KR101644025B1 - Superhydrophobic Surface Body and Method for Fabricating Superhydrophobic Surface Body Using iCVD - Google Patents

Abstract

The present invention relates to a method for producing a superhydrophobic surface body using a chemical vapor deposition reactor (iCVD) using an ultra-hydrophobic surface body and an initiator having improved mechanical strength and chemical strength, comprising the steps of: (a) step; (b) depositing a super hydrophobic monomer on a crosslinking agent deposited on an upper surface of the substrate; (c) depositing a crosslinking agent on the lower surface of the substrate; And (d) depositing a super-hydrophobic monomer on a crosslinking agent deposited on the lower surface of the substrate to produce a super-hydrophobic surface body. The super-hydrophobic surface body according to the present invention has excellent mechanical strength and chemical strength, Separation of oil from water, energy conversion, protection of electronic equipment, regulation of cell substrate junctions in the biomedical field, reduction of fluid resistance in microfluidic devices, and the like.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a superhydrophobic surface body and a method for manufacturing the superhydrophobic surface body using a chemical vapor deposition reactor (iCVD)

The present invention relates to a method of preparing a superhydrophobic surface body by using a chemical vapor deposition reactor (iCVD) using an ultra-hydrophobic surface body and an initiator, and more particularly, to a method of manufacturing a superhydrophobic surface body by depositing a cross- (ICVD) using an initiator having an improved strength, and a method for producing a superhydrophobic surface body using the chemical vapor deposition reactor (iCVD).

Hydrophobicity refers to the property of an object that has no affinity for water. Hydrophobicity is related to the surface tension, which is the internal force generated by the imbalance of molecular forces when two different materials form a contact surface with each other. If the force acting between the water and the surface of the object is stronger than the cohesive force between the molecules of the water, the water molecule receives a strong attraction to the surface of the object, so that the surface of the object is wetted. In the opposite case, the water does not wet the surface of the object.

This hydrophobicity can be confirmed by measuring the contact angle (?) Between the surface and the water measured on the surface of the object, and when the contact angle between the surface of the object and water is more than 150 °, it is said to have superhydrophobicity.

An object having a superhydrophobic surface can effectively prevent surface agglomeration of other materials including water due to low surface energy and has an effect of preventing foreign materials such as human fingerprints and foreign substances such as dust from adhering to the surface. Therefore, an object having a superhydrophobic surface can be widely applied to exterior materials of electronic products, which are polluted by organic matter, and building materials in which prevention of humidity and foreign matter contamination is essential. Especially, if stainless steel excellent in corrosion resistance including chromium has a superhydrophobic surface, application value of exterior materials and building materials of home electric appliances such as refrigerators, mobile phones, televisions and the like will be greatly increased.

A method conventionally used to impart superhydrophobicity to the surface of an object, in particular stainless steel, is a method of coating a surface with a fluorine-based hydrophobic substance such as titanium or Teflon. The method of forming titanium or titanium oxide on the double surface is disadvantageous in that the contact angle with water is less than 150 deg., The hydrophobic property is weak, and there is a problem that the manufacturing cost is increased due to the use of the vacuum evaporation method.

The method of coating the fluorine-based hydrophobic material such as Teflon is excellent in the super-hydrophobic property, but since the vacuum evaporation method is also used, the manufacturing cost is greatly increased for the large-sized. In order to solve this problem, a method of coating the surface of an object at atmospheric pressure has been studied. However, since the fluorine-based hydrophobic substance itself is an expensive material, the problem of manufacturing cost still remains.

Therefore, it is urgent to develop a technique for imparting super-hydrophobicity to the surface of a large area at a low price.

Meanwhile, U.S. Patent No. 7651760 discloses a method for producing a superhydrophobic surface body using a chemical vapor deposition reactor (iCVD) using electrospinning and an initiator. However, the chemical strength and mechanical There was a problem in using because of its weak strength.

As a result of intensive efforts to solve the above problems, the inventors of the present invention have found that, prior to the deposition of monomers on a substrate for the preparation of a super hydrophobic surface body, the cross-linking agent is first deposited and the monomers having super hydrophobic properties are subjected to chemical vapor deposition It has been confirmed that a superhydrophobic surface body having improved mechanical strength and chemical strength can be produced by depositing a layered structure using a reactor (iCVD) or a copolymer of a monomer and a cross-linking agent, and completing the present invention .

An object of the present invention is to provide a superhydrophobic surface body having improved mechanical strength and chemical strength and a method of manufacturing the same.

In order to accomplish the above object, the present invention provides a method for manufacturing a semiconductor device, comprising: (a) depositing a cross-linking agent on both sides of a substrate; And (b) depositing a super-hydrophobic monomer on both sides of the substrate on which the cross-linking agent is deposited to produce a super-hydrophobic surface body, wherein the cross-linking agent is deposited on the surface of the super- hydrophobic surface body using a chemical vapor deposition reactor (iCVD) And a manufacturing method thereof.

(A) depositing a cross-linking agent on the top surface of the substrate; (b) depositing a super hydrophobic monomer on a crosslinking agent deposited on an upper surface of the substrate; (c) depositing a crosslinking agent on the lower surface of the substrate; And (d) depositing a super-hydrophobic monomer on a crosslinking agent deposited on the lower surface of the substrate to produce a super-hydrophobic surface body. The method of manufacturing a super-hydrophobic surface body using a chemical vapor deposition reactor (iCVD) ≪ / RTI >

The present invention also provides a superhydrophobic surface body on which a crosslinking agent is deposited on the upper and lower surfaces of a substrate, and a superhydrophobic polymer is deposited on the deposited crosslinking agent.

The present invention also provides a method for producing a superhydrophobic surface using a chemical vapor deposition reactor (iCVD) using an initiator comprising the steps of depositing a copolymer of a superhydrophobic monomer and a crosslinking agent on the upper and lower surfaces of a substrate, respectively, A method for producing a sieve is provided.

The present invention also provides a superhydrophobic surface body on which a copolymer of a superhydrophobic monomer and a crosslinking agent is deposited on the upper and lower surfaces of a substrate.

The present invention also provides a method of manufacturing a semiconductor device comprising the steps of: (a) depositing 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane on both sides of a substrate; And (b) on both sides of the substrate on which the 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane has been deposited, 1H, 1H, 2H, 2H-perfluorodecyl (ICVD) using an initiator comprising the steps of: (a) forming a superhydrophobic surface body by depositing an acrylate monomer on the surface of the superhydrophobic surface body;

The present invention also provides a method of manufacturing a semiconductor device, comprising: (a) depositing 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane on the top surface of a substrate; (b) 1, 1H, 2H, 2H-perfluorodecyl acrylate (hereinafter referred to as " perfluorodecyl acrylate ") on 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane Depositing a monomer; (c) depositing 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane on the underside of the substrate; And (d) depositing 1H, 1H, 2H, 2H-perfluorodecyl acrylate on 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane deposited on the lower surface of the substrate (ICVD) using an initiator comprising the steps of: (i) depositing a monomethylketone monomethylketone monomethyl ether and a monomethyl ether monomethyl ether to produce a superhydrophobic surface material.

