CN104479437B - Preparation method for super-hydrophobic self-luminous coating - Google Patents
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Abstract
The invention provides a preparation method for a super-hydrophobic self-luminous coating. The method comprises the following two steps of 1, uniformly mixing a high-molecular polymer monomer, a cross-linking agent, an initiating agent, nano-particles and long-lasting phosphor materials to obtained a mixture; 2, uniformly coating the surface of a base material with the mixture, and carrying out polymerization to obtain the super-hydrophobic self-luminous coating. The preparation method for the super-hydrophobic self-luminous coating overcomes the shortcomings of the prior art, the application range of the long-lasting phosphor materials is widened, and meanwhile the problem that the super-hydrophobic self-luminous coating is decomposed or the luminous intensity is reduced when water is encountered is solved. The preparation method for the super-hydrophobic self-luminous coating is simple in process and high in universality, and the manufacturing cost is saved.
Description
Technical field
The present invention relates to one kind by being coated to long after glow luminous material and adulterate, prepare super-hydrophobic spontaneous
The method of light coating, belongs to coating technology field.
Background technology
Long after glow luminous material is a kind of " green " source material, stores light spoke under natural light or artificial light sources are irradiated
Penetrate energy, after light source cuts off, remain to discharge the energy of storage in the form of visible ray, present bright distinguishable light, be
Preferably meet an urgent need and indicate light source.Going deep into Recent study, its persistence has also brought up to little more than ten from several seconds
When.There are illumination functions, the effect of emergent instruction can be played, but the long after glow luminous material pair of a lot of good luminescence property
Water is very sensitive, easily decomposes in humid air, luminescent decay, finally loses luminous power.Therefore how to make long-persistence luminous
Material avoids the interference of steam, and can be used for humidity or the field such as the emergency lighting under harsh environmental conditions or instruction, for
Further expand its range of application and there is very important Research Significance.
Superhydrophobic surface material refers to that water droplet is rounded in material surface, and its contact angle is more than 150 degree, and therefore performance is come from
Cleaning, a series of excellent properties such as anti-pollution.By manufacturing suitable surface roughness or by low surface in material surface
The modification of energy material, can prepare super-hydrophobic surface.Such material is in national defence, industry, agricultural, medical science and daily life
In all have broad application prospects.
At present, the preparation of super-hydrophobic self-luminous coating being related in the present invention and performance study are there is not yet document report.
Content of the invention
The technical problem to be solved in the present invention is the interference how making long after glow luminous material avoid steam, and can be used for tide
Emergency lighting under wet or harsh environmental conditions or instruction.
In order to solve above-mentioned technical problem, the technical scheme is that and a kind of preparation of super-hydrophobic self-luminous coating is provided
Method it is characterised in that: the method is made up of following 2 steps:
Step 1: will be uniform to high molecular polymer monomer, cross-linking agent, initiator, nano-particle and long after glow luminous material
Mixing, obtains mixture；
Step 2: said mixture is uniformly coated on substrate surface, polymerization, obtain super-hydrophobic self-luminous coating.
Preferably, described high molecular polymer monomer is polydimethylsiloxane pdms, polyamide pa, poly terephthalic acid
Glycol ester pet, polrvinyl chloride pvc, Merlon pc, polystyrene ps, ethylene-vinyl acetate copolymer eva, polyethylene
Octene elastic composite poe, polyethylene pe, polymethyl methacrylate pmma, polyurethane pu, polypropylene pp or derivatives thereof
One of；
Described cross-linking agent is amino resins, acrylic amide, imines, epoxy compound species, silicone coupling agents, isocyanide
One of acid esters；
Described initiator is light trigger or thermal initiator；
Described nano-particle is nano-oxide, nano composite oxide or nano metal and alloy；
Described long after glow luminous material is rare-earth sulfide long-lasting phosphor, rare earth silicate long-lasting phosphor or dilute
One of native aluminate long afterglow luminous body；
Described base material is one of glass, silicon chip, timber, metal, pottery, rubber, fabric, building.
Preferably, described light trigger is one of radical polymerization light trigger or Cationic photoinitiator,
Described thermal initiator is one of peroxide, azo-initiator.
