CN113126438A - Red sensitive photopolymer holographic dry plate and preparation method thereof - Google Patents
Red sensitive photopolymer holographic dry plate and preparation method thereof Download PDFInfo
- Publication number
- CN113126438A CN113126438A CN202110473135.XA CN202110473135A CN113126438A CN 113126438 A CN113126438 A CN 113126438A CN 202110473135 A CN202110473135 A CN 202110473135A CN 113126438 A CN113126438 A CN 113126438A
- Authority
- CN
- China
- Prior art keywords
- photopolymer
- dry plate
- polyvinyl alcohol
- red
- sensitive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 52
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 52
- 238000003756 stirring Methods 0.000 claims abstract description 32
- 239000000178 monomer Substances 0.000 claims abstract description 20
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims abstract description 19
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 19
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 18
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003504 photosensitizing agent Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- DNDJEIWCTMMZBX-UHFFFAOYSA-N n,n-dimethyl-7-methyliminophenothiazin-3-amine;hydrochloride Chemical compound [Cl-].C1=CC(=[N+](C)C)C=C2SC3=CC(NC)=CC=C3N=C21 DNDJEIWCTMMZBX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 108010010803 Gelatin Proteins 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 229920000159 gelatin Polymers 0.000 claims abstract description 14
- 239000008273 gelatin Substances 0.000 claims abstract description 14
- 235000019322 gelatine Nutrition 0.000 claims abstract description 14
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 14
- 239000011521 glass Substances 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 230000000295 complement effect Effects 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 27
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 abstract description 11
- 229920000642 polymer Polymers 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000005281 excited state Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 150000003254 radicals Chemical class 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 3
- 239000011232 storage material Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 125000000030 D-alanine group Chemical group [H]N([H])[C@](C([H])([H])[H])(C(=O)[*])[H] 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002605 large molecules Chemical class 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Images
Classifications
-
- 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
- G03F7/09—Photosensitive materials characterised by structural details, e.g. supports, auxiliary layers
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C1/00—Photosensitive materials
- G03C1/005—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
- G03C1/015—Apparatus or processes for the preparation of emulsions
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Architecture (AREA)
- Structural Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Holo Graphy (AREA)
Abstract
The invention relates to the technical field of polymer photosensitive materials, in particular to a red-sensitive photopolymer holographic dry plate and a preparation method thereof. The red-sensitive photopolymer has good diffraction effect. The preparation method comprises the following steps: firstly, adding polyvinyl alcohol into deionized water, and stirring to fully dissolve the polyvinyl alcohol to prepare polyvinyl alcohol gelatin; then, sequentially adding monomer acrylamide, complementary monomer N, N' -methylene bisacrylamide, photoinitiator triethanolamine and photosensitizer methylene blue or azure I into 5-10ml of deionized water, fully and uniformly stirring to completely dissolve the monomers, adding the solution into polyvinyl alcohol gelatin, and uniformly stirring to form photopolymer sol; and finally, uniformly coating the photopolymer sol on a clean glass substrate, and drying in a dark room to obtain the photopolymer dry plate sensitive to red light.
Description
Technical Field
The invention relates to the technical field of polymer photosensitive materials, in particular to a red-sensitive photopolymer holographic dry plate and a preparation method thereof.
Background
In the present situation, silver salt emulsion storage materials are most commonly used, but the materials have many disadvantages, and because of the photosensitive characteristics of the materials, the materials can only be used in a dark room, which undoubtedly brings inconvenience to holographic experiments. In addition, the silver salt emulsion storage material is severely restricted in practicality and commercialization due to the reasons of low diffraction efficiency, difficulty in selection of response wavelength, high manufacturing cost and the like, and thus a novel material is sought.
Photopolymer materials offer an absolute advantage over silver salt latex storage materials, both in terms of performance and fabrication process.
In terms of performance, the photopolymer material has the advantages of wide spectral response range, large refractive index modulation degree, high diffraction efficiency and the like;
in terms of manufacturing process, the method has the advantages of relatively simple synthesis and manufacturing conditions, large-area production, relatively low cost and the like;
thus, the value of the photopolymer is higher both commercially and in practical use, which has also made it a hot spot for research in recent years both at home and abroad.