The present invention also relates to a process for the preparation of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane polymers deposited on the top and bottom surfaces of a substrate, - tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane on which a 1H, 1H, 2H, 2H-perfluorodecyl acrylate polymer is deposited.

The present invention also relates to a process for the preparation of 4,6,8,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane and 1H, 1H, 2H, 2H-perfluorodecyl acrylate (ICVD) using an initiator comprising the steps of: preparing a superhydrophobic surface body by vapor-depositing a copolymer of a monomer to prepare a superhydrophobic surface body, respectively.

The present invention also relates to a process for the preparation of 4,6,8,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane and 1H, 1H, 2H, 2H-perfluorodecyl acrylate A superhydrophobic surface body on which a copolymer of a monomer is deposited.

The superhydrophobic surface body according to the present invention is excellent in mechanical strength and chemical strength and can be used for separation of oil from water, energy conversion, protection of electronic equipment, regulation of cell substrate bonding in biomedical fields, reduction of fluid resistance in microfluidic devices, etc. Can be used for various purposes.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic diagram of a superhydrophobic surface body manufactured by a method of producing a superhydrophobic surface body using a chemical vapor deposition reactor (iCVD) using an initiator according to the present invention (A: deposition in a layered structure, B: Use of a copolymer of a crosslinking agent).
FIG. 2 shows the result of FT-IR measurement of a superhydrophobic surface body on which a pPFDA layer was formed by depositing PFDA monomer and PFDA monomer.
3 shows the results of FT-IR measurement of the intermediate or finished product of the superhydrophobic surface material prepared in Examples and Comparative Examples of the present invention.
4 is a photograph of the superhydrophobic surface body prepared in Examples and Comparative Examples of the present invention after washing with soapy water and observed with SEM (A: superfine hydrophobic surface body manufactured in Comparative Example 1, x 1300 magnification; B : The superhydrophobic surface body prepared in Example 1, x 600 magnification).
FIG. 5 is a photograph of a superhydrophobic surface body prepared in Examples and Comparative Examples of the present invention, washed with soapy water and observed with XPS (A: superfine hydrophobic surface body prepared in Example 1, and B: And C: the superhydrophobic surface body prepared in Comparative Example 1).
FIG. 6 is a photograph of the contact angle measured by the ultrasonic treatment of the super-hydrophobic surface material prepared in Examples and Comparative Examples of the present invention. FIG.
7 is a photograph (A: washing with water, B: washing with soapy water, C: washing with soap water in a washing machine for 40 minutes). Fig. 7 is a photograph of the contact angle measured by the washing treatment of the superhydrophobic surface body prepared in Examples and Comparative Examples of the present invention , D: washing 5 times for 40 minutes in a washing machine with soapy water).
8 is a photograph (A: left at 16 캜 for 24 hours and B: left at 120 캜 for 24 hours) of the contact angle according to the temperature condition of the superhydrophobic surface body prepared in Examples and Comparative Examples of the present invention.
9 is a photograph of the contact angle measured by the solvent treatment of the superhydrophobic surface material prepared in Examples and Comparative Examples of the present invention
10 is a photograph showing the oleophobicity of the superhydrophobic surface body manufactured in the embodiment of the present invention.
11 (a) is an SEM photograph of the superhydrophobic surface body manufactured in Example 1 of the present invention, and the right side of FIG. 11 (b) is a photograph of a digital camera after annealing at 120 ° C. for 24 hours, 11 (b) is a photograph of a digital camera after annealing the super-hydrophobic surface body manufactured in Comparative Example 1 at 120 ° C. for 24 hours, FIG. 11 (c) is a photograph of V4D4 and p (V4D4) FT-IR graph of the laminated polymer.
The left side of FIG. 12A is a SEM image before the deposition of the polymer on the polyester mesh and a drop of water droplets (FIG. 12A). On the right side of FIG. 12A, FIG. 12B is a view showing the measurement of the transmittance of the glass coated with the laminated polymer. FIG. 12B is a graph showing the SEM image after the deposition of the polymer and the drop of water droplets (FIG.
13 (b) is an EDS (Energy Dispersive Spectroscopy) element mapping image of fluorine, and FIG. 13 (c) is an SEM image of the surface of the superhydrophobic surface body prepared in Example 1 of the present invention. 13 (a) and the EDS element mapping picture of Fig. 13 (b).
14 is a photograph (SEM and AFM) of a surface of a superhydrophobic surface body and an uncoated polyester produced according to an embodiment of the present invention ((a) uncoated polyester, (b) (D) an uncoated Si wafer, (e) a superhydrophobic surface body according to Example 3, (f) a deposition condition A superhydrophobic surface body which is deposited in a rugged manner).
Fig. 15 is a view schematically showing that an air pocket is formed due to a rugged structure to exhibit super-hydrophobic properties.
16 is a graph showing changes in the contact angle after chemical and mechanical stress ((a) heat treatment, (b) ultrasonic treatment, (c) solvent treatment, and (d) hysteresis curve before and after treatment).
17 is a graph (a) showing a change in contact angle according to the number of times of washing of the superhydrophobic surface body according to Example 1 of the present invention, and FIG. 17 ), After washing (c), and after the erosion treatment (d).
Figure 18 is a contact angle measured after immersing for 24 hours in Example 1 H ₂ SO ₄ respectively, the second hydrophobic surface material according to (a), KOH (b) , H 2 O 2 (c) according to the present invention, H ₂ SO ₄ (d), and KOH (e).

In the present invention, when a crosslinking agent is first deposited and a monomer having a super-hydrophobic property is deposited in a laminated structure using a chemical vapor deposition reactor (iCVD) using an initiator, , The mechanical strength and the chemical strength can be improved.

In the present invention, a crosslinking agent is deposited on a substrate, and monomers having super hydrophobic properties are deposited in a laminated structure using a chemical vapor deposition reactor (iCVD) using an initiator to prepare a superhydrophobic surface body. As a result, it was confirmed that the prepared superhydrophobic surface body had higher mechanical strength and chemical strength than those without crosslinking agent.

Accordingly, in one aspect, the present invention provides a method of manufacturing a semiconductor device, comprising: (a) depositing a cross-linking agent on both sides of a substrate; And (b) depositing a super-hydrophobic monomer on both sides of the substrate on which the cross-linking agent is deposited to produce a super-hydrophobic surface body, wherein the cross-linking agent is deposited on the surface of the super- hydrophobic surface body using a chemical vapor deposition reactor (iCVD) And a manufacturing method thereof.

