CN104441357B - Method for preparing resin film layer with ultralow roughness - Google Patents

Method for preparing resin film layer with ultralow roughness Download PDF

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Publication number
CN104441357B
CN104441357B CN201410718478.8A CN201410718478A CN104441357B CN 104441357 B CN104441357 B CN 104441357B CN 201410718478 A CN201410718478 A CN 201410718478A CN 104441357 B CN104441357 B CN 104441357B
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carrier
resin film
film layer
roughness
liquid phase
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CN104441357A (en
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王鹏
张盾
陆洲
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Institute of Oceanology of CAS
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Institute of Oceanology of CAS
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Abstract

The invention relates to a method for preparing a resin film layer with ultralow roughness, in which a liquid phase surface is used as a template. With the liquid phase surface as the template, resin is covered on the surface of the template, and the resin film layer with ultralow roughness can be copied by the cured resin. The resin film layer with ultralow roughness, prepared in the invention, can be applied to such fields as marine fouling, drag reduction, etc.

Description

A kind of method preparing the resin film layer with ultralow roughness
Technical field
The present invention relates to a kind of is template using " liquid phase " surface, preparation has the side of the resin film layer of ultralow roughness Method.
Background technology
Surface roughness is one of key factor of impact material property, also can affect some performances on surface.For example, table Surface roughness can strengthen the apparent wettability on surface, in addition, the presence of surface roughness can affect between surface attachments and surface Active force etc..The preparation therefore with special roughness surface is most important with application for the exploitation of functional material.
Low surface roughness surface is with a wide range of applications in actual industrial.It is experimentally confirmed that low coarse low surface Affixing probability and the adhesive force of material surface antibacterial can be significantly reduced, this is opening of new anti-marine biofouling attachment material Send out and foundation is provided.In addition, low roughness surface can significantly reduce the resistance of drop and its surface, can be applicable to draft reduction material Exploitation.The method being presently used for reducing solid metal surface roughness is a lot, and conventional method includes mechanical polishing, electrochemistry Polishing etc..But for organic polymer layers, the resin film layer especially commonly used in industry, its low roughness surface construction method is very Few.
Content of the invention
It is an object of the invention to provide a kind of method preparing ultralow roughness resin film layer.
For achieving the above object, the technical solution used in the present invention is:
A kind of method preparing the resin film layer with ultralow roughness, with " liquid phase " surface resin is covered as template In its surface, the resin film layer of the reproducible excess of export low roughness of the resin after solidification.
Described " liquid phase " surface is the surface in surface of solid phase carriers preparation with coarse structure, and adopts low-surface-energy thing Confrontation film is modified, and the carrier surface after modification covers one layer of liquid good with surface matching, then by micro structure Capillarity, that is, carrier surface formed one layer of continuous, smooth " liquid phase " surface.
Described carrier is the test button that metallic aluminium or surface cover aluminium coat;Described low-surface energy substance be containing- (cf2)nThe silane of-group;The described liquid good with surface matching is by group-(cf2)nThe polyethers of-composition.
The preparation on described " liquid phase " surface:
(1) the constructing of carrier surface coarse structure: as anode, rustless steel is negative electrode to the carrier after to clean, in volume ratio Carry out the electrochemical polish of carrier, polishing voltage is 12-15v DC voltage, during polishing in perchloric acid for 1:4 and ethanol solution Between be 2-3 minute;Subsequently, as anode, stainless steel electrode is negative electrode to the aluminum after to polish, and the aqueous solution of 0.4m ethanedioic acid is electrolysis Liquid, prepares coarse pellumina using anodic oxidation mode in metal surface, two interpolars apply 70-80v DC voltage, during oxidation Between be 2-4 minute, temperature be room temperature;
(2) carrier surface is modified: the sample that surface after anodic oxidation is had coarse structure is immersed in containing 5-10% (volume Percentage ratio) the ethanol solution of tridecafluoro-n-octyltriethoxysilane in soak 5-10 minute, in 140-150 DEG C of environment after taking-up Middle process 5-10 minute;
(3) covering of " liquid phase " skin covering of the surface: polyethers is added to the specimen surface after process, and sample is tilted 20-25 ° and put Put 1-2 hour, cover one layer of liquid good with surface chemical property matching on surface, by the capillarity of micro structure, carry Body surface face forms one layer of continuous, smooth " liquid phase " surface.
Described carrier carries out ultrasonic vibration cleaning using deionized water to its surface.
Cover in template surface using epoxy resin, then use 1wt.% dibutyl phthalate as diluent, As firming agent, hardening time is 24-48h to 0.5wt.% triethylene diamine mixture at room temperature.
Advantage for present invention:
With " liquid phase " surface as template, a step prepares the resin film layer on low roughness surface to the present invention.And be not required to Use main equipment.The neck such as marine anti-pollution, drag reduction be can be applicable to by the resin film layer with ultralow roughness prepared by the present invention Domain.
Brief description
Fig. 1 be provided in an embodiment of the present invention with " liquid phase " surface as template, the resin with ultralow roughness of preparation The line scanning result figure of apparent height.
Specific embodiment
Embodiment 1
(1) ultrasonic vibration cleaning is carried out to pure aluminum substrate surface using deionized water;
(2) as anode, rustless steel is negative electrode to the metallic aluminium after to clean, molten with ethanol in the perchloric acid for 1:4 for the volume ratio In liquid, (temperature is less than 3 DEG C) carries out the electrochemical polish of aluminum, and polishing voltage is 15v DC voltage, and polishing time is 2 minutes;With Afterwards, as anode, stainless steel electrode is negative electrode to the aluminum after to polish, and the aqueous solution of 0.4m ethanedioic acid is electrolyte, using anodic oxygen Change mode prepares coarse pellumina in metal surface, and two interpolars apply 70v DC voltage, and oxidization time is 2 minutes, and temperature is Room temperature;
(3) sample that the surface after anodic oxidation is had coarse aluminium oxide structure is immersed in containing 1% (percent by volume) The ethanol solution of tridecafluoro-n-octyltriethoxysilane in soak 10 minutes, after taking-up in 140 DEG C of environment process 10 minutes;
(4) PFPE is dropped to the specimen surface after process, and sample is tilted 20 ° and place 2 hours, by micro- knot The capillarity of structure, carrier surface forms one layer of continuous, smooth " liquid phase " surface.
(5) by commercially available epoxy resin uniform fold to " liquid phase " surface, after resin polymerization solidification, reproducible go out low thick Rugosity surface, the line scanning result of its apparent height is as shown in Figure 1.As shown in Figure 1, its apparent height rises and falls and is less than 20nm.