Disclosure of Invention
In view of this, the present invention provides a red-sensitive photopolymer holographic dry plate and a method for preparing the same.
In order to solve the problems in the prior art, the technical scheme of the invention is as follows: a preparation method of a red sensitive photopolymer holographic dry plate is characterized by comprising the following steps: the preparation method comprises the following steps:
firstly, adding polyvinyl alcohol into deionized water, and stirring to fully dissolve the polyvinyl alcohol to prepare polyvinyl alcohol gelatin;
then, sequentially adding monomer acrylamide, complementary monomer N, N' -methylene bisacrylamide, photoinitiator triethanolamine and photosensitizer methylene blue or azure I into 5-10ml of deionized water, fully and uniformly stirring to completely dissolve the monomers, adding the solution into polyvinyl alcohol gelatin, and uniformly stirring to form photopolymer sol;
and finally, uniformly coating the photopolymer sol on a clean glass substrate, and drying in a dark room to obtain the photopolymer dry plate sensitive to red light.
Further, the polyvinyl alcohol gelatin is 5-30 wt% aqueous solution;
the concentrations of the acrylamide, the N, N' -methylene bisacrylamide, the triethanolamine and the methylene blue or azure I are respectively 0.25-0.4mol/L, 0.04-0.07mol/L, 0.25-0.4mol/L, 4 x 10-4-7 x 10-4mol/L and 7.5 x 10-4mol/L to 9.5 x 10-4 mol/L.
Further, the polyvinyl alcohol gelatin is preferably 10-20 wt% aqueous solution;
the concentration of the acrylamide, the N, N' -methylene bisacrylamide, the triethanolamine and the methylene blue or azure I is preferably 0.3-0.35mol/L, 0.05-0.06mol/L, 0.3-0.35mol/L, 5 x 10-4-6 x 10-4mol/L and 8 x 10-4mol/L-9 x 10-4mol/L respectively.
Further, the stirring temperature is 60-80 ℃ and the stirring time is 1 hour when preparing the polyvinyl alcohol gelatin.
Further, the temperature of stirring the photopolymer sol was 40 ℃ and the stirring time was 1 hour.
Further, the glass substrate coated with the photopolymer sol is dried in a dark room under a yellow safety lamp.
Further, the prepared photopolymer dry plate is placed under the conditions that the humidity is 65-75% and the temperature is 20-25 ℃ for 36-48 hours.
Further, when the dry plate is coated, a manual coating method or a machine coating method is adopted.
The photopolymer holographic dry plate sensitive to red light is prepared by the preparation method.
Compared with the prior art, the invention has the following advantages:
1) the binder of the method is polyvinyl alcohol, the monomer is acrylamide, the complementary monomer is N, N' -methylene bisacrylamide, the photoinitiator is triethanolamine, and the photosensitizer is methylene blue or azure I (the peak value of the wavelength absorbed by the methylene blue is 667nm, and the peak value of the wavelength absorbed by the azure I is 649 nm). The photosensitizer forms a photosensitizer excited state under the irradiation of laser, the photoinitiator reacts with the photosensitizer excited state to generate photoinitiator ionic free radicals, and finally, the photoinitiator ionic free radicals react with monomers to form a photopolymer.
2) The dry plate prepared by the invention can be used for holographic photographing even in daytime or under the background of external stray light, and is mainly sensitive to red light;
3) experiments show that the red-sensitive photopolymer dry plate prepared by the invention has good diffraction effect, and the absorption peak value of the red-sensitive photopolymer dry plate reaches 85% in a narrow bandwidth region at 650 nm.
Description of the drawings:
FIG. 1 is a schematic diagram of the exposure light path of the present invention for a red sensitive photopolymer holographic dry plate;
FIG. 2 is a diffraction pattern for a red sensitive photopolymer holographic dry plate after exposure;
FIG. 3 is a graph of the spectral absorption of a red sensitive photopolymer holographic dry plate.
