CN106199775A - A kind of porous hemispherical array films with broadband, comprehensive its antireflective properties and preparation method thereof - Google Patents
A kind of porous hemispherical array films with broadband, comprehensive its antireflective properties and preparation method thereof Download PDFInfo
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- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
Abstract
A kind of porous hemispherical array films with broadband, comprehensive its antireflective properties and preparation method thereof, belongs to materials science field.The present invention utilizes mask etching method, physical gas-phase deposite method, colloidal self-assembly method etc., and whole process operation is easy, and process low consumption is cleaned, and controllability is high.The time etched by control and condition, can be prepared the porous hemispherical array of different pore size size and the degree of depth, thus realize its its antireflective properties.There is porous layer aggregated(particle) structure on porous hemispherical array prepared by the present invention, make sample surfaces reduce along with incident angle of light increases reflectance, thus obtain broadband, comprehensive antireflective plasma foil on the semispherical surface of bending.The level plasma structure prepared, may apply in the actual application such as photoelectric device, display device.
Description
Method field
The invention belongs to materials science field, be specifically related to a kind of there is broadband, comprehensive its antireflective properties
Porous hemispherical array films and preparation method thereof.
Background method
The attention that people are numerous has been attracted, because it is at camera gun at suprabasil antireflection film layer[1], the sun
Can battery[2]、LEDs[3], photodetector[4], light sensing and image[5,6]Huge effect has been played Deng in application.Substantial amounts of
Silicon[7], metal-oxide[8], polymer[9]And carbon[10]Micro-nano cone and the rod structure prepared Deng material have good antireflective
Energy.Recently, it has been found that metal nano-micro structure interacts with incident light the surface plasma body resonant vibration of generation[11]Have very well
Its antireflective properties, referred to as plasma antireflective.Subsequently, some novel plasma antireflection film layers are prepared out also
And its broadband, comprehensive reflection preventing ability are studied[12]。
But the preparation on curved surfaces of this plasma antireflection film layer is also not carried out.More for meeting
Potential application, in addition it is also necessary to plasma its antireflective properties has deeper understanding and further explores.One of them
Particularly challenge is exactly to prepare broadband, comprehensive plasma antireflection film layer on curved surfaces.This plasma membrane
Special effect can be played in photoelectric device and display device.
Summary of the invention
It is an object of the invention to provide a kind of have broadband, the porous hemispherical array films of comprehensive its antireflective properties and
Its preparation method.
The present invention utilizes mask etching method, physical gas-phase deposite method, colloidal self-assembly method etc., whole process operation
Simplicity, process low consumption cleaning, controllability is high.The time etched by control and condition, can prepare different pore size size with deep
The porous hemispherical array of degree, thus realize its its antireflective properties.
The present invention is as a example by realizing porous hemispherical array films, it is achieved have broadband, comprehensive its antireflective properties many
The preparation of hole hemispherical array films, specifically comprises the following steps that
1) substrate (the smooth substrate: glass, piezoid, silicon chip that hydrophilic treated is crossed is taken；Bending substrate: polydimethylsiloxanes
Alkane (PDMS), polyethylene terephthalate (PET), polypropylene (PP) etc.), the rotating speed with 1000～3000rpm by 10～
The toluene solution of the polystyrene (PS) of 100mg/mL is spun in this substrate, then this substrate is placed in room temperature environment natural
