CN112379473A - Flexible tunable deep ultraviolet band-pass filter and preparation method thereof - Google Patents
Flexible tunable deep ultraviolet band-pass filter and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a flexible tunable deep ultraviolet band-pass filter and a preparation method thereof, wherein a refractive index adjusting material and an organic polymer matrix are uniformly mixed to be used as a main composite material; mixing the micro-nano scale scattering material with the main composite material, adding a curing agent, and uniformly stirring to prepare an optical scattering material; and pouring the optical scattering material into a PMMA (polymethyl methacrylate) mold after vacuum defoaming to be cured into a film, so as to realize the manufacture of the optical filter film, wherein the optical filter films form the flexible tunable deep ultraviolet band-pass optical filter. According to the flexible tunable deep ultraviolet band-pass filter and the preparation method thereof, the preparation of the flexible tunable deep ultraviolet band-pass filter is realized through a simple multiple doping manufacturing process, and the flexible tunable deep ultraviolet band-pass filter has the advantages of low manufacturing cost, simple manufacturing process, flexibility and tunability, no need of surface grinding, no incident angle dependency and the like.
Description
Technical Field
The invention relates to the technical field of preparation of deep ultraviolet band-pass filters, in particular to a flexible tunable deep ultraviolet band-pass filter and a preparation method thereof.
Background
In daily life, optical filters made of rigid materials such as glass substrates are widely visible, such as filters of cameras, filter films of mobile phone screens, band-pass filters used in optical signal transmission processes, and the like. However, with the gradual heating of wearable optical devices, there is an increasing demand for various devices such as filters and sensors made of flexible materials. How to manufacture a flexible material device with a light filtering function becomes a subject which needs to be researched and developed vigorously.
The preparation method of the general flexible light filtering material comprises the following steps: based on the absorption or reflection characteristics of a special dielectric material, a filtering material is manufactured on the surface of the flexible light-transmitting material through multilayer coating and internal doping; or, based on the characteristics of optical interference and the like, a special structure is made of flexible materials to achieve the purpose of filtering light. In fact, the optical filter manufactured based on these methods often affects the practical effect and cost of the optical filter due to the problems of strain, incident light angle sensitivity, etc., and the optical filter manufactured based on rigid materials such as glass substrate has poor biocompatibility. Therefore, developing a new tunable filter material independent of incident light angle or strain would be of great significance to the development of low-cost, wearable optical devices.
Disclosure of Invention
The invention aims to provide a flexible tunable deep ultraviolet band-pass filter and a preparation method thereof, which realize the preparation of the flexible tunable deep ultraviolet band-pass filter through a simple multiple doping manufacturing process and have the advantages of low manufacturing cost, simple manufacturing process, flexibility and tunability, no need of surface grinding, no incident angle dependency and the like.
In order to achieve the purpose, the invention provides the following scheme:
a flexible tunable deep ultraviolet bandpass filter, the filter comprising: the optical filter thin film is formed by curing and film-forming an optical scattering material, wherein the optical scattering material comprises an organic polymer matrix, and a refractive index adjusting material and a micro-nano scale scattering material which are doped in the organic polymer matrix.
Further, the organic polymer matrix is polydimethylsiloxane PDMS material, polymethyl methacrylate PMMA or polystyrene PS or polyethylene terephthalate PET.
Further, the refractive index adjusting material is semiconductor colloidal quantum dots, perovskite quantum dots, nano compounds, nano metal compounds, organic polymers with different molecular weights or organic dyes.
Further, the micro-nano scale scattering material is ultraviolet transmission CaF2、SiO2、MgF2Or BaF2。
The invention also provides a preparation method of the flexible tunable deep ultraviolet band-pass filter, which is used for the flexible tunable deep ultraviolet band-pass filter and comprises the following steps:
s1, uniformly mixing the refractive index adjusting material and the organic polymer matrix to obtain a main composite material;
s2, mixing the scattering material with the micro-nano scale with the main composite material, adding a curing agent, and uniformly stirring to prepare the optical scattering material;
s3, pouring the optical scattering material into a PMMA mould to be solidified into a film after vacuum defoaming, and realizing the manufacture of the optical filter film, wherein the optical filter films form the flexible tunable deep ultraviolet band-pass optical filter.