Detailed Description
The invention provides a preparation method of a photopolymer holographic dry plate sensitive to red light, which comprises the following steps:
firstly, adding polyvinyl alcohol into deionized water, and stirring to fully dissolve the polyvinyl alcohol to prepare polyvinyl alcohol gelatin;
then, sequentially adding monomer acrylamide, complementary monomer N, N' -methylene bisacrylamide, photoinitiator triethanolamine and photosensitizer methylene blue or azure I into 5-10ml of deionized water, fully and uniformly stirring to completely dissolve the monomers, adding the solution into polyvinyl alcohol gelatin, and uniformly stirring (the stirring temperature is 40 ℃ and the stirring time is 1 hour) to form photopolymer sol;
and finally, uniformly coating the sol on a clean glass substrate, and drying in a dark room to obtain the red light sensitive photopolymer dry plate.
Invention sheetThe compound is acrylamide with molecular formula of C3H5NO, molecular weight 71.08.
The complementary monomer is N, N' -methylene bisacrylamide and the molecular formula is C7H10N2O2And the molecular weight is 154.17.
The photoinitiator is triethanolamine with molecular formula of C6H15NO3And the molecular weight is 149.19.
The photosensitizer is methylene blue or azure I, and the molecular formula of the methylene blue is C16H18Cl4I4O5Molecular weight 373.9, and absorption wavelength peak around 667 nm; azure I molecular formula C15H16ClN3S, molecular weight 305.83, and absorption wavelength peak around 649 nm. Azure I adopted by the invention.
The aqueous solution of polyvinyl alcohol is used as a binder, and the aqueous solution of polyvinyl alcohol is 5-30 wt% aqueous solution, preferably 10-20 wt% aqueous solution.
Wherein, the dosage of the acrylamide is 0.25-0.4mol/L of the polyvinyl alcohol aqueous solution, preferably 0.3-0.35mol/L of the polyvinyl alcohol aqueous solution; aqueous polyvinyl alcohol solutions in which the amount of N, N' -methylenebisacrylamide used is from 0.04 to 0.07mol/L, preferably from 0.05 to 0.06 mol/L; the dosage of the triethanolamine is 0.25 to 0.4mol/L of polyvinyl alcohol aqueous solution, preferably 0.3 to 0.35 mol/L; the methylene blue is used in an amount of 4 × 10-4-7×10-4mol/L aqueous polyvinyl alcohol solution, preferably 5X 10-4-6×10-4mol/L; the dosage of azure I is 7.5 × 10-4mol/L-9.5×10-4mol/L aqueous polyvinyl alcohol solution, preferably 8X 10- 4mol/L-9×10-4mol/L。
The photopolymerization process is a process of combining small molecules or monomers into large molecules or polymers, and several conditions are necessary for completing the process: firstly, the invention selects proper monomer; and preparing a corresponding initiator. Different monomers, different initiators, different photosensitive wavelengths and different quantum yields. Therefore, the invention adopts the combination to ensure that the prepared photopolymer holographic dry plate has higher diffraction efficiency.
The following is the reaction formula for photopolymer formation:
as shown in the formula, DYE is a photosensitizer*The photosensitizer is in a photosensitizer excited state, and the photosensitizer is irradiated by laser to obtain light energy hv and absorb photons with specific wavelength, so that the photosensitizer excited state is formed. Am is a photoinitiator, and the photoinitiator reacts with the excited state of the photosensitizer to generate photoinitiator ion free radicals Am*Meanwhile, the photosensitizer is bleached to form photosensitizer bleaching LDYE. Finally, the photoinitiator ionic free radical and the monomer M are subjected to polymerization reaction to form a photopolymer P, wherein lambda and lambda' are reaction constants.