It is dried, thus in substrate, obtains polystyrene/toluene thin film that thickness is 200～2000nm；
2) 1～5mL, concentration be the deionization moisture of polystyrene microsphere of 1～20wt%, a diameter of 0.2～0.8 μm
Dissipate the deionized water adding 1～3mL in liquid, be centrifuged 3～5 minutes under 9000～14000rpm rotating speeds, obtain after centrifugal
Solids add 1～3mL deionized water and is again centrifuged, repeating to add deionized water and centrifugal process 4～7 times；
Ethanol and the mixed liquor of deionized water that 1～5mL volume ratio is 1:1 is added, 9000 in the last centrifugal solids obtained
～under 14000rpm rotating speed centrifugal 5～10 minutes, repeat to add ethanol and deionized water mixed liquor and centrifugal process 4～20 times,
Add, in the last centrifugal solids obtained, the ethanol and the mixed liquor of deionized water that 1～5mL volume ratio is 1:1, thus
Obtain ethanol and the deionized water dispersion liquid of hydrophobic polystyrene microsphere；0.1～0.5mL is drawn hydrophobic poly-with disposable syringe
The ethanol of phenylethylene micro ball and deionized water dispersion liquid, be added drop-wise to fill in the container of deionized water, hydrophobic polystyrene microsphere
Gas-liquid interface at air-deionized water is arranged as monolayer, add 50～200 μ L, concentration be 1～10wt% dodecyl
Sulfonate surfactants makes hydrophobic polystyrene microsphere close-packed arrays each other, substrate (the smooth substrate: glass crossed by hydrophilic treated
Glass, piezoid, silicon chip；Bending substrate: polydimethylsiloxane (PDMS), polyethylene terephthalate (PET), polypropylene
(PP) etc.) compact arranged for monolayer hydrophobic polystyrene microsphere is held up, be placed on natural drying in inclined plane, thus in substrate
Obtain a diameter of 0.2～0.8 μm monolayer compact arranged hydrophobic polystyrene micro-sphere array of sequential 2 D；
1～5mL, concentration be 1～20wt%, a diameter of 2～5 μm the deionized water dispersion liquid of polystyrene microsphere in
Add the deionized water of 1～3mL, be centrifuged 3～5 minutes under 4000～8800rpm rotating speeds, in the solids obtained after centrifugal
Add 1～3mL deionized water and be again centrifuged, repeating to add deionized water and centrifugal process 4～7 times；Finally from
Gains in depth of comprehension to solids in add 1～5mL volume ratio be ethanol and the mixed liquor of deionized water of 1:1,4000～8800rpm
Under rotating speed centrifugal 5～10 minutes, repeat to add ethanol and deionized water mixed liquor and centrifugal process 4～20 times, last centrifugal
The solids obtained adds ethanol and the mixed liquor of deionized water that 1～5mL volume ratio is 1:1, thus obtains hydrophobic poly-
The ethanol of phenylethylene micro ball and deionized water dispersion liquid；0.1～0.5mL hydrophobic polystyrene microsphere is drawn with disposable syringe
Ethanol and deionized water dispersion liquid, be added drop-wise to fill in the container of deionized water, hydrophobic polystyrene microsphere air-go from
The gas-liquid interface of sub-water is arranged as monolayer, add 50～200 μ L, concentration be 1～10wt% dodecyl sodium sulfate surface
Activating agent makes hydrophobic polystyrene microsphere close-packed arrays each other, by step 1) polystyrene prepared/toluene film substrate will be single
The compact arranged hydrophobic polystyrene microsphere of layer holds up, and is placed on natural drying in inclined plane, thus obtains two dimension in substrate and have
The a diameter of 2～5 μm monolayer compact arranged hydrophobic polystyrene micro-sphere array of sequence；
3) by step 2) a diameter of 0.2～0.8 compact arranged hydrophobic polystyrene of μm monolayer of sequential 2 D for preparing
Micro-sphere array substrate is placed in reactive plasma etching machine, etching air pressure be 5～10mTorr, etching temperature be 10～
20 DEG C, oxygen gas flow rate is 10～50sccm, under conditions of etching power is 30～100W, etches 100～300 seconds；In this mistake
Cheng Zhong, polystyrene microsphere is etched and tapers into；Then etched sample is placed on the sample of vacuum evaporation coating film device
