CN108707336A - PDMS/C Super hydrophobic compound films and preparation method thereof - Google Patents
PDMS/C Super hydrophobic compound films and preparation method thereof Download PDFInfo
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- CN108707336A CN108707336A CN201810607024.1A CN201810607024A CN108707336A CN 108707336 A CN108707336 A CN 108707336A CN 201810607024 A CN201810607024 A CN 201810607024A CN 108707336 A CN108707336 A CN 108707336A
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- 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
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- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The present invention relates to a kind of PDMS/C Super hydrophobic compound films, including dimethyl silicone polymer and the carbon black that is uniformly distributed in dimethyl silicone polymer, the water contact angle of Super hydrophobic compound film is 155 ° -160 °.The present invention also provides preparation methods, include the following steps:The mixture of dimethyl silicone polymer and carbon black is formed between two opposite substrates, based surface applies the power towards mixture, then cures at 150 DEG C -160 DEG C, to form Super hydrophobic compound film between substrate.Carbon black materials are embedded in PDMS by the present invention only with physical compression mode, and simple and quick, economic and environment-friendly, prepared laminated film not only has excellent super-hydrophobicity, but also is also equipped with characteristic that is wear-resistant and being protected from light protection simultaneously.
Description
Technical field
The present invention relates to based superhydrophobic thin films technical field more particularly to a kind of PDMS/C Super hydrophobic compound films and its preparations
Method.
Background technology
The super-hydrophobic i.e. self-cleaning property of lotus leaf is from ancient times just known, therefore also leaves " going out mud without contaminating "
Good reputation.Water droplet can form pearl shape in lotus leaf surface and cannot steadily rest on surface, as long as slightly swinging or tilting droplet
It will be tumbled from blade face, the pollutants such as the dust of lotus leaf surface adherency can be taken away while droplet tumbles, to keep lotus leaf table
Face it is clean, this self-cleaning phenomenon of lotus leaf surface is referred to as lotus leaf effect.Lotus has been opened in the use of scanning electron microscope
The veil of the hydrophobic secret of leaf, promotes Barthlott to propose " lotus leaf effect " concept in theory, and opens a new table
Face application field.
Super hydrophobic surface can be prepared by multiple technologies, but can be mainly divided into two kinds of approach:One is in low table
Face can construct microcosmic coarse structure on the surface of substance;Another kind is the modification low-surface-energy object on the surface of coarse structure
Matter.With the development of experiment technology of preparing, some highly sophisticated devices and excellent low-surface energy substance are applied.Researcher is
Through the based superhydrophobic thin films that can prepare different-shape coarse structure by different physics, chemical method.These methods are main
Including phase detachment technique, etching method, electrochemical deposition method, sol-gel method, layer-by-layer and Electrospinning Method.
Although researchers have prepared the super-hydrophobic table with very big static contact angle and minimum roll angle in laboratory
Face.But or corresponding preparation method needs expensive and complicated precision equipment or is exactly preparation process complexity, only
Rest on the experimental study stage, it is difficult to realize large-scale industrial production.Furthermore prepared superhydrophobic surface structure is loosely
Gu, it usually needs follow-up silicic acid anhydride (mainly chemical modification), the ability for adapting to external environment is poor, in natural conditions
Under, surface layer coarse structure is easy to aging, destroys, to lose super-hydrophobicity.These defects make artificial based superhydrophobic thin films mesh
It is preceding to be also difficult to walk out laboratory.Therefore, at low cost, excellent durability based superhydrophobic thin films how are prepared by simple method
It is the main direction of experimental study from now on.
Invention content
In order to solve the above technical problems, the object of the present invention is to provide a kind of PDMS/C Super hydrophobic compound films and its preparations
Carbon black materials are embedded in PDMS, simple and quick, economic and environment-friendly, prepared THIN COMPOSITE by method only with physical compression mode
Film not only has excellent super-hydrophobicity, but also is also equipped with characteristic that is wear-resistant and being protected from light protection simultaneously.
