CN109507766A - In flexibility, remote dual-band infrared absorbing membrane and preparation method thereof - Google Patents
In flexibility, remote dual-band infrared absorbing membrane and preparation method thereof Download PDFInfo
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- CN109507766A CN109507766A CN201811226654.0A CN201811226654A CN109507766A CN 109507766 A CN109507766 A CN 109507766A CN 201811226654 A CN201811226654 A CN 201811226654A CN 109507766 A CN109507766 A CN 109507766A
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/003—Light absorbing elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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Abstract
The present invention provides in a kind of flexibility, remote dual-band infrared absorbing membrane and preparation method thereof, this method is using ethyl orthosilicate, the polyvinyl alcohol of high alcoholysis degree, catalyst, modifying agent as raw material, it is using the method for sol-gel that polyvinyl alcohol and nano silica is compound, by the hydrolysis of ethyl orthosilicate, the crosslinking of silicon dioxide gel and polyvinyl alcohol, shrink, film forming procedure, obtain in strong, the flexible composite film that remote dual-band infrared absorbs.In most of, compared with remote red absorbing material, film of the present invention is slightly narrow to the wave-length coverage of infrared Absorption, selectivity is stronger, is suitble to preparation to the demanding infrared components of wavelength selection, can be applied to infrared Absorption, infrared sensor, the fields such as heat-insulated, anti-infrared radiation, stealthy of filtering.
Description
Technical field
The invention belongs to infrared absorbing material technical field, be related in a kind of flexibility, remote dual-band infrared absorbing membrane and
Preparation method.
Background technique
In infrared light detecting and Infrared stealthy materials field, concerned by people is 3-5 μm of medium-wave infrared (MWIR) and 8-12 μ
M LONG WAVE INFRARED (LWIR), the wave band are that the infrared system of air contact often selects service band.The infrared absorptivity of material
It is the vital technical indicator determined whether such device is advanced.In traditional, Far-infrared Absorption material be mostly inorganic
Material such as mercury cadmium telluride HgCdTe, vanadium oxide VOX, silicon nitride, tungsten bronze compound etc., the complex process of such material preparation is former
Material is expensive, it is difficult to which the device of large area is processed into preparation.Therefore, scientist continuously attempts to use in different method reductions, far
The price of dual-band infrared absorbing material and its filming performance of raising, such as Chinese patent (ZL201610566514.2) are described
One kind be based on carbon nanometer infrared absorption layer, devise an infrared absorption layer, the invention using carbon nanometer and silicon nitride material
Carbon nanomaterial it is expensive, absorbed layer preparation process is complicated；Microelectronics, Peking University research institute Wang Xin et al. uses plasma
Body enhances chemical vapor deposition (PECVD)-SiC Infrared Absorbing Thin Film, and required the device is complicated, expensive.In addition, red in order to improve
The filming performance of outer absorbing material, the polymer for having document report to form a film by the inorganic infrared absorbing material of nanoscale and easily carry out
Physics is compound, but this physics composite material disperses uneven, nano inoganic particle there are inorganic material in the polymer to be held
Easy cluster, and the problem of mutually separating can occur, therefore leverage its practical application.
Summary of the invention
The object of the present invention is to provide in a kind of flexibility, remote dual-band infrared absorbing membrane and preparation method thereof, solve
Problems of the prior art.