In sample platform, sample normal is 0～50 ° with the angle (i.e. angle of incidence) of deposition direction, 5 × 10-4～1 × 10-3The vacuum of Pa
Lower thermal evaporation deposition Aurum metallicum, deposition velocity isThe thickness of deposited gold film is 50～100nm；By thermal evaporation deposition
The substrate of complete gold film puts in toluene ultrasonic 3～10min, and ultrasonic power is 40～100W, removes polystyrene microsphere and obtains week
Phase be 0.2～0.8 μm, aperture be the gold nano pore membrane array substrate of 100～200nm；
4) by step 2) a diameter of 2～5 μm monolayer compact arranged hydrophobic polystyrene microsphere of sequential 2 D for preparing
Array substrate is placed in 80～110 DEG C of baking ovens 0.1～1 hour, then takes out stand-by；
5) by step 3) prepare gold nano pore membrane array substrate tilt after be immersed in dilute with water 10～20 at leisure
In the aqueous solution of Fluohydric acid. again (Fluohydric acid. is commercialization analytical pure product, and mass fraction is 40%), make gold nano pore membrane battle array
Row depart from substrate and are suspended in water/Air Interface；Then by step 4) substrate that obtains picks up the gold nano pore membrane of suspension gently
Array, natural air drying in room temperature environment；
6) by step 5) prepare substrate be placed in reactive plasma etching machine, etching air pressure be 5～
Under conditions of 10mTorr, etching temperature are 10～20 DEG C, oxygen gas flow rate is 10～50sccm, etching power is 30～100W, carve
Lose 100～300 seconds；In this process, with gold nano pore membrane array as mask, by tight for a diameter of 2～5 following μm monolayers
The hydrophobic polystyrene micro-sphere array of arrangement is etched into porous pattern, then removes gold nano pore membrane array with gold etching agent；Then
Being placed on the sample stage of vacuum evaporation coating film device by etched sample, sample normal (i.e. enters with the angle of deposition direction
Firing angle) it is 0～50 °, 5 × 10-4～1 × 10-3Thermal evaporation deposition argent under the vacuum of Pa, deposition velocity is The thickness of deposition silverskin is 50～100nm, obtains one of the present invention and has broadband, comprehensive its antireflective properties
Porous hemispherical array films；
Separately take the sample that step 4 obtains to be placed on the sample stage of vacuum evaporation coating film device, sample normal and deposition side
To angle (i.e. angle of incidence) be 0～50 °, 5 × 10-4～1 × 10-3Thermal evaporation deposition argent is carried out under the vacuum of Pa,
Deposition velocity isDeposit thickness is 50～100nm, obtains hemispherical Shell array films, as reference sample；
By step 6) sample prepared is placed on the sample stage of fiber spectrometer, tests its reflectivity properties；Change incidence
The direction of light, the reflectivity properties of test different directions incident illumination.
By step 6) sample prepared is placed on and screen vertical, the position of horizontal range screen 10～30cm.Then use
A branch of wavelength is that the laser of 635nm irradiates, it was demonstrated that its its antireflective properties in actual applications.
Step 1) described in smooth substrate be sheet glass, piezoid, silicon chip；Bending substrate is polydimethylsiloxane
(PDMS), polyethylene terephthalate (PET), polypropylene (PP) etc..The hydrophilic treated of substrate is that substrate is put into quality
In the mixed solution of the concentrated sulphuric acid of mark 98% and the hydrogen peroxide of mass fraction 30%, heating in water bath is to 70～90 DEG C, keeps 3
～8 hours, then use deionized water cyclic washing, nitrogen dries up；The volume ratio of concentrated sulfuric acid solution and hydrogenperoxide steam generator is 7:
3。
Each step operation of the present invention is simple, and controllability is strong, has porous level to tie on the porous hemispherical array of preparation
Structure, make sample surfaces along with incident angle of light increase reflectance reduce, thus bending semispherical surface on obtain broadband,
Comprehensive antireflective plasma foil.The level plasma structure prepared, may apply to photoelectric device, display
In the actual application such as part.
