CN109777358A - Graphene-based anti-/ deicing integration fold film of one kind and preparation method thereof - Google Patents
Graphene-based anti-/ deicing integration fold film of one kind and preparation method thereof Download PDFInfo
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Abstract
Graphene-based anti-/ deicing integration fold film of one kind and preparation method thereof belongs to the technical field of aerial anti-/ deicing in real time.The invention solves the technical problems of extreme environment anti-icing and deicing difficulty.Fold film (FSGF) of the invention is to first pass through dry method transfer rGO is transferred on 4910 substrate film of acrylic acid VHB of biaxial tension, by the retraction of basilar memebrane, obtains fold rGO film；Then pass throughMethod grows SiO on the surface rGO2Nanoparticle, finally by made from FDTS modification of surfaces.Fold film of the invention still maintains anti-icing performance when temperature is -20 DEG C；, can at low voltage meanwhile when temperature is -20 DEG C, 30s realizes complete deicing and defrosting, shows excellent anti-icing and deicing performance, and anti-/ deicing field has huge application prospect in real time in the sky.
Description
Technical field
The invention belongs to the technical fields of aerial anti-/ deicing in real time；Not only there is ultra-hydrophobicity but also tool more particularly to a kind of
Have the novel graphite alkenyl of electric heating property it is micro--receive the preparation method of hierarchical structure fold film.
Background technique
The large area accumulated ice of aircraft surfaces will lead to frequent flight delay；Wing accumulated ice will lead to flight resistance increase,
Both wings weight is unbalanced, or even air crash accident can occur；Cockpit windscreen accumulated ice will affect the visual field and judgement of pilot etc..Product
Ice not only makes troubles to the trip of winged Passenger On Board, or even threatens to their life, while air crash also can be to land
On people or building cause injures and deaths or damage.
It, can be by its own super-hydrophobic spy currently, super hydrophobic material is considered as the optimal selection in anti-/ deicing field
Property, using the air layer captured when contacting between water droplet and film, reduce solid-liquid contact area, when surface slightly inclination angle, supercooling
Drop can bounce off super hydrophobic material surface before icing, realize the anti-icing performance under low temperature with this.But in extreme circumstances, such as
Under the conditions of low temperature and high relative humidity or cryogenic condensation, anchorage effect will form between drop and material, increase between drop and material
Adhesion strength loses anti-icing performance, while bringing difficulty to de-icing work.
Summary of the invention
The invention solves the technical problems of extreme environment anti-icing and deicing difficulty；And provide it is a kind of it is graphene-based it is anti-/
Deicing integration fold film and preparation method thereof.The VHB 4910 that rGO is transferred to stretching is shifted in the present invention by dry method
On substrate film, by the retraction of basilar memebrane, fold rGO film is obtained；Pass throughMethod, on the surface rGO, growth SiO2 is received
Rice corpuscles obtains FSGF finally by FDTS modification of surfaces.Test the anti-icing performance of FSGF, electric defrosting and electro-thermal deicing
Can, show excellent anti-deicing characteristic.It is fold film lightweight of the present invention, super-hydrophobic, high electric heating, flexible.Of the invention
Film is by the modified SiO of FDTS2What/rGO fold (FSGF) obtained, there is good superhydrophobic characteristic and excellent electric heating
Performance has great importance to aerial anti-icing and real-time deicing.
