KR101766970B1 - Functional Coating Film Manufacturing Method and Functional Coating Film - Google Patents

Functional Coating Film Manufacturing Method and Functional Coating Film Download PDF

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KR101766970B1
KR101766970B1 KR1020150144309A KR20150144309A KR101766970B1 KR 101766970 B1 KR101766970 B1 KR 101766970B1 KR 1020150144309 A KR1020150144309 A KR 1020150144309A KR 20150144309 A KR20150144309 A KR 20150144309A KR 101766970 B1 KR101766970 B1 KR 101766970B1
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South Korea
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electron beam
coating film
functional coating
metal
post
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KR1020150144309A
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Korean (ko)
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KR20170044521A (en
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정채환
윤성민
조은애
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한국생산기술연구원
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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
    • B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
    • B05D1/12—Applying particulate materials
    • 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
    • B05D3/02—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 baking
    • B05D3/0254—After-treatment
    • 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
    • B05D3/145—After-treatment
    • 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
    • B05D3/145—After-treatment
    • B05D3/147—Curing
    • 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
    • B05D7/14—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 to metal, e.g. car bodies
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on 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; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Laminated Bodies (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

The present invention provides a method for manufacturing a functional coating film and a functional coating film having functions such as abrasion resistance and corrosion resistance by irradiating an electron beam for a short time in a post-treatment process of a metal coating film.
As an example, a step of synthesizing a ceramic precursor; Spray coating the ceramic precursor on a metal surface; Drying the surface of the spray coated metal; And a step of post-treating the surface of the coated metal with an electron beam.

Description

Technical Field [0001] The present invention relates to a functional coating film,

The present invention relates to a method for producing a functional coating film and a functional coating film for irradiating an electron beam in a post-treatment process of a metal coating film.

In recent years, materials that have properties that can withstand corrosion, abrasion, etc. in almost all industrial fields, such as aerospace industry, automobile industry, and electronic industry, are required. In order to satisfy the physical properties, a surface treatment technique for forming a coating film with a material having properties such as corrosion resistance and abrasion resistance has been developed.

Ceramics have excellent corrosion resistance and abrasion resistance at high temperatures and are widely used as coating films for metals. However, there is a discrepancy between metal and ceramics lattice, a difference in thermal expansion coefficient at the interface, and so the bonding is not easy. Therefore, post-treatment is required to develop the function of corrosion resistance and abrasion resistance of the ceramic and to strengthen the metal-ceramic bonding.

As a post-treatment method, a method of treating a coating film formed using an electric furnace after a ceramic film is formed on a metal surface is generally used. The treatment using the electric furnace has a merit of being able to treat in a large amount, but it takes a long time to reduce the yield. Therefore, there is a need for a post-processing method that can solve the above problems.

The present invention provides a method for manufacturing a functional coating film and a functional coating film having functions such as abrasion resistance and corrosion resistance by irradiating an electron beam for a short time in a post-treatment process of a metal coating film.

The method for preparing a functional coating film according to the present invention comprises: synthesizing a ceramic precursor; Spray coating the ceramic precursor on a metal surface; Drying the surface of the spray coated metal; And post-treating the surface of the coated metal with an electron beam.

The ceramic precursor may be an inorganic polymer.

The inorganic polymer may be one of Polycarbosilane (PCS), Polymethylsilane (PMS), Polytitanomethylsilane (PTMS), Dimethylaluminum isopropoxide (DMAI) or Trimethylaluminum (TMA).

Further, the ceramic precursor may be spray-coated by a sol-gel method.

Further, when the surface of the coated metal is post-treated with an electron beam, the chamber, which is a space in which the electron beam is irradiated to the metal surface, may be in a vacuum state.

Further, when the surface of the coated metal is post-treated with an electron beam, an argon (Ar) plasma discharge may be used for the electron beam apparatus.

Further, at the argon (Ar) plasma discharge, the flow rate of the argon (Ar) may be 25 (sccm).

Further, when the surface of the coated metal is post-treated with an electron beam, the RF power of the electron beam apparatus may be 200 (W) and the DC voltage may be 1.5 (keV).

Further, when the surface of the coated metal is post-treated with an electron beam, the electron beam may be irradiated for a predetermined time or longer.

The predetermined time may be 5 minutes.

In addition, the functional coating film of the present invention can be produced by any one of the above-mentioned methods for producing a functional coating film.

In addition, the coating film produced by the above-mentioned production method may be a SiO 2 , Al 2 O 3 , TiO 2 or metal-ceramic intermixed bonding material.

The functional coating film production method and the functional coating film of the present invention can irradiate an electron beam in the post treatment process of the functional coating film on the metal surface to shorten the processing time and improve the quality and production yield of the functional coating film as compared with the case of using the electric furnace.