On the one hand, the present invention provides a kind of PDMS/C Super hydrophobic compound films, including dimethyl silicone polymer
(PDMS) and the carbon black that is uniformly distributed in dimethyl silicone polymer, the water contact angle of PDMS/C Super hydrophobic compound films are
155 ° -160 °, it is preferable that the water contact angle of Super hydrophobic compound film is 158 °.
Carbon black film has natural super-hydrophobicity, but can not directly apply to practical matter always, and reason is its machine
Tool intensity is very low, is easily destroyed.And carbon black be probably passed through in the carbon particle of tens rans by grain size one by one it is random
Physics stacked combination at unordered chain dendritic morphology (Fig. 1), exactly have benefited from this structure so that carbon blacksurface have very
High roughness just creates its remarkable super-hydrophobicity.But the microcosmic caking property between these nano particles is naturally just very weak,
Therefore the mechanical strength for resulting in its macroscopic view is very poor.PDMS carries out carbon black structure certain external fixed reinforcing as binder,
The wearability of structure is greatly improved, and retains its super-hydrophobicity simultaneously, and carbon black also assigns laminated film with photophobism simultaneously.
On the other hand, the present invention also provides a kind of preparation methods of above-mentioned PDMS/C Super hydrophobic compound films, including
Following steps:
The mixture of dimethyl silicone polymer and carbon black is formed between two opposite substrates, based surface applies court
To the power of mixture, then cure at 150 DEG C -160 DEG C, to form the super-hydrophobic THIN COMPOSITEs of the PDMS/C between substrate
Film.
Further, the material of substrate is glass, silicon chip or metal.
Further, the pressure of the power of application is 650-1250Pa.
Further, gravity can be used in the power of application, and counterweight is such as compressed on substrate surface, easy to operate.
Further, the method for the mixture of formation dimethyl silicone polymer and carbon black includes between two opposite substrates
Following steps:In the surface modification dimethyl silicone polymer layer of the first substrate, silica aerogel layer is deposited on the surface of the second substrate, then
The silica aerogel layer of the dimethyl silicone polymer layer of first substrate surface and the second substrate surface is contacted with each other and fitted closely.
Further, the thickness of dimethyl silicone polymer layer is 8-20 microns.
Further, the thickness of silica aerogel layer is according to above-mentioned selected dimethyl silicone polymer layer thickness, with silica aerogel layer and poly- two
The ratio between thickness of methylsiloxane layer is 1-1.3:1 is advisable.
Further, include the following steps in the method for the surface modification dimethyl silicone polymer layer of the first substrate:
(S1) by the main glue of PDMS and curing agent with 10:1 quality forms colloid than mixing, excludes the bubble in colloid, obtains
To PDMS solution;
(S2) PDMS solution is spin-coated on the first substrate surface.
In step (S1), also colloid is diluted using diluent to obtain the PDMS solution of good fluidity,
In order to ensure its mobility, the main glue of PDMS:It is 1 with diluent mass ratio:1-3.
The abrasion resistance that the thickness of dimethyl silicone polymer layer can influence finally formed Super hydrophobic compound film is different, gathers
The dimethyl siloxane layer the thick more rub resistance.
Further, before curing, further include the steps that the second substrate of removal, to be formed on the surface of the first substrate
Super hydrophobic compound film.
According to the above aspect of the present invention, the present invention has at least the following advantages:
1, the commercially available PDMS of method selection of the invention and carbon black are raw material, and material is cheap, simple and easy to get, nontoxic
It is pollution-free, it is simple for process, it is not necessarily to expensive device, does not need high-temperature process and follow-up silicic acid anhydride, low energy consumption, to environment friend
It is good, it is widely portable to be prepared in the various substrate material surfaces such as glass, silicon chip, metal.
2, preparation method using the present invention is gone out using PDMS composite carbon black material preparations a kind of with anti abrasive for the first time
Hydrophobic polymer film, and film is opaque, can be used for the special occasion for being protected from light requirement of shelter.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, below with presently preferred embodiments of the present invention and after coordinating attached drawing to be described in detail such as.