In order to solve the above technical problems, the graphene-based anti-/ deicing integration fold film (FSGF) of one kind is in the present invention
It first passes through dry method transfer rGO is transferred on 4910 substrate film of acrylic acid VHB of biaxial tension, by the retraction of basilar memebrane,
Obtain fold rGO film；Then pass throughMethod grows SiO on the surface rGO2Nanoparticle modifies table finally by FDTS
Made from face；It is realized particular by following step:
Step 1: rGO (redox graphene) film to be transferred to the acrylic acid VHB of biaxial tension using dry method
On 4910 substrate films；
Step 2: then first discharging substrate film along a uniaxial direction, make its retraction, then discharges the base in another uniaxial direction
Bottom film, makes it retract to original size, obtains rGO fold film；
Step 3: cationic surfactant is added in ammonia water mixture, it is uniformly mixed, is then placed in step 2 and obtains
RGO fold film, magnetic agitation 5h~7h under heating water bath are obtained, then instills ethyl orthosilicate dropwise, heat preservation is stirred after being added dropwise
It mixes, is dried after then taking out；
Step 4: then through step 3 treated fold film surface, drying, i.e., the diluted FDTS of n-hexane is dripped to
Obtain graphene-based anti-/ deicing integration fold film (FSGF)；
Wherein, ammonia water mixture is prepared by deionized water, dehydrated alcohol and ammonium hydroxide.
The hexane solution of FDTS is obtained with n-hexane dilution FDTS.
It further limits, rGO described in step 1 (redox graphene) film carries out in the steps below: by oxygen
Graphite aqueous solution is diluted to 0.1mg/mL, and taking 3mL to be filtered by vacuum to diameter is 50mm, the polytetrafluoroethyl-ne that aperture is 0.45 μm
On alkene film, 50 DEG C of dryings obtain GO film, then GO film are put into HI solution, in 90~100 DEG C of baking ovens restore 1~
1.5h is put into 6h in 120 DEG C of baking ovens, removes the HI of excess surface after taking-up.
Further limit, the graphene oxide the preparation method is as follows:
The concentrated sulfuric acid that 23ml mass concentration is 98% is added in the beaker of 250mL, ice bath is cooled to -1 DEG C~1 DEG C,
It carries and 1g natural graphite is added, stir 40min~60min, 6g KMnO is added by several times4, 2.5h~3h is stirred, ice bath is then changed,
35 DEG C~45 DEG C waters bath with thermostatic control are placed in, solution starts to become viscous after stirring 40min~50min, then will stablize in water at 40 DEG C
It~50 DEG C, is then transferred in 80 DEG C of thermostat water baths and stirs, 80mL distilled water is added by several times, after stirring 10min~20min, add
Enter 60mL distilled water dilution, then plus 10.81mL 30% hydrogen peroxide and 60mL deionized water composition mixed solution, solution become
For golden yellow, with deionized water centrifuge washing to solution pH value 5~6.
Further limiting, the prestrain of the acrylic acid substrate film of biaxial tension described in step 1 is 300%~
400%.
It further limits, 30mg~50mg cationic surfactant is added in ammonia water mixture in step 3,
Wherein, ammonia water mixture is prepared by the ammonium hydroxide of 40mL deionized water, 10mL dehydrated alcohol and 1mL~2mL.
It further limits, cationic surfactant is cetyl trimethylammonium bromide (CTAB) in step 3.
It further limits, the dosage of ethyl orthosilicate is 1mL~2mL in step 3.
It further limits, the concentration of the solution of FDTS is 1% (quality), the use of the hexane solution of FDTS in step 3
Amount is 10 μ L.
Further limit, in step 3 bath temperature be 40 DEG C~45 DEG C, magnetic stirring speed be 400r/min~
500r/min。
It further limits, is dried at 40 DEG C~60 DEG C in step 3.
The present invention passes through rGO microns of folds of preparation and SiO2Nanoparticle combine formed special it is micro--receive hierarchical structure,
Modified simultaneously using low-surface energy substance FDTS prevented/deicing surface FSGF using the superhydrophobic characteristic of fold film makes water
One layer of air layer is captured when contacting between drop and fold film, to reduce solid-liquid contact area, when surface slightly inclination angle,
Supercooling drop can bounce off material surface before icing, realize the anti-icing performance under low temperature with this.Meanwhile water droplet is on the surface FSGF
When upper, the contact angle under low temperature is larger, so that the free energy barrier of droplet nucleation is higher, ice nucleation rate is smaller, has delayed solid-liquid
The time of interface heterogeneous nucleation；Meanwhile the air layer captured between solid-liquid effectively slows down the heat between surface and drop
Exchange, to realize the purpose for delaying super-cooling waterdrop to freeze.Simultaneously as grapheme material has excellent electric conductivity,
By Joule heat principle, the ice sheet contacted between fold film can be melted, reduce the adhesion strength between ice and material, shaken
It moves, wind-force, it can be achieved that quick deicing under the external forces such as gravity.