Further, in the step S1, the content of the refractive index adjusting material is 0 to 90 vol.%.
Further, in the step S2, the content of the micro-nano-scale scattering material is 0.1 to 90 wt.%, and the particle size is 1 to 50000 nm.
Further, in step S2, the weight ratio of the mixture of the organic polymer matrix and the organic polymer matrix is not less than 10: curing agent was added at a ratio of 0.1.
Further, in step S3, the optical scattering material is vacuum defoamed, poured into a PMMA mold, and then placed into an environment at a temperature of less than 100 ℃ to be cured for more than 4 hours, and then taken out, so as to obtain an optical filter thin film with a thickness of 0.01-10 mm.
Further, in step S3, the flexible tunable deep ultraviolet band pass filter is formed by one, two, three, or four filter films.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects: the invention provides a flexible tunable deep ultraviolet band-pass filter and a preparation method thereof.A nano particle or a material with different refractive indexes is dispersed in an organic polymer matrix material with a common refractive index to adjust the refractive index dispersion of a composite matrix material; secondly, adding a specific scattering particle material with the refractive index similar to that of the composite matrix material; finally, after the scattering particle material and the composite matrix material are uniformly mixed, injection molding and curing are carried out to form a film, and the manufacture of the thin film optical filter is completed; the preparation method of the flexible tunable deep ultraviolet band-pass filter is realized through a simple multiple doping manufacturing process, the transparent wavelength of the flexible tunable deep ultraviolet band-pass filter can be changed along with the variety and concentration of dopants, the tunable characteristic is realized, the preparation method has the advantages of low cost, simplicity in manufacturing, flexibility, no need of surface grinding, no incident angle dependency and the like, and the preparation method can be applied to the technical fields of ultraviolet sterilization, disinfection, filtering, biochemical material detection, specific optical sensing and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
Fig. 1 is a schematic view of a process for manufacturing a flexible tunable deep ultraviolet band-pass filter according to an embodiment of the present invention;
fig. 2 is a schematic flow chart of a manufacturing process of a flexible tunable deep ultraviolet band-pass filter according to a second embodiment of the present invention;
FIG. 3 is a schematic diagram of a simulated index matching principle of the present invention;
FIG. 4 is a schematic diagram of a simulated transmittance spectrum according to the present invention;
FIG. 5 is a schematic diagram of a transmission spectrum of a filter material doped with nano-quantum dots according to an embodiment of the present invention;
FIG. 6 is a schematic diagram of the transmission spectrum of a second light filtering material doped with low molecular weight PDMS according to an embodiment of the present invention;
reference numerals: 11. a PDMS matrix; 12. CdSe/ZnS quantum dots; 13. CaF2Micro-nano particle materials; 14. a PMMA die groove; 15. a PMMA cover plate; 21. low molecular PDMS; 22. a PDMS matrix; 23. low molecular weight PDMS and PDMS matrix mixture; 24. CaF2Micro-nano particle materials; 25. a PMMA die groove; 26. and a PMMA cover plate.
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 invention aims to provide a flexible tunable deep ultraviolet band-pass filter and a preparation method thereof, which utilize the refractive index matching among mixed materials to achieve the scattering property of transmitting light at a specific wavelength and scattering light with other wavelengths, can realize the transparent wavelength tuning function by changing the doped materials, and only manufacture a novel filtering film with the filtering property by mixing and doping, thereby having profound significance for realizing the micro integration, the printable and the wearable of optical equipment.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
The invention provides a flexible tunable deep ultraviolet band-pass filter, which comprises: the optical filter thin film is formed by curing and film-forming an optical scattering material, wherein the optical scattering material comprises an organic polymer matrix, and a refractive index adjusting material and a micro-nano scale scattering material which are doped in the organic polymer matrix.
The organic polymer matrix is a polydimethylsiloxane PDMS material, polymethyl methacrylate PMMA or polystyrene PS, polyethylene terephthalate PET and other common thermoplastic optical functional polymer materials.
