CN109438980A - A kind of light absorber and preparation method thereof - Google Patents
A kind of light absorber and preparation method thereof Download PDFInfo
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- CN109438980A CN109438980A CN201811122872.XA CN201811122872A CN109438980A CN 109438980 A CN109438980 A CN 109438980A CN 201811122872 A CN201811122872 A CN 201811122872A CN 109438980 A CN109438980 A CN 109438980A
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- 239000006096 absorbing agent Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 239000000243 solution Substances 0.000 claims abstract description 49
- 229920006231 aramid fiber Polymers 0.000 claims abstract description 40
- 239000002121 nanofiber Substances 0.000 claims abstract description 38
- 239000002082 metal nanoparticle Substances 0.000 claims abstract description 32
- 239000004760 aramid Substances 0.000 claims abstract description 31
- 229920003235 aromatic polyamide Polymers 0.000 claims abstract description 31
- 239000011259 mixed solution Substances 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 239000011159 matrix material Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000010931 gold Substances 0.000 claims description 31
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 27
- 229910052737 gold Inorganic materials 0.000 claims description 27
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 22
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 18
- 239000002105 nanoparticle Substances 0.000 claims description 15
- 206010016654 Fibrosis Diseases 0.000 claims description 14
- 230000004761 fibrosis Effects 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 9
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N dimethyl sulfoxide Natural products CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 9
- 229920000271 Kevlar® Polymers 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000004761 kevlar Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 4
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- 238000002156 mixing Methods 0.000 claims description 2
- 239000002070 nanowire Substances 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- BDRTVPCFKSUHCJ-UHFFFAOYSA-N molecular hydrogen;potassium Chemical compound [K].[H][H] BDRTVPCFKSUHCJ-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 230000031700 light absorption Effects 0.000 abstract description 11
- 230000002045 lasting effect Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 20
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- 235000013339 cereals Nutrition 0.000 description 14
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- 238000012545 processing Methods 0.000 description 4
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- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- FTCZPMDTJZCISS-UHFFFAOYSA-N C1(=CC=CC=C1)N(C1=C(C=CC=C1)NC=O)C=O Chemical compound C1(=CC=CC=C1)N(C1=C(C=CC=C1)NC=O)C=O FTCZPMDTJZCISS-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229920000561 Twaron Polymers 0.000 description 1
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 description 1
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- 230000032900 absorption of visible light Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
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- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
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- 239000000047 product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 239000004762 twaron Substances 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- G02B1/002—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/003—Light absorbing elements
-
- 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
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
-
- 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
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
-
- 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
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0831—Gold
-
- 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
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
-
- 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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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Engineering & Computer Science (AREA)
- Optics & Photonics (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a kind of light absorber and preparation method thereof, preparation method includes: S1. using aramid fiber as raw material, prepares aramid nano-fiber solution；S2. metal nanoparticle solution is prepared；S3. the metal nanoparticle solution by aramid nano-fiber solution and step S2 preparation prepared by step S1 is mixed with mixed solution；S4. the mixed solution prepared by step S3, removal solvent obtain nano compound film light absorber；Using aramid nano-fiber as matrix, metal nanoparticle is supported in the aramid nano-fiber matrix light absorber.The light absorber has super flexibility, has enough and lasting mechanical strengths, and be conducive to be used widely in wearable and non-planar photo-thermal device；Efficient, full angle, broadband light absorption may be implemented on visible light and near-IR frequency；Preparation method is simple and efficient, and is easy to scale.
Description
Technical field
The present invention relates to technical field of composite materials more particularly to a kind of light absorber and preparation method thereof.
Background technique
It is always the main of science and technology that ideal light absorber, which has the high-selenium corn efficiency of comprehensive (full angle) to light,
Target.In recent years, the light absorber based on Meta Materials (such as plasma light absorber) has obtained widely grinding in many fields
Study carefully and develop, Meta Materials are the artificial structure's materials being made of sub-wavelength cell array, have excellent electromagnetic performance.Meta Materials
Absorbing material generally can be divided into narrowband absorbing material and broadband absorbing material.Narrowband meta-material absorber invariably rely on it is specific
The resonance effects of the structure of the light interaction of frequency.In contrast, broadband meta-material absorber dependent on its electromagnetic response with
The unrelated structure of frequency, therefore light can be absorbed in big bandwidth.Therefore, broadband meta-material absorber answers extensive photon
With having a great attraction, for example, solar energy-thermal energy collecting, for the sensor platform of full light spectrum image-forming and Photoelectric Detection.
