CN113138437A - Broadband near-infrared absorption optical filter and preparation method thereof - Google Patents
Broadband near-infrared absorption optical filter and preparation method thereof Download PDFInfo
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- CN113138437A CN113138437A CN202110248140.0A CN202110248140A CN113138437A CN 113138437 A CN113138437 A CN 113138437A CN 202110248140 A CN202110248140 A CN 202110248140A CN 113138437 A CN113138437 A CN 113138437A
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- infrared absorbent
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- 230000003287 optical effect Effects 0.000 title claims abstract description 56
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000002250 absorbent Substances 0.000 claims abstract description 29
- 230000002745 absorbent Effects 0.000 claims abstract description 25
- 239000002952 polymeric resin Substances 0.000 claims abstract description 20
- 229920003002 synthetic resin Polymers 0.000 claims abstract description 20
- 239000008187 granular material Substances 0.000 claims abstract description 17
- 238000001746 injection moulding Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 7
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 7
- 239000004417 polycarbonate Substances 0.000 claims abstract description 6
- 229920000515 polycarbonate Polymers 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 3
- -1 free radical arylamine compound Chemical class 0.000 claims description 7
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 150000002941 palladium compounds Chemical class 0.000 claims description 4
- 238000007747 plating Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910052787 antimony Inorganic materials 0.000 claims description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical group [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000006096 absorbing agent Substances 0.000 claims 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims 1
- 238000002834 transmittance Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 2
- 238000000862 absorption spectrum Methods 0.000 description 6
- 238000000411 transmission spectrum Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000003063 flame retardant Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/22—Absorbing filters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D11/00—Producing optical elements, e.g. lenses or prisms
- B29D11/00634—Production of filters
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/14—Protective coatings, e.g. hard coatings
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/208—Filters for use with infrared or ultraviolet radiation, e.g. for separating visible light from infrared and/or ultraviolet radiation
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/22—Absorbing filters
- G02B5/223—Absorbing filters containing organic substances, e.g. dyes, inks or pigments
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Toxicology (AREA)
- Manufacturing & Machinery (AREA)
- Ophthalmology & Optometry (AREA)
- Mechanical Engineering (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a broadband near-infrared absorption optical filter and a preparation method thereof; the raw materials and the weight portions of each component are as follows: 0.1-0.2 part of low-band near-infrared absorbent, 0.05-0.08 part of medium-band near-infrared absorbent, 0.4-0.6 part of high-band near-infrared absorbent and 100 parts of optical polymer resin granules; polycarbonate or polymethyl methacrylate optical polymer resin granules with high visible light transmittance are selected as base materials, and the broadband near-infrared absorption filter is obtained by using a method of injection molding after mixing optical polymer resin granules and an absorbent. The optical filter has good cut-off performance for laser within the range of 700nm to 1800nm, and simultaneously ensures certain visible light transmittance; the optical filter has high impact strength and flame retardance.
Description
Technical Field
The invention relates to the technical field of laser protection material materials, in particular to a broadband near-infrared absorption optical filter and a preparation method thereof.
Background
The laser has the characteristics of good monochromaticity, good coherence, high brightness and the like, so that the laser can be widely applied to the fields of medical treatment, processing, military affairs and the like. With the use of laser, great harm is brought to human eyes and photoelectric sensor devices, and how to effectively protect the human eyes and the photoelectric sensor devices is emphasized by people. The high-power near-infrared band laser is widely used in industrial mechanical processing such as welding, cutting, punching and the like, and dangerous reflection must be effectively shielded through an infrared filter. The existing near-infrared filter has a narrow protection waveband range and is difficult to adapt to the current situation of rapid development of increasing laser spectral lines and broadband continuous tunable lasers. The laser protection material is earlier researched in foreign countries, some laser safety irradiation limits are provided in the United states as early as 1962, multi-band goggles capable of protecting army soldiers at 532nm, 694nm and 1064nm are equipped for the army soldiers in the gulf war, the narrow absorption band is provided, and the optical density of the protection band reaches more than 4; the near-infrared laser protection plastic with strong absorption at a wave band of 780-1500 nm is developed by the national-segment latent et al (research on the near-infrared wave band laser protection plastic [ J ]. laser journal, 2001, 22(6): 57-59.). Chinese patent document CN103809231A discloses "an ultraviolet-near infrared dual-band absorption filter and a preparation method thereof", wherein the filter has good cut-off performance for laser with the wave bands of 200 nm-400 nm and 700 nm-900 nm, and simultaneously ensures a certain transmittance in the visible light region. The near infrared filter which has the protection range of the wide waveband of 700nm to 1800nm and simultaneously keeps a certain transmittance in the visible light region has not been reported in domestic documents. It is therefore highly desirable to develop a broadband near infrared absorption filter.