Accompanying drawing explanation
Fig. 1 is the flow chart of preparation porous hemispherical array；Figure denotes material and the primary operational step of various utilization
Suddenly；Wherein, substrate 1, polystyrene/toluene thin film 2,330nm polystyrene microsphere 3,3 μm polystyrene microsphere 4, Jenner's metre hole
Film 5, porous hemispherical array 6, silverskin 7；
Fig. 2 is that (A top view, B side view and 45 ° tilt figure to porous hemispherical array scanning ultramicroscope (SEM) photo
(illustration in figure B), C (A partial enlargement 1 times figure, scale is 1 μm))；The structural parameters signal of D porous hemispherical dome structure unit
(polystyrene microsphere 4, silverskin 7, D represents the cycle (the biggest ball size 2～5 μm) of porous hemispherical array films, P represents Jenner
Metre hole film covers the cycle (i.e. bead size 0.2～0.8nm) of plate, H represents the degree of depth (100～200nm) of etched hole, d represents many
The bore dia (100～200nm) of empty hemispherical array films)；
The spectrogram that Fig. 3 fiber spectrometer records.(A black line represents the reflectance spectrum of hemispherical Shell array films, and red line represents
The reflectance spectrum of porous hemispherical array films, illustrate the anti-reflection performance of porous hemispherical array films wave-length coverage be 400～
Broadband between 1000nm all very well, the incident illumination of B different angles time, the reflectance spectrum of porous hemispherical array films, explanation
Porous hemispherical array films has omnibearing anti-reflection performance)；
Fig. 4 is its antireflective properties exemplary plot of porous hemispherical array films, and correspondence is embodiment 11.((wavelength is A laser
635nm) be irradiated on conventional silver mirror, it can be seen that screen (screen is vertical with the position relationship of silver mirror, horizontal range 10～
30cm) upper flare is very strong, B laser is irradiated on hemispherical Shell array films it can be seen that on screen flare the most weak, explanation
The anti-reflection performance of porous hemispherical array films, C laser half are radiated on silver mirror, and second half is radiated at porous hemispherical array films
On, it can be seen that irradiate flare on the screen of silver mirror part very strong, and irradiate the screen of porous hemispherical array films part
Upper flare is hardly visible, and is radiated at many completely by anti-reflection performance, the D laser of comparative illustration porous hemispherical array films
On the hemispherical array films of hole, it can be seen that on screen, flare is hardly visible, the anti-reflection of porous hemispherical array films is described
Performance is the best).
Detailed description of the invention
Embodiment 1: the preparation of hydrophilic glass sheet
Sheet glass used diamant is cut out to 2.5cm length, and 3.5cm is roomy little, put into concentrated sulphuric acid (mass fraction 98%) with
In the mixed solution (volume ratio is 7:3) of hydrogen peroxide (mass fraction 30%), heating in water bath is to 80 DEG C, keeps 5 hours, to obtain final product
To hydrophilic glass sheet；Mixed solution is poured in waste liquid bottle, the sheet glass deionized water cyclic washing obtained 4 times, and use nitrogen
Air-blowing is done.
Embodiment 2: the preparation of polystyrene PS/ toluene thin film
Polystyrene microsphere is dissolved in toluene, is configured to the solution that concentration is 10mg/mL.Utilize desk-top sol evenning machine with
The rotating speed spin coating of 3000rpm 30 seconds, is spun on hydrophilic glass sheet, then places it in natural air drying in room temperature environment,
To the polystyrene PS/ toluene thin film that 200nm is thick.
Embodiment 3: the preparation of hydrophobic polystyrene microsphere
At normal temperatures, 1mL, 5wt%, a diameter of 330nm polystyrene microsphere aqueous dispersions in add 3mL deionization
Water, is centrifuged 5 minutes with 14000rpm rotating speed, draws the supernatant, adds 3mL deionized water also in left solids
Again it is centrifuged, hereafter repeats this process 7 times.After drawing the supernatant the last time, in solids, add 1mL's
Ethanol and the mixed liquor of 1mL deionized water, be centrifuged 5 minutes with 14000rpm rotating speed, draws the supernatant, then consolidating of leaving over
State thing add identical ethanol and the mixed liquor of deionized water and is centrifuged by identical method, hereafter repeating this centrifugal process
16 times, after drawing the supernatant the last time, solids is eventually adding 1mL ethanol and 1mL deionized water, obtains hydrophobic
The ethanol of a diameter of 330nm polystyrene microsphere of 10wt% and the dispersion liquid of deionized water；
At normal temperatures, 1mL, 5wt%, a diameter of 3 μm polystyrene microsphere aqueous dispersions in add 3mL deionization
Water, is centrifuged 5 minutes with 8000rpm rotating speed respectively, draws the supernatant, adds 3mL deionization in left solids
Water is also centrifuged again, hereafter repeats this process 7 times.After drawing the supernatant the last time, add in solids
The ethanol of 1mL and 1mL deionized water, be centrifuged 5 minutes with 8000rpm rotating speed, draws the supernatant, then in the solids left over
In add identical ethanol and the mixed liquor of deionized water and be centrifuged by identical method, hereafter repeat this centrifugal process 16
Secondary, after drawing the supernatant the last time, solids is eventually adding 1mL ethanol and 1mL deionized water, obtains hydrophobic
A diameter of 3 μm polystyrene microsphere ethanol and dispersion liquids of deionized water of 10wt%.
The preparation of embodiment 4: six side closelypacked monolayer polystyrene colloid crystal
The second of the hydrophobic polystyrene microsphere of a diameter of 330nm of 0.2mL embodiment 3 preparation is drawn with disposable syringe
Alcohol aqueous dispersions, slowly drips on the interface of air-deionized water of culture dish, stands a moment, adds along culture dish side
50 μ L concentration are the aqueous solution of the sodium lauryl sulphate of 10wt%, and it is closelypacked that polystyrene microsphere can be subsequently formed six sides
Monolayer.With hydrophilic glass sheet as substrate, it extend into below the water surface, slowly upwards carry below close monolayer polystyrene microsphere
Rise, be placed in inclined-plane natural drying, thus obtain a diameter of closelypacked polystyrene colloid of 330nm monolayer on the glass substrate
Crystal；
The ethanol of the hydrophobic polystyrene microsphere of a diameter of 3 μm of 0.2mL embodiment 3 preparation is drawn with disposable syringe
Aqueous dispersions, slowly drips on the interface of air-deionized water of culture dish, stands a moment, adds 50 μ along culture dish side
L concentration is the aqueous solution of the sodium lauryl sulphate of 10wt%, and polystyrene microsphere can be subsequently formed the six closelypacked lists of side
Layer.There is the sheet glass of PS/ toluene as substrate with the spin coating of embodiment 2 preparation, extend into below the water surface, from close monolayer polyphenyl
Slowly it is lifted up below ethylene microsphere, is placed in inclined-plane natural drying, thus in PS/ toluene substrate of glass, obtains 3 μm monolayers
Closelypacked polystyrene colloid crystal.
Embodiment 5: the preparation of gold nano pore membrane array
The substrate of glass of the sequential 2 D monolayer polystyrene microsphere array of above-mentioned prepared a diameter of 330nm is placed in instead
In answering property plasma etching machine, being 10mTorr at etching air pressure, etching temperature is 20 DEG C, and oxygen gas flow rate is 50sccm, etching
Under conditions of power is 100W, etch 180 seconds；In this process, microsphere is etched and tapers into；Then by etched sample
Product are placed on the sample stage of vacuum evaporation coating film device, and sample normal is 0 ° with the angle (i.e. angle of incidence) of deposition direction, 5
×10-4Carrying out thermal evaporation deposition Aurum metallicum under the vacuum of Pa, deposition velocity isDeposit thickness is 100nm；Will evaporation
Ultrasonic 3min in toluene is put in complete substrate, and power is 40w, and remove microsphere obtaining the cycle is 330nm, and aperture is the gold of 200nm
Nano-pore membrane array substrate；
Embodiment 6: the method increasing colloidal crystal and the adhesiveness of substrate
The PS/ toluene glass base of the sequential 2 D monolayer polystyrene microsphere array of a diameter of 3 μm that embodiment 4 is prepared
The end, is placed in 20min in 110 DEG C of baking ovens, then takes out stand-by；
Embodiment 7: the transfer of gold nano pore membrane
Gold nano pore membrane array substrate embodiment 5 prepared tilts to be immersed in the hydrogen fluorine of dilute with water 10 times at leisure
10s in aqueous acid (mass fraction 40% of solution before dilution), makes gold nano pore membrane array depart from substrate and be suspended in water/sky
Vapor interface.The substrate obtained by embodiment 6 picks up the gold nano pore membrane array of suspension, natural air drying in room temperature environment gently.
Embodiment 8: the preparation of porous hemispherical array
Sample prepared by embodiment 7 is placed in reactive plasma etching machine, is 10mTorr at etching air pressure, carves
Erosion temperature is 20 DEG C, and oxygen gas flow rate is 50sccm, under conditions of etching power is 100W, etches 240 seconds；In this process,
Gold nano pore membrane array is as mask, and etching 3 following μm microspheres is porous pattern, removes gold nano pore membrane battle array with gold etching agent
Row, (structural parameters of porous hemispherical array structure unit represent porous half for (such as Fig. 2 D): D to obtain porous hemispherical array
The cycle (the biggest ball size 3 μm) of ball array film, P represent gold nano pore membrane and cover the cycle (i.e. bead size 330nm) of plate, H
Represent the degree of depth (150nm) of etched hole, the bore dia (200nm) of the many empty hemispherical array films of d representative).
Embodiment 9: the evaporation coating method of argent
The sample of embodiment 8 is placed on the sample stage of vacuum evaporation coating film device, sample normal and deposition direction
Angle (i.e. angle of incidence) is 0 °, 5 × 10-4Vacuum under carry out thermal evaporation deposition argent, deposition velocity isHeavy
Long-pending thickness is 50nm, obtains porous hemispherical array films.
Embodiment 10: detection porous hemispherical array films broadband, the comprehensive method subtracting emission characteristic
The sample of embodiment 9 is placed on the sample stage of fiber spectrometer, tests its reflectivity properties；It is 400 at wavelength
～1000nm scope, when angle of incidence is 0 °, the reflectance of porous hemispherical array films is about 0.5%, it was demonstrated that its wideband
Band its antireflective properties, corresponding diagram 3A.Changing the direction (angle of incidence is respectively 0 °, 15 °, 25 °, 35 °, 45 °) of incident illumination, test is not
With reflectivity properties during incident illumination direction.Find that the reflectance of porous hemispherical array films also subtracts along with incident angle of light increases
Little, and minima reaches 0.05%.Demonstrate its comprehensive its antireflective properties, corresponding diagram 3B.
Embodiment 11: prove the method that porous hemispherical array films its antireflective properties is applied in real life
The sample of preparation is placed on and screen vertical, the position of horizontal range screen 20cm.Then with a branch of wavelength it is
The laser of 635nm irradiates sample, it was demonstrated that its its antireflective properties in actual applications, corresponding diagram 4.
The above, be only presently preferred embodiments of the present invention, not the method scheme of the present invention is made any form
On restriction.Any simple modification, equivalent that above example is made by the method essence of every foundation present invention change and repair
Decorations, each fall within protection scope of the present invention.
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Claims (9)
1. having a preparation method for the porous hemispherical array films of broadband, comprehensive its antireflective properties, its step is as follows:
1) take the substrate that hydrophilic treated is crossed, the rotating speed with 1000～3000rpm by 10～100mg/mL the toluene of polystyrene
Solution is spun in this substrate, and then this substrate be placed on natural drying in room temperature environment, thus obtains thickness in substrate and be
The polystyrene of 200～2000nm/toluene thin film；
2) in substrate, prepare a diameter of 0.2～0.8 compact arranged hydrophobic polyphenyl second of μm monolayer of sequential 2 D respectively
The a diameter of 2～5 μm monolayer compact arranged hydrophobic polystyrene micro-sphere array of alkene micro-sphere array and sequential 2 D；
3) by step 2) a diameter of 0.2～0.8 μm monolayer compact arranged hydrophobic polystyrene microsphere of sequential 2 D for preparing
Array substrate is placed in reactive plasma etching machine, etches 100～300 seconds；In this process, polystyrene microsphere quilt
Etching tapers into；Then being placed on by etched sample on the sample stage of vacuum evaporation coating film device, sample normal is with heavy
The angle in long-pending direction is 0～50 °, and the thickness of deposited gold film is 50～100nm；First is put in the substrate of complete for thermal evaporation deposition gold film
In benzene ultrasonic 3～10min, ultrasonic power is 40～100W, and remove polystyrene microsphere obtaining the cycle is 0.2～0.8 μm, aperture
It it is the gold nano pore membrane array substrate of 100～200nm；
4) by step 2) a diameter of 2～5 μm monolayer compact arranged hydrophobic polystyrene micro-sphere array of sequential 2 D for preparing
Substrate is placed in 80～110 DEG C of baking ovens 0.1～1 hour, then takes out stand-by；
5) by step 3) prepare gold nano pore membrane array substrate tilt after be immersed in the hydrogen fluorine diluting 10～20 times at leisure
In acid solution, gold nano pore membrane array is made to depart from substrate and be suspended in water/Air Interface；Then by step 4) substrate that obtains is light
Gently pick up the gold nano pore membrane array of suspension, natural air drying in room temperature environment；
6) by step 5) prepare substrate be placed in reactive plasma etching machine, etch 100～300 seconds；In this process
In, with gold nano pore membrane array as mask, by following a diameter of 2～5 μm monolayer compact arranged hydrophobic polystyrene microsphere
Array is etched into porous pattern, then removes gold nano pore membrane array with gold etching agent；Then etched sample is placed on very
On the sample stage of empty evaporating and coating equipment, sample normal is 0～50 ° with the angle of deposition direction, and the thickness of deposition silverskin is 50
～100nm, obtain the porous hemispherical array films with broadband, comprehensive its antireflective properties.
A kind of system of the porous hemispherical array films with broadband, comprehensive its antireflective properties
Preparation Method, it is characterised in that: be 1～5mL, concentration be the polystyrene microsphere of 1～20wt%, a diameter of 0.2～0.8 μm
Deionized water dispersion liquid adds the deionized water of 1～3mL, under 9000～14000rpm rotating speeds centrifugal 3～5 minutes, from
The solids obtained after the heart add 1～3mL deionized water and is again centrifuged, repeating add deionized water and be centrifuged
Journey 4～7 times；Add, in the last centrifugal solids obtained, ethanol and the mixing of deionized water that 1～5mL volume ratio is 1:1
Liquid, is centrifuged 5～10 minutes under 9000～14000rpm rotating speeds, repeats to add ethanol and deionized water mixed liquor and centrifugal process
4～20 times, add, in the last centrifugal solids obtained, the ethanol and the mixing of deionized water that 1～5mL volume ratio is 1:1
Liquid, thus obtain ethanol and the deionized water dispersion liquid of hydrophobic polystyrene microsphere；With disposable syringe draw 0.1～
The ethanol of 0.5mL hydrophobic polystyrene microsphere and deionized water dispersion liquid, be added drop-wise to fill in the container of deionized water, hydrophobic poly-
Phenylethylene micro ball is arranged as monolayer at the gas-liquid interface of air-deionized water, adds 50～200 μ L, concentration is 1～10wt%
Dodecyl sodium sulfate surfactant make hydrophobic polystyrene microsphere close-packed arrays each other, the substrate crossed by hydrophilic treated will
Monolayer compact arranged hydrophobic polystyrene microsphere holds up, and is placed on natural drying in inclined plane, thus obtains two dimension in substrate
Orderly a diameter of 0.2～0.8 μm monolayer compact arranged hydrophobic polystyrene micro-sphere array.