The realization of broadband light absorber based on Meta Materials has been achieved for huge progress.For example, having hyperbolic space color
Scattered nano-patterning anisotropy Meta Materials have been proved to have effective optical absorption under visible and near-IR frequency.
The Meta Materials made of the nanoporous template of noble-metal coated also show excellent wide band absorption performance.In addition, such as nitrogen
The refractory material for changing titanium and vanadium dioxide has recently been used as constructing nanostructure broadband meta-material absorber.However, still having one
A little limitations hinder the practical application of these meta-material absorbers.Firstly, nanostructure meta-material absorber is usually by from upper
Nano-fabrication methods under and manufacture, such as electron beam lithography (EBL) and focused ion beam (FIB) milling, this is inherently limited
The greatest physical size and output of absorber are made.Second, most of broadband Meta Materials absorbing material is all in rigid substrate
Upper preparation, such as glass and silicon wafer.This makes these devices lack flexibility, and largely limits them and have
Application in the wearable and other electro-optical system of non-planar surfaces.Although having carried out one under Terahertz and optical frequency
A little experiments are attempted, and succeed and are realized the preparation of Meta Materials on flexible substrates, but the intensity of periodicity metamaterial structure
It is not so good as flexible substrate with strain, it reduce the overall mechanical properties of device.Therefore, using large area, it is high-throughput from lower and
Upper technology is still challenging to prepare the flexible membrane with high-performance, full angle and broadband light absorption.
Summary of the invention
To solve the above problems, the present invention proposes a kind of light absorber and preparation method thereof, which has super soft
Property, efficient, full angle, broadband light absorption may be implemented on visible light and near-IR frequency；Preparation method is simple and efficient, easily
In scale.
The preparation method of light absorber provided by the invention, comprising: S1. prepares aramid nano-fiber using aramid fiber as raw material
Solution；S2. metal nanoparticle solution is prepared；S3. it prepared by the step S1 aramid nano-fiber solution prepared and step S2
Metal nanoparticle solution is mixed with mixed solution；S4. the mixed solution prepared by step S3, it is multiple that removal solvent obtains nanometer
Close film light absorber；Using aramid nano-fiber as matrix, metal nanoparticle is supported on the aramid fiber and receives the light absorber
On rice fibre substrate.
Preferably, the aramid fiber includes the Kevlar of E.I.Du Pont Company, and the metal nanoparticle includes gold nano grain, silver
One of nano particle, copper nano particles are a variety of, in the nano compound film metal nanoparticle content be 2.8% with
On.
Preferably, the step S1 includes: and impregnates to carry out fibrosis in the solution after aramid fiber is dried in vacuo by S11., then
It pulls cleaning out and is dried in vacuo to obtain fibrosis aramid fiber；S12. the fibrosis aramid fiber that step S11 is obtained is mixed with alkali and solvent
Uniform stirring, after solution from it is colourless become aubergine oily solution after, be added inorganic agent, obtain aramid nano-fiber solution.
Further preferably, the vacuum drying condition before the aramid fiber in the step S11 are as follows: 60-65 DEG C, dry
18h–24h；Vacuum drying condition after fibrosis is 60 DEG C -70 DEG C, dry 48h.Alkali in the step S12 is hydroxide
Potassium, and the mass ratio of potassium hydroxide and aramid fiber is 1:1-2:1；The solvent is N, N- dimethyl sulfoxide；The inorganic agent is phosphorus
The mixed solution of acid and water.
Still more preferably, the volume ratio of the phosphoric acid and water is 1:2-2:1；The volume of the inorganic agent accounts for mixed solution
The percentage of total volume is 1.0%-10%.
Preferably, the step S4 includes: and mixed solution prepared by step S3 is obtained nanometer to answer by way of suction filtration
Close film light absorber.
