CN106526719B - Homogeneity bilayer SiO2The automatically cleaning antireflective film compound with polytetrafluoroethylene (PTFE) and preparation method - Google Patents
Homogeneity bilayer SiO2The automatically cleaning antireflective film compound with polytetrafluoroethylene (PTFE) and preparation method Download PDFInfo
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- CN106526719B CN106526719B CN201710013416.0A CN201710013416A CN106526719B CN 106526719 B CN106526719 B CN 106526719B CN 201710013416 A CN201710013416 A CN 201710013416A CN 106526719 B CN106526719 B CN 106526719B
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- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/18—Coatings for keeping optical surfaces clean, e.g. hydrophobic or photo-catalytic films
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- G—PHYSICS
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- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
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Abstract
A kind of homogeneity bilayer SiO2The automatically cleaning antireflective film compound with polytetrafluoroethylene (PTFE) and preparation method, the antireflective film are combined by compact silicon dioxide layer, porous silicon dioxide nano stick layer and polytetrafluorethylenano nano stick；Preparation method is using electron beam evaporation methods, and compact silicon dioxide, porous silica and polytetrafluorethylenano nano stick laminated film that three layers of refractive index are gradually successively decreased are sequentially depositing in transparent or semitransparent substrate.The laminated film is respectively provided with the multi-angle incident light in visible-range good anti-reflection effect, compared with the double-deck silicon oxide film of non-ptfe composite nanometer rods, the laminated film is while anti-reflection effect is improved, also there is good thermal stability, hydrophobicity and the mechanical adhesion with matrix, the application request of the surfaces anti-reflections such as optical device, automatically cleaning solar cell, photonic device, colour filter, optical recorder can be met.
Description
Technical field
The present invention relates to a kind of homogeneity bilayer SiO2The automatically cleaning antireflective film compound with polytetrafluoroethylene (PTFE) and preparation method belong to
In nano material and optical anti-reflection technical field of film preparation.
Background technology
Anti-reflection film is widely used in the fields such as machinery, electronics, laser, medicine, due to that can effectively reduce light reflection, increases
Add the transmission capacity of light, be applied primarily to all kinds of optical lens, photoelectric device, digital information display, dielectric film, electronics
Antireflection antireflecting coating needed for film, optoelectronic film, colour filter, optical recorder etc..It is mainly by substrate deposit one
Layer or the film that changes in gradient of multilayer refractive index make the interfacial refraction rate between outermost layer film and environment be down to or close to 1
To reduce the reflection of light.
Be mostly hydrophilic nmature however, as current most of anti-reflective coating layer surface, during use can by environment steam,
The pollution of dust granule and the anti-reflective for reducing film, the in addition heat of basis material and thin-film material in film deposition process
The difference of the coefficient of expansion, the imperfection of structural arrangement or structural rearrangement and cause interface internal stress excessive, lead to film
Mechanicalness is poor, in actual application, easily because of the factors such as absorption of the washing away of steam, grease and organic pollution in environment
It causes the damage of film microstructure or even film separation can be caused to lose the characteristic of automatically cleaning and anti-reflection.
Therefore it needs to develop new anti-reflection membrane preparation technology, while the effect of film anti-reflection is improved, it may have good
Good thermal stability, hydrophobicity and the mechanical adhesion with matrix, to meet application request.
Invention content
The object of the present invention is to provide a kind of homogeneity bilayer silica and the compound automatically cleaning antireflective film of polytetrafluoroethylene (PTFE),
Make it while the effect of film anti-reflection is improved, it may have good thermal stability, hydrophobicity and glued with the machinery of matrix
Attached power, to meet application request.
It is yet another object of the invention to provide a kind of homogeneity bilayer silica automatically cleanings compound with polytetrafluoroethylene (PTFE) to subtract
The preparation method of anti-film.
In order to achieve the above object, the present invention adopts the following technical scheme that：
A kind of homogeneity bilayer silica and the compound automatically cleaning antireflective film of polytetrafluoroethylene (PTFE), it is characterised in that:The anti-reflection
Film is that the compact silicon dioxide layer, porous silicon dioxide nano stick layer and polytetrafluorethylenano nano stick gradually to be successively decreased by refractive index is answered
It closes.