The substrate is not particularly limited, but may be glass, metal, metal oxide, wood, paper, fiber, plastic, rubber, leather, silicon wafer or the like, depending on the purpose of use. The plastic may be polyethylene (PE), polypropylene (PP), polystyrene (PS), polyethylene terephthalate (PET), polyamides (PA) ), Polyvinyl chloride (PVC), polyurethanes (PU), polycarbonate (PC), polyvinylidene chloride (PVDC), polytetrafluoroethylene (PTFE) Polyetheretherketone (PEEK), polyetherimide (PEI), and the like.

The crosslinking agent is used for improving the durability of the super hydrophobic surface body, that is, the mechanical strength and the chemical strength, and it is possible to use a compound containing two or more vinyl groups, and 2,4,6,8-tetramethyl (2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane; V4D4), 1,3,5-trimethyl-1,3,5- 1,3,5-trimethyl-1,3,5-trivinyl-cyclotrisiloxane (V3D3), divinylbenzene (DVB), diethyleneglycol divinylether (DEGDVE) (Ethylene glycol dimethacrylate), ethylene glycol dimethacrylate (EGDMA), 1,3-diethenyl-1,1,3,3-tetramethyl-disiloxane (1,3-diethyl -1,1,3,3-tetramethyl-disiloxane (V2D2), and the like.

The chemical strength means a strength to withstand a chemical impact. It is weak in strength to be dissolved by an acid or to react with a specific gas.

1H, 1H, 2H, 2H, 2H-perfluorodecylacrylate (PFDA), perfluoro (1H) But are not limited to, perfluorodecyl methacrylate (PFDMA), dodecafluoroheptyl acrylate, pentafluorophenyl methacrylate, 3,3,4,4,5,5,6,6 , 7,7,8,8,9,9,9-pentadecafluorononyl acrylate (3,3,4,4,5,5,6,6,7,7,8,8,9,9,9 , 9-pentadecafluorononyl acrylate), 2-methyl-3,3,4,4,5,5,6,6,7,7,8,8,9,9,9-pentadecafluorononyl acrylate (2 3,3,4,4,5,5,6,6,7,7,8,8,9,9,9-pentadecafluorononyl acrylate), 3,3,4,4,5,5,6 , 6,7,7,8,8,8-tridecafluorooctyl acrylate (3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl acrylate) , 2-methyl-3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl acrylate (2-methyl-3,3,4,4 , 5, 5, 6, 6,7,7,8,8,8-tridecafluorooctyl acrylate), 3,3,4,4,5,5,6,6,7,7,7-undecafluoroheptyl acrylate (3,3, 4,4,5,5,6,6,7,7,7-undecafluoroheptyl acrylate), 2-methyl-3,3,4,4,5,5,6,6,7,7,7-undeca Fluoroheptyl acrylate (2-methyl-3,3,4,4,5,5,6,6,7,7,7-undecafluoroheptyl acrylate), 3,3,4,4,5,5,6, (3,3,4,4,5,5,6,6,6-nonafluorohexyl acrylate), 2-methyl-3,3,4,4,5,5,6 , 6,6-nonafluorohexyl acrylate (2-methyl-3,3,4,4,5,5,6,6,6-nonafluorohexyl acrylate), 3,3,4,4,5,5, 6,6,7,7,8,8,9,9,10,10,11,11,11-nonadecafluoroundecyl acrylate (3,3,4,4,5,5,6,6 , 7,7,8,8,9,9,10,10,11,11,11-nonadecafluoroundecyl acrylate), 2-methyl-3,3,4,4,5,5,6,6,7,7 , 8,8,9,9,10,10,11,11,11-nonadecafluoroundecyl acrylate (2-methyl-3,3,4,4,5,5,6,6,7, 7,8,8,9,9,10,10,11,11,11-nonadecafluoroundecyl acrylate), 3,3,4,4,5,5,6,6,7,7,8,8,9, 9,10,10,11,11,12,12,12-HENEICO < / RTI > fluorododecyl acrylate (3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12,12-heneicosafluorododecyl acrylate), 2- Methyl-3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12,12-Hanescoflorododde (2-methyl-3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12,12- heneicosafluorododecyl acrylate), 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12,13,13,13- Tricosafluorotridecyl acrylate (3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12,13, 13,13-tricosafluorotridecyl acrylate), 2-methyl-3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,11,11,12, 12,13,13,13-tricosafluorotridecyl acrylate (2-methyl-3,3,4,4,5,5,6,6,7,7,8,8,9,9,10, 10,11,11,12,12,13,13,13-tricosafluorotridecyl acrylate), 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10, 10,11,11,12,12,13,13,14,14,14-pentacosafluorotetradecyl acrylate (3,3,4,4,5,5,6,6,7,7,8 , 8,9,9,10,10,11,11,12,12,13,13,14,14,14-pentacosafluorotetradecyl acrylate), 2-methyl-3,3,4,4,5,5,6 , 6,7,7,8,8,9,9,10,10,11,11,12,12,13,13,14 , 14,14-pentacosafluorotetradecyl acrylate (2-methyl-3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10, 11,12,12,13,13,14,14,14-pentacosafluorotetradecyl acrylate), and the like.

In the present invention, the superhydrophobic surface body means a surface body having a contact angle of the object surface and water exceeding 150 °.

A chemical vapor deposition reactor (iCVD) using an initiator used in the present invention is a device for decomposing an initiator of a gas phase into radicals to cause polymerization of a monomer. As the initiator, peroxide such as tert-butyl peroxide (TBPO) is mainly used, which is a volatile substance having a boiling point of about 110 ° C., and pyrolysis occurs at about 150 ° C. Benzophenone, which decomposes by heat such as tert-butyl peroxide (TBPO) to form radicals, and decomposes by light such as UV to form radicals, may also be used.

The iCVD process does not seem to be much different from the conventional inorganic thin film deposition CVD process because the thin film is deposited by the energy supply of the heated filament heat source or UV. However, the iCVD process is performed at a low filament temperature between 200 ° C. and 350 ° C. And the temperature of the substrate surface on which the polymer thin film is deposited can be kept as low as 10 to 50 ° C. Because of these low surface temperatures, iCVD can be used to coat polymer films on multiple substrates that are susceptible to mechanical and chemical impacts, such as paper or cloth. And since the process is done in vacuum from 50 mTorr to 1000 mTorr, no high vacuum equipment is needed and the amount of monomer and initiator is controlled by the injection valve.

The deposition in the step (a) may be performed for 10 to 60 minutes while maintaining the temperature of the substrate at 25 to 45 ° C and the pressure of the chamber in the reactor at 150 to 250 mTorr. If the temperature of the substrate is less than 25 ° C, the deposition may be foggy. If the temperature of the substrate is more than 45 ° C, the deposition rate may be slowed. If the pressure of the chamber in the reactor is less than 150mTorr or more than 250mTorr There is a problem that the deposition is not performed or the deposition rate is slowed down. And. Since the deposition time is related to the deposition thickness, when the deposition time exceeds 10 to 60 minutes, the deposition thickness becomes thin or thick.