The present invention also provides a kind of light absorbers, comprising: aramid nano-fiber matrix, and it is supported on the aramid fiber nanometer
Metal nanoparticle on fibre substrate.
Preferably, the aramid fiber includes the Kevlar of E.I.Du Pont Company；The metal nanoparticle includes gold nano grain, silver
One of nano particle, copper nano particles are a variety of；Metal nanoparticle content is 2.8% or more in the light absorber.
Beneficial effects of the present invention:
1. the present invention selects aramid fiber for raw material, and prepares aramid nano-fiber (ANFs) as matrix, because of aramid fiber nanometer
The excellent mechanical strength of fibre substrate (performances such as tension, counter-bending are high), so that film light absorber possesses super flexibility, tool
There are enough and lasting mechanical strengths, and is conducive to be used widely in wearable and non-planar photo-thermal device.
2. be different from the prior art it is middle use top-down preparation method, the present invention is by aramid nano-fiber solution and gold
Metal nano-particle solution is mixed, and obtains nano compound film light absorber after removing solvent, this method is at low cost and is easy to
Amplification.Meanwhile the nano compound film light absorber that this method prepares, aramid nano-fiber self assembly simultaneously form porous three
Wiki matter, metal nanoparticle are supported on nanofiber between nanofiber.The metal nanoparticle adulterated in film
Content and diameter are optimised, and the metal nanoparticle of high dispersive is because its local surface plasma resonance effect realizes brilliant
Broadband, efficient, omnidirectional's light absorption；Light absorber in compared to the prior art, the metal nanoparticle of unit square is significantly
It reduces, further reduces the cost of light absorber.
3. based on the chemical/thermal stability that aramid nano-fiber is excellent, even if being acted in efficient light absorption and photothermal conversion
Lower film surface temperature sharply increases, and light absorber will not burn or deform, its physical property can still be maintained under high temperature
And function-stable.
Detailed description of the invention
Fig. 1 is the specific preparation flow schematic diagram of light absorber (PMF) in the embodiment of the present invention.
Fig. 2 is the fibrosis schematic diagram of aramid line in the embodiment of the present invention.
Fig. 3 is the nanosizing schematic diagram of aramid fiber in the embodiment of the present invention.
Fig. 4 is the aramid nano-fiber scanning electron microscope (SEM) photograph obtained after different disposal agent processing in the embodiment of the present invention.
Fig. 5 is the gold nano grain and its transmission electron microscope of the different-grain diameter of gold kind growth method preparation in the embodiment of the present invention
Figure, particle diameter distribution a-b:20nm, 30nm, 40nm, 60nm, 80nm, 110nm.
Fig. 6 is that the different gold content PMF pictorial diagrams of suction method preparation, a-h gold content difference are utilized in the embodiment of the present invention
Are as follows: 0,1.4%, 2.8%, 4.3%, 5.7%, 7.1%, 8.6%, 9.9%.
When Fig. 7 is gold nano grain partial size difference in the super flexible plasma light absorber of the embodiment of the present invention (A), gold
Influence when nano particle (partial size 58nm) content difference when (B) and incidence angle different (C) to absorption.
Fig. 8 is the scanning electron microscope (SEM) photograph and its surface topography of super flexible plasma light absorber in the embodiment of the present invention.
Fig. 9 is that the flexibility of super flexible plasma light absorber in the embodiment of the present invention tests (A), bending performance test
(B) and its Young's modulus performance test (C).
Figure 10 is the research of super flexible plasma light absorber light thermal property in the embodiment of the present invention.
Specific embodiment
Following specific embodiment provided by the invention and all possible combination between them.For succinct
Purpose, the no various specific combinations for recording embodiment one by one of the application, it will be understood that the application specifically records simultaneously
Disclose all possible combination of the specific embodiment.
The present invention provides a kind of super flexible nano laminated film light absorber and preparation method thereof, includes the following steps: S1.
Using aramid fiber as raw material, aramid nano-fiber solution is prepared；S2. metal nanoparticle solution is prepared；S3. the virtue prepared by step S1
Synthetic fibre nanofiber solution and the metal nanoparticle solution of step S2 preparation are mixed with mixed solution；S4. it prepared by step S3
Mixed solution, removal solvent simultaneously be dried to obtain nano compound film light absorber；The light absorber is with aramid nano-fiber
For matrix, metal nanoparticle is supported in the aramid nano-fiber matrix.