The following are detailed procedures for preparing the red-sensitive photopolymer:
a. at normal room temperature, a beaker is filled with a proper amount of deionized water, then the beaker is placed into a larger vessel filled with water, the vessel is placed on a multi-head magnetic heating stirrer, a switch is turned on, the temperature is regulated to 60-80 ℃, the rotating speed is set to be 400rad/min, then the weighed polyvinyl alcohol is slowly poured into the beaker, the polyvinyl alcohol is stirred and dissolved for about 1 hour, and polyvinyl alcohol sol with the mass percentage concentration of 10-20 wt% is obtained after the polyvinyl alcohol sol is completely dissolved;
b. weighing a proper amount of acrylamide and N, N ' -methylene bisacrylamide, dissolving the acrylamide and the N, N ' -methylene bisacrylamide in 5ml of deionized water by using a small beaker, putting the small beaker on a stirrer, heating to about 30 ℃, and fully stirring for about 20 minutes to fully dissolve the acrylamide and the N, N ' -methylene bisacrylamide;
c. c, dripping a proper amount of triethanolamine into the solution obtained in the step b by using a plastic dropper, heating to 30 ℃, and stirring for about 5 minutes to fully and uniformly mix the triethanolamine and the solution;
d. weighing a proper amount of methylene blue under the safety environment of a yellow lamp, adding the methylene blue into the solution obtained in the step c, and stirring for 30 minutes to fully and uniformly dissolve the methylene blue;
e. and (c) slowly pouring the prepared solution in the step (d) into the polyvinyl alcohol sol in the step (a) and stirring for 30 minutes to ensure that the solution is sufficiently and uniformly mixed, and shaking to remove bubbles in the solution to obtain a bubble-free and uniform photosensitive mixed solution. Then the sol in the beaker is sealed by a black reagent bottle, wrapped by black paper and placed in a dark dry place to prepare the photopolymer sol, and the prepared dry plate is placed in a dark room with the humidity of 65-75% and the temperature of 20-25 ℃ for 36-48 hours.
The dry board preparation method is generally divided into two methods, one is a manual smearing method and the other is a machine smearing method.
The manual smearing method comprises the steps of dripping 2-3ml of sol on a clean glass sheet by using a plastic dropper, then enabling the sol to naturally flow, enabling the sol to be evenly smeared on the surface of the glass sheet, and finally placing the glass sheet into a dark and dry box to be dried for 36-48 hours.
Machine coating is to use a spin coater to coat the dry plate. Firstly, putting a clean optical glass sheet into a spin coater, sucking the sheet, dripping about 3ml of sol on the glass sheet by using a plastic dropper, and then adjusting the rotating speed, wherein the low rotating speed is set to be 400rad/min and the time is 18s, and the high rotating speed is set to be 1400rad/min and the time is 30 s. And taking out the dry plate after coating, and putting the dry plate into a dark dry box for drying for 36-48 hours. After drying, the dry photopolymer film required in the experiment is obtained.
After obtaining the red light sensitive photopolymer holographic dry plate, preferably using a He-Ne laser as a light source, using a key as a material object, adopting a transmission holographic imaging method, selecting a certain light intensity ratio of object light to reference light and reference light intensity, setting the angles of the two beams of light, and obtaining an image of the object after exposure.
As shown in fig. 1, it is a schematic diagram of the exposure light path of the red-sensitive photopolymer holographic dry plate, and in this exposure, a mach zehnder light path diagram is selected, La is He-Ne laser, L1 is beam expander, L2 is collimator lens, P1 and P2 are 5: 5 spectroscope, M1, M2 plane mirrors, Sam dry plate sample. Laser emitted by a laser is expanded by L1, collimated by L2, split by P1 to form object light and reference light, reflected by M1 and M2, converged at one point, and irradiated on a dry plate sample to form interference fringes on the dry plate. FIG. 2 is a diffraction diagram of the holographic dry plate of the red sensitive photopolymer after exposure, wherein the central bright spot is a zero-order diffraction spot, and the two small spots beside the bright spot are first-order diffraction spots.
The sensitive wave band of the material is mainly concentrated on a red light wave band, and the peak wavelength is about 650 nm. As shown in FIG. 3, the absorption peak of the red-sensitive photopolymer reaches 85% in a narrow bandwidth region at 650nm, and according to the photoreaction mechanism of the holographic recording material, the photosensitizer component in the recording medium in the holographic recording process can only absorb photons of a specific photosensitive band to initiate a photochemical reaction.