Technical scheme is as follows:
In a kind of flexibility, the preparation method of remote dual-band infrared absorbing membrane, specifically includes the following steps:
Step 1 measures ethyl alcohol, ethyl orthosilicate and deionized water according to volume ratio 3:3:1 and mixes, and adds hydrochloric acid tune PH to 2-4,
It is stirred 5-7 hours under room temperature, obtains transparent silicon dioxide gel；
Step 2 weighs the single-necked flask that polyvinyl alcohol addition of the alcoholysis degree greater than 98% is furnished with condenser pipe, and deionized water is added, adds
Heat stirs 2-3 hours to 90 DEG C, until polyvinyl alcohol is completely dissolved, obtains the polyethylene that polyvinyl alcohol mass percent is 1.5%
Alcoholic solution, temperature are down to room temperature, for use；
Step 3, by the stand-by poly-vinyl alcohol solution of the resulting silicon dioxide gel of the first step and second step according to PVA/SiO2It rubs
You mix than 1:0.7 ~ 1.3, the modifying agent for accounting for mixed liquor gross mass 2 ~ 5% are added, the modifying agent is only in 3-3.5 μm and 8-10
There is the functional group of infrared absorption at μm, then high-speed stirred, ageing to 18 ~ 23 Pa.S of viscosity；
Step 4, using spin-coating method under 1800 revs/min of revolving speed, film is prepared as substrate using the silicon wafer of polishing, in 60 DEG C of vacuum
Drying box is heat-treated 1-2 hours, and 0 DEG C of ice water is quickly cooled down, and obtains remote dual-band infrared absorbing membrane in transparence.
Further, the modifying agent selects cetyl trimethylammonium bromide, ethyl trimethoxy silane, long chain silane
One kind.
According to above-mentioned preparation method preparation flexibility in, remote dual-band infrared absorbing membrane.
The beneficial effects of the present invention are:
The method of the present invention belongs to chemically composited method, it is prepared in, the compatibility performance of remote dual-band infrared absorbing membrane it is good, no
Two-phase laminated flow easily occurs, film is uniform, excellent in optical properties.It is raw materials used based on ethyl orthosilicate and polyethylene glycol, price
It is cheap, nontoxic.Therefore, provided by the invention in, the preparation method of remote dual-band infrared absorbing membrane, low in raw material price,
Environmental protection, preparation process is simple, mid and far infrared absorptivity is high, flexility is excellent, is suitble to be processed into the infrared-sensitive list of large area
Member.In most of, compared with remote red absorbing material, slightly narrow to the wave-length coverage of infrared Absorption, selectivity is stronger, is suitble to preparation
To the demanding infrared components of wavelength selection, can be applied to infrared Absorption, infrared sensor, heat-insulated, the anti-infrared radiation that filters,
Stealthy equal fields.
Detailed description of the invention
Fig. 1 is in flexibility, the preparation technology flow chart of remote dual-band infrared absorbing membrane；
Fig. 2 is during experiment is resulting, the infrared absorpting light spectra of remote dual-band infrared absorbing membrane；
Fig. 3 be prepared by embodiment 1 in, the infrared spectrogram of remote dual-band infrared absorbing membrane；
Fig. 4 be prepared by embodiment 2 in, the infrared spectrogram of remote dual-band infrared absorbing membrane.
Specific embodiment
Below by specific embodiment combination attached drawing, invention is further described in detail.Wherein different embodiments
Middle similar component uses associated similar element numbers.In the following embodiments, many datail descriptions be in order to
The application is better understood.However, those skilled in the art can recognize without lifting an eyebrow, part of feature
It is dispensed, or can be substituted by other elements, material, method in varied situations.In some cases, this Shen
Please it is relevant it is some operation there is no in the description show or describe, this is the core in order to avoid the application by mistake
More descriptions are flooded, and to those skilled in the art, these relevant operations, which are described in detail, not to be necessary, they
Relevant operation can be completely understood according to the general technology knowledge of description and this field in specification.
The present invention propose it is a kind of flexibility in, remote dual-band infrared absorbing membrane and its preparation method, and pass through the preparation
Method prepares in flexibility, remote dual-band infrared absorbing membrane, and the appearance of this method and product solves several present in technology
A major defect: (1) in most of, the problem that remote dual-band infrared absorbing material ir-absorbance is not high enough；(2) in, remote wave
The inorganic material expensive starting materials of section infrared absorption are toxic, preparation process is complicated, is difficult to the problem of forming a film；(3) in, remote wave band it is infrared
The problems such as inorganic-organic composite material bad dispersibility of absorption, mutually separation are seriously, bad mechanical property and preparation process are complicated.
Basic principle of the invention is: the invention is with ethyl orthosilicate, the polyvinyl alcohol of high alcoholysis degree, catalyst, modification
Agent is raw material, using the method for sol-gel that polyvinyl alcohol and nano silica is compound, by the water of ethyl orthosilicate
Solution, the crosslinking of silicon dioxide gel and polyvinyl alcohol, shrink, film forming procedure, obtain in strong, remote dual-band infrared absorbs
Flexible composite film.