Aramid fiber full name is poly- phenyl-diformyl phenylenediamine, main Twaron and E.I.Du Pont Company's production including the production of Di Ren company
Kevlar, have the excellent performances such as superhigh intensity, high-modulus and high temperature resistant, acid-fast alkali-proof, light-weight.
In step S1, aramid fiber successively passes through fibrosis and hydrolysis, forms nanofiber.
In step S2, metal nanoparticle includes one of gold nano grain, silver nano-grain, copper nano particles or more
Kind, partial size 1nm-200nm, particle diameter distribution is 20nm -110nm.The preparation of metal nanoparticle can use the prior art
In the preparation of any metal nanoparticle method.
In step S3, nanofiber solution prepared by step S1 is stirred and is warming up to boiling, step S2 is then added
The metal nanoparticle solution of preparation stops heating after mixing evenly, spare；
In step S4, first using pressurization suction filtration/freeze-drying/drying/supercritical CO2The modes such as cleaning remove solvent, then permanent
Nano compound film is prepared in temperature drying.
It With reference to embodiment and compares attached drawing invention is further described in detail, wherein aramid fiber is selected
The Kevlar of E.I.Du Pont Company, metal nanoparticle select golden (Au) nano particle.It is emphasized that following the description is only to show
Example property, the range and its application being not intended to be limiting of the invention.
The specific preparation flow of light absorber (PMF) is as shown in Figure 1, the specific steps are as follows:
S11. the fibrosis of aramid fiber
1.5g aramid fiber is weighed, fiber is shredded with scissors, is dried in vacuo for 24 hours at 60-65 DEG C.Then by drying, shredded
Aramid fiber be placed in the dry N-methylpyrrolidone solution for filling 100ml, impregnate 48 hours or so (as shown in Figure 2).Then
Fiber is pulled out, is constantly cleaned with deionized water, N-Methyl pyrrolidone solution contained in fiber is removed, after cleaning
Fiber is placed in 70 DEG C of vacuum oven, 48 hours or so dry.Obtained substance is the product of aramid fiber, fine
The degree of scatter of dimension is higher than before, is easier to disperse in the solution of sequential hydrolysis step.
S12. the hydrolysis of fibrosis aramid fiber
Firstly, weigh aramid fiber and potassium hydroxide is added in suitable round-bottomed flask, wherein potassium hydroxide and aramid fiber
Mass ratio controls between 1:1 to 2:1.
In the present embodiment, aramid fiber and each 1.0g of potassium hydroxide are weighed.Then by the aramid fiber of the fibrosis prepared in S11
It is transferred in the round-bottomed flask, and the N of 350ml, N- dimethyl sulfoxide (DMSO) is added into bottle.Next fibrosis will be filled
The round-bottomed flask of aramid fiber, potassium hydroxide and dimethyl sulfoxide is placed on magnetic stirring apparatus and stirs, with the increasing in reaction time
Add the color of substance in flask that significant change occurs.As shown in figure 3, when solution becomes uniform aubergine oily solution by colourless
When, inorganic agent is added into round-bottomed flask.Inorganic agent are as follows: the mixed solution of phosphoric acid and water.Different inorganic agents is added can be to virtue
The final form of synthetic fibre nanofiber generates different influences, as shown in figure 4, (phosphoric acid is the phosphorus bought on the market through phosphoric acid
Acid, its general mass concentration are 85%, similarly hereinafter) and the aramid nano-fiber that handles of mixed solution of water both remained without blocky,
Also it does not hydrolyze excessively, even thickness, space three-dimensional structure is more three-dimensional, is more advantageous to subsequent use；And individually through phosphorus
The uniformity coefficient of aramid nano-fiber after acid or water process is all good without the mixed solution of phosphoric acid and water, as shown in figure 4, through water
The aramid nano-fiber of processing is easily excessively hydrolyzed, and has biggish hole, the aramid nano-fiber space three handled through phosphoric acid
It is not three-dimensional enough to tie up structure.