Graphene-based anti-/ deicing integration fold the film (FSGF) of the present invention when temperature is -20 DEG C, when surface angle >=
At 16.1 °, anti-icing performance is still maintained；When temperature is -10 DEG C, compared with rGO planar film, water droplet freezing time can postpone about
6.8 again；, can at low voltage meanwhile when temperature is -20 DEG C, 30s realizes complete deicing and defrosting, shows excellent
Anti-icing and deicing performance, anti-/ deicing field has huge application prospect in real time in the sky.
Detailed description of the invention
The SEM image of Fig. 1 FSGF；
Contact angle and roll angle of the water droplet on FSGF under Fig. 2 different temperatures；
The process that Fig. 3 delays super-cooling waterdrop to freeze；
Fig. 4 applies the temperature rise figure of FSGF under DC voltage；
Fig. 5 electric defrosting process；
Fig. 6 electro-thermal deicing process.
Specific embodiment
Embodiment 1: the graphene-based anti-/ deicing integration fold film (FSGF) of one kind is by following steps in the present embodiment
Suddenly it realizes:
Step 1: rGO (redox graphene) film is transferred to the biaxial tension that prestrain is 400% using dry method
Acrylic acid substrate film on；
Step 2: then first discharging substrate film along a uniaxial direction, make its retraction, then discharges the base in another uniaxial direction
Bottom film, makes it retract to original size, obtains rGO fold film；
Step 3: 30mg cetyl trimethylammonium bromide (CTAB) is added in ammonia water mixture, it is uniformly mixed, so
After be put into step 2 and obtain rGO fold film, under 40 DEG C of heating water baths magnetic agitation 6h, then instilling dosage dropwise is 1mL
Rear insulated and stirred 12h is added dropwise in ethyl orthosilicate, dries under the conditions of 50 DEG C after then taking out；
Step 4: being then the FDTS (1H, 1H, 2H, 2H- perfluoro decyl trichlorosilane) of 1% (quality) by 10 μ L concentration
Hexane solution drip to through step 3 treated fold film surface, be put into vacuum drying oven, 50 DEG C of drying 3h are to get arriving
Graphene-based anti-/ deicing integration fold film (FSGF)；
Wherein, ammonia water mixture is prepared by 40mL deionized water, 10mL dehydrated alcohol and 1~2mL ammonium hydroxide；
Preparing for rGO film described in step 1 is as follows:
The preparation of step 1. graphene oxide
The concentrated sulfuric acid that 23ml mass concentration is 98% is added in the beaker of 250mL, ice bath is cooled to -1~1 DEG C.Add
Enter 1g natural graphite, stirs 40~60min, 6g KMnO is added by several times4, stir 2.5~3h.Ice bath is changed, is placed in 35~45 DEG C
Water bath with thermostatic control, solution starts to become viscous after stirring 40~50min, stablizes in last water at 40~50 DEG C or so.It is transferred to 80 DEG C
It is stirred in thermostat water bath, 80mL distilled water is added by several times, after stirring 10~20min, the dilution of 60mL distilled water is added.Again plus
The mixed solution of hydrogen peroxide and 60mL the deionized water composition of 10.81mL 30%, solution become golden yellow, with deionized water from
The heart is washed to solution pH value 5~6 or so.