Description of the drawings
Fig. 1 is the Electronic Speculum shape appearance figure of carbon black;
Fig. 2 is the preparation flow figure of PDMS/C Super hydrophobic compound films;
Fig. 3 is photo and the water contact angle test result in kind of PDMS/C Super hydrophobic compound films;
Fig. 4 is the SEM pattern test results of PDMS/C Super hydrophobic compound films;
Reference sign:
The second substrates of 1-;2- carbon blacks;3-PDMS;The first substrates of 4-;5-PDMS/C Super hydrophobic compound films.
Specific implementation mode
With reference to the accompanying drawings and examples, the specific implementation mode of the present invention is described in further detail.Implement below
Example is not limited to the scope of the present invention for illustrating the present invention.
Embodiment 1
A kind of preparation method of PDMS/C Super hydrophobic compound films is present embodiments provided, is carried out according to the flow of Fig. 2, tool
Body method is as follows:
(1) select glass slide (material is glass) be used as the first substrate 4 and the second substrate 1, and through acetone, ethyl alcohol, go from
Sub- water is cleaned by ultrasonic 10min, is dried up under nitrogen spare.
(2) by the main glue of PDMS and curing agent (main glue and curing agent be all DOW CORNING 184) with 10:1 mass ratio mixing, puts
The ultrasound in ultrasonic machine is set after ten minutes, to place into plasma machine and vacuumize 10min bubble removings;Again by obtained PDMS with
Diluent (n-hexane) presses 1:1 ratio (mass ratio) mixed configuration PDMS solution for standby.
(3) the PDMS solution of above-mentioned configuration is added dropwise in step (1) treated the first substrate 4, and utilizes photoresist spinner
With 2000r/min rotating speed spin coatings, the first substrate 4 coated with PDMS 3 is obtained, the thickness of PDMS 3 is 9.5 microns.In reality
Operation in, directly the PDMS solution of agent without dilution can also be used with certain rotating speed whirl coating.The difference and difference of rotating speed
Dilution ratio (mass ratio of PDMS and diluent) can cause finally obtained sample thickness (identical whirl coating parameter, be added
Diluent is more, and colloid is diluter, and the glue got rid of is thinner) (colloids more thick more rub resistance) different with abrasion resistance.
(4) step (1) is taken treated the second substrate 1, place it in baking above kerosene flame, deposition of thick is 11 microns
Carbon black 2 after, obtain deposition carbon black 2 the second substrate 1.Second substrate 1 is buckled in the first substrate 4, and make carbon black 2 with
PDMS 3 is contacted, and is then stood on 1 upper surface of the second substrate is pressed in the counterweight (equivalent pressure is about 930Pa) of 100g
10s makes the PDMS 3 in the first substrate 4 pour and penetrates into carbon black 2, and the first substrate 4 is directly taken by force from 1 surface of the second substrate
Carbon black 2 is taken, then takes counterweight and the second substrate 1 away.
(5) the first substrate 4 with PDMS and carbon black is put into 150 DEG C of pressurizes in baking oven and cures 20min, i.e., in the first base
4 surface of bottom forms PDMS/C Super hydrophobic compound films 5.The step can make carbon black be fully uniformly mixed with PDMS, and make
PDMS cures.
Above-mentioned product is characterized, a drop water, photo in kind such as Fig. 3 a is added dropwise to the first substrate surface after solidification
Shown, Fig. 3 b are the water contact angle test results of PDMS/C Super hydrophobic compound films, the results showed that, method of the invention is successfully
It is prepared for the super-hydrophobic PDMS/C laminated films that one layer of contact angle is up to 158 °.
In above method, the thickness (being selected in 8-20 micron ranges) and step (4) of PDMS 3 in (3) are changed the step
The thickness of the carbon black 2 of middle deposition, and the ratio between carbon black 2 and the thickness of dimethyl silicone polymer 3 are controlled in 1-1.3:It, can in 1 range
To adjust the water contact angle (155 ° -160 °) of prepared PDMS/C Super hydrophobic compound films, that is, change its hydrophobic performance.
