange and methylene blue into deionized water, heating in a constant-temperature water bath at 35 ℃, and uniformly stirring to obtain a photosensitizer solution;
sixthly, respectively adding the monomer solution and the graphene oxide solution into the polyvinyl alcohol solution for mixing, adding the photosensitizer solution after uniformly stirring, and finally removing bubbles by using an ultrasonic method to obtain the photopolymer sol;
seventhly, uniformly coating a proper amount of the photopolymer sol on a clean substrate, standing for 40h, naturally airing, and fully volatilizing moisture to obtain the photopolymer holographic recording material.
And (c) carrying out the step (c) under the conditions of a dark room environment, a temperature of 21 ℃ and a relative humidity of 45%.
Example 5
The photopolymer holographic recording material doped with graphene oxide comprises the following components in percentage by mass: polyvinyl alcohol 43%, acrylamide 14.6%, methylene bisacrylamide 2%, triethanolamine 40%, eosin Y + erythrosine B + acridine orange + methylene blue 0.3%, and graphene oxide 0.1%. Wherein, the polyvinyl alcohol is 1788 type with alcoholysis degree of 88%. Wherein, the polyvinyl alcohol is 1790 type with alcoholysis degree of 90%. The preparation method comprises the following steps:
firstly, cleaning a substrate, cutting an optical glass sheet into sizes of 60mm multiplied by 0.5mm, firstly cleaning the optical glass sheet in an ultrasonic cleaner by using absolute ethyl alcohol, then washing the optical glass sheet by using deionized water, and finally drying the optical glass sheet in a drying oven for later use;
adding 43g of polyvinyl alcohol into deionized water, stirring at normal temperature for 10min, after full swelling, heating in water bath to gradually increase the temperature to 80 ℃, stirring while heating, and simultaneously limiting the temperature increase speed to 130 ℃/h and the stirring speed to 90r/min, and dissolving for 4h to obtain a polyvinyl alcohol solution;
thirdly, adding 14.6g of acrylamide and 2g of methylene bisacrylamide into deionized water, heating and uniformly stirring in a constant-temperature water bath at 45 ℃, then adding 40g of photoinitiator triethanolamine into the mixture, and continuously and uniformly stirring to obtain a monomer solution;
adding 0.1g of graphene oxide into deionized water, heating in a constant-temperature water bath at 45 ℃, and uniformly stirring to obtain a graphene oxide solution;
adding 0.3g of photosensitizer eosin Y, erythrosin B, acridine orange and methylene blue into deionized water, heating in a constant-temperature water bath at 45 ℃, and uniformly stirring to obtain a photosensitizer solution;
sixthly, respectively adding the monomer solution and the graphene oxide solution into the polyvinyl alcohol solution for mixing, adding the photosensitizer solution after uniformly stirring, and finally removing bubbles by using an ultrasonic method to obtain the photopolymer sol;
seventhly, uniformly coating a proper amount of the photopolymer sol on a clean substrate, standing for 44h, naturally airing, and fully volatilizing moisture to obtain the photopolymer holographic recording material.
And (c) carrying out the step (c) under the conditions of a dark room environment, the temperature of 24 ℃ and the relative humidity of 55%.
Claims (7)
1. A preparation method of a photopolymer holographic recording material doped with graphene oxide is characterized by comprising the following steps:
the components of the photopolymer holographic recording material doped with graphene oxide comprise polyvinyl alcohol, acrylamide, methylene bisacrylamide, triethanolamine, a photosensitizer and graphene oxide; the weight percentages of the components are as follows: 40-60% of polyvinyl alcohol, 10-30% of acrylamide, 0-10% of methylene bisacrylamide, 20-40% of triethanolamine, 0.05-0.3% of photosensitizer and 0.1-10% of graphene oxide;
the method comprises the following steps:
cleaning a substrate: cutting the optical glass sheet into proper sizes, firstly ultrasonically cleaning the optical glass sheet by using absolute ethyl alcohol, then washing the optical glass sheet by using deionized water, and then drying the optical glass sheet for later use;
preparing a polyvinyl alcohol solution, a monomer solution, a graphene oxide solution and a photosensitizer solution respectively;
respectively adding the monomer solution and the graphene oxide solution into the polyvinyl alcohol solution for mixing, adding the photosensitizer solution after uniformly stirring, and finally removing bubbles by using an ultrasonic method to prepare the photopolymer sol;
uniformly coating the photopolymer sol on a clean substrate, standing for 36-48 h for natural airing, and fully volatilizing moisture to obtain a photopolymer holographic recording material;
and the step two-four is carried out in a darkroom environment at the temperature of 20-25 ℃ and the relative humidity of 40-60%.
2. The method for preparing a graphene oxide-doped photopolymer holographic recording material according to claim 1, wherein the alcoholysis degree of the polyvinyl alcohol is 80-99%.
3. The method for preparing a graphene oxide-doped photopolymer holographic recording material according to claim 1, wherein the photosensitizer is selected from one or more of the following: eosin Y, erythrosin B, methylene blue, acridine orange.
4. The method for preparing a graphene oxide-doped photopolymer holographic recording material according to claim 1, wherein the method for preparing a polyvinyl alcohol solution comprises: adding polyvinyl alcohol into deionized water, stirring at normal temperature for 10min, fully swelling, heating in a water bath to 60-90 ℃, stirring while heating, limiting the temperature rise speed to be not more than 150 ℃/h, and the stirring speed to be 60-100 r/min, and dissolving for 4h to obtain a polyvinyl alcohol solution.
5. The method for preparing the graphene oxide-doped photopolymer holographic recording material according to claim 4, wherein the method for preparing the monomer solution comprises: adding acrylamide and methylene bisacrylamide into deionized water, heating in a constant-temperature water bath at 30-50 ℃, uniformly stirring, adding triethanolamine, and continuously uniformly stirring to obtain a monomer solution.
6. The method for preparing a graphene oxide-doped photopolymer holographic recording material according to claim 4, wherein the method for preparing a graphene oxide solution comprises: adding graphene oxide into deionized water, heating in a constant-temperature water bath at 30-50 ℃, and uniformly stirring to obtain a graphene oxide solution.
7. The method for preparing the graphene oxide-doped photopolymer holographic recording material according to claim 4, wherein the method for preparing the photosensitizer solution comprises: adding a photosensitizer into deionized water, heating in a constant-temperature water bath at 30-50 ℃, and uniformly stirring to obtain a photosensitizer solution.
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| CN111007697A (en) * | 2019-12-13 | 2020-04-14 | 北京航空航天大学 | Water-soluble photopolymer based on refractive index modulation and holographic recording material |
| CN112885417B (en) * | 2021-01-21 | 2023-08-01 | 福建师范大学 | GO doped PQ-PMMA photopolymer holographic storage material, preparation method thereof and holographic optical disk |
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| CN1963664A (en) * | 2006-12-07 | 2007-05-16 | 河南大学 | Photosensitive hologram recording material of shortwave wide band and preparing method of the same |
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