A kind of system of the porous hemispherical array films with broadband, comprehensive its antireflective properties
Preparation Method, it is characterised in that: be 1～5mL, concentration be 1～20wt%, a diameter of 2～5 μm polystyrene microsphere go from
Sub-aqueous dispersions adds the deionized water of 1～3mL, is centrifuged 3～5 minutes under 4000～8800rpm rotating speeds, after centrifugal
To solids in add 1～3mL deionized water and be again centrifuged, repeat to add deionized water and centrifugal process 4～7
Secondary；Add, in the last centrifugal solids obtained, ethanol and the mixed liquor of deionized water that 1～5mL volume ratio is 1:1,
It is centrifuged 5～10 minutes under 4000～8800rpm rotating speeds, repeats to add ethanol and deionized water mixed liquor and centrifugal process 4～20
Secondary, add, in the last centrifugal solids obtained, the ethanol and the mixed liquor of deionized water that 1～5mL volume ratio is 1:1, from
And obtain ethanol and the deionized water dispersion liquid of hydrophobic polystyrene microsphere；0.1～0.5mL is drawn hydrophobic with disposable syringe
The ethanol of polystyrene microsphere and deionized water dispersion liquid, be added drop-wise to fill in the container of deionized water, and hydrophobic polystyrene is micro-
Ball is arranged as monolayer at the gas-liquid interface of air-deionized water, add 50～200 μ L, concentration be 1～10wt% dodecane
Base sulfonate surfactants makes hydrophobic polystyrene microsphere close-packed arrays each other, by step 1) polystyrene/toluene of preparing
Compact arranged for monolayer hydrophobic polystyrene microsphere is held up by film substrate, is placed on natural drying in inclined plane, thus in substrate
On obtain a diameter of 2～5 μm monolayer compact arranged hydrophobic polystyrene micro-sphere array of sequential 2 D.
A kind of system of the porous hemispherical array films with broadband, comprehensive its antireflective properties
Preparation Method, it is characterised in that: the etching air pressure of reactive plasma etching is 5～10mTorr, etching temperature is 10～20
DEG C, oxygen gas flow rate be 10～50sccm, etching power be 30～100W.
A kind of system of the porous hemispherical array films with broadband, comprehensive its antireflective properties
Preparation Method, it is characterised in that: the vacuum of vacuum vapor plating is 5 × 10-4～1 × 10-3Pa, deposition velocity is
A kind of system of the porous hemispherical array films with broadband, comprehensive its antireflective properties
Preparation Method, it is characterised in that: substrate is smooth substrate or bending substrate.
A kind of system of the porous hemispherical array films with broadband, comprehensive its antireflective properties
Preparation Method, it is characterised in that: smooth substrate is sheet glass, piezoid or silicon chip；Bending substrate is polydimethylsiloxane, poly-right
PET or polypropylene.
A kind of system of the porous hemispherical array films with broadband, comprehensive its antireflective properties
Preparation Method, it is characterised in that: the hydrophilic treated of substrate is that substrate is put into concentrated sulphuric acid and the mass fraction of mass fraction 98%
In the mixed solution of the hydrogen peroxide of 30%, heating in water bath is to 70～90 DEG C, keeps 3～8 hours, then with deionized water repeatedly
Washing, nitrogen dries up；The volume ratio of concentrated sulfuric acid solution and hydrogenperoxide steam generator is 7:3.
9. a porous hemispherical array films with broadband, comprehensive its antireflective properties, it is characterised in that: it is to be wanted by right
The method described in 1～8 any one is asked to prepare.
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| CN111272730A (en) * | 2020-02-11 | 2020-06-12 | 南京信息工程大学 | High-sensitivity optical fiber surface plasmon sensor and preparation method thereof |
| CN111272730B (en) * | 2020-02-11 | 2022-08-02 | 南京信息工程大学 | High-sensitivity optical fiber surface plasmon sensor and preparation method thereof |
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