The deposition in the step (b) may be performed for 5 to 60 minutes while maintaining the temperature of the substrate at 25 to 45 ° C and the pressure of the chamber in the reactor at 50 to 200 mTorr. If the temperature of the substrate is less than 25 ° C, the deposition can be foggy. If the temperature of the substrate is more than 45 ° C, the deposition rate is decreased. If the pressure in the chamber is less than 50mTorr or more than 200mTorr There is a problem that the deposition is not performed or the deposition rate is slowed down. And. Since the deposition time is related to the deposition thickness, when the deposition time exceeds 5 to 60 minutes, the deposition thickness becomes thin or thick.

In particular, the deposition of the step (a) or the step (b) may be performed while maintaining the temperature of the substrate at 25 to 35 ° C, preferably 25 to 32 ° C, and more preferably 25 to 30 ° C . Within the temperature range, the surface of the super-hydrophobic surface body changes to a rough structure to create an air pocket, so that the contact angle between the surface of the object and water becomes super-hydrophobic exceeding 150 °, and hysteresis occurs. There is an effect that the phenomenon does not occur.

In another aspect, the present invention relates to a superhydrophobic surface body on which a cross-linking agent is deposited on the upper and lower surfaces of a substrate, and a super-hydrophobic polymer is deposited on the deposited cross-linking agent.

In another preferred embodiment of the present invention, a polymer is deposited on the top and bottom surfaces of a substrate, a 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane polymer, Perfluorodecyl acrylate polymer deposited on 4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane. The present invention relates to a superhydrophobic surface body on which a 1H, 1H, 2H, 2H-perfluorodecyl acrylate polymer is deposited.

The superhydrophobic surface body has a transmittance of 95% or more, preferably 98% or more, shows water repellency, preserves hierarchical nanostructure even after applying mechanical and chemical stress , And the superhydrophobic property that the contact angle of superhydrophobic surface body and water exceeds 150 ° is maintained.

In another aspect, the present invention relates to a method of manufacturing a semiconductor device comprising the steps of: (a) depositing 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane on both sides of a substrate; And (b) on both sides of the substrate on which the 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane has been deposited, 1H, 1H, 2H, 2H-perfluorodecyl (ICVD) using an initiator comprising the step of vapor-depositing an acrylate monomer to produce a superhydrophobic surface body. The present invention also relates to a method for producing a superhydrophobic surface body using a chemical vapor deposition reactor (iCVD).

In one aspect of the present invention, there is provided a method of manufacturing a semiconductor device, comprising the steps of: (a) providing a substrate having a temperature of 25 to 45 DEG C and a chamber pressure of 50 to 200 mTorr, - tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane; And (b) maintaining the temperature of the substrate at 25 to 45 占 폚 and the pressure of the chamber in the reactor at 50 to 200 mTorr while stirring the 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetra Depositing 1H, 1H, 2H, 2H-perfluorodecyl acrylate monomers on both sides of a substrate on which siloxane is deposited for 5 to 60 minutes to prepare a superhydrophobic surface body, (ICVD) to produce a superhydrophobic surface body.

In the present invention, it was confirmed that a superhydrophobic surface body having improved mechanical strength and chemical strength can be produced even when a cross-linking agent and a monomer are deposited on an upper surface of a substrate and then a cross-linking agent and a monomer are sequentially deposited on the lower surface of the substrate.

Accordingly, in another aspect, the present invention provides a method of manufacturing a semiconductor device, comprising: (a) depositing a cross-linking agent on an upper surface of a substrate; (b) depositing a super hydrophobic monomer on a crosslinking agent deposited on an upper surface of the substrate; (c) depositing a crosslinking agent on the lower surface of the substrate; And (d) depositing a super-hydrophobic monomer on a crosslinking agent deposited on the lower surface of the substrate to produce a super-hydrophobic surface body. The method of manufacturing a super-hydrophobic surface body using a chemical vapor deposition reactor (iCVD) ≪ / RTI >

As the substrate, the cross-linking agent and the monomer, the same ones as described above can be used.

The deposition of the step (a) and the step (c) is performed for 10 to 60 minutes while maintaining the temperature of the substrate at 25 to 45 ° C and the pressure of the chamber in the reactor at 150 to 250 mTorr. If the temperature of the substrate is less than 25 ° C, the deposition may be foggy. If the temperature of the substrate is more than 45 ° C, the deposition rate may be slowed. If the pressure of the chamber in the reactor is less than 150mTorr or more than 250mTorr There is a problem that the deposition is not performed or the deposition rate is slowed down. Since the deposition time is related to the deposition thickness, when the deposition time exceeds 10 to 60 minutes, there is a problem that the deposition thickness becomes thin or thick.

The deposition of the step (b) and the step (d) is performed for 5 to 60 minutes while maintaining the temperature of the substrate at 25 to 45 ° C and the pressure of the chamber in the reactor at 50 to 200 mTorr. If the temperature of the substrate is less than 25 ° C, the deposition can be foggy. If the temperature of the substrate is more than 45 ° C, the deposition rate is decreased. If the pressure in the chamber is less than 50mTorr or more than 200mTorr There is a problem that the deposition is not performed or the deposition rate is slowed down. Since the deposition time is related to the deposition thickness, when the deposition time exceeds 5 to 60 minutes, the deposition thickness becomes thin or thick.

In particular, the deposition of (a), (b), (c) or (d) may be performed at a temperature of 25 to 35 ° C, preferably 25 to 32 ° C, 25 to 30 < 0 > C.

Within the temperature range, the surface of the super-hydrophobic surface body changes to a rough structure to create an air pocket, so that the contact angle between the surface of the object and water becomes super-hydrophobic exceeding 150 °, and hysteresis occurs. There is an effect that the phenomenon does not occur.

In another aspect, the present invention provides a method of manufacturing a semiconductor device, comprising: (a) depositing 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane on the top surface of a substrate; (b) 1, 1H, 2H, 2H-perfluorodecyl acrylate (hereinafter referred to as " perfluorodecyl acrylate ") on 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane Depositing a monomer; (c) depositing 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane on the underside of the substrate; And (d) depositing 1H, 1H, 2H, 2H-perfluorodecyl acrylate on 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane deposited on the lower surface of the substrate (ICVD) using an initiator comprising the steps of: (i) depositing a monomethylketone monomethyl ether and a monomethyl ether monomer to produce a superhydrophobic surface material.