For further understanding of the present invention, the following embodiments are provided to illustrate the technical solutions of the present invention in detail, and the scope of the present invention is not limited by the following embodiments.
Example 1
a. At normal room temperature, a beaker is filled with a proper amount of deionized water, then the beaker is placed into a larger vessel filled with water, the vessel is placed on a multi-head magnetic heating stirrer, a switch is turned on, the temperature is regulated to 60-80 ℃, the rotating speed is set to be 400rad/min, then the weighed polyvinyl alcohol is slowly poured into the beaker, the polyvinyl alcohol is stirred and dissolved for about 1 hour, and the polyvinyl alcohol sol with the mass percentage concentration of 15 wt% is obtained after the polyvinyl alcohol sol is completely dissolved.
b. An appropriate amount of acrylamide and N, N '-methylenebisacrylamide was weighed so that the concentrations of acrylamide and N, N' -methylenebisacrylamide in the polyvinyl alcohol solution were 0.3mol/L and 0.05mol/L, respectively, and was dissolved in 5ml of deionized water using a small beaker, which was placed on a stirrer and heated to about 30 ℃ and sufficiently stirred for about 20 minutes to be sufficiently dissolved.
c. And d, dripping an appropriate amount of triethanolamine into the solution obtained in the step b by using a plastic dropper to ensure that the concentration of the triethanolamine in the polyvinyl alcohol solution is 0.3mol/L, heating to 30 ℃, and stirring for about 5 minutes to fully and uniformly mix the triethanolamine and the solution.
d. Weighing an appropriate amount of methylene blue under a yellow lamp safety environment, adding the methylene blue into the solution obtained after the step c, and enabling the concentration of the methylene blue in the polyvinyl alcohol solution to be 5 x 10-4And (3) stirring for 30 minutes to fully and uniformly dissolve the components.
e. And (c) slowly pouring the prepared solution in the step (d) into the polyvinyl alcohol sol in the step (a) and stirring for 30 minutes to ensure that the solution is sufficiently and uniformly mixed, and shaking to remove bubbles in the solution to obtain a bubble-free and uniform photosensitive mixed solution. The sol in the beaker was then sealed with a black reagent bottle and wrapped with black paper and placed in a dark dry place.
And (3) taking 2-3ml of sol, naturally flowing the sol to uniformly coat the surface of the glass sheet, and finally drying the glass sheet in a dark dry box for 36-48 hours to obtain the photopolymer dry film.
Example 2
At normal room temperature, a beaker is filled with a proper amount of deionized water, then the beaker is placed into a larger vessel filled with water, the vessel is placed on a multi-head magnetic heating stirrer, a switch is turned on, the temperature is regulated to 60-80 ℃, the rotating speed is set to be 400rad/min, then the weighed polyvinyl alcohol is slowly poured into the beaker, the polyvinyl alcohol is stirred and dissolved for about 1 hour, and the polyvinyl alcohol sol with the mass percentage concentration of 15 wt% is obtained after the polyvinyl alcohol sol is completely dissolved.
b. An appropriate amount of acrylamide and N, N '-methylenebisacrylamide was weighed so that the concentrations of acrylamide and N, N' -methylenebisacrylamide in the polyvinyl alcohol solution were 0.35mol/L and 0.06mol/L, respectively, and was dissolved in 5ml of deionized water with a small beaker, which was placed on a stirrer and heated to about 30 ℃ and sufficiently stirred for about 20 minutes to be sufficiently dissolved.
c. And d, dripping an appropriate amount of triethanolamine into the solution obtained in the step b by using a plastic dropper to ensure that the concentration of the triethanolamine in the polyvinyl alcohol solution is 0.35mol/L, heating to 30 ℃, and stirring for about 5 minutes to fully and uniformly mix the triethanolamine and the solution.
d. Weighing proper amount of azure I in a yellow lamp safety environment, adding the azure I into the solution obtained after the step c, and enabling the concentration of the azure I in the polyvinyl alcohol solution to be 8 x 10-4And (3) stirring for 30 minutes to fully and uniformly dissolve the components.
e. And (c) slowly pouring the prepared solution in the step (d) into the polyvinyl alcohol sol in the step (a) and stirring for 30 minutes to ensure that the solution is sufficiently and uniformly mixed, and shaking to remove bubbles in the solution to obtain a bubble-free and uniform photosensitive mixed solution. The sol in the beaker was then sealed with a black reagent bottle and wrapped with black paper and placed in a dark dry place.