The refractive index regulating material is semiconductor colloid quantum dot CdSe/ZnS, CdSeS/ZnS, perovskite quantum dot and other types of quantum dot particle materials, or MgF2，TiO2Nano compounds, nano metal compounds such as Au and Ag, organic polymers with different molecular weights, organic dyes and the like. Wherein the content of the refractive index adjusting material is 0-90 vol.%. The colloid quantum dots in the refractive index adjusting material are binary, ternary or quaternary mononuclear quantum dots, or binary, ternary or quaternary core-shell quantum dots, or surface hydroxylation, amination or silanization function modified quantum dot materials.
The micro-nano scale scattering material is ultraviolet transmission CaF2，SiO2，MgF2，BaF2And the like, or other micro-nano scale particle materials with the refractive index similar to that of the organic polymer matrix. Wherein the particle size is 1-50000nm and the doping concentration is 0.1-90 wt.%.
The film thickness of the flexible thin film filter is 0.01-10 mm.
The invention can realize the tunability of the transparent wavelength of the scattering material by mixing different types of micro-nano particles, dyes or low-refractive-index polymer materials and the original PDMS matrix material. The refractive index adjusting material is introduced for tuning the center wavelength of the flexible thin film filter, and the tuning range is 200-800 nm.
The invention also provides a preparation method of the flexible tunable deep ultraviolet band-pass filter, which is used for the flexible tunable deep ultraviolet band-pass filter and comprises the following steps:
s1, uniformly mixing the refractive index adjusting material and the organic polymer matrix to obtain a main composite material;
s2, mixing the scattering material with the micro-nano scale with the main composite material, adding a curing agent, and uniformly stirring to prepare the optical scattering material;
s3, pouring the optical scattering material into a PMMA mould to be solidified into a film after vacuum defoaming, and realizing the manufacture of the optical filter film, wherein the optical filter films form the flexible tunable deep ultraviolet band-pass optical filter.
Wherein, in the step S2, the weight ratio of the mixture to the organic polymer matrix is more than or equal to 10: curing agent was added at a ratio of 0.1.
In the step S3, the optical scattering material is defoamed in vacuum, poured into a PMMA mold and a cover plate, and then placed into an environment of less than 100 ℃ to be cured for more than 4 hours, and then taken out, so as to obtain an optical filter thin film with a thickness of 0.01-10 mm. The flexible tunable deep ultraviolet band-pass filter is composed of one layer, two layers, three layers or four layers of filter films.
Example one
As shown in fig. 1, in the first embodiment of the present invention, a method for preparing a flexible tunable deep ultraviolet bandpass filter is provided, where a refractive index adjusting material is CdSe/ZnS quantum dots, and a CdSe/ZnS quantum dot-based doping scattering filter material is used as a preparation method, and the method includes the following specific steps:
s1, mixing a solution of CdSe/ZnS quantum dots 12 dispersed in toluene with a PDMS matrix 11, wherein the PDMS matrix is SIM-360, and putting the PDMS matrix into an ultrasonic device to completely evaporate the toluene in the mixture; the quantum dots respectively have the PDMS concentrations of 0 wt.%, 0.14 wt.%, 0.43 wt.%, 0.83 wt.% and 1.4 wt.%, and then the PDMS is put into a stirrer with the rotation speed higher than 1440/1440rpm (revolution/rotation) for 200s and stirred until the PDMS is uniform, in the embodiment, only CdSe/ZnS quantum dots are added to regulate the refractive index;
s2, adding CaF into the mixed solution2Micro-nano particulate material 13 at a concentration of 30 wt.% (relative to PDMS);
s3, putting the solution into a stirrer with the rotation speed of 1440/1440rpm (revolution/rotation) for stirring for 200S, and repeating the process for 1-4 times until the solution is uniformly stirred;
s4, adding a curing agent according to the weight ratio of 10:1 of PDMS, and uniformly stirring at the rotation speed of 1440/475rpm (revolution/rotation) for 90S;
s5, injecting the solution into a PMMA mold groove 14 with the depth of 0.3mm, placing the PMMA mold groove into a vacuum chamber to remove bubbles, finally covering a PMMA cover plate 15, placing the PMMA cover plate into a 50-degree environment to cure for 28 hours, and taking out the PMMA cover plate to obtain an optical filter film with the thickness of 0.3 mm.