According to a preferred embodiment of the present invention, there is provided a method of manufacturing a semiconductor device, comprising the steps of: (a) forming a first electrode on a substrate with a temperature of 25 to 45 DEG C and a chamber pressure of 150 to 250 mTorr, Depositing tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane for 10 to 60 minutes; (b) a step of heating the substrate while keeping the temperature of the substrate at 25 to 45 DEG C and the pressure of the chamber in the reactor at 50 to 200 mTorr, Depositing 1H, 1H, 2H, 2H-perfluorodecyl acrylate monomer onto 8-tetravinylcyclotetrasiloxane for 5 to 60 minutes; (c) While maintaining the temperature of the substrate at 25 to 45 DEG C and the pressure of the chamber in the reactor at 150 to 250 mTorr, a solution of 2,4,6,8-tetravinyl-2,4,6,8-tetravinyl Depositing cyclotetrasiloxane for 10 to 60 minutes; And (d) maintaining the temperature of the substrate at 25 to 45 DEG C and the pressure of the chamber in the reactor at 50 to 200 mTorr, and depositing 2,4,6,8-tetramethyl-2,4,6 , And depositing 1H, 1H, 2H, 2H-perfluorodecyl acrylate monomers on 8-tetravinylcyclotetrasiloxane for 5 to 60 minutes to prepare a superhydrophobic surface body. The chemical vapor deposition reactor (iCVD) to produce a superhydrophobic surface body.

On the other hand, in the present invention, instead of vapor-depositing a crosslinking agent on a substrate and depositing a monomer on the deposited crosslinking agent, a superhydrophobic surface body having improved mechanical strength and chemical strength even when a copolymer of a monomer and a crosslinking agent is deposited on the substrate .

Accordingly, in another aspect, the present invention provides a chemical vapor deposition reactor (iCVD) using an initiator, comprising the steps of depositing a copolymer of a superhydrophobic monomer and a crosslinking agent on the upper and lower surfaces of a substrate, respectively, The present invention relates to a method for producing a superhydrophobic surface body using the above-

The copolymer is a copolymer of a cross-linking agent for enhancing durability and a monomer having a super-hydrophobic property, and is a copolymer of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane and 1H, 1H, 2H, 2H-perfluorodecyl acrylate monomer, a copolymer of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane and perfluorodecyl methacrylate monomer A copolymer of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane and dodecafluoroheptyl acrylate monomer, a copolymer of 2,4,6,8-tetramethyl- A copolymer of 2,4,6,8-tetravinylcyclotetrasiloxane and pentafluorophenyl methacrylate monomer, a copolymer of 1,3,5-trimethyl-1,3,5-trivinylcyclotrisiloxane and 1H, 1H, 2H, 2H-perfluorodecyl acrylate monomer, a copolymer of 1,3,5-trimethyl-1,3,5-trivinylcyclotrisiloxane and perfluorodecyl methacrylate monomer Copolymers of 1,3,5-trimethyl-1,3,5-trivinylcyclotrisiloxane and dodecafluoroheptyl acrylate monomers, copolymers of 1,3,5-trimethyl-1,3,5-tri Copolymers of vinylcyclotrisiloxane and pentafluorophenyl methacrylate monomer, copolymers of divinylbenzene, diethylene glycol divinyl ether and 1H, 1H, 2H, 2H-perfluorodecyl acrylate monomers, divinylbenzene , Copolymers of diethylene glycol divinyl ether and perfluorodecyl methacrylate monomer, copolymers of divinylbenzene, diethylene glycol divinyl ether and dodecafluoroheptyl acrylate monomer, divinylbenzene, diethylene glycol Copolymers of divinyl ether and pentafluorophenyl methacrylate monomers, copolymers of diethylene glycol diacrylate and 1H, 1H, 2H, 2H-perfluorodecyl acrylate monomers, diethylene glycol diacrylate And a perfluorodecyl methacrylate monomer, a copolymer of diethylene glycol diacrylate and dodecafluoroheptyl acrylate monomer, a copolymer of diethylene glycol diacrylate and pentafluorophenyl methacrylate monomer , Copolymers of ethylene glycol dimethacrylate and 1H, 1H, 2H, 2H-perfluorodecyl acrylate monomers, copolymers of ethylene glycol dimethacrylate and perfluorodecyl methacrylate monomers, ethylene glycol dimethacrylate A copolymer of acrylate and dodecafluoroheptyl acrylate monomer, a copolymer of ethylene glycol dimethacrylate and pentafluorophenyl methacrylate monomer, and the like. The polymerization ratio of the copolymer is preferably 40 to 60:60 to 40.

The deposition is performed for 5 to 60 minutes while maintaining the temperature of the substrate at 25 to 45 DEG C and the pressure of the chamber in the reactor at 50 to 200 mTorr. If the temperature of the substrate is less than 25 ° C, the deposition can be foggy. If the temperature of the substrate is more than 45 ° C, the deposition rate is decreased. If the pressure in the chamber is less than 50mTorr or more than 200mTorr There is a problem that the deposition is not performed or the deposition rate is slowed down. Since the deposition time is related to the deposition thickness, when the deposition time exceeds 5 to 60 minutes, the deposition thickness becomes thin or thick.

In particular, the deposition can be performed while maintaining the temperature of the substrate at 25 to 35 캜, preferably 25 to 32 캜, and more preferably 25 to 30 캜.

Within the temperature range, the surface of the super-hydrophobic surface body changes to a rough structure to create an air pocket, so that the contact angle between the surface of the object and water becomes super-hydrophobic exceeding 150 °, and hysteresis occurs. There is an effect that the phenomenon does not occur.

In another aspect, the present invention relates to a superhydrophobic surface body on which a copolymer of a superhydrophobic monomer and a crosslinking agent is deposited on the upper and lower surfaces of a substrate.

A preferred embodiment of the present invention also relates to a process for the preparation of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane and 1H, 1H, 2H, 2H-purple And a superhydrophobic surface body on which a copolymer of ruroodecyl acrylate monomer is deposited.

The superhydrophobic surface body has a transmittance of 95% or more, preferably 98% or more, shows water repellency, preserves hierarchical nanostructure even after applying mechanical and chemical stress , And the superhydrophobic property that the contact angle of superhydrophobic surface body and water exceeds 150 ° is maintained.

According to another aspect of the present invention, there is provided a process for producing 2,4,6,8-tetramethyl-2,4,6-tetramethyl-2,4,6-tetramethyl- , 6,8-tetravinylcyclotetrasiloxane and 1H, 1H, 2H, 2H-perfluorodecyl acrylate monomers for 10 to 60 minutes to prepare a superhydrophobic surface body, And a method for producing a superhydrophobic surface body using a chemical vapor deposition reactor (iCVD).

[Example]

Hereinafter, the present invention will be described in more detail with reference to Examples. It is to be understood by those skilled in the art that these embodiments are only for illustrating the present invention and that the scope of the present invention is not construed as being limited by these embodiments.