Referring to Fig. 1, in a kind of flexibility, the preparation method of remote dual-band infrared absorbing membrane, the specific steps are as follows:
Step 1 measures ethyl alcohol, ethyl orthosilicate and deionized water according to volume ratio 3:3:1 and mixes, and adds hydrochloric acid tune PH to 2-4,
It is stirred 5-7 hours under room temperature, obtains silicon dioxide gel；
Step 2 weighs the single-necked flask that polyvinyl alcohol addition of the alcoholysis degree greater than 98% is furnished with condenser pipe, and deionized water is added, adds
Heat stirs 2-3 hours to 90 DEG C, until polyvinyl alcohol is completely dissolved, obtains the polyethylene that polyvinyl alcohol mass percent is 1.5%
Alcoholic solution, temperature are down to room temperature, for use；
Step 3, by the stand-by poly-vinyl alcohol solution of the resulting silicon dioxide gel of the first step and second step according to PVA/SiO2It rubs
You mix than 1:0.7 ~ 1.3, the modifying agent for accounting for mixed liquor gross mass 2 ~ 5% are added, the modifying agent is only in 3-3.5 μm and 8-10
There is the functional group of infrared absorption at μm, then high-speed stirred, ageing to viscosity 18-23Pa.S；
Step 4, using spin-coating method under 1800 revs/min of revolving speed, prepare film by substrate of polished silicon slice, it is dry in 60 DEG C of vacuum
Dry case is heat-treated 1-2 hours, and 0 DEG C of ice water is quickly cooled down, and obtains remote dual-band infrared absorbing membrane in transparence.
Step 5 tests institute's made membrane in, the infrared spectroscopy of far infrared band by infrared spectrometer.
Above-mentioned modifying agent can select cetyl trimethylammonium bromide, ethyl trimethoxy silane, long chain silane one
Kind.
As above method preparation gained it is a kind of it is flexible in, remote dual-band infrared absorbing membrane, in the material it is main at
It is divided into polyvinyl alcohol and earth silicon material, analysis ,-OH, CH contained in the material is constituted by the molecule of polyvinyl alcohol2
In 3362,2924cm-1At (3-3.4 μm of wavelength) and C-OH is in 1095cm-1Cm (9.13 μm of wavelength) has infrared absorption, and just
The earth silicon material obtained after silicate hydrolyzate is 958-1There are the absorption peaks of Si-OH at (10.4 μm).It is solidifying by colloidal sol
Hydroxyl on the hydroxyl and polyvinyl alcohol on silica that glue method obtains occurs condensation reaction and obtains being located at 1100cm-1Left and right
The absorption band of Si-O-Si antisymmetric stretching vibration Qiang Erkuan at (8-10 μm of wavelength).The material remote wave in is red in addition to this
Functional group of the outer segment again without other strong infrared absorptions.Therefore, from the angle analysis of materials chemistry molecule functional group's infrared absorption,
The material has in 3-3.4 μm of wavelength and the strong infrared absorption performance of 8-10 μm of two waveband, other regions are infrared light transmission area,
So that the Infrared Absorbing Thin Film has very strong selectivity and sensitivity.
Referring to fig. 2, Fig. 2 is the infrared absorpting light spectra infrared spectroscopy of remote dual-band infrared absorbing membrane during experiment is resulting
Analysis, there are strong infrared absorptions at 3-3.4 μm of wavelength with 8-10 μm for the material as seen from Figure 2, especially at 8-10 μm
Place's infrared absorption nearly reaches 100%.In 3362,2924cm in figure-1At (3-3.4 μm of wavelength) and C-OH is in 1095cm-1(wave
It is 9.13 μm long) at infrared absorption be respectively belonging to the-OH of polyvinyl alcohol and silica surface, the and-CH of PVA2Cm's
Absorption peak；958-1(10.4 μm of wavelength) belongs at the earth silicon material obtained after teos hydrolysis that there are Si-OH
Absorption peak；In 1100cm-1It is flexible that strong and wide absorption band at left and right (i.e. 8-10 μm of wavelength) belongs to Si-O-Si antisymmetry
Vibration, the map structure and above-mentioned analysis are completely the same.
The present invention is further detailed below by several specific embodiments:
Example 1:
Measure ethyl alcohol: ethyl orthosilicate: deionized water is the volume ratio of 3:3:1, adds hydrochloric acid tune PH to 2-4, stirs 5-7 under room temperature
Hour；The single-necked flask that alcoholysis degree addition a certain amount of greater than 98% polyvinyl alcohol is furnished with condenser pipe is weighed, deionized water is added,
90 DEG C of heating is stirred 2-3 hours, until PVA is completely dissolved, obtains the solution that polyvinyl alcohol mass percent is 1.5%, temperature drop
To room temperature, for use；
By silicon dioxide gel obtained as above and stand-by poly-vinyl alcohol solution according to PVA/SiO2Molar ratio is 1:1.1 (two
The molal quantity of silica is equal to the molal quantity of ethyl orthosilicate) mixing, the modification ethyl trimethoxy silicon that gross mass is 2% is added
Alkane, then high-speed stirred, ageing to viscosity are 21 Pa.S.Using spin-coating method under 1800 revs/min of revolving speed, with polished silicon slice
Film is prepared for substrate, is heat-treated 1.5 hours in 60 DEG C of vacuum ovens, 0 DEG C of ice water is quickly cooled down, and is obtained remote in transparence
Dual-band infrared absorbing membrane.Institute's made membrane is tested in, the infrared spectroscopy of far infrared band by infrared spectrometer.Gained is thin
The infrared spectroscopy of film as shown in figure 3, as shown in Figure 3 the film have at 3.0-3.2 μm and 8.2-10.2 μm of two waveband it is strong red
Outer absorption.
Example 2:
Measure ethyl alcohol: ethyl orthosilicate: deionized water is the volume ratio of 3:3:1, adds hydrochloric acid tune PH to 2-4, stirring 6 is small under room temperature
When；The single-necked flask that alcoholysis degree addition a certain amount of greater than 98% polyvinyl alcohol is furnished with condenser pipe is weighed, deionized water is added, adds
90 DEG C of heat stirs 3 hours, until PVA is completely dissolved, obtains the solution that polyvinyl alcohol mass percent is 3%, and temperature is down to room temperature,
For use；
By silicon dioxide gel obtained as above and stand-by poly-vinyl alcohol solution according to PVA/SiO2Molar ratio is 1:0.8 (two
The molal quantity of silica is equal to the molal quantity of ethyl orthosilicate) mixing, the modifying agent cetyl front three that gross mass is 5% is added
Base ammonium bromide, then high-speed stirred, ageing to viscosity to 19Pa.S.Using spin-coating method under 1800 revs/min of revolving speed, with polishing
Silicon wafer is that substrate prepares film, is heat-treated 1 hour in 60 DEG C of vacuum ovens, 0 DEG C of ice water is quickly cooled down, and is obtained in transparence
Remote dual-band infrared absorbing membrane.Institute's made membrane is tested in, the infrared spectroscopy of far infrared band by infrared spectrometer.Gained
The infrared spectroscopy of film is as shown in figure 4, the film has by force at 2.9-3.5 μm and 8.2-10.8 μm of two waveband as seen from the figure
Infrared absorption.
Use above specific case is illustrated the present invention, is merely used to help understand the present invention, not to limit
The system present invention.For those skilled in the art, according to the thought of the present invention, can also make several simple
It deduces, deform or replaces.