The preparation of step 2.rGO film
Graphene oxide water solution prepared by step 1 is diluted to 0.1mg/mL, takes 3mL to be filtered by vacuum to diameter and is
50mm, aperture is on 0.45 μm of polytetrafluoroethylene film, 50 DEG C of dryings obtains GO film；GO film is put into HI solution,
1~1.5h is restored in 90~100 DEG C of baking ovens, and 6h in 120 DEG C of baking ovens is put into after taking-up, removes the HI of excess surface.
The pattern picture of FSGF prepared by the present embodiment as shown in Figure 1, upper right corner illustration structure thus enlarged drawing.From
It can be seen that prepared FSGF is the particle with nanometer above the pleated structure of micron in figure, for it is micro--receive hierarchical structure,
Middle micron fold width is about 22.0 μm, and 36.4 μm are spaced about between fold, and nano surface silica particle diameter is about
100nm。
The water contact angle (WCA) of FSGF and roll angle (SA) are as shown in Figure 2 under the conditions of Different hypothermia, it can be seen that even if working as
When temperature is -20 DEG C, if surficial inclination >=16.1 °, water droplet can also be flicked, and maintain good anti-icing performance.
When material surface temperature be -10 DEG C, freezing process such as Fig. 3 institute of the 10 μ L water droplets on plane rGO film and the surface FSGF
Show, it can be seen that water droplet delays about 6.8 times in FSGF freezing time, shows the good performance for delaying to freeze.
Electric heating property of the FSGF at low dc voltage (5~15V) as shown in figure 4, temperature can rise to highest in 20s,
The characteristics of showing low energy consumption and being rapidly heated.
Electricity when material surface temperature is -20 DEG C, under conditions of relative humidity > 90%, and FSGF both end voltage is 15V
Hot defrosting process is as shown in figure 5, defrosting completely can be achieved in FSGF in 30s.
When material surface temperature is -20 DEG C, under conditions of relative humidity is 35 ± 5%, when FSGF both end voltage is 15V,
As shown in fig. 6, when energization 23s, ice melts and is formed completely with fold film contacts layer for the removal process of the frozen droplets of 10 μ L
Water layer reduces the adhesion strength between ice and material, and when the inclination angle FSGF is 30 °, ice drop is slid under the effect of gravity, realizes fast
Fast deicing.
Embodiment 2: the graphene-based anti-/ deicing integration fold film (FSGF) of one kind is by following steps in the present embodiment
Suddenly it realizes:
Step 1: rGO (redox graphene) film is transferred to the biaxial tension that prestrain is 400% using dry method
Acrylic acid substrate film on；
Step 2: then first discharging substrate film along a uniaxial direction, make its retraction, then discharges the base in another uniaxial direction
Bottom film, makes it retract to original size, obtains rGO fold film；
Step 3: 50mg cetyl trimethylammonium bromide (CTAB) is added in ammonia water mixture, it is uniformly mixed, so
After be put into step 2 and obtain rGO fold film, under 45 DEG C of heating water baths magnetic agitation 6h, then instilling dosage dropwise is 2mL
Rear insulated and stirred 12h is added dropwise in ethyl orthosilicate, dries under the conditions of 50 DEG C after then taking out；
Step 4: being then the FDTS (1H, 1H, 2H, 2H- perfluoro decyl trichlorosilane) of 1% (quality) by 10 μ L concentration
Hexane solution drip to through step 3 treated fold film surface, be put into vacuum drying oven, 50 DEG C of drying 3h are to get arriving
Graphene-based anti-/ deicing integration fold film (FSGF)；
Wherein, ammonia water mixture is prepared by 40mL deionized water, 10mL dehydrated alcohol and 1~2mL ammonium hydroxide；
The step of preparation method with embodiment 1 of rGO film described in step 1 and technological parameter are identical.
Claims (11)
1. a kind of graphene-based anti-/ deicing integration fold film (FSGF), it is characterised in that the fold film first passes through dry
RGO is transferred on 4910 substrate film of acrylic acid VHB of biaxial tension by method transfer, by the retraction of basilar memebrane, obtains fold
RGO film；Then pass throughMethod grows SiO on the surface rGO2Nanoparticle, finally by made from FDTS modification of surfaces.