Example  One: Superhydrophobic Surface body  Produce

1H, 1H, 2H, 2H-perfluorodecylacrylate (PFDA, Aldrich 97%), which is a monomer, was added to a reservoir of an iCVD reactor (Daeki Hi-Tech Co., 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane (V4D4, < RTI ID = 0.0 > Alfa 97%) were added and both were heated to 70 ° C and the initiator tert-butyl peroxide (TBPO) (Aldrich, 98%) was placed in the initiator bar and kept at room temperature.

First, V4D4 was deposited on the upper surface of a polyester mesh (100% polyester, Puritech PRT-S1091) as a substrate having a size of 8 × 8 cm, and then PFDA was deposited thereon.

When the crosslinking agent V4D4 is deposited, the temperature of the filament in the reactor is maintained at 200 ° C, the substrate temperature in the reactor is kept at 35 ° C, and the pressure of the chamber in the reactor is maintained at 200mTorr while flowing V4D4 and TBPO in the iCVD reactor at a ratio of 1: Minute deposition was carried out to prepare a polyester mesh on which 100 nm thick pV4D4 (poly-V4D4) was deposited.

Then, PFDA was deposited on the top surface of the polyester mesh on which pV4D4 (poly-V4D4) was deposited.

During the PFDA deposition, the PFDA and TBPO were flown into the iCVD reactor at a ratio of 1: 1, while the filament temperature in the reactor was maintained at 200 ° C, the substrate temperature in the reactor was maintained at 40 ° C, and the chamber pressure in the reactor was maintained at 100 mTorr. To deposit a 300 mesh-thick polyester mesh deposited with pPFDA (poly-PFDA).

Next, in the same manner, a superhydrophobic surface body (PFDA_V4D4_LBL) was prepared by depositing V4D4 and PFDA on the bottom surface of the polyester mesh in a laminated structure.

In order to determine the optimal substrate temperature and chamber pressure for deposition of PFDA and V4D4, deposition was performed under different conditions of substrate temperature and chamber pressure, respectively. In the case of PFDA, the substrate temperature was set to 40 ° C. In the case of V4D4, the substrate temperature was set to 35 ° C. In the case of the PFDA, the chamber pressure was maintained at 100mTorr and the chamber pressure was maintained at 100mTorr. The chamber pressure was adjusted to 0 to 400 mTorr, and the results are shown in Tables 1 and 2. The results are shown in Tables 1 and 2.

10 15 20 25 30 35 40 45 50 55 60 PFDA foggy foggy foggy Deposited Deposited Deposited Deposited Deposited Slow deposition rate Slow deposition rate Slow deposition rate V4D4 foggy foggy foggy Deposited Deposited Deposited Deposited Deposited Slow deposition rate Slow deposition rate Slow deposition rate

As shown in Table 1, both PFDA and V4D4 confirmed that the deposition was smooth when the temperature of the substrate was 25 to 45 ° C.

0mTorr 50 mTorr 100 mTorr 150mTorr 200 mTorr 250 mTorr 300 mTorr 350mTorr 400mTorr PFDA No deposition Deposited Deposited Deposited Deposited No deposition No deposition No deposition No deposition V4D4 No deposition No deposition No deposition Deposited Deposited Deposited No deposition No deposition No deposition

As shown in Table 2, when the chamber pressure is 50 to 200 mTorr for PFDA, and when the chamber pressure is 150 to 250 mTorr for V4D4, deposition is smoothly performed.

Example  2: V4D4 - PFDA  Copolymer Superhydrophobic Surface body  Produce

A solution of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane (V4D4) and 1H, 1H, 2H, 2H (V4D4) in an iCVD reactor (Daeki Hi- (Copolymerization ratio: 1: 1) of perfluorodecyl acrylate (PFDA) monomer was heated to 70 ° C and tertiary butyl peroxide (TBPO) (Aldrich, 98% And kept at room temperature.

First, on the upper and lower surfaces of a polyester mesh (100% polyester, Puritech PRT-S1091) as a substrate having a size of 8 x 8 cm, 2,4,6,8-tetramethyl-2,4,6,8-tetravinyl cyclo A copolymer of tetrasiloxane (V4D4) and 1H, 1H, 2H, 2H-perfluorodecyl acrylate (PFDA) monomer was deposited.

When the copolymer of V4D4-PFDA was deposited, the copolymer of V4D4-PFDA and TBPO were flowed in the iCVD reactor at a ratio of 1: 1, the temperature of the filament in the reactor was 200 ° C, the substrate temperature in the reactor was 35 ° C, (PFDA_V4D4_copolymer) having a thickness of 200 nm and a V4D4-PFDA copolymer deposited thereon was prepared by maintaining the pressure at 250 mTorr for 30 minutes.

Example  3: Superhydrophobic Surface body  Produce

1H, 1H, 2H, 2H-perfluorodecylacrylate (PFDA, Aldrich 97%), which is a monomer, was added to a reservoir of an iCVD reactor (Daeki Hi-Tech Co., 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane (V4D4, < RTI ID = 0.0 > Alfa 97%) were added and both were heated to 70 ° C and the initiator tert-butyl peroxide (TBPO) (Aldrich, 98%) was placed in the initiator bar and kept at room temperature.

First, V4D4 was deposited on a Si wafer (Si wafer, LG siltron) of 8 × 8 cm size, and PFDA was deposited thereon.

When the crosslinking agent V4D4 is deposited, the temperature of the filament in the reactor is maintained at 200 ° C, the substrate temperature in the reactor is kept at 35 ° C, and the pressure of the chamber in the reactor is maintained at 200mTorr while flowing V4D4 and TBPO in the iCVD reactor at a ratio of 1: Minute deposition was performed to produce a Si wafer on which 100 nm thick pV4D4 (poly-V4D4) was deposited.

Then, PFDA was deposited on the top surface of the Si wafer on which pV4D4 (poly-V4D4) was deposited.

During the PFDA deposition, the PFDA and TBPO were flown into the iCVD reactor at a ratio of 1: 1, while the filament temperature in the reactor was maintained at 200 ° C, the substrate temperature in the reactor was maintained at 40 ° C, and the chamber pressure in the reactor was maintained at 100 mTorr. To deposit a Si wafer deposited with 300 nm thick pPFDA (poly-PFDA).

Next, in the same manner, a super-hydrophobic surface body (PFDA_V4D4_LBL) was prepared by depositing V4D4 and PFDA on the lower surface of a Si wafer in a laminated structure.

Comparative Example  One: Superhydrophobic Surface body  Produce

1H, 1H, 2H, 2H-perfluorodecylacrylate (PFDA, Aldrich 97%), which is a monomer, was added to a reservoir of an iCVD reactor (Daeki Hi-Tech Co., And the mixture was heated to 70 ° C. and an initiator, tert-butyl peroxide (TBPO) (Aldrich, 98%), was placed in an initiator bottle and kept at room temperature.