In above-mentioned technical proposal, the dense oxide silicon layer thickness is 90~99nm；Porous silicon dioxide nano stick thickness
It is 63%~67% to spend for 85~90nm, porosity；Polytetrafluorethylenano nano stick layer thickness is 140~150nm, porosity is
80%~83%.
The technical characteristic of the present invention also resides in：The refractive index of dense oxide silicon layer is 1.21~1.45, and porous silica is received
The refractive index of rice stick layer is 1.17~1.21, and the refractive index of polytetrafluorethylenano nano stick layer is 1~1.17.
The preparation side of a kind of homogeneity bilayer silica provided by the invention and the compound automatically cleaning antireflective film of polytetrafluoroethylene (PTFE)
Method, it is characterised in that this method comprises the following steps：
1) using electron beam evaporation methods, angle of deposit is first set as 0 °, is deposited in transparent or semitransparent substrate
The compact silicon dioxide layer that a layer thickness is 90~99nm, refractive index is 1.21~1.45；
2) angle of deposit is set as 80 °, in the dense porous silicon dioxide layer of acquisition, deposition a layer thickness for 85~
The porous silicon dioxide nano stick layer that 90nm, porosity are 63%~67%, refractive index is 1.17~1.21
3) angle of deposit is set as 85 °, deposition pressure 10-4~10-5Pa, in the porous silicon dioxide nano of acquisition
On stick layer deposit a layer thickness be 140~150nm, the polytetrafluoroethylene (PTFE) that refractive index is 1~1.17, porosity is 80%~83%
Nanometer rods layer.
In method described above, the substrate is using quartz plate, BK7, SF5, LAK14, FTO or sends in Simon Rex glass
Any, their refractive index is between 1.45~1.95.
The present invention has the following advantages and the technique effect of high-lighting：1. antireflection：By in three layers of folding of substrate deposit
Penetrate the film that rate changes in gradient, segmentation reduces refractive index difference of the matrix with environment to light, make outermost layer film and environment it
Between interfacial refraction rate be down to or reduced close to 1 the reflection of light.2. high stability and self-cleaning property：Due to high molecular material ratio
The good mechanochemistry properties such as intensity is high, not soluble in water, wear-resisting, self-lubricating are coated in anti-reflection film surface, can be notable
Thermostabilization, hydrophobicity and the mechanical adhesion with matrix of film are improved, it in actual use will not be by environment steam, ash
The pollution of dirt particle and the anti-reflective for reducing film.3. in the case where not influencing material antireflection rate, can effectively improve thin
Film failure intensity, while film surface wetting type can be changed to the greatest extent, it is made to become hydrophobicity from hydrophily.
Description of the drawings
Fig. 1 is homogeneity bilayer SiO provided by the invention2Compound high stability automatically cleaning subtracts with polytetrafluoroethylene (PTFE) (PTFE)
The schematic cross-section of anti-film.
Wherein：1- substrates；2- densifications SiO2Layer；The porous SiO of 3-2Nanometer rods layer；4- polytetrafluorethylenano nano stick layers.
Fig. 2 is the homogeneity bilayer SiO of the present invention2The cross-sectional scans Electronic Speculum in kind of compound automatically cleaning antireflective film is shone with PTFE
Piece.
Fig. 3 is the homogeneity bilayer SiO of the present invention2The reality of the Normal incidence reflectance rate of the automatically cleaning antireflective film compound with PTFE
Test value and calculated value.
Wherein：Ds representatives are vertical using three layers of compound antireflective film in BK7 deposition on glass of optical software calculating
Incident reflectivity；De is represented according to optical software result of calculation, utilizes the compound antireflective film of electron beam evaporation equipment experiment deposition
Normal incidence reflectance rate.
Fig. 4 is the homogeneity bilayer SiO of the present invention2The automatically cleaning antireflective film compound with PTFE is in the different incidence angles of visible ray
Three-dimensional reflection rate under degree, different wave length.
Fig. 5 is the homogeneity bilayer SiO of the present invention2It is vertical anti-with the room temperature of high stability automatically cleaning antireflective film that PTFE is compound
Penetrate rate and the vertical reflectivity after 100 DEG C of annealings.