Wherein, the volume ratio of the preferred phosphoric acid of inorganic agent and deionized water is 1:2-2:1, most preferably 1:2,2:2,2:1；Add
The volume for entering inorganic agent accounts for the percentage of overall solution volume in round-bottomed flask and controls between 1.0% -10% as needed.
It is worth noting that: compared to other highly basic (sodium hydroxide, barium hydroxide etc.), only potassium hydroxide and fiber
Change aramid fiber, DMSO solution are hydrolyzed and by the processing of inorganic agent, can just obtain ideal aramid nano-fiber.
S2. the preparation of golden (Au) nano particle
The gold nano grain of gold kind method preparation is mainly used in the present embodiment.Particle diameter distribution mainly has: 20nm,
30nm, 40nm, 60nm, 80nm, 110nm, it is specific the preparation method is as follows:
S21. seed liquor is prepared
19.0mL high purity water is measured with graduated cylinder to be placed in flask.The tetra chlorauric acid solution of 0.17mL is accurately measured with liquid-transfering gun
(1wt%) is added in 50.0mL round-bottomed flask, and adjustment magnetite revolving speed makes solution stirring acutely, then is accurately measured with liquid-transfering gun
0.172mL sodium citrate solution (0.75wt%) rapidly joins the sodium borohydride solution (0.1M) that 0.6mL is newly prepared immediately, can
To observe that solution becomes yellowish red color by colourless rapid intensification therewith, timing later continues stirring 4 hours, then regathers molten
Liquid, be put into refrigerator be kept in dark place it is spare.
It is to be noted that seed liquor needs fresh configuration, standing time, overlong time can occur no more than 24 hours
Ageing, seed slowly agglomeration is unfavorable to the size and regular pattern of control nanoparticle in this way, according to expense number
The amount of substance needed for being adjusted with equal proportion, to meet the needs of practical operation.
S22. crystal seed is grown
It takes a 50.0mL flask to set up device, measures 20mL high purity water with graduated cylinder and pour into flask, add one
Appropriately sized magneton adjusts suitable revolving speed.Successively measured with liquid-transfering gun 4.0mL polyvinylpyrrolidone (PVP) solution,
2.0mL ascorbic acid solution, 1.5mL potassium iodide (KI) solution, 5.1mL chlorauric acid solution (1wt%) are added in flask.Keep molten
Liquid is sufficiently stirred down, quickly with liquid-transfering gun be added different volumes S21 in prepare seed liquor (0.018mL, 0.072mL,
0.144mL, 0.36mL, 1.44mL, 2.88mL) come prepare different particle size distribution (20nm, 30nm, 40nm, 60nm, 80nm,
10min is stirred in gold nano grain 110nm), timing.After reaction, cooled to room temperature is subsequently moved within clean brown
In sample bottle, labelled paper places into refrigerator and is protected from light storage.As shown in figure 5, sample is finally by uv-vis spectra UV-
Vis and transmission electron microscope TEM carries out phenetic analysis.
S3. the preparation of nanofiber, nano particle mixed solution
The preparation of nanofiber and nano particle mixed solution is received using the aramid fiber as above prepared in the present embodiment
Rice fiber solution and gold nano grain are mixed with.Main preparation methods are as follows: it is high-purity that 200ml being added in a. round-bottomed flask
Water (deionized water), is stirred continuously, and is heated to boiling；B. the aramid nano-fiber prepared in 20ml step S12 is measured with graduated cylinder
Solution is stirred continuously heating, until mixed solution boils again, contains gold nano for what is prepared in the S22 of certain volume rapidly
The mixed solution of particle is added in the mixed solution to have boiled, after solution is again stirring for being uniformly mixed, stops heating, standby
With.
S4. the preparation of thin-film material
As shown in Figure 1, the present embodiment is thin using super flexible, the efficient, full angle of method preparation of decompression suction filtration, wide band absorption
Film.It is specific the preparation method is as follows:
Pressure-reduction filter device is assembled, two layers of suction filtration paper is put into bottle,suction, adds water-wet to moisten, turns on the power switch.Then
The mixed solution prepared in step S3 is quickly transferred in bottle,suction, when filtrate is down to film surface in Buchner funnel, edge
Buchner funnel inner wall is slowly added to boiling water (20% -50% or so that volume is mixed solution are added) into funnel, continues to filter
It is flowed out to no liquid by Buchner funnel end, continues to filter after five minutes, close decompression suction filter pump power switch.For same
Particle size prepares the different film of gold content with same method to be used to test gold content difference to material absorptive energy etc.