2. a kind of preparation method of graphene-based anti-/ deicing integration fold film (FSGF) as described in claim 1, special
Sign is that the preparation method is realized by following step:
Step 1: rGO (redox graphene) film to be transferred to 4910 base of acrylic acid VHB of biaxial tension using dry method
On the film of bottom；
Step 2: then first discharging substrate film along a uniaxial direction, make its retraction, then discharge another uniaxial direction substrate it is thin
Film makes it retract to original size, obtains rGO fold film；
Step 3: cationic surfactant is added in ammonia water mixture, it is uniformly mixed, is then placed in step 2 acquisition
RGO fold film, magnetic agitation 5h~7h under heating water bath, then ethyl orthosilicate is instilled dropwise, rear insulated and stirred is added dropwise,
It is dried after then taking out；
Step 4: then dripping to the diluted FDTS of n-hexane through step 3 treated fold film surface, dry to get arriving
Graphene-based anti-/ deicing integration fold film (FSGF)；
Wherein, ammonia water mixture is prepared by deionized water, dehydrated alcohol and ammonium hydroxide.
3. preparation method according to claim 2, it is characterised in that rGO described in step 1 (redox graphene) film
It carries out in the steps below: graphene oxide water solution is diluted to 0.1mg/mL, take 3mL to be filtered by vacuum to diameter to be
50mm, aperture is on 0.45 μm of polytetrafluoroethylene film, 50 DEG C of dryings obtains GO film, then GO film is put into HI solution
In, 1~1.5h is restored in 90~100 DEG C of baking ovens, and 6h in 120 DEG C of baking ovens is put into after taking-up, removes the HI of excess surface.
4. preparation method according to claim 3, it is characterised in that the graphene oxide the preparation method is as follows:
The concentrated sulfuric acid that 23ml mass concentration is 98% is added in the beaker of 250mL, ice bath is cooled to -1 DEG C~1 DEG C, is added
1g natural graphite stirs 40min~60min, 6g KMnO is added by several times4, 2.5h~3h is stirred, ice bath is then changed, is placed in 35
DEG C~45 DEG C of waters bath with thermostatic control, and solution starts to become viscous after stirring 40min~50min, then it will stablize in water at 40 DEG C~50 DEG C,
It is then transferred in 80 DEG C of thermostat water baths and stirs, 80mL distilled water is added by several times, after stirring 10min~20min, 60mL is added and steams
Distilled water dilution, then plus 10.81mL 30% hydrogen peroxide and 60mL deionized water composition mixed solution, solution becomes golden yellow,
With deionized water centrifuge washing to solution pH value 5~6.
5. preparation method according to claim 2, it is characterised in that the acrylic bottom of biaxial tension described in step 1 is thin
The prestrain of film is 300%~400%.
6. preparation method according to claim 2, it is characterised in that in step 3 that 30mg~50mg cationic surface is living
Property agent is added in ammonia water mixture, wherein ammonia water mixture is by 40mL deionized water, 10mL dehydrated alcohol and 1mL~2mL
Ammonium hydroxide prepare.
7. the preparation method according to claim 2 or 6, it is characterised in that cationic surfactant is 16 in step 3
Alkyl trimethyl ammonium bromide (CTAB).
8. preparation method according to claim 2, it is characterised in that in step 3 the dosage of ethyl orthosilicate be 1mL~
2mL。
9. preparation method according to claim 2, it is characterised in that in step 3 n-hexane dilute FDTS to concentration be 1%
(quality), the dosage of the diluted FDTS of n-hexane are 10 μ L.
10. preparation method according to claim 2, it is characterised in that bath temperature is 40 DEG C~45 DEG C in step 3, magnetic
Power mixing speed is 400r/min~500r/min.
11. preparation method according to claim 6, it is characterised in that dried at 40 DEG C~60 DEG C in step 3.
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