Fig. 6 is the homogeneity bilayer SiO of the present invention2It is vertical anti-with the room temperature of high stability automatically cleaning antireflective film that PTFE is compound
Penetrate rate and the vertical reflectivity after 200 DEG C of annealings.
Specific embodiment
A kind of homogeneity bilayer SiO provided by the invention2The compound automatically cleaning antireflective film with polytetrafluoroethylene (PTFE) (PTFE), be
Transparent or semitransparent substrate surface is sequentially depositing compact silicon dioxide layer 2, the porous dioxy that three layers of refractive index are gradually successively decreased
What SiClx nanometer rods layer 3 and polytetrafluorethylenano nano stick layer 4 were combined.Fig. 1 is homogeneity bilayer SiO provided by the invention2With
The schematic cross-section of the compound automatically cleaning antireflective film of polytetrafluoroethylene (PTFE), incident light is in air-anti-reflection membrane interface, PTFE nanometer rods
Layer-porous SiO2Nanometer rods bed boundary, bilayer SiO2Reflection and transmission occur at interface and antireflective film-substrate interface.
Refractive index per layer film is controlled by the incident angle of electron beam evaporation plating, and thickness is different according to substrate and adjusts.It causes
The refractive index of close silicon oxide layer is 1.21~1.45, and the refractive index of porous oxidation silicon nanorod layer is 1.17~1.21, polytetrafluoro
The refractive index of ethylene nanometer rods layer is 1~1.17.Their thickness is respectively 90~99nm, 85~90nm, 140~150nm；Its
In porous SiO2The porosity of layer and PTFE nanometer rods layers is respectively 63%~67%, 80%~83%.It is described transparent or semi-transparent
Bright substrate is using quartz plate, BK7, SF5, LAK14, FTO or sends any one of Simon Rex glass, their refractive index exists
Between 1.45~1.95.
Preparation method provided by the invention is：First with TFCalc optical software simulated dual-layers SiO2With PTFE is compound subtracts
The thickness and refractive index of anti-film are found and optimize anti-reflection parameter.Then, it is calculated according to simulation, deposits refraction in substrate successively
The fine and close SiO that rate is gradually successively decreased2Layer, porous SiO2The laminated film of layer and PTFE nanometer rods layers, wherein densification SiO2Layer, it is porous
SiO2The refractive index of layer and PTFE nanometer rods layers is controlled by the incident angle of electron beam evaporation plating, further according to the difference point of base material
Their thickness is not adjusted.
Its specific preparation method includes the following steps：
1) at room temperature, substrate is fixed on the sample stage of electron beam evaporation deposition machine；Using SiO2It, will for evaporation material
Electron beam equipment vacuum is evacuated to 3 × 10-4Pa；
2) angle of deposit is first set as 0 °, a layer thickness is deposited in transparent or semitransparent substrate and is caused for 90~99nm
Close silicon dioxide layer, the refractive index of dense oxide silicon layer is 1.21~1.45；Substrate using quartz plate, BK7, SF5, LAK14,
FTO sends any one of Simon Rex glass, their refractive index is between 1.45~1.95.
3) angle of deposit is set as 80 °, in the fine and close SiO by 2) obtaining2On layer, deposition a layer thickness is 85~90nm
Porous SiO2Nanometer rods layer, porosity are 63%~67%；The refractive index of porous oxidation silicon nanorod layer is 1.17~1.21；
4) angle of deposit is set as 85 °, vacuum degree 10-4~10-5Pa, in the porous SiO 3) obtained2On nanometer rods layer
Deposition a layer thickness is 140~150nmPTFE nanometer rods, and porosity is 80%~83%, the folding of polytetrafluorethylenano nano stick layer
It is 1~1.17 to penetrate rate.
The present invention is illustrated with reference to the accompanying drawings and examples.Following embodiments are illustrative, are not limits
Qualitatively, it is impossible to limit protection scope of the present invention with following embodiments.