Claims (5)

1. a kind of method preparing the resin film layer with ultralow roughness it is characterised in that: with " liquid phase " surface as template, will Resin covers in its surface, the resin film layer of the reproducible excess of export low roughness of the resin after solidification;
Described " liquid phase " surface is the surface in surface of solid phase carriers preparation with coarse structure, and adopts low-surface energy substance pair Film is modified, and the carrier surface after modification covers one layer of liquid good with surface matching, then by the hair of micro structure Spy uses, and forms one layer of continuous, smooth " liquid phase " surface in carrier surface.
2. the preparation as described in claim 1 have the resin film layer of ultralow roughness method it is characterised in that: described carrier Test button for metallic aluminium or surface covering aluminium coat;Described low-surface energy substance is containing-(cf2)nThe silane of-group;Described Good liquid is by group-(cf with surface matching2)nThe polyethers of-composition.
3. the preparation as described in claim 1 have the resin film layer of ultralow roughness method it is characterised in that: described " liquid The preparation on phase " surface:
(1) the constructing of carrier surface coarse structure: as anode, rustless steel is negative electrode to the carrier after to clean, and is 1:4 in volume ratio Perchloric acid and ethanol solution in carry out the electrochemical polish of carrier, polishing voltage is 12-15v DC voltage, and polishing time is 2-3 minute;Subsequently, as anode, stainless steel electrode is negative electrode to the aluminum after to polish, and the aqueous solution of 0.4m ethanedioic acid is electrolyte, Coarse pellumina is prepared in metal surface using anodic oxidation mode, two interpolars apply 70-80v DC voltage, oxidization time For 2-4 minute, temperature is room temperature;
(2) carrier surface is modified: the sample that surface after anodic oxidation is had coarse structure is immersed in containing 5-10% (volume basis Than) tridecafluoro-n-octyltriethoxysilane ethanol solution in soak 5-10 minute, after taking-up in 140-150 DEG C of environment locate Reason 5-10 minute;
(3) covering of " liquid phase " skin covering of the surface: polyethers is added to the specimen surface after process, and sample is tilted 20-25 ° of placement 1- 2 hours, cover one layer of liquid good with surface chemical property matching on surface, by the capillarity of micro structure, carrier table Face forms one layer of continuous, smooth " liquid phase " surface.
4. the preparation as described in claim 3 have the resin film layer of ultralow roughness method it is characterised in that: described carrier Ultrasonic vibration cleaning is carried out to its surface using deionized water.
5. a kind of as described in claim 1 prepare the method with ultralow roughness resin film layer it is characterised in that: adopt ring Oxygen tree fat covers in template surface, then uses dibutyl phthalate as diluent, triethylene diamine as firming agent, Room temperature lower hardening time is 24-48h.
CN201410718478.8A 2014-12-01 2014-12-01 Method for preparing resin film layer with ultralow roughness Active CN104441357B (en)

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CN104441357B true CN104441357B (en) 2017-01-25

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CN107364057A (en) * 2017-07-10 2017-11-21 天津工业大学 A kind of preparation method of different roughness template

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JP2005231047A (en) * 2004-02-17 2005-09-02 Konica Minolta Medical & Graphic Inc Method for manufacturing aluminum support for lithographic printing plate, aluminum support for lithographic printing plate and lithographic printing plate material/image forming method
JP4683289B2 (en) * 2006-01-13 2011-05-18 富士フイルム株式会社 Method for producing thermoplastic resin film
CN101125936A (en) * 2006-08-14 2008-02-20 日立麦克赛尔株式会社 Method for modifying surface of plastic member, method for forming metal film, and method for producing plastic member

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