And (3) taking 2-3ml of sol, naturally flowing the sol to uniformly coat the surface of the glass sheet, and finally drying the glass sheet in a dark dry box for 36-48 hours to obtain the photopolymer dry film.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and it should be noted that those skilled in the art should make modifications and variations without departing from the principle of the present invention.
Claims (9)
1. A preparation method of a red sensitive photopolymer holographic dry plate is characterized by comprising the following steps: the preparation method comprises the following steps:
firstly, adding polyvinyl alcohol into deionized water, and stirring to fully dissolve the polyvinyl alcohol to prepare polyvinyl alcohol gelatin;
then, sequentially adding monomer acrylamide, complementary monomer N, N' -methylene bisacrylamide, photoinitiator triethanolamine and photosensitizer methylene blue or azure I into 5-10ml of deionized water, fully and uniformly stirring to completely dissolve the monomers, adding the solution into polyvinyl alcohol gelatin, and uniformly stirring to form photopolymer sol;
and finally, uniformly coating the photopolymer sol on a clean glass substrate, and drying in a dark room to obtain the photopolymer dry plate sensitive to red light.
2. The method for preparing the red-sensitive photopolymer holographic dry plate according to claim 1, wherein the method comprises the following steps: the polyvinyl alcohol gelatin is 5-30 wt% aqueous solution;
the concentrations of the acrylamide, the N, N' -methylene bisacrylamide, the triethanolamine and the methylene blue or azure I are respectively 0.25-0.4mol/L, 0.04-0.07mol/L, 0.25-0.4mol/L, 4 x 10-4-7 x 10-4mol/L and 7.5 x 10-4mol/L to 9.5 x 10-4 mol/L.
3. The method for preparing a red-sensitive photopolymer holographic dry plate according to claim 1 or 2, wherein: the polyvinyl alcohol gelatin is preferably 10-20 wt% aqueous solution;
the concentration of the acrylamide, the N, N' -methylene bisacrylamide, the triethanolamine and the methylene blue or azure I is preferably 0.3-0.35mol/L, 0.05-0.06mol/L, 0.3-0.35mol/L, 5 x 10-4-6 x 10-4mol/L and 8 x 10-4mol/L-9 x 10-4mol/L respectively.
4. The method for preparing the red-sensitive photopolymer holographic dry plate according to claim 3, wherein the method comprises the following steps: the stirring temperature is 60-80 ℃ and the stirring time is 1 hour when preparing the polyvinyl alcohol gelatin.
5. The method for preparing the red-sensitive photopolymer holographic dry plate according to claim 4, wherein the method comprises the following steps: the temperature of stirring of the photopolymer sol was 40 ℃ and the stirring time was 1 hour.
6. The method for preparing the red-sensitive photopolymer holographic dry plate according to claim 5, wherein the method comprises the following steps: and drying the glass substrate coated with the photopolymer sol in a dark room under a yellow safety lamp environment.
7. The method for preparing the red-sensitive photopolymer holographic dry plate according to claim 6, wherein the method comprises the following steps: the prepared photopolymer dry plate is placed under the conditions that the humidity is 65-75 percent and the temperature is 20-25 ℃ for 36-48 hours.
8. The method for preparing the red-sensitive photopolymer holographic dry plate according to claim 7, wherein the method comprises the following steps: the dry plate is coated by a manual coating method or a machine coating method.