Embodiment：
1) bilayer SiO in TFCalc optical softwares simulation BK7 substrate of glass is utilized2With the thickness of the compound antireflective films of PTFE and
Refractive index is found and optimizes anti-reflection parameter, its light normal-incidence reflection rate at reference wavelength 550nm is made to be down to 0；Wherein
The reflectivity of BK7 glass is 4.267%, is 1.52 in the refractive index of 550nm reference wavelengths；
2) SiO that refractive index is gradually successively decreased is deposited in substrate successively2/SiO2/ PTFE nanometer rods laminated films.Specific step
It is rapid as follows：
A. clean BK7 substrate of glass is fixed on the sample stage of electron beam evaporation deposition machine；
B. at room temperature, using SiO2For evaporation material, it is to incite somebody to action that the chamber of electron beam evaporation deposition machine is evacuated to vacuum degree
Electron beam equipment vacuum is evacuated to 10-4~10-5Pa；
C. angle of deposit is set as 0 °, it is 99nm densifications SiO that a layer thickness is deposited in BK7 substrates2Layer；
D. angle of deposit is set as 80 °, in the fine and close SiO of acquisition2On layer, deposition a layer thickness is the porous SiO of 85nm2
Nanometer rods；
F. angle of deposit is set as 85 °, in the porous SiO of acquisition2It is 145nm that a layer thickness is deposited on nanometer rods layer
PTFE nanometer rods.
3) with reference to Fig. 1, Fig. 2, the refractive index of laminated film is from fine and close SiO2Layer is continuously decreased to PTFE nanometer rods layers.It is porous
SiO2Nanometer rods layer, PTFE nanometer rods layers refractive index be respectively depending on their porosity, have macroporosity film folding
It is small to penetrate rate.Its refractive index is respectively 1.19,1.15~1.17 at 550nm reference wavelengths, corresponding porosity is respectively 66%,
82%.
As seen from Figure 3, the reflectivity of the substrate is down to from 4.267% close to 0 in visible-range, and is tested
As a result it is consistent with analog result.As shown in table 1：Wherein ds represents being somebody's turn to do in BK7 deposition on glass calculated using optical software
The Normal incidence reflectance rate of three layers of compound antireflective film；De is represented according to optical software result of calculation, utilizes electron beam evaporation equipment
Test the Normal incidence reflectance rate of the compound antireflective film of deposition.
1 homogeneity bilayer SiO of table2The reflectivity % of the high stability automatically cleaning antireflective film compound with PTFE
Meanwhile our light that also analyze when different wave length enter the reflection of the compound antireflective film from incidence angles degree
Rate.Such as Fig. 4, in 450~650nm range of wavelengths, the mass reflex rate of the antireflective film is less than 1%, in 400~450nm wavelength
In section, reflectivity also only has 1~1.5% or even in 650~750nm range of wavelengths, and reflectivity reduces also obvious, card
Understand the compound good anti-reflection effect of antireflective film.
4) finally in order to illustrate the excellent thermostabilization of the laminated film, hydrophobicity and and matrix adhesion, by it with being not coated with
Cover the double-deck SiO of PTFE nanometer rods2Film has carried out Experimental comparison：
Specific experiment is：The laminated film is made annealing treatment in 100 DEG C, 200 DEG C respectively, measures film to visible ray
Reflectivity, nanometer failure intensity and deionized water contact angle.
1. after annealed processing, the laminated film is little to the reflectivity changes of visible ray, maximum deviation is ± 1%.
2. before annealing, uncoated PTFE nanometer rods layer homogeneity bilayer SiO2The mechanical adhesion of antireflective film and BK-7 matrixes
Power is only 9.6LC, homogeneity bilayer SiO of the invention2The high stability automatically cleaning antireflective film compound with PTFE and BK-7 matrixes
Mechanical adhesion is up to 77LC, and after the annealed processing of film, the two is improved, the former increases to failure intensity from 9.6LC
21.2LC, the latter's failure intensity increase to 85LC from 77LC.Illustrate that temperature changes that the mechanical adhesion of film will not be generated to disappear
Pole influences.Experimental result refers to table 2：
The borderline failure intensity of 2 two kinds of antireflective films of table
3. before and after annealing, uncoated PTFE nanometer rods layer homogeneity bilayer SiO2The contact angle of antireflective film does not change,
It is 7 °；The homogeneity bilayer SiO of the present invention2The contact angle of the high stability automatically cleaning antireflective film compound with PTFE changes less, but
It is up to 150 ° or more.Illustrate that PTFE nanometer rods layers can effectively improve the wetability of interface surface.Interface is made to be become by Superhydrophilic
For super-hydrophobicity
The contact angle of 3 two kinds of antireflective films of table
Embodiment 1 fully meets the technique effect of the present invention, i.e.,：
1) antireflection：By the film changed in gradient in three layers of refractive index of substrate deposit, segmentation reduces matrix and ring
Border is down to the interfacial refraction rate between outermost layer film and environment or reduces the anti-of light close to 1 to the refractive index difference of light
It penetrates.