First, PFDA was deposited on the upper and lower surfaces of a polyester mesh (100% polyester, Puritech PRT-S1091) as a substrate having a size of 8 × 8 cm.

During the PFDA deposition, the PFDA and TBPO were flown into the iCVD reactor at a ratio of 1: 1, while the filament temperature in the reactor was maintained at 200 ° C, the substrate temperature in the reactor was maintained at 40 ° C, and the chamber pressure in the reactor was maintained at 100 mTorr. (Poly-PFDA) -deposited polyester mesh was deposited to produce a superhydrophobic surface body (PFDA).

Experimental Example  1: Using FT-IR Function machine  Confirm

The intermediate and finished product of the super-hydrophobic surface material prepared in Example 1, Example 2, and Comparative Example 1 were measured with an FT-IR spectrometer (BRUKER) and are shown in FIGS. 2 and 3 . 2, the case of the deposition by pPFDA PFDA monomer, 1100cm ^-1 and 1700cm ^-1 functional group in the vicinity of the position (functional group) is present, but, 1600cm ^-1 vinyl group (vinyl group), near position is missing .

As shown in FIG. 3, it was confirmed that both the copolymer and the laminated structure (LBL) contained both functional groups of PFDA and V4D4.

Experimental Example  2: SEM  Check coating by measurement

The super-hydrophobic surface material prepared in Comparative Example 1 and Example 1 was washed with soapy water, observed with an SEM (Nova 230, FEI company), and photographed and shown in FIG.

As a result, it was found that the superfacial surface (A) deposited only with PFDA had a large surface coating peeling, whereas the superficial hydrophobic surface (PFDA_V4D4_LBL) (B) deposited with a cross- Respectively.

2-1: Annealing  Depending on the treatment SEM  Measure

The changes observed after the annealing treatment of the super-hydrophobic surface material prepared in Comparative Example 1 and Example 1 at 120 ° C for 24 hours were observed.

11 (b), a morphologically significant change was observed when the pPFDA-coated coating was annealed at 120 ° C for 24 hours. A phenomenon that the surface of the superficial body is formed into a very irregularly shaped lump by the dewetting phenomenon mainly occurs. However, when the laminated superhydrophobic surface body was subjected to the annealing treatment at 120 ° C for 24 hours, no significant change occurred as shown in the right photograph of FIG. 11 (b).

From the above results, it can be seen that the strong cohesive force between p (PFDA) and the substrate is generated by the covalent bond formed by the continuous deposition of p (V4D4) intermediate layer and p (PFDA). When the cohesive force between the layers is increased, the stability of the superhydrophobic surface body is improved and the annealing treatment is not changed for 24 hours at 120 ° C.

2-2: According to droplet loading treatment SEM  Measure

(SEM) (Nova 230, FEI company) before and after deposition of the polyhydrophobic polymer on the polyester mesh, and photographed and shown in FIG.

12 (b), optically excellent transparency was exhibited within the range of visible light. The transmittance of the super-hydrophobic polymer layer was measured at over 98% in the wavelength range of 380-780 nm, and no change in color occurred after lamination.

Referring to FIG. 13, it can be confirmed that the pPFDA deposited on the outer surface is well deposited through the EDAX image. (FIG. 13 (a)), a photograph (FIG. 13 (b)) which maps the F element to the same fiber (FIG. 13 . As shown in FIG. 13 (c), pPFDA was well deposited on the outer surface of the fiber to confirm that there was a fluorine element.

2-3: Dependent on deposition conditions SEM  Measure

Blue ink was dripped onto the nonwoven polyester mesh, the super-hydrophobic surface material prepared in Example 1, and the super-hydrophobic surface material which was deposited rugely by controlling the deposition conditions, and then SEM (Nova 230, FEI company) And photographed, and the results are shown in Fig.

The polyester mesh without the deposition was soft, and the polyester mesh was wetted with the blue ink falling (Fig. 14 (a)). However, the super-hydrophobic surface material prepared in Example 1 showed water-repellency to water (Fig. 14 (b)).

When the substrate temperature in the iCVD reactor was lowered from 40 캜 to 30 캜, p (PFDA) crystals of nanometer scale were formed and the surface of the polyester superhydrophobic surface body became uneven (Fig. 14 c)).

In other words, it was confirmed that the surface of the super hydrophobic surface body can be changed into a rugged structure by controlling the parameters of the iCVD process. Such a rugged structure causes an air pocket as shown in FIG. 15 to have a super-hydrophobic property.

2-4: According to washing SEM  Measure

The water droplets were dropped before and after washing the super-hydrophobic surface material prepared in Example 1, observed with an SEM (Nova 230, FEI company), and photographed and shown in FIG. 17 (c), it was confirmed that the hierarchical nanostructure was preserved even after washing.

2-5: Depending on acid and base treatment SEM  Measure

After immersing the superhydrophobic surface material of Example 1 according to the present invention in H ₂ SO ₄ (pH 2, Daejung,> 95%) and KOH (pH 12, Aldrich, 90%) for 24 hours, SEM (Nova 230, FEI company, and photographed as shown in Figs. 18 (d) and 18 (e). It was confirmed that the nanostructure of the layer was preserved even after the acid and base treatment.

Experimental Example  3: XPS  Check durability through measurement

The superficial hydrophobic surface materials prepared in Examples 1 and 2 and Comparative Example 1 were measured by X-ray photoelectron spectroscopy (XPS) (Multilab 2000, Thermo) before and after washing with soapy water, And the results are shown in Fig.

As a result, it was confirmed that the superfine hydrophobic surface body (A) prepared in Example 1 showed almost no change in F1s peak before and after washing with soapy water. That is, it was found that the durability was excellent because there was no change in the fluoro group.

For reference, in Fig. 5, si2p, C1s, O1s and F1s peaks indicate how much each element is present on the surface.

Experimental Example  4: Superhydrophobic Surface Contact angle  Confirm

4-1: According to ultrasonic treatment Superhydrophobic Surface Contact angle  Confirm

Ultrasonic waves were applied to the super-hydrophobic surface materials prepared in Examples 1 and 2 and Comparative Example 1 for 24 hours, and then one drop of distilled water (10 μl) was dropped on the super-hydrophobic surface material. DSA, KRUSS), and photographs thereof are shown in FIG.

As shown in FIG. 6, the superhydrophobic surface body (C) prepared in Example 1, the super hydrophobic surface body (B) prepared in Example 2, and the superhydrophobic surface body (A) prepared in Comparative Example 1 Both ultrasound treatment maintained a superhydrophilic surface.

4-2: According to washing Superhydrophobic Surface Contact angle  Confirm

The superhydrophobic surface bodies prepared in Examples 1 and 2 and Comparative Example 1 were washed (A) by water, soapy water (B) by hand, washed with soapy water for 40 minutes in a washing machine (C) After washing (D), one drop of distilled water (10)) was dropped on the superfacial surface, and the contact angle was measured with a contact angle analyzer (DSA, KRUSS).