1 is a flowchart illustrating a method of manufacturing a functional coating film according to an embodiment of the present invention.
2 is a cross-sectional view of an electron beam apparatus used in a post-process of a functional coating film according to an embodiment of the present invention.
3A is a graph showing changes in surface temperature of an object according to changes in RF power of an electron beam apparatus used in a post-treatment process of a functional coating film according to an embodiment of the present invention.
FIG. 3B shows a surface temperature change of an object according to a change in DC voltage of an electron beam apparatus used in a post-process of a functional coating film according to an embodiment of the present invention.
FIG. 4A is a photograph of a functional coating film according to an embodiment of the present invention after electron beam irradiation for 15 minutes. FIG.
FIG. 4B is a photograph of the functional coating film according to an embodiment of the present invention when the electron beam is irradiated for 10 minutes in the post-treatment.
FIG. 4C is a photograph of the functional coating film according to another embodiment of the present invention after electron beam irradiation for 5 minutes. FIG.
FIG. 4D is a photograph of an electron beam irradiated for 5 minutes during the post-treatment of the functional coating film on the metal surface according to another embodiment of the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.

The embodiments of the present invention are described in order to more fully explain the present invention to those skilled in the art, and the following embodiments may be modified into various other forms, It is not limited to the embodiment. Rather, these embodiments are provided so that this disclosure will be more faithful and complete, and will fully convey the scope of the invention to those skilled in the art.

In the following drawings, thickness and size of each layer are exaggerated for convenience and clarity of description, and the same reference numerals denote the same elements in the drawings. As used herein, the term "and / or" includes any and all combinations of one or more of the listed items. In the present specification, the term " connected "means not only the case where the A member and the B member are directly connected but also the case where the C member is interposed between the A member and the B member and the A member and the B member are indirectly connected do.

The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the singular forms "a," "an," and "the" include singular forms unless the context clearly dictates otherwise. Also, " comprise, " and / or "comprising, " when used in this specification, are intended to be interchangeable with the said forms, numbers, steps, operations, elements, elements and / And does not preclude the presence or addition of one or more other features, integers, operations, elements, elements, and / or groups.

Although the terms first, second, etc. are used herein to describe various elements, components, regions, layers and / or portions, these members, components, regions, layers and / It is obvious that no. These terms are only used to distinguish one member, component, region, layer or section from another region, layer or section. Thus, a first member, component, region, layer or section described below may refer to a second member, component, region, layer or section without departing from the teachings of the present invention.

1 is a flowchart illustrating a method of manufacturing a functional coating film according to an embodiment of the present invention. Hereinafter, each step of FIG. 1 will be described.

Referring to FIG. 1, a method of fabricating a functional coating film according to an embodiment of the present invention includes synthesizing a ceramic precursor (S1).

Ceramics refers to a compound composed of a combination of a metallic element and a non-metallic element such as oxide, nitride, carbide and the like whose main material is an inorganic material. The ceramic can be produced by pyrolyzing an inorganic polymer which is a precursor. Since the inorganic polymer has solubility and meltability, it is easy to control the viscosity and has good wettability, so that it can be mixed at a molecular level and can be used for coating. The inorganic polymer forming the ceramic coating layer may be selected from the group consisting of Polycarbosilane (PCS), Polymethylsilane (PMS), Polytitanomethylsilane (PTMS), Polyvinylsilane (PVS), Polyborazine (PBN), Aminopropyltriethoxysilane (APTES), Aminopropyltrimethoxysilane (MPTES), 3-mercaptopropyltrimethoxysilane (MPTMS), Tetraethyl Orthosilicate (TEOS), TMOS (Tetramethyl Orthosilicate) and TPOS (Tetrapropyl Orthosilicate), and aluminum polymer compounds such as dimethylaluminum isopropoxide (DMAI), trimethylaluminum (TMA), aluminum nitrate nonahydrate, aluminum isopropoxide, and aluminum sec butoxide. Titanium isopropoxide and tetraethylorthosilicate may be used as the titanium polymer composite. The magnesium polymer composite may include at least one of gnesium nitrate, magnesium acetate tetrahydrate , And magnesium methoxide, and zinc dust Zinc nitrate, and Zinc acetate. The zirconia polymer composite may be at least one of zirconium oxynitrate hydrate, zirconium nitrate oxide dihydrate, and zirconium npropoxide. However, the present invention is not limited thereto.

The inorganic polymer is produced by mixing the reactants at a predetermined ratio, and can be mass-produced within 30 minutes.