2) high stability, self-cleaning property：Since high molecular material specific strength is high, not soluble in water, wear-resisting, self-lubricating etc. is good
Mechanochemistry property, be coated in anti-reflection film surface, can significantly improve the thermostabilization of film, hydrophobicity and with matrix
Mechanical adhesion, in actual use will not by environment steam, dust granule pollution and reduce the anti-reflective of film.
Claims (2)
1. a kind of preparation method of homogeneity bilayer silica and the compound automatically cleaning antireflective film of polytetrafluoroethylene (PTFE), it is characterised in that
This method comprises the following steps：
1) using electron beam evaporation methods, angle of deposit is first set as 0 °, one layer is deposited in transparent or semitransparent substrate
The compact silicon dioxide layer that thickness is 90~99nm, refractive index is 1.21~1.45；
2) angle of deposit is set as 80 °, on the compact silicon dioxide layer of acquisition, deposition a layer thickness is 85~90nm, hole
The porous silicon dioxide nano stick layer that gap rate is 63%~67%, refractive index is 1.17~1.21；
3) angle of deposit is set as 85 °, deposition pressure 10-4~10-5Pa, on the porous silicon dioxide nano stick layer of acquisition
Deposition a layer thickness is 140~150nm, the polytetrafluorethylenano nano stick that refractive index is 1~1.17, porosity is 80%~83%
Layer is received to get to the compact silicon dioxide layer, porous silicon dioxide nano stick layer and polytetrafluoroethylene (PTFE) gradually to be successively decreased by refractive index
The compound automatically cleaning antireflective film of rice stick layer.
2. a kind of homogeneity bilayer silica according to claim 1 and the compound automatically cleaning antireflective film of polytetrafluoroethylene (PTFE)
Preparation method, which is characterized in that the substrate is using quartz plate, BK7, SF5, LAK14, FTO or sends appointing in Simon Rex glass
One kind, their refractive index is between 1.45~1.95.
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| CN107337356B (en) * | 2017-06-28 | 2020-05-22 | 清华大学 | Preparation method of polytetrafluoroethylene and aluminum oxide atomic layer composite antireflection film |
| CN108648883B (en) * | 2018-05-15 | 2020-08-25 | 华东师范大学 | Preparation method of transparent conductive film compounded by double-layer anti-reflection structure and graphene |
| CN109765645A (en) * | 2019-03-15 | 2019-05-17 | 深圳大学 | A kind of porous pectinate texture optical thin film and preparation method thereof |
| CN110423567B (en) * | 2019-07-22 | 2021-06-22 | 苏州盛达飞智能科技股份有限公司 | Low refractive index film and centrifuge vessel for producing the same |
| CN110698078A (en) * | 2019-08-29 | 2020-01-17 | 信义光伏产业(安徽)控股有限公司 | Coated glass and manufacturing method thereof |
| CN111320396A (en) * | 2020-02-14 | 2020-06-23 | 云南师范大学 | Preparation method of anti-radiation silicon oxide anti-reflection film |
| CN111722308A (en) * | 2020-08-21 | 2020-09-29 | 深圳市汇顶科技股份有限公司 | Optical element and preparation method thereof |
| CN113149458B (en) * | 2021-02-26 | 2023-08-22 | 中建材玻璃新材料研究院集团有限公司 | Color photovoltaic module cover plate glass and preparation method thereof |
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