Fig. 4 is the SEM pattern tests of PDMS/C Super hydrophobic compound films as a result, it is with coarse structure, therein
It is mutually bonded between grain.Embedding viscous effect by PDMS to carbon black structure, this layer film are still protected after tap water washes away 30 minutes
Stay stable super-hydrophobicity.
The above is only a preferred embodiment of the present invention, it is not intended to restrict the invention, it is noted that for this skill
For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is several improvement and
Modification, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (8)
1. a kind of PDMS/C Super hydrophobic compound films, it is characterised in that:Including dimethyl silicone polymer and it is uniformly distributed in institute
The carbon black in dimethyl silicone polymer is stated, the water contact angle of the PDMS/C Super hydrophobic compound films is 155 ° -160 °.
2. a kind of preparation method of PDMS/C Super hydrophobic compound films described in claim 1, which is characterized in that including following step
Suddenly:
The mixture that dimethyl silicone polymer and carbon black are formed between two opposite substrates applies court to the surface of the substrate
To the power of mixture, then cure at 150 DEG C -160 DEG C, it is super-hydrophobic compound to form the PDMS/C between the substrate
Film.
3. preparation method according to claim 2, it is characterised in that:The material of the substrate is glass, silicon chip or metal.
4. preparation method according to claim 2, it is characterised in that:The pressure of the power of application is 650-1250Pa.
5. preparation method according to claim 2, which is characterized in that form poly dimethyl silicon between two opposite substrates
The method of the mixture of oxygen alkane and carbon black includes the following steps:In the surface modification dimethyl silicone polymer layer of the first substrate,
The surface of second substrate deposits silica aerogel layer, then by the dimethyl silicone polymer layer of the first substrate surface and the second substrate surface
Silica aerogel layer contacts with each other and fits closely.
6. preparation method according to claim 5, it is characterised in that:The thickness of the dimethyl silicone polymer layer is 8-20
Micron.
7. preparation method according to claim 5, it is characterised in that:The thickness of the silica aerogel layer and dimethyl silicone polymer layer
The ratio between degree is 1-1.3:1.
8. preparation method according to claim 5, it is characterised in that:Before curing, further include removal second base
The step of bottom, to form the PDMS/C Super hydrophobic compound films on the surface of the first substrate.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111499898A (en) * | 2020-04-08 | 2020-08-07 | 国网山西省电力公司电力科学研究院 | Preparation method of carbon nano composite film and application of carbon nano composite film in laser ultrasonic detection |
CN112646485A (en) * | 2020-12-01 | 2021-04-13 | 中国矿业大学(北京) | Preparation method of hydrophobic wax-proof composite coating and hydrophobic wax-proof composite coating |
CN115181310A (en) * | 2022-07-13 | 2022-10-14 | 电子科技大学长三角研究院(湖州) | Optical actuator and preparation method thereof |
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CN106219996A (en) * | 2016-07-14 | 2016-12-14 | 苏州大学 | Method for constructing high-adhesion super-hydrophobic surface |
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CN106219996A (en) * | 2016-07-14 | 2016-12-14 | 苏州大学 | Method for constructing high-adhesion super-hydrophobic surface |
Non-Patent Citations (1)
Title |
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徐成云: ""基于PDMS与炭黑的超疏水涂层的制备"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111499898A (en) * | 2020-04-08 | 2020-08-07 | 国网山西省电力公司电力科学研究院 | Preparation method of carbon nano composite film and application of carbon nano composite film in laser ultrasonic detection |
CN112646485A (en) * | 2020-12-01 | 2021-04-13 | 中国矿业大学(北京) | Preparation method of hydrophobic wax-proof composite coating and hydrophobic wax-proof composite coating |
CN115181310A (en) * | 2022-07-13 | 2022-10-14 | 电子科技大学长三角研究院(湖州) | Optical actuator and preparation method thereof |
CN115181310B (en) * | 2022-07-13 | 2023-07-25 | 电子科技大学长三角研究院(湖州) | Optical actuator and preparation method thereof |
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Application publication date: 20181026 |