Disclosure of Invention
The invention aims to solve the technical problem that the existing near-infrared absorption filter has a narrow protection waveband, and provides a broadband near-infrared absorption filter with a protection waveband of 700 nm-1800 nm.
The technical scheme of the invention is as follows: optical polymer resin particles with high visible light transmittance are selected as a matrix material, the optical polymer resin particles and the near-infrared absorbent are blended, and then the broadband near-infrared absorption filter with the near-infrared absorbent molecules uniformly distributed in the optical polymer is obtained by adopting an injection molding method.
The specific technical scheme of the invention is as follows: the broadband near-infrared absorption optical filter comprises the following raw materials in parts by weight: 0.1-0.2 part of low-band near-infrared absorbent, 0.05-0.08 part of medium-band near-infrared absorbent, 0.4-0.6 part of high-band near-infrared absorbent and 100 parts of optical polymer resin granules; the main absorption wave band of the optical filter is 700 nm-1800 nm.
The low-waveband near-infrared absorbent is an octaphenoxy octaphenylamino metal phthalocyanine compound; the mid-band near-infrared absorbent is a sulfodiene palladium compound; the high-waveband near-infrared absorbent is an antimony hexa-butyl cyanide hexafluoride free radical arylamine compound; the optical polymer resin granules are polycarbonate or polymethyl methacrylate.
The invention also provides a method for preparing the broadband near-infrared absorption optical filter, which comprises the following steps:
(1) drying the optical polymer resin granules in a dryer at 100-120 ℃ for 4 h;
(2) accurately weighing optical polymer resin granules and near-infrared absorbent powder according to parts by weight, loading the optical polymer resin granules and the near-infrared absorbent powder into a mixer, adding a small amount of white oil to mix, wherein the rotating speed of the mixer is 60r/min, and the mixing time is 10min to obtain dark green semitransparent master batches;
(3) injection molding the dark green semitransparent master batch prepared in the step (2) to prepare a broadband near-infrared absorption optical filter;
(4) and (4) plating a hard film on the surface of the broadband near-infrared absorption optical filter prepared in the step (3) to improve the hardness of the surface of the optical filter.
The invention prepares the broadband near-infrared absorption optical filter by uniformly doping the near-infrared absorbent into an optical polymer matrix in a mode of blending the near-infrared absorbent and optical polymer resin particles by adopting an injection molding method; the laser protection optical density of the prepared near-infrared absorption optical filter is more than 4 in the range of 700 nm-1800 nm, and the permeability of other bands of visible light is good; the optical filter provided by the invention has good mechanical properties, wherein the impact strength of the optical filter material taking polycarbonate as a matrix is 72kJ/m2(ii) a The invention providesThe filter has flame retardance and a flame retardant grade V0. The invention has the advantages of simple preparation process, high production efficiency, adjustable thickness and shape of the prepared optical filter and low production cost.
Drawings
FIG. 1 is an absorption spectrum of a filter prepared according to example 1, with wavelength (nm) on the abscissa and optical density on the ordinate;
fig. 2 is a transmission spectrum of the optical filter prepared according to example 1, with wavelength (nm) on the abscissa and transmittance (%) on the ordinate;
FIG. 3 is an absorption spectrum of a filter prepared according to example 2, with wavelength (nm) on the abscissa and optical density on the ordinate;
fig. 4 is a transmission spectrum of the optical filter prepared according to example 2, with the wavelength (nm) on the abscissa and the transmittance (%) on the ordinate.
Detailed Description
The present invention will be described below by way of specific embodiments, but is not limited thereto and is applicable to various kinds of near-infrared absorption filters in this wavelength range.
Example 1
(1) Selecting polymethyl methacrylate optical polymer resin granules, and drying the granules in a dryer at 100 ℃ for 4 h;
(2) accurately weighing octaphenoxy octaphenylamino metal phthalocyanine compound (molecular formula: C) as low-waveband near-infrared absorbent128H88PbN16O8)1g of a compound; sulfodiene palladium compounds (molecular formula: C) as mid-band near-infrared absorbent52H52PdS6N4O4) 0.5 g; high-band near-infrared absorbent hexabutylcyanoantimony hexafluoride free radical arylamine compound (molecular formula: C)36H36N16SbF6) 4g of the total weight of the mixture; 1000g of the dried polymethyl methacrylate optical polymer resin pellets; loading into a mixer, adding a small amount of white oil for mixing, wherein the rotating speed of the mixer is 60r/min, and the mixing time is 10min to obtain dark green semitransparent master batches;
(3) and setting parameters of the injection molding machine according to the injection molding process requirement of the polymethyl methacrylate. Performing injection molding on the dark green semitransparent master batch prepared in the step (2) to prepare a broadband near-infrared absorption optical filter;
(4) and (4) plating a hard film on the surface of the broadband near-infrared absorption optical filter prepared in the step (3) to improve the hardness of the surface of the optical filter.
And (3) carrying out absorption spectrum and transmission spectrum tests on the sample obtained in the step (4) in a range of 200-1800 nm by using an Shimadzu (SHIMADZU) UV-3600 ultraviolet visible near infrared spectrophotometer, wherein the absorption spectrum is shown in a figure 1, and the transmission spectrum is shown in a figure 2.
Example 2
(1) Selecting polycarbonate optical polymer resin granules, and drying the granules in a dryer at 120 ℃ for 4 hours;
(2) accurately weighing octaphenoxy octaphenylamino metal phthalocyanine compound (molecular formula: C) as low-waveband near-infrared absorbent128H88PbN16O8)2g of the total weight of the mixture; sulfodiene palladium compounds (molecular formula: C) as mid-band near-infrared absorbent52H52PdS6N4O4) 0.8 g; high-band near-infrared absorbent hexabutylcyanoantimony hexafluoride free radical arylamine compound (molecular formula: C)36H36N16SbF6) 6g of a mixture; 1000g of the dried polymethyl methacrylate optical polymer resin pellets; loading into a mixer, adding a small amount of white oil for mixing, wherein the rotating speed of the mixer is 60r/min, and the mixing time is 10min to obtain dark green semitransparent master batches;
(3) setting parameters of an injection molding machine according to the injection molding process requirements of polycarbonate, and performing injection molding on the dark green semitransparent master batch prepared in the step (2) to prepare a broadband near-infrared absorption optical filter;
(4) and (4) plating a hard film on the surface of the broadband near-infrared absorption optical filter prepared in the step (3) to improve the hardness of the surface of the optical filter.
And (4) carrying out absorption spectrum and transmission spectrum tests on the sample obtained in the step (4), wherein the absorption spectrum is shown in figure 3, and the transmission spectrum is shown in figure 4.
The samples obtained in example 2 were also subjected to a notched impact strength test and a flame retardancy test. The test result shows that the notch impact strength of the sample is 72kJ/m2Flame retardant performance V0 rating.
The foregoing is a detailed description of the invention in conjunction with specific embodiments thereof, and it is not intended that the invention be limited to these specific embodiments. It should be understood by those skilled in the art that various changes and substitutions may be made in accordance with the technical solution and the inventive concept of the present invention, and the same properties or uses should be considered as the protection scope of the present invention.