9. The red-sensitive photopolymer holographic dry plate prepared by the method of any one of claims 1 to 8.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110473135.XA CN113126438A (en) | 2021-04-29 | 2021-04-29 | Red sensitive photopolymer holographic dry plate and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110473135.XA CN113126438A (en) | 2021-04-29 | 2021-04-29 | Red sensitive photopolymer holographic dry plate and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN113126438A true CN113126438A (en) | 2021-07-16 |
Family
ID=76781037
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202110473135.XA Pending CN113126438A (en) | 2021-04-29 | 2021-04-29 | Red sensitive photopolymer holographic dry plate and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN113126438A (en) |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5213915A (en) * | 1989-05-19 | 1993-05-25 | Agency Of Industrial Science & Technology, Ministry Of International Trade & Industry | Holographic recording material and method for holographic recording |
CN1448782A (en) * | 2003-05-09 | 2003-10-15 | 中国科学院上海光学精密机械研究所 | Dual wavelength sensitive photopolymer holographic recording material and preparation method thereof |
CN108931887A (en) * | 2017-05-22 | 2018-12-04 | 北京航空航天大学 | Red-sensitive photopolymer material, preparation method and application |
-
2021
- 2021-04-29 CN CN202110473135.XA patent/CN113126438A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5213915A (en) * | 1989-05-19 | 1993-05-25 | Agency Of Industrial Science & Technology, Ministry Of International Trade & Industry | Holographic recording material and method for holographic recording |
CN1448782A (en) * | 2003-05-09 | 2003-10-15 | 中国科学院上海光学精密机械研究所 | Dual wavelength sensitive photopolymer holographic recording material and preparation method thereof |
CN108931887A (en) * | 2017-05-22 | 2018-12-04 | 北京航空航天大学 | Red-sensitive photopolymer material, preparation method and application |
Non-Patent Citations (1)
Title |
---|
高云龙: "光致聚合物的制备及其全息性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》, no. 1, 15 January 2019 (2019-01-15), pages 37 - 38 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US4139853A (en) | Laserbeam recording | |
CN108563101A (en) | Warm and humid sensitive intelligent device of a kind of photoresist, micro-nano and preparation method thereof | |
JPH0619040A (en) | Optical recording composition, film and method | |
Kinoshita et al. | Large photoinduced refractive index changes of a polymer containing photochromic norbornadiene groups | |
Navarro-Fuster et al. | Biophotopol’s energetic sensitivity improved in 300 μm layers by tuning the recording wavelength | |
CN113126438A (en) | Red sensitive photopolymer holographic dry plate and preparation method thereof | |
CN113527594B (en) | Composite initiator holographic photopolymer and method for preparing holographic recording film by using same | |
CN113589648B (en) | Double-monomer holographic photopolymer and method for preparing holographic recording film material from same | |
Weiss et al. | Organic materials for real-time holographic recording | |
CN108931887B (en) | Red sensitive photopolymer material, preparation method and application | |
JP2567257B2 (en) | Color filter | |
RU2541521C2 (en) | Liquid composition for photopolymerisation-able film for hologram recording, method of composition obtaining, method of obtaining said film | |
CN1963664A (en) | Photosensitive hologram recording material of shortwave wide band and preparing method of the same | |
CA1315591C (en) | Visible ray-recording hologram material | |
Hai et al. | Holographic property of photopolymers with different amine photoinitiators | |
Sharma et al. | Uniform holographic films of acrylamide/polyvinyl alcohol photopolymer using an automatic film applicator based on doctor blade technique | |
Fontanilla-Urdaneta et al. | Diffraction efficiency study of holographic gratings in dichromated poly (vinyl alcohol) NiCl2· 6H2O doped | |
WO2022251546A2 (en) | System and method for high resolution 3d nanofabrication | |
JPH09281878A (en) | Photosensitive agent for hologram, photosensitive material for hologram, hologram and its production | |
JP2000310932A (en) | Hologram recording material and hologram recording medium | |
SUCHITHRA | REVIEW ON PHOTOPOLYMER BASED HOLOGRAPHIC RECORDING MEDIUM | |
Leite | Photopolymerizable nanocomposites for holographic applications | |
Toxqui-López et al. | PVA glue as a recording holographic medium | |
Ibarra-Torres et al. | Holographic materials composed by rosin with ammonium dichromate (R) | |
CN116917808A (en) | Improved colour fading |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |