CN105855151B - A kind of long-acting hydrophobic oleophobic process of surface treatment - Google Patents

A kind of long-acting hydrophobic oleophobic process of surface treatment Download PDF

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CN105855151B
CN105855151B CN201610249744.6A CN201610249744A CN105855151B CN 105855151 B CN105855151 B CN 105855151B CN 201610249744 A CN201610249744 A CN 201610249744A CN 105855151 B CN105855151 B CN 105855151B
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hydrophobic oleophobic
long
silicon dioxide
surface treatment
substrate
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CN105855151A (en
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金碧
曹朝贵
连华景
张先超
李明仁
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Runner Xiamen Corp
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/002—Pretreatement
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/10—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by other chemical means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/14—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by electrical means
    • B05D3/141—Plasma treatment
    • B05D3/142—Pretreatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/50—Multilayers
    • B05D7/52—Two layers
    • B05D7/54—No clear coat specified
    • B05D7/544—No clear coat specified the first layer is let to dry at least partially before applying the second layer
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/06—Coating with compositions not containing macromolecular substances
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2350/00—Pretreatment of the substrate
    • B05D2350/30—Change of the surface
    • B05D2350/33—Roughening
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2355/00—Characterised by the use of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08J2323/00 - C08J2353/00
    • C08J2355/02—Acrylonitrile-Butadiene-Styrene [ABS] polymers

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The present invention discloses a kind of long-acting hydrophobic oleophobic process of surface treatment, comprising the following steps: and one, shaggy micro nano structure is obtained in substrate surface etching；Two, substrate surface dip-coating hydrophilic nano silicon dioxide gel after etching is dried to obtain transparent silicon dioxide film；Three, in handover layer surface dip-coating perfluor acid anhydrides alkyl triethoxysilane, it is dried to obtain hydrophobic oleophobic layer.The present invention can obtain the preferable hydrophobic oleophobic layer of compactness, so that processing surface has better hydrophobic oleophobic performance and stronger wearability.

Description

A kind of long-acting hydrophobic oleophobic process of surface treatment
Technical field
The present invention relates to technical field of surface, refer in particular to a kind of long-acting hydrophobic oleophobic process of surface treatment.
Background technique
In the prior art, hydrophobic oleophobic membrane preparation method first is that method preparation by toasting after dip-coating, this method The disadvantage is that process flow is longer, need to consume more raw material, baking temperature is higher, and general plastic material can not high temperature resistant, It causes higher cost and influences to use.
Hydrophobic oleophobic membrane preparation method second is that using physical vapor deposition (PVD) or chemical vapor deposition (CVD) side Method preparation.It is that there is no chemical reactions in deposition process that physical vapour deposition (PVD), which prepares the shortcomings that hydrophobic coating, so coating Binding force is bad, and wearability is poor and service life is shorter.Chemical vapor deposition prepares reaction gas and be easy to cause cracking, and shadow Ring hydrophobic effect, and the slower higher cost of deposition velocity.
In the prior art, without hydrophobic oleophobic layer obtained from etching processing with rub resistance, anticorrosion ability be not bad The disadvantages of, in view of this, the present invention proposes a kind of long-acting hydrophobic oleophobic process of surface treatment, thus this case generates.
Summary of the invention
The purpose of the present invention is to provide a kind of long-acting hydrophobic oleophobic process of surface treatment, are preferably dredged with obtaining compactness Water oleophobic layer, so that processing surface has better hydrophobic oleophobic performance and stronger wearability.
To reach above-mentioned purpose, solution of the invention are as follows:
A kind of long-acting hydrophobic oleophobic process of surface treatment, comprising the following steps:
One, shaggy micro nano structure is obtained in substrate surface etching；
Two, substrate surface dip-coating hydrophilic nano silicon dioxide gel after etching is dried to obtain transparent silicon dioxide Film；
Three, in handover layer surface dip-coating perfluor acid anhydrides alkyl triethoxysilane, it is dried to obtain hydrophobic oleophobic layer.
Further, after substrate surface etching, substrate is cleaned: wiping substrate with being stained with spirituous non-dust cloth first Surface Visible pollutant, then the substrate cleaned is placed in pure solution ethanol: the in the mixed solvent ultrasound that acetone volume ratio is 1:2 10min removes surface grease and dust, then with remaining solvent is removed in the deionized water containing cleaning agent, finally spend from Sub- water rinses, and is dried for standby.
Further, substrate is one of plastics, metal, ceramics, glass, woven fabric or rubber.
Further, lithographic method is one of plasma etching, chemical etching or photoengraving.
Further, hydrophilic nano silicon dioxide gel is obtained by following methods: ethyl orthosilicate: dehydrated alcohol: distillation Water: ethyl orthosilicate, dehydrated alcohol and distilled water are uniformly mixed, according to molar ratio=1:6:4:0.05 in magnetic agitation by ammonium hydroxide The lower dropwise addition ammonium hydroxide of device stirring is 9-10 to pH, 2h is stirred after completion of dropwise addition, condensation reaction is hydrolyzed, and stands overnight ageing reaction Up to transparence nano silicon dioxide sol.
Further, in step 2, will be etched after substrate be at the uniform velocity immersed in containing mass concentration be 2% polyvinyl alcohol Or in the silicon dioxide gel of polyethylene glycol, impregnated, is reached after 30-90nm thickness in 80- with the pull rate of 5-9cm/min Dry 3-5min at 100 DEG C.
Further, in step 3, the substrate of the transparent silicon dioxide film of 30-90nm thickness immerses perfluor acid anhydrides dip-coating It in alkyl triethoxysilane, is impregnated with the pull rate of 1-6cm/min, then dry 20-30min at 100-150 DEG C, natural The cooling hydrophobic oleophobic layer that 10-1000nm thickness can be obtained.
Further, silicon dioxide film with a thickness of 30-90nm.
Further, hydrophobic oleophobic layer with a thickness of 10-1000nm.
After adopting the above scheme, the present invention first performs etching acquisition rough surface to substrate surface, in rough surface dip-coating Silicon dioxide gel is dried to obtain transparent silicon dioxide film；The low-surface-energy of silicon dioxide film and perfluor siloxane polymer is total Same-action, so that substrate is firmly combined with silicon dioxide film, silicon dioxide film is finer and close in conjunction with hydrophobic oleophobic layer, so that obtaining Surface have better hydrophobic oleophobic performance and stronger wearability.
Using present invention process handle product have excellent performance, after 1KG steel wool friction testing 3000 times with The contact angle of water is also greater than 110 °, and the hydrophobic oleophobic layer obtained compared with no etching processing has better rub resistance.The simple process It is easy, it can be widely applied to the surface treatment of different substrate materials, continuous production can be achieved in industrialization.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail.
Embodiment one
A kind of long-acting hydrophobic oleophobic process of surface treatment, comprising the following steps:
One, the preparation of hydrophilic nano silicon dioxide gel: ethyl orthosilicate: dehydrated alcohol: distilled water: ammonium hydroxide is according to rubbing You are ratio=1:6:4:0.05, and ethyl orthosilicate, dehydrated alcohol and distilled water are uniformly mixed, are added under magnetic stirrer Ammonia spirit is 9-10 to pH, 2h is stirred after completion of dropwise addition, condensation reaction is hydrolyzed, and stands overnight ageing and reacts up to transparent Shape nano silicon dioxide sol is spare.
Two, copper sheet substrate substrate etching: is immersed into the H that mass concentration is 10%2O2Solution etches 30min, surface are formed Even rough layer.
Three, substrate cleaning: first be stained with spirituous non-dust cloth wipe it is etched after copper sheet surface naked eyes visible contamination Object, then the copper sheet cleaned is placed in the in the mixed solvent ultrasound 10min of pure solution ethanol-acetone (v:v=1:2), remove surface oil Rouge and dust, then with remaining solvent is removed in the deionized water containing cleaning agent, finally rinsed again with deionized water, it dries standby With.
Four, the preparation of transparent silicon dioxide film: the copper sheet of cleaning is at the uniform velocity immersed with hanger after will be etched contains Mass concentration is to be impregnated with the pull rate of 5cm/min in the silicon dioxide gel of 2% polyvinyl alcohol, reach after 30nm 100 DEG C Lower dry 3min.
Five, the preparation of long-acting hydrophobic oleophobic layer: the substrate that dip-coating has the transparent silicon dioxide film of 30nm thickness is immersed complete It in fluoric acid acid anhydride alkyl triethoxysilane, is impregnated with the pull rate of 3cm/min, then dry 20min at 120 DEG C, naturally cold But the long-acting hydrophobic oleophobic layer of 300nm thickness can be obtained in processing product surface.
Crocking resistance tests (GB/T 30693-2014):
Number Rub preceding and water contact angle ° Rub 1000 times and water contact angle ° Rub 2000 times and water contact angle ° Rub 3000 times and water contact angle °
a 116 103 94 86
b 121 118 116 112
Not through over etching pre-treatment, other steps are same as above a
B passes through etching processing, other steps are as above.
Embodiment two
A kind of long-acting hydrophobic oleophobic process of surface treatment, comprising the following steps:
One, the preparation of hydrophilic nano silicon dioxide gel: ethyl orthosilicate: dehydrated alcohol: distilled water: ammonium hydroxide is according to rubbing You are ratio=1:6:4:0.05, and ethyl orthosilicate, dehydrated alcohol and distilled water are uniformly mixed, are added under magnetic stirrer Ammonia spirit is 9-10 to pH, 2h is stirred after completion of dropwise addition, condensation reaction is hydrolyzed, and stands overnight ageing and reacts up to transparent Shape nano silicon dioxide sol is spare.
Two, substrate etching: by ABS electroplated product, using plasma etching 10min, surface forms uniform rough layer.
Three, substrate cleaning: first be stained with spirituous non-dust cloth wipe it is etched after ABS electroplated product surface naked eyes can See pollutant, then the copper sheet cleaned is placed in the in the mixed solvent ultrasound 10min of pure solution ethanol-acetone (v:v=1:2), removes Surface grease and dust, then with remaining solvent is removed in the deionized water containing cleaning agent, finally rinsed again with deionized water, It is dried for standby.
Four, the preparation of transparent silicon dioxide film: the ABS electroplated product of cleaning is at the uniform velocity soaked with hanger after will be etched Enter is to be impregnated in the silicon dioxide gel of 2% polyvinyl alcohol with the pull rate of 6cm/min, after reaching 50nm containing mass concentration Dry 3min at 80 DEG C.
Five, the preparation of long-acting hydrophobic oleophobic layer: the substrate that dip-coating has the transparent silicon dioxide film of 50nm thickness is immersed complete It in fluoric acid acid anhydride alkyl triethoxysilane, is impregnated with the pull rate of 2cm/min, then dry 20min at 100 DEG C, naturally cold But the long-acting hydrophobic oleophobic layer of 600nm thickness can be obtained in processing product surface.
Crocking resistance tests (GB/T 30693-2014):
Number Rub preceding and water contact angle ° Rub 1000 times and water contact angle ° Rub 2000 times and water contact angle ° Rub 3000 times and water contact angle °
a 118 108 101 92
b 125 123 119 115
Not through over etching pre-treatment, other steps are same as above a
B passes through etching processing, other steps are as above.
Embodiment three
A kind of long-acting hydrophobic oleophobic process of surface treatment, comprising the following steps:
One, the preparation of hydrophilic nano silicon dioxide gel: ethyl orthosilicate: dehydrated alcohol: distilled water: ammonium hydroxide is according to rubbing You are ratio=1:6:4:0.05, and ethyl orthosilicate, dehydrated alcohol and distilled water are uniformly mixed, are added under magnetic stirrer Ammonia spirit is 9-10 to pH, 2h is stirred after completion of dropwise addition, condensation reaction is hydrolyzed, and stands overnight ageing and reacts up to transparent Shape nano silicon dioxide sol is spare.
Two, substrate etching: by ceramic product, 30min is etched using ultraviolet light, surface forms uniform rough layer.
Three, substrate cleaning: first be stained with spirituous non-dust cloth wipe it is etched after surface of ceramic products naked eyes it is visible Pollutant, then the copper sheet cleaned is placed in the in the mixed solvent ultrasound 10min of pure solution ethanol-acetone (v:v=1:2), remove table Face grease and dust, then with remaining solvent is removed in the deionized water containing cleaning agent, finally rinsed again with deionized water, it dries It does spare.
Four, the preparation of transparent silicon dioxide film: the ceramic product of cleaning is at the uniform velocity immersed with hanger after will be etched It is to be impregnated in the silicon dioxide gel of 2% polyvinyl alcohol with the pull rate of 5cm/min, after reaching 50nm containing mass concentration Dry 5min at 100 DEG C.
Five, the preparation of long-acting hydrophobic oleophobic layer: the substrate that dip-coating has the transparent silicon dioxide film of 50nm thickness is immersed complete It in fluoric acid acid anhydride alkyl triethoxysilane, is impregnated with the pull rate of 8cm/min, then dry 30min at 100 DEG C, naturally cold But the long-acting hydrophobic oleophobic layer of 200nm thickness can be obtained in processing product surface.
Crocking resistance tests (GB/T 30693-2014):
Number Rub preceding and water contact angle ° Rub 1000 times and water contact angle ° Rub 2000 times and water contact angle ° Rub 3000 times and water contact angle °
a 112 103 94 81
b 118 115 113 110
Not through over etching pre-treatment, other steps are same as above a
B passes through etching processing, other steps are as above.
Example IV
A kind of long-acting hydrophobic oleophobic process of surface treatment, comprising the following steps:
One, the preparation of hydrophilic nano silicon dioxide gel: ethyl orthosilicate: dehydrated alcohol: distilled water: ammonium hydroxide is according to rubbing You are ratio=1:6:4:0.05, and ethyl orthosilicate, dehydrated alcohol and distilled water are uniformly mixed, are added under magnetic stirrer Ammonia spirit is 9-10 to pH, 2h is stirred after completion of dropwise addition, condensation reaction is hydrolyzed, and stands overnight ageing and reacts up to transparent Shape nano silicon dioxide sol is spare.
Two, substrate etching: kirsite substrate is immersed into the HCl solution that mass concentration is 5% and etches 10min, surface is formed Even rough layer.
Three, substrate cleaning: first be stained with spirituous non-dust cloth wipe it is etched after zinc alloy product surface naked eyes can See pollutant, then the copper sheet cleaned is placed in the in the mixed solvent ultrasound 10min of pure solution ethanol-acetone (v:v=1:2), removes Surface grease and dust, then with remaining solvent is removed in the deionized water containing cleaning agent, finally rinsed again with deionized water, It is dried for standby.
Four, the preparation of transparent silicon dioxide film: the zinc alloy product of cleaning is at the uniform velocity soaked with hanger after will be etched Enter is to be impregnated in the silicon dioxide gel of 2% polyvinyl alcohol with the pull rate of 3cm/min, after reaching 60nm containing mass concentration Dry 5min at 100 DEG C.
Five, the preparation of long-acting hydrophobic oleophobic layer: the substrate that dip-coating has the transparent silicon dioxide film of 60nm thickness is immersed complete It in fluoric acid acid anhydride alkyl triethoxysilane, is impregnated with the pull rate of 3cm/min, then dry 20min at 100 DEG C, naturally cold But the long-acting hydrophobic oleophobic layer of 650nm thickness can be obtained in processing product surface.
Crocking resistance tests (GB/T 30693-2014):
Number Rub preceding and water contact angle ° Rub 1000 times and water contact angle ° Rub 2000 times and water contact angle ° Rub 3000 times and water contact angle °
a 108 96 92 83
b 126 121 118 115
Not through over etching pre-treatment, other steps are same as above a
B passes through etching processing, other steps are as above.
The above description is only a preferred embodiment of the present invention, and not to the limitation of this case design, all designs according to this case are closed The equivalent variations that key is done each falls within the protection scope of this case.

Claims (9)

1. a kind of long-acting hydrophobic oleophobic process of surface treatment, which comprises the following steps:
One, shaggy micro nano structure is obtained in substrate surface etching；
Two, substrate surface dip-coating hydrophilic nano silicon dioxide gel after etching is dried to obtain transparent silicon dioxide film；
Three, there is the substrate surface dip-coating perfluor acid anhydrides alkyl triethoxysilane of transparent silicon dioxide film in dip-coating, is dried to obtain Hydrophobic oleophobic layer.
2. a kind of long-acting hydrophobic oleophobic process of surface treatment as described in claim 1, which is characterized in that substrate surface etches it Afterwards, substrate is cleaned: wipes substrate surface Visible pollutant, then the substrate that will be cleaned with being stained with spirituous non-dust cloth first Be placed in pure solution ethanol: acetone volume ratio is the in the mixed solvent ultrasound 10min of 1:2, removes surface grease and dust, then with containing There is the deionized water of cleaning agent to remove remaining solvent, is finally rinsed, be dried for standby with deionized water.
3. a kind of long-acting hydrophobic oleophobic process of surface treatment as described in claim 1, which is characterized in that substrate is plastics, gold One of category, ceramics, glass, woven fabric or rubber.
4. a kind of long-acting hydrophobic oleophobic process of surface treatment as described in claim 1, which is characterized in that lithographic method be it is equal from One of son etching, chemical etching or photoengraving.
5. a kind of long-acting hydrophobic oleophobic process of surface treatment as described in claim 1, which is characterized in that hydrophilic nano dioxy SiClx colloidal sol is obtained by following methods: ethyl orthosilicate: dehydrated alcohol: distilled water: ammonium hydroxide according to molar ratio=1:6:4:0.05, Ethyl orthosilicate, dehydrated alcohol and distilled water are uniformly mixed, it is 9-10 that ammonium hydroxide is added dropwise under magnetic stirrer to pH, is dripped 2h is stirred after adding, condensation reaction is hydrolyzed, stand overnight ageing and react up to transparence nano silicon dioxide sol.
6. a kind of long-acting hydrophobic oleophobic process of surface treatment as described in claim 1, which is characterized in that, will be through in step 2 Substrate after etching is at the uniform velocity immersed in the silicon dioxide gel of the polyvinyl alcohol or polyethylene glycol that are 2% containing mass concentration, with The pull rate of 5-9cm/min impregnates, and 3-5min is dried at 80-100 DEG C after reaching 30-90nm thickness.
7. a kind of long-acting hydrophobic oleophobic process of surface treatment as described in claim 1, which is characterized in that in step 3, will soak The substrate for being coated with the transparent silicon dioxide film of 30-90nm thickness immerses in perfluor acid anhydrides alkyl triethoxysilane, uses 1-6cm/ The pull rate of min impregnates, and then 10-1000nm thickness can be obtained in dry 20-30min at 100-150 DEG C, natural cooling Hydrophobic oleophobic layer.
8. a kind of long-acting hydrophobic oleophobic process of surface treatment as described in claim 1, which is characterized in that the thickness of silicon dioxide film Degree is 30-90nm.
9. a kind of long-acting hydrophobic oleophobic process of surface treatment as described in claim 1, which is characterized in that the thickness of hydrophobic oleophobic layer Degree is 10-1000nm.
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