Claims (3)
1. The broadband near-infrared absorption optical filter comprises the following raw materials in parts by weight: 0.1-0.2 part of low-band near-infrared absorbent, 0.05-0.08 part of medium-band near-infrared absorbent, 0.4-0.6 part of high-band near-infrared absorbent and 100 parts of optical polymer resin granules; the main absorption wave band of the optical filter is 700 nm-1800 nm.
2. The broadband near infrared absorbing filter of claim 1, wherein the low band near infrared absorber is octaphenoxy octaphenylamino metal phthalocyanine based compound; the mid-band near-infrared absorbent is a sulfodiene palladium compound; the high-waveband near-infrared absorbent is an antimony hexa-butyl cyanide hexafluoride free radical arylamine compound; the optical polymer resin granules are polycarbonate or polymethyl methacrylate.
3. A method of making the broadband near-infrared absorbing filter of claim 1, comprising the steps of:
(1) drying the optical polymer resin granules in a dryer at 100-120 ℃ for 4 h;
(2) accurately weighing optical polymer resin granules and near-infrared absorbent powder according to parts by weight, loading the optical polymer resin granules and the near-infrared absorbent powder into a mixer, adding a small amount of white oil to mix, wherein the rotating speed of the mixer is 60r/min, and the mixing time is 10min to obtain dark green semitransparent master batches;
(3) injection molding the dark green semitransparent master batch prepared in the step (2) to prepare a broadband near-infrared absorption optical filter;
(4) and (4) plating a hard film on the surface of the broadband near-infrared absorption optical filter prepared in the step (3) to improve the hardness of the surface of the optical filter.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110248140.0A CN113138437A (en) | 2021-03-08 | 2021-03-08 | Broadband near-infrared absorption optical filter and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110248140.0A CN113138437A (en) | 2021-03-08 | 2021-03-08 | Broadband near-infrared absorption optical filter and preparation method thereof |
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| CN113138437A true CN113138437A (en) | 2021-07-20 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115124825A (en) * | 2022-08-01 | 2022-09-30 | 广州市博泰光学科技有限公司 | PC high-definition optical lens and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103809231A (en) * | 2014-01-27 | 2014-05-21 | 南京工业大学 | UV (Ultraviolet)-NIR (Near-Infrared) dual band absorbing optical filter and preparation method thereof |
| US20180149783A1 (en) * | 2016-11-30 | 2018-05-31 | Samsung Electronics Co., Ltd. | Optical filter and camera module and electronic device |
| CN109143439A (en) * | 2018-08-31 | 2019-01-04 | 苏州讯能光电科技有限公司 | A kind of high-low temperature resistant Near infrared absorbing filter and preparation method thereof |
| CN109504072A (en) * | 2018-07-23 | 2019-03-22 | 广州市辉乐医药科技有限公司 | A kind of eyeglass of high visible light multistage protection laser |
-
2021
- 2021-03-08 CN CN202110248140.0A patent/CN113138437A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103809231A (en) * | 2014-01-27 | 2014-05-21 | 南京工业大学 | UV (Ultraviolet)-NIR (Near-Infrared) dual band absorbing optical filter and preparation method thereof |
| US20180149783A1 (en) * | 2016-11-30 | 2018-05-31 | Samsung Electronics Co., Ltd. | Optical filter and camera module and electronic device |
| CN109504072A (en) * | 2018-07-23 | 2019-03-22 | 广州市辉乐医药科技有限公司 | A kind of eyeglass of high visible light multistage protection laser |
| CN109143439A (en) * | 2018-08-31 | 2019-01-04 | 苏州讯能光电科技有限公司 | A kind of high-low temperature resistant Near infrared absorbing filter and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 段潜: "《新型近红外滤光塑料研究》", 《精密工程》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115124825A (en) * | 2022-08-01 | 2022-09-30 | 广州市博泰光学科技有限公司 | PC high-definition optical lens and preparation method thereof |
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Application publication date: 20210720 |