Fig. 5 is a diagram showing the original spectrum result of the filter film tested by the spectrophotometer. As the concentration of doped CdSe/ZnS quantum dots increases, the transparent wavelength is red-shifted more.
Example two
As shown in fig. 2, the second embodiment provides a method for manufacturing a flexible tunable deep ultraviolet bandpass filter. The second embodiment is a preparation method of a low-molecular PDMS 21-based doped scattering filter material, which comprises the following specific steps:
s1, selecting low-molecular PDMS-RTV thin inner to mix with the PDMS matrix 22, wherein the PDMS matrix is selected from SIM-360, the mixing concentrations are 0 vol.%, 10 vol.%, 20 vol.% and 50 vol.%, respectively, and the mixture is put into a stirrer with the rotation speed of 1440/1440rpm (revolution/rotation) for 200S to be stirred until the mixture is uniform, and only the low-molecular PDMS is added in the embodiment to regulate the refractive index; forming a mixture 23 of low molecular PDMS and PDMS matrix;
s2, adding CaF into the mixed solution2Micro-nano particulate material 24 at a concentration of 30 wt.% (relative to PDMS);
s3, putting the solution into a stirrer with the rotation speed of 1440/1440rpm (revolution/rotation) for stirring for 200S, and repeating the process for 1-4 times until the solution is uniformly stirred;
s4, adding a curing agent according to the weight ratio of 10:1 of PDMS, and uniformly stirring at the rotation speed of 1440/475rpm (revolution/rotation) for 90S;
s5, injecting the solution into a PMMA mold groove 25 with the depth of 1mm, placing the PMMA mold groove into a vacuum chamber to remove bubbles, finally covering a PMMA cover plate 26, placing the PMMA cover plate into a 50-degree environment to be cured for 28 hours, and taking out the PMMA cover plate to obtain the optical filter film with the thickness of 1.1 mm.
As shown in fig. 6, which is a graph of the original spectrum result of the spectrophotometer test corresponding to the filter thin film, the transparent wavelength is blue-shifted more as the concentration of the doped low molecular weight PDMS is increased.
The spectrum testing apparatus and testing procedure of the second embodiment are the same as those of the first embodiment.
In the embodiment of the invention, RTV thinker and SIM-360 are 2 PDMS of Japan shiner chemical company, RTV thinker is low molecular weight PDMS, and SIM-360 is high molecular weight PDMS. The two kinds of products belong to common products in the market, and have high ultraviolet transmittance and moderate viscosity. The spectrophotometer is an ultraviolet-visible spectrophotometer V-630 of Japan Spectroscopy.
The invention is based on the principle of refractive index matching and utilizes CaF2The fundamental property of the particles in the long wavelength region is higher refractive index than the ordinary PDMS matrix (1.41). As the wavelength becomes shorter, the organic polymer PDMS matrix generally has an increased refractive index dispersion curve due to strong absorption, and the corresponding CaF2The dispersion curves rise slowly so that the dispersion curves of the two will intersect at a certain wavelength, theoretically, for light of the corresponding wavelength at the intersection point, when the two materials are mixed together, the refractive index difference is 0, and the light wave can directly pass through the mixture medium without scattering. But in other wavelength regions the two have different degrees of difference in refractive index, which will result in different degrees of scattering. Therefore, such a hybrid material will allow light of a particular wavelength to pass through while scattering light of other wavelengths. Meanwhile, the CaF is changed by changing the refractive index dispersion of the PDMS matrix, namely based on the effective medium theory, such as doping a high-refractive-index nano material to improve the refractive index of the PDMS matrix or mixing low-refractive-index PDMS to reduce the dispersion curve of the original PDMS matrix2And the refractive index intersection point of PDMS, and the tuning of the transparent wavelength is realized. FIG. 3 shows the refractive index dispersion plots of PDMS and CaF2At a certain wavelength of the light beam, the light beams intersect,and the refractive index dispersion of the original PDMS matrix is changed by doping nano materials or low-refractive index PDMS and the like, so that the mixed material and CaF2At other wavelengths. A filter separately made based on such a hybrid material will exhibit transparency at different wavelengths as shown in fig. 4. Therefore, the optical filter prepared by the method has the advantages of simple manufacturing process, low cost and no influence of the incident light angle and self strain on the optical filter performance, and is expected to be used in the fields of environmental purification equipment, ultraviolet sterilization and disinfection instruments, specific refractive index sensors and the like in the future.