It influencing, prepared sample such as Fig. 6, a-h gold content is respectively as follows: 0,1.4%, 2.8%, 4.3%, 5.7%, 7.1%, 8.6%,
9.9%, particle size is all 58nm.
By the semi-finished product film filtered by being taken out in Buchner funnel, it is placed in drying box, in 65 DEG C of normal pressure, dries
24 hours.Film is stripped out from filter paper with pocket knife after drying.So far the super flexible plasma light absorber system
It is standby to finish.
It is commonly lyophilized, dries in compared to the prior art, supercritical CO2The mode of the removal solvent such as cleaning, by adding
The flexibility of the nano compound film that the mode that pressure filters is prepared, the nano compound film of preparation is more preferable and more sharp
For collecting and transporting；In addition, it requires instrument and equipment, low, preparation method is simple and efficient, processing cost is low.
Actual sample test
For light absorber prepared by the present embodiment, further characterization test is done to its structural property, specifically includes that knot
Structure characterization and performance test.
Firstly, the influence of partial size, content and the incidence angle of gold nano grain to absorption in measurement light absorber.Such as Fig. 7 A
Shown, influence of the partial size of gold nano grain to light absorption be not when gold nano grain content is 5.7%, in absorber
Together.In the absorption of visible light region (380-780nm) and the different light absorbers of near-infrared short wavelength regions (780-1100nm) to light
Substantially it is attained by 95% or more, even if its light absorption of near-infrared Long wavelength region 85% or more, wherein partial size is 58nm
Gold nano grain effect be better than other partial size assimilation effects.As shown in Figure 7 B, when Au nano-particle content is 2.8% or more
When, absorber reaches 82% or more to the absorption of light；When Au nano-particle content is 4.3% or more, the absorption of light is reached
90% or more.When the content of gold nano grain reaches 5.7% or more, light absorber is best to the assimilation effect of light, the suction
Receive device visible light region (380-780nm) and near-infrared short wavelength regions (780-1100nm) to the absorption of light be up to 99% with
On, i.e., in near-infrared Long wavelength region its light absorption also 90% or more, and this absorption will not be with the change of incident light angle
Change has apparent fluctuation (Fig. 7 C), and by comparing selecting partial size for 58nm, the golden composite membrane that content is 5.7% is as research pair
As surface texture is as shown in figure 8, surface has porous and high dispersive gold nano grain.The gold nano of these high dispersives
Particle is realized effective optics due to the porous structure of its local surface plasma resonance effect and thin-film material and inhaled
It receives.
Secondly, the optical absorber also has fabulous flexibility.As shown in Figure 9 A, the film absorber can fold,
Curling, is convenient for carrying.Furthermore super flexible plasma light absorber has the good resistant to bending, characteristic that stretches, such as Fig. 9 B and
It shown in 9C, is stretched even across 800 times, film still has good mechanical flexibility.
Finally, the Photothermal characterisation of super flexible plasma light absorber is characterized, it is latent in Photo-thermal technology application to assess it
Power.As shown in Figure 10, super flexible plasma light absorber and real is illuminated using the broadband laser source with different output power
Shi Jilu temperature.Incident laser spot diameter is 4mm, and output power density range is from 4.7mW/mm2To 30.4mW/mm2.It can be with
It can be clearly seen, the heat of all generations all height limitations are around incident laser spot area.This is because aramid fiber Nanowire
Tie up the low (0.048Wm of thermal conductivity-1k-1), the thermal energy of generation is not easy to be transmitted to adjacent area, so that the local temperature of PMF can be anxious
Play rises.Each heating-cooling is recycled, power supply opens and closes 1 minute (line chart) respectively.Super flexible plasma light
The temperature-responsive of absorber is all very fast during heating and cooling.For example, when super flexible plasma light absorber quilt
30.4mW/mm2Laser output power irradiation when, from room temperature (20.5 DEG C) be heated to equilibrium temperature (147.2 DEG C) only need it is big
About 4.8s.Once light source is closed, super flexible plasma light absorber returns to the cooling procedure of room temperature also less than 5s.With different
Output power collects the equilibrium temperature of the super flexible plasma light absorber of laser light source exposure, it shows good linear
Correlation: Ts (DEG C)=3.69 × P (mW/mm2)+31.85, wherein Ts and P respectively represent equilibrium temperature and output power of power supply.