Preferably, the launch wavelength of described long after glow luminous material is in the range of 400～800nm；Described step 1 preparation
In mixture, the mass content of long after glow luminous material is 5%～30%.
Preferably, the ratio of described high molecular polymer monomer and initiator is 1: 1～20: 1, described step 1 preparation
In mixture, the content of cross-linking agent is 0.1wt%～5wt%.
Preferably, described nano-particle includes inorganic nanoparticles silicon dioxide, titanium dioxide, silver, ferrum oxide, titanium dioxide
Stannum, carborundum, politef microgranule, carbon, zirconium dioxide.
Preferably, the particle size range of described nano-particle is 10～200nm；The concentration range of described nano-particle is 5%
～30%.
Preferably, the method that described mixture is uniformly coated on during substrate surface includes rubbing method, pinch-band technic or template；
Described rubbing method includes drop coating, spin coating, roller coat, blade coating or brushing, and the speed of spin coating is 0.1～10.0kr/min, the pressure of roller coat
Power is 1～100n, and the speed of blade coating is 1～99mm/s, and the volume of drop coating is 1～100ml；Between described template and pinch-band technic
It is 10～1000 μm away from thickness.
Preferably, in described step 2, the condition of polymerization is: heating induction is polymerized or by causing light irradiation；Heating side
Formula is placement 1～5h at 60～120 DEG C；Initiation light is ultraviolet region or the wavelength 400～800nm of wavelength 250～420nm
Visible region, light application time 1～30 minute, intensity of illumination is 1mw/cm2～2w/cm2.
Preferably, the thickness of described super-hydrophobic self-luminous coating is 10～1000 μm, and launch wavelength is 400～800nm.
The present invention is by carrying out high molecular polymer cladding to the long after glow luminous material of different emission scope and mixing
Miscellaneous, the super-hydrophobic self-luminous coating of the different substrate materials compatibility can be obtained.This coating not only has super-hydrophobic automatic cleaning performance, solution
Long after glow luminous material of having determined meets the problem of water unstable, and has pervasive substrate compatibility it is adaptable to different substrate materials table
Face, and can be applicable to various humidity or the emergency lighting under harsh environmental conditions and instruction.The addition of long after glow luminous material
Not only increase the hydrophobicity of polymeric film, and there is long-persistence luminous performance.Under the irradiation of natural light, can be rapid
Absorb sunlight and slowly discharge.By changing species and the ratio of dopant material, different colours can be obtained and answer
Luminescent film with function.
The method that the present invention provides overcomes the deficiencies in the prior art, is extending the range of application of long after glow luminous material
While, solve it and meet the difficult problem that water decomposition or luminous intensity reduce.Method of the present invention process is simple, has saved and has been prepared into
This, and universality is strong.
Brief description
Fig. 1 is the super-hydrophobic effect of the coating preparing in embodiment 2；
Fig. 2 is the super-hydrophobic effect of the coating preparing in embodiment 3.
Specific embodiment
For making the present invention become apparent, hereby with several preferred embodiments, it is described in detail below.
Embodiment 1
The long-lasting phosphor that 0.05g launching light is blue (peak value is 456nm) add 1g pmma polymer monomer and
In the mixture of initiator 2- hydroxy-2-methyl-to ethoxy ether phenylacetone (ratio of monomer and initiator is 20: 1),
And adding the cross-linking agent VTES (vtes) that mass content is 0.1%, mass content is 5% hydrophobic dioxy
SiClx nanoparticle (particle size range be 10nm～100nm), continuously stirred until long-lasting phosphor and monomer, nano-particle mixes
Close uniformly, using knife coating, said mixture dripped on the glass sheet, use coating machine even spread, coating speed is 99mm/s,
Then irradiate 1min under the ultraviolet light in 250～420nm wave-length coverage, light intensity magnitude is 1mw, prepares the indigo plant of 10 μ m-thick
The super-hydrophobic luminescent coating of color, water droplet static contact angle on the coating layer is about 155 °.
Embodiment 2
The long-lasting phosphor that 2.5g launching light is green (peak value is 510nm) adds 25g pa high molecular polymer list
In the mixture of body and aqueouss azo initiator azo diisobutyl amidine hydrochlorate (ratio of monomer and initiator is 10: 1), and
Add the cross-linking agent phenolic resin that mass content is 1%, mass content is that (particle size range is for 30% titanium dioxide nano-particle
10nm～200nm), continuously stirred said mixture is dropped on silicon chip using knife coating until mixture mix homogeneously, with apply
Cloth machine even spread, coating speed is 1mm/s, then places 1h at 120 DEG C and dries, obtains the doping long afterglow of 1000 μ m-thick
The pa film of luminous body-green super-hydrophobic self-luminous coating.As shown in Figure 1, preparation-obtained self-luminous applies as stated above
Layer, is 150 ° with the water droplet contact angle that static contact angle records.
Embodiment 3
The long-lasting phosphor that 3g launching light is red (peak value is 780nm) adds 5g pet monomer and initiator hexichol
In the mixture of ketone (dp) (ratio of monomer and initiator is 1: 1), and add the cross-linking agent n that mass content is 5%, n '-
Methylene-bisacrylamide, mass content is 30% tin dioxide nano-particle (particle size range is 10nm～200nm), continues
Stir until mixture mix homogeneously, using spin-coating method: said mixture is dropped on plank base material, is uniformly revolved with sol evenning machine
Apply, spin speed is 1kr/min, under the ultraviolet light in 250～420nm wave-length coverage, then irradiate 5min, light intensity magnitude is
2w, obtains the super hydrophobic surface of pet film-redness that thickness is 100 μm, as shown in Figure 2, preparation-obtained as stated above
Self-luminous coating, reaches 153 ° with the water droplet contact angle that static contact angle records.
Embodiment 4
The long-lasting phosphor that 1g launching light is blue (peak value is 456nm) adds 1g pvc monomer and initiator azo
In the mixture of bis-isobutyronitrile (ratio of monomer and initiator is 1: 1), and just add the cross-linking agent 2- that mass content is 0.5%
Fourth amino -4,6- bis- dredges base s-triazine, mass content be 10% nanometer silicon carbide particle (particle size range be 50nm～
200nm), continuously stirred until mixture mix homogeneously；Using spin-coating method: said mixture is dropped on metal aluminium flake, uses platform
The uniform spin coating of formula sol evenning machine, spin speed is 10kr/min, then irradiates under the ultraviolet light in 250～420nm wave-length coverage
1min, light intensity magnitude is 2w, obtains the super-hydrophobic luminescent coating of pvc film-blueness that thickness is 10 μm, prepared as stated above
The self-luminous coating obtaining, reaches 155 ° with the water droplet contact angle that static contact angle records.
Embodiment 5
The long-lasting phosphor that 0.1g launching light is red (peak value is 780nm) adds 1g pc monomer and initiator mistake
Aoxidize (ratio of monomer and initiator is 10: 1) in the mixture of two dicyclohexyl carbonate, and the friendship that mass content is 1%
Connection agent pmma, mass content is 15% polytetrafluorethylenano nano particle (particle size range is 50nm～200nm), continuously stirred straight
To said mixture mix homogeneously, using knife coating, said mixture is dropped on potsherd, with the uniform roller coat of Glass rod, pressure
Size is 10n, then places 3h at 80 DEG C and dries, the super-hydrophobic self-luminous obtaining pc film-redness that thickness is 1 μm applies
Layer, is more than 150 ° with the contact angle of light-emitting area.
Embodiment 6
The long-lasting phosphor that 7.5g launching light is green (peak value is 510nm) adds 25g pa monomer and initiator mistake
Aoxidize (ratio of monomer and initiator is 20: 1) in the mixture of two diisopropyl carbonate, and the friendship that mass content is 5%
Connection agent carbodiimide cross-linker, mass content is 30% Nano silver grain (particle size range is 10nm～100nm), persistently stirs
Mix until long-lasting phosphor mix homogeneously, dropped in said mixture on sheet rubber using knife coating, use Glass rod even roller
Apply, pressure size is 0.1n, at 120 DEG C, then place 1h dry, obtain the super-hydrophobic of pa film-green that thickness is 1000 μm
Luminescent coating.It is about 152 ° with the contact angle of light-emitting area.
Embodiment 7
The long-lasting phosphor that 2.5g launching light is red (peak value is 780nm) adds 10g pe monomer and initiator mistake
In the mixture of oxidation diisopropylbenzene (DIPB) (dcp) (ratio of monomer and initiator is 10: 1), and the friendship that mass content is 0.5%
Connection agent vinyl triethoxyl silicon burns, and mass content is 30% ferric oxide nano particles (particle size range is 10nm～200nm),
Continuously stirred then use pinch-band technic confinement preparation on silicon chip until long-lasting phosphor mix homogeneously, control between intermediate plate away from
Dry from for 500 μm, then placing 5h at 60 DEG C, prepare the super-hydrophobic luminous painting of pe film-redness that thickness is 500 μm
Layer.It is about 155 ° with the contact angle of light-emitting area.
Embodiment 8
The long-lasting phosphor that 0.1g launching light is green (peak value is 510nm) adds 1g pdms monomer and initiator
In the mixture of azodiisobutyronitrile (ratio of monomer and initiator is 1: 1), and the styrene that mass content is 0.1% is made
For cross-linking agent, mass content is 20% carbon nano-particles (particle size range is 10nm～200nm), continuously stirred until long afterglow
Luminous body mix homogeneously, then monomer being added the groove depth of well in advance is in 10 μm of mould, places 5h and dry at 60 DEG C,
Prepare the super-hydrophobic luminescent coating of pdms film-green that thickness is 10 μm.It is about 152 ° with the contact angle of light-emitting area.
Embodiment 9
The long-lasting phosphor that 0.05g launching light is red (peak value is 780nm) adds 10g pet monomer and initiator
In the mixture of azodiisobutyronitrile initiator (ratio of monomer and initiator is 1: 1), and the friendship that mass content is 0.5%
Connection agent vinyl chloride, mass content be 30% Nano particles of silicon dioxide and carborundum mixture (particle size range be 10nm～
200nm), continuously stirred until said mixture mix homogeneously, the groove depth then monomer being added well in advance is 100 μm of mould
In tool, place 2h at 120 DEG C and dry, prepare the super-hydrophobic luminescent coating of pt film-redness that thickness is 100 μm.With send out
The contact angle of optical surface is about 151 °.
Embodiment 10
The long-lasting phosphor that 6g launching light is green (peak value is 510nm) adds 20g poe monomer and initiator fluorine
Change (ratio of monomer and initiator is 20: 1) in the mixture of diphenyl titanium cyclopentadienyl, and the cross-linking agent that mass content is 0.1%
Carbodiimides, mass content is 20% titanium dioxide nano-particle and nano SiO 2 particle mixture (particle size range
For 10nm～200nm), continuously stirred until long-lasting phosphor mix homogeneously, then monomer is added the groove depth of well in advance
For, in 1000 μm of moulds, then irradiating 30min under the visible ray in 400～800nm wave-length coverage, light intensity magnitude is 2w,
Prepare the super-hydrophobic luminescent coating of pt film-green that thickness is 1000 μm.It is about 156 ° with the contact angle of light-emitting area.
Embodiment 11
The long-lasting phosphor that 5g launching light is red (peak value is 780nm) adds 15g pu monomer and initiator double
In the mixture of (pentafluorophenyl group) titanium cyclopentadienyl (ratio of monomer and initiator is 10: 1), and the cross-linking agent that mass content is 5%
Polyethylene glycol oxide, mass content be 10% polytetrafluorethylenano nano particle and the mixture of carbon nano-particle (particle size range is
10nm～200nm), continuously stirred until long-lasting phosphor mix homogeneously, the groove depth then monomer being added well in advance is
In 500 μm of mould, under the visible ray in 400～800nm wave-length coverage, then irradiate 30min, light intensity magnitude is 1w, preparation
Obtain the super-hydrophobic luminescent coating of pu film-redness that thickness is 500 μm.It is about 151 ° with the contact angle of light-emitting area.
Embodiment 12
The long-lasting phosphor that 3g launching light is green (peak value is 510nm) adds 7g pp monomer and initiator peroxide
Change (ratio of monomer and initiator is 20: 1) in the mixture of di-t-butyl, and the cross-linking agent that mass content is 0.1%
Pmma, mass content is 5% ferriferrous oxide nano-particle (particle size range be 10nm～200nm), continuously stirred until length
Afterglow body mix homogeneously, is dropped in said mixture on sheet rubber using knife coating, and with the uniform roller coat of Glass rod, pressure is big
Little for 1n, at 120 DEG C, then place 1h dry, obtain the super-hydrophobic luminescent coating of ps film-green that thickness is 200 μm.
It is about 152 ° with the contact angle of light-emitting area.
Embodiment 13
The long-lasting phosphor that 0.5g launching light is green (peak value is 510nm) adds 1g eva monomer and initiator 1-
In the mixed solution of hydroxycyclohexyl phenyl ketone (ratio of monomer and initiator is 1: 1), and mass content is 0.1%
The poly- dially phthalate of cross-linking agent, mass content be 30% zirconium dioxide nanoparticles (particle size range be 10nm～
200nm), continuously stirred until long-lasting phosphor mix homogeneously, the folder that thickness is 10 μm is fed the mixture into using pinch-band technic
In piece, it is to cause light using ultraviolet region (250～420nm), light application time is 2 minutes, intensity of illumination is 1mw/cm2, preparation
Obtain the super-hydrophobic luminescent coating of pu film-green that thickness is 10 μm.It is about 152 ° with the contact angle of light-emitting area.
Claims (1)
1. a kind of preparation method of super-hydrophobic self-luminous coating it is characterised in that: the method is made up of following 2 steps:
Step 1: high molecular polymer monomer, cross-linking agent, initiator, nano-particle and long after glow luminous material are uniformly mixed
Close, obtain mixture；
Described high molecular polymer monomer is polyethylene terephthalate pet, polrvinyl chloride pvc, Merlon pc, poly- second
Alkene octene elastic composite poe, one of polyethylene pe, polypropylene pp or derivatives thereof；
Described cross-linking agent is one of amino resins, imines, epoxy compound species, silicone coupling agents；
Described initiator is one of radical polymerization light trigger or Cationic photoinitiator；
Described nano-particle include inorganic nanoparticles silicon dioxide, titanium dioxide, silver, ferrum oxide, tin ash, carborundum,
Politef microgranule, carbon, zirconium dioxide；
Described long after glow luminous material is rare-earth sulfide long-lasting phosphor, and the launch wavelength of long after glow luminous material is 400
In the range of～800nm；In the mixture of described step 1 preparation, the mass content of long after glow luminous material is 30%；
The ratio of described high molecular polymer monomer and initiator is 1: 1～20: 1, crosslinked in the mixture of described step 1 preparation
The content of agent is 0.1wt%～5wt%；
The mass content of described nano-particle is 30%, and size is 10nm～200nm；
Step 2: said mixture is uniformly coated on substrate surface, polymerization, obtain super-hydrophobic self-luminous coating；
The method that in described step 2, mixture is uniformly coated on during substrate surface includes rubbing method, pinch-band technic or template；Described
Rubbing method includes drop coating, spin coating, roller coat, blade coating or brushing, and the speed of spin coating is 0.1～10.0kr/min, and the pressure of roller coat is 1
～100n, the speed of blade coating is 1～99mm/s, and the volume of drop coating is 1～100ml；The spacing of described template and pinch-band technic is thick
Spend for 10～1000 μm；
In described step 2 polymerization condition be: by cause light irradiation, cause light be wavelength 250～420nm ultraviolet region or
The visible region of wavelength 400～800nm, light application time 1～30 minute, intensity of illumination is 1mw/cm2～2w/cm2；
The thickness of described super-hydrophobic self-luminous coating is 10～1000 μm, and launch wavelength is 400～800nm；
Described base material is one of glass, silicon chip, timber, metal, pottery, rubber, fabric.
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