The invention adopts PDMS as the matrix material, which has excellent flexibility, biocompatibility and larger thermo-optic coefficient, so that the deep ultraviolet filtering material can be used for developing wearable photonic devices and environment sterilization and disinfection equipment; the use of nanoscale quantum dot crystals and the like as refractive index adjusting materials provides the possibility of integrating high performance light sources and filters onto very small organic thin films.
The invention adopts a simple multiple doping method to manufacture the flexible scattering filter material, and combines the principle of refractive index matching and the effective medium theory to realize the characteristics of transparency and transparent wavelength tunability of the filter material at specific wavelength. Compared with absorption type, reflection type and interference type filters, the filter made of the material has the advantages that the filtering performance is not limited by incident light angles, the processing process is simple, and the manufacturing cost of devices is greatly reduced. The flexible tunable deep ultraviolet band-pass filter provided by the invention can be integrated with optical systems such as a planar lens and the like, can be integrated with a bendable flexible optical device system, and can be applied to the technical fields of ultraviolet sterilization, disinfection, filtering, biochemical material detection, specific optical sensing and the like.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. A flexible tunable deep ultraviolet bandpass filter comprising: the optical filter thin film is formed by curing and film-forming an optical scattering material, wherein the optical scattering material comprises an organic polymer matrix, and a refractive index adjusting material and a micro-nano scale scattering material which are doped in the organic polymer matrix.
2. The flexible tunable deep ultraviolet bandpass filter of claim 1 wherein the organic polymer matrix is Polydimethylsiloxane (PDMS), Polymethylmethacrylate (PMMA), Polystyrene (PS), or polyethylene terephthalate (PET).
3. The flexible tunable deep ultraviolet bandpass filter according to claim 1, wherein the refractive index adjusting material is a semiconductor colloidal quantum dot, a perovskite quantum dot, a nano compound, a nano metal compound, an organic polymer or an organic dye with different molecular weights.
4. The flexible tunable deep ultraviolet bandpass filter of claim 1, wherein the micro-nano scale scattering material is an ultraviolet transparent CaF2、SiO2、MgF2Or BaF2。
5. A method for preparing a flexible tunable deep ultraviolet band-pass filter, which is used for preparing the flexible tunable deep ultraviolet band-pass filter as claimed in any one of claims 1 to 4, and comprises the following steps:
s1, uniformly mixing the refractive index adjusting material and the organic polymer matrix to obtain a main composite material;
s2, mixing the micro-nano scale scattering material with the main composite material, adding a curing agent, and uniformly stirring to prepare an optical scattering material;
s3, pouring the optical scattering material into a PMMA mould to be solidified into a film after vacuum defoaming, and realizing the manufacture of the optical filter film, wherein the optical filter films form the flexible tunable deep ultraviolet band-pass optical filter.
6. The method for preparing a flexible tunable deep ultraviolet bandpass filter according to claim 5, wherein in the step S1, the content of the refractive index adjusting material is 0-90 vol.%.
7. The method for preparing the flexible tunable deep ultraviolet band-pass filter according to claim 5, wherein in the step S2, the content of the micro-nano scattering material is 0.1-90 wt.%, and the particle size is 1-50000 nm.
8. The method for preparing the flexible tunable deep ultraviolet band-pass filter according to claim 5, wherein in the step S2, the weight ratio of the mixture of the organic polymer matrix and the flexible tunable deep ultraviolet band-pass filter is greater than or equal to 10: curing agent was added at a ratio of 0.1.
9. The method for preparing the flexible tunable deep ultraviolet band-pass filter according to claim 5, wherein in step S3, the optical scattering material is defoamed in vacuum, poured into a PMMA mold, and then placed into an environment with a temperature less than 100 ℃ to be cured for more than 4 hours, and then taken out, so as to obtain the filter film with a thickness of 0.01-10 mm.
10. The method as claimed in claim 5, wherein in step S3, the tunable deep ultraviolet band pass filter is composed of one, two, three or four layers of filter films.
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