Claims (3)
1. in a kind of flexibility, the preparation method of remote dual-band infrared absorbing membrane, which is characterized in that specifically includes the following steps:
Step 1 measures ethyl alcohol, ethyl orthosilicate and deionized water according to volume ratio 3:3:1 and mixes, and adds hydrochloric acid tune PH to 2-4,
It is stirred 5-7 hours under room temperature, obtains transparent silicon dioxide gel；
Step 2 weighs the single-necked flask that polyvinyl alcohol addition of the alcoholysis degree greater than 98% is furnished with condenser pipe, and deionized water is added, adds
Heat stirs 2-3 hours to 90 DEG C, until polyvinyl alcohol is completely dissolved, obtains the polyethylene that polyvinyl alcohol mass percent is 1.5%
Alcoholic solution, temperature are down to room temperature, for use；
Step 3, by the stand-by poly-vinyl alcohol solution of the resulting silicon dioxide gel of the first step and second step according to PVA/SiO2Mole
It is mixed than 1:0.7 ~ 1.3, the modifying agent for accounting for mixed liquor gross mass 2 ~ 5% is added, the modifying agent is only in 3-3.5 μm and 8-10 μm
There is the functional group of infrared absorption at place, then high-speed stirred, ageing to 18 ~ 23 Pa.S of viscosity；
Step 4, using spin-coating method under 1800 revs/min of revolving speed, film is prepared as substrate using the silicon wafer of polishing, in 60 DEG C of vacuum
Drying box is heat-treated 1-2 hours, and 0 DEG C of ice water is quickly cooled down, and obtains remote dual-band infrared absorbing membrane in transparence.
2. preparation method according to claim 1, which is characterized in that the modifying agent selects cetyl trimethyl bromination
One kind of ammonium, ethyl trimethoxy silane, long chain silane.
3. according to claim 1 preparation method preparation flexibility in, remote dual-band infrared absorbing membrane.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116695446A (en) * | 2023-07-12 | 2023-09-05 | 吴江市兴业纺织有限公司 | Fabric with infrared shielding function and preparation method thereof |
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| CN103011619A (en) * | 2013-01-14 | 2013-04-03 | 大连工业大学 | Method for preparing network interpenetrating polyvinyl alcohol/silicon dioxide composite coating |
| CN103183479A (en) * | 2013-04-16 | 2013-07-03 | 浙江大学 | Preparation method of anti-reflection thin film with photo-transformation function |
| US20150301247A1 (en) * | 2012-11-02 | 2015-10-22 | Konica Minolta, Inc. | Optical reflection film, infrared shielding film, and process for producing the same |
| CN107075289A (en) * | 2014-10-16 | 2017-08-18 | 住友大阪水泥股份有限公司 | Surface modification of metals oxide particle dispersion liquid and its manufacture method, surface modification of metals oxide particle silicone resin complex composition, surface modification of metals oxide particle silicone resin compound, optical component and light-emitting device |
| CN107233802A (en) * | 2017-06-13 | 2017-10-10 | 江苏理工学院 | A kind of polyvinyl alcohol/nano silicon titanium hybridized film and preparation method thereof |
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2018
- 2018-10-22 CN CN201811226654.0A patent/CN109507766A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150301247A1 (en) * | 2012-11-02 | 2015-10-22 | Konica Minolta, Inc. | Optical reflection film, infrared shielding film, and process for producing the same |
| CN103011619A (en) * | 2013-01-14 | 2013-04-03 | 大连工业大学 | Method for preparing network interpenetrating polyvinyl alcohol/silicon dioxide composite coating |
| CN103183479A (en) * | 2013-04-16 | 2013-07-03 | 浙江大学 | Preparation method of anti-reflection thin film with photo-transformation function |
| CN107075289A (en) * | 2014-10-16 | 2017-08-18 | 住友大阪水泥股份有限公司 | Surface modification of metals oxide particle dispersion liquid and its manufacture method, surface modification of metals oxide particle silicone resin complex composition, surface modification of metals oxide particle silicone resin compound, optical component and light-emitting device |
| CN107233802A (en) * | 2017-06-13 | 2017-10-10 | 江苏理工学院 | A kind of polyvinyl alcohol/nano silicon titanium hybridized film and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116695446A (en) * | 2023-07-12 | 2023-09-05 | 吴江市兴业纺织有限公司 | Fabric with infrared shielding function and preparation method thereof |
| CN116695446B (en) * | 2023-07-12 | 2024-02-02 | 吴江市兴业纺织有限公司 | Fabric with infrared shielding function and preparation method thereof |
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Application publication date: 20190322 |