The coefficient of determination (R2) it is 0.9954.Linear correlation means to be easy to by adjusting power to control temperature, and vice versa.
Have benefited from the superior heat-stability of golden (fusing point: 1064 DEG C) and aramid fiber (decomposition temperature > 500 DEG C), PMF is at such high temperatures
Its physical property and function-stable can still be maintained.
The above content is combine it is specific/further detailed description of the invention for preferred embodiment, cannot recognize
Fixed specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs,
Without departing from the inventive concept of the premise, some replacements or modifications can also be made to the embodiment that these have been described,
And these substitutions or variant all shall be regarded as belonging to protection scope of the present invention.
Claims (10)
1. a kind of preparation method of light absorber characterized by comprising
S1. using aramid fiber as raw material, aramid nano-fiber solution is prepared；
S2. metal nanoparticle solution is prepared；
S3. the metal nanoparticle solution of aramid nano-fiber solution and step S2 preparation prepared by step S1 is mixed with mixed
Close solution；
S4. the mixed solution prepared by step S3, removal solvent obtain nano compound film light absorber；The light absorber with
Aramid nano-fiber is matrix, and metal nanoparticle is supported in the aramid nano-fiber matrix.
2. preparation method as described in claim 1, which is characterized in that the aramid fiber includes the Kevlar of E.I.Du Pont Company；It is described
Metal nanoparticle includes one of gold nano grain, silver nano-grain, copper nano particles or a variety of, described nano combined thin
Metal nanoparticle content is 2.8% or more in film.
3. preparation method as described in claim 1, which is characterized in that the step S1 includes:
S11. it is impregnated after aramid fiber being dried in vacuo and carries out fibrosis in the solution, then pull cleaning out and be dried in vacuo to obtain fibrosis
Aramid fiber；
S12. the fibrosis aramid fiber that step S11 is obtained is uniformly mixed stirring with alkali and solvent, becomes purple from colourless to solution
After Red oil solution, inorganic agent is added, obtains aramid nano-fiber solution.
4. preparation method as claimed in claim 3, which is characterized in that the vacuum before aramid fiber in the step S11
Drying condition are as follows: 60 DEG C -65 DEG C, dry 18h-24h；Vacuum drying condition after fibrosis is 60 DEG C -70 DEG C, dry 48h.
5. preparation method as claimed in claim 3, which is characterized in that alkali in the step S12 is potassium hydroxide, and hydrogen-oxygen
The mass ratio for changing potassium and aramid nano-fiber is 1:1-2:1；The solvent is N, N- dimethyl sulfoxide；The inorganic agent is phosphoric acid
With the mixed solution of water.
6. preparation method as claimed in claim 5, which is characterized in that the volume ratio of the phosphoric acid and water is 1:2-2:1；It is described
The percentage that the volume of inorganic agent accounts for mixed solution total volume is 1.0%-10%.
7. preparation method as described in claim 1, which is characterized in that the step S4 includes: the mixing for preparing step S3
Solution obtains nano compound film light absorber by way of suction filtration.
8. a kind of light absorber characterized by comprising aramid nano-fiber matrix, and it is supported on the aramid fiber Nanowire
Metal nanoparticle in Wiki matter.
9. light absorber as claimed in claim 8, which is characterized in that the aramid fiber includes the Kevlar of E.I.Du Pont Company；It is described
Metal nanoparticle includes one of gold nano grain, silver nano-grain, copper nano particles or a variety of.
10. light absorber as claimed in claim 8, which is characterized in that metal nanoparticle content is in the light absorber
2.8% or more.
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