As shown in FIG. 7, it was confirmed that the superhydrophobic surface body manufactured in Example 1 retains super-hydrophobicity even when hand-washed with soapy water (B).

4-3: Temperature dependent Superhydrophobic Surface Contact angle  Confirm

The superfine hydrophobic surface bodies prepared in Examples 1 and 2 and Comparative Example 1 were allowed to stand at 16 ° C and 120 ° C for 24 hours, respectively, and one drop of distilled water (10 μl) was dropped on the superfacial surface body. (DSA, KRUSS), and photographs thereof are shown in FIG.

As shown in FIG. 8, it was confirmed that the superhydrophobic surface bodies prepared in Examples 1 and 2 and Comparative Example 1 retained the superhydrophobic surface at 16 ° C and 120 ° C, respectively.

4-4: Solvent treatment Superhydrophobic Surface Contact angle  Confirm

The super-hydrophobic surface materials prepared in Examples 1 and 2 and Comparative Example 1 were immersed in Ethanol, Acetone, Toluene, IPA (isopropyl alcohol) and THF (Tetrahydrofuran) for 48 hours, One drop of distilled water (10 mu l) was dropped and the contact angle was measured with a contact angle analyzer (DSA, KRUSS), and a photograph thereof was shown in Fig.

As shown in FIG. 9, it was confirmed that both the super-hydrophobic surface materials prepared in Examples 1 and 2 and Comparative Example 1 retained the super-hydrophobic surface even when the solvent was treated.

4-5: Chemical and mechanical stress Superhydrophobic Surface Contact angle  Confirm

The ultrafine hydrophobic surface bodies prepared in Example 1 and Comparative Example 1 were subjected to heat treatment (the same as in 4-3), ultrasonic treatment (same as in 4-1), solvent treatment , The contact angle was measured with a contact angle analyzer (DSA, KRUSS), and the change in the contact angle was shown in Figs. 16 (a), 16 (b) and 16 (c).

As shown in Figs. 16 (a) to 16 (c), it was confirmed that both of the super-hydrophobic surface materials produced in Example 1 and Comparative Example 1 retained the super-hydrophobic surface.

4-6: According to acid and base treatment Superhydrophobic Surface Contact angle  Confirm

The superhydrophobic surface body according to Example 1 was treated with H ₂ SO ₄ (pH 2, Daejung,> 95%), KOH (pH 12, Aldrich, 90%) and H ₂ O ₂ (Daejung,> 30% After dipping and drying, a drop (10 μl) of distilled water was dropped on the super-hydrophobic surface body and the contact angle was measured with a contact angle analyzer (DSA, KRUSS) Respectively.

As shown in Figs. 18 (a) to 18 (c), it was confirmed that both of the super-hydrophobic surface materials produced in Example 1 and Comparative Example 1 retained the super-hydrophobic surface.

Experimental Example  5: Superhydrophobic Surface  pollution Oleophobicity  Confirm

FIG. 10 shows a photograph of a drop of pump oil in the polyester mesh used as the substrate and the superhydrophobic surface body prepared in Example 1. FIG.

As shown in FIG. 10, it was confirmed that the pump oil was absorbed in the case of the polyester mesh, whereas the pump oil was not absorbed in the super-hydrophobic surface body prepared in Example 1. [

Experimental Example  6: According to washing Superhydrophobic Surface  Element ratio analysis

Table 1 shows the percentages of elements of carbon, oxygen, silicon, and fluorine by XPS analysis after washing the super-hydrophobic surface material prepared in Example 1 with water, respectively.

element carbon Oxygen silicon Fluorine Before washing 40.46 6.31 0.84 52.39 After washing (50cycles) 45.87 8.07 1.08 44.08

From Table 3, it can be seen that the ratio of fluorine was slightly decreased after 50 washing cycles, and the ratio of Si element was slightly increased. This indicates that the frictional wear of p (PFDA) exposes the surface of p (V4D4).

While the present invention has been particularly shown and described with reference to specific embodiments thereof, those skilled in the art will appreciate that such specific embodiments are merely preferred embodiments and that the scope of the present invention is not limited thereto will be. Accordingly, the actual scope of the present invention will be defined by the appended claims and their equivalents.

Claims (14)

delete delete delete delete delete delete delete delete delete delete A method for producing a superficial hydrophobic surface body of a layered structure using a chemical vapor deposition reactor (iCVD) using an initiator comprising the steps of:
(a) a layer of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane polymer is deposited on both sides of the substrate at 25 to 30 DEG C under a pressure of 150 to 250 mTorr Gt; 10 to < / RTI > 60 minutes; And
(b) On the both surfaces of the substrate on which the polymer layer of the 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane is deposited, 1H, 1H, 2H, 2H-perfluoro Decyl acrylate polymer layer was deposited at 25 to 30 ° C for 5 to 60 minutes while maintaining the pressure of the chamber in the reactor at 50 to 200 mTorr to deposit 2,4,6,8-tetramethyl-2,4 , A 6,8-tetravinylcyclotetrasiloxane polymer layer was deposited on the deposited 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane polymer layer, and 1H, 1H, 2H , A 2H-perfluorodecyl acrylate polymer layer is deposited, and a contact angle of an object surface with water is more than 150 °.
A method for producing a superficial hydrophobic surface body of a layered structure using a chemical vapor deposition reactor (iCVD) using an initiator comprising the steps of:
(a) a layer of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane polymer is deposited on the upper surface of the substrate at 25 to 30 DEG C to maintain the chamber pressure at 150 to 250 mTorr For 10 to 60 minutes ;
(b) 1, 1H, 2H, 2H-perfluorodecyl (2-ethylhexyl) is deposited on the 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane polymer layer deposited on the top surface of the substrate Acrylate polymer layer at 25 to 30 DEG C for 5 to 60 minutes while maintaining the pressure of the chamber in the reactor at 50 to 200 mTorr;
(c) a layer of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane polymer is deposited on the lower surface of the substrate at 25 to 30 DEG C to maintain the chamber pressure at 150 to 250 mTorr ; And
(d) depositing 1H, 1H, 2H, 2H-perfluorodecyl (meth) acrylate on the 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane polymer layer deposited on the lower surface of the substrate Acrylate polymer layer was deposited at 25-30 占 폚 while maintaining the pressure of the chamber in the reactor at 50-200 mTorr to form 2,4,6,8-tetramethyl-2,4,6,8-tetra Vinyl cyclotetrasiloxane polymer layer was deposited on the deposited 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane polymer layer, and 1H, 1H, 2H, 2H-perfluoro A decyl acrylate polymer layer is deposited on the surface of the substrate, and the contact angle of the object surface with water is more than 150 °.
delete delete

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