The inorganic polymer is spray-coated by a sol-gel method (S2). The sol-gel method is a technique for producing a thin film by dissolving the inorganic polymer in a dispersion medium to prepare a sol, applying the sol to the surface of the electrodeposition to form a thin film, Method. The inorganic polymer is dissolved in the dispersion medium to form a colloidal coating solution.

The dispersion medium is methanol (CH 3 OH), ethanol (CH 3 CH 2 OH), propanol (CH 3 CH 2 CH 2 OH ), butanol (CH 3 CH 2 CH 2 CH 2 OH), acetone (C 3 H 6 O ), Toluene (C 6 H 5 CH 3 ), ddethylformamide, xylene, distilled water (H 2 O), hydrochloric acid (HCl) It is not.

The sol-gel method is generally capable of low-temperature synthesis, and even a multicomponent material can be made homogeneous. The coating solution in which the inorganic compound is dissolved may be sprayed onto the surface of the metal to be coated with the spray. In this case, electrostatic coating or the like may be used to increase the coating efficiency. The electrostatic coating allows electric charge to be applied to the coating liquid before spraying the coating liquid, and the coated body can be uniformly coated by being grounded or reversely charged.

The surface of the coated metal is dried (S3). When the inorganic polymer is dissolved in the dispersion medium, hydrolysis and condensation polymerization are performed, so that an organic matter exists in the coating solution. Therefore, the coating liquid is dried to evaporate the organic material.

The surface of the coated metal is post-treated with an e-beam (S4). The electron beam can generate a coating film by heat-treating the dried metal surface coated with the coating solution with an electron beam. Ceramics and metals have many differences in properties such as lattice structure, bond type, and thermal expansion coefficient, which makes the bonding difficult. Therefore, the surface is heat-treated with the electron beam to strengthen the bonding between the metal and the ceramic. In addition, the heat treatment by the electron beam causes the inorganic polymer to transfer to the ceramic system, thereby exhibiting the functions of ceramics such as abrasion resistance and corrosion resistance.

The coating film formed by the post-treatment may be any one selected from the group consisting of SiO 2 , Al 2 O 3 , TiO 2, MgO, ZnO, and ZrO 2 , but is not limited thereto.

In the case of using an electric furnace, the post-treatment takes 60 to 120 minutes depending on the material, and the heat treatment by the electron beam can be performed within 15 minutes. In addition, when an electric furnace is used, products to be dried can be collected and processed at one time, but pin holes, voids, and the like may be defective in the coating film. However, the electron beam apparatus 100 can reduce the defective rate by applying energy in one direction to the electric furnace, which is an omni-directional energy supplying method.

2 is a cross-sectional view of an electron beam apparatus used in a post-process of a functional coating film according to an embodiment of the present invention. Hereinafter, the electron beam apparatus will be described with reference to the step of post-processing (S4) the surface of the coated metal with an electron beam (e-beam).

2, the electron beam apparatus 100 includes an electron beam generating apparatus 110, a chamber 120, and an object 130.

The electron beam generating apparatus 110 is an electron gun for generating an electron beam, and the electron gun includes a cathode electrode, an anode electrode, a grid lens, RF bias, and DC bias. An RF bias is electrically connected to the cathode electrode and the anode electrode. That is, a constant voltage of RF bias is applied to the cathode electrode, and a negative voltage of RF bias is applied to the anode electrode. Argon (Ar) or the like is plasma discharged by the voltage applied to the cathode electrode and the anode electrode, and electrons are extracted, and the extracted electrons generate an electron beam through the cathode electrode. Also, a DC bias is electrically connected to the grid lens. A magnetic field is formed in the grid lens to focus the electron beam.

The chamber 120 is provided with a space for accommodating the object therein and the electron beam generator 110 is installed in the chamber 120 so that the generated electron beam is vertically irradiated onto the object 130 . The chamber 120 is grounded, and the pressure inside the chamber 120 is adjustable. The electron beam generated in the electron beam generating apparatus 110 is irradiated inside the chamber 120.

The object 130 is accommodated in the chamber 120, and the accommodated object 130 is irradiated with an electron beam. The object 130 may be a metal coated on the surface of the coating liquid. Therefore, the electron beam generated in the electron beam generating apparatus 110 can be irradiated to the metal coated on the surface of the coating solution to be post-treated.

The electron beam apparatus 100 may adjust the electron beam energy by adjusting the RF power and the DC voltage, and may adjust the pressure inside the chamber 120 to be vacuum.

3A is a graph showing changes in surface temperature of an object according to changes in RF power of an electron beam apparatus used in a post-treatment process of a functional coating film according to an embodiment of the present invention. FIG. 3B shows a surface temperature change of an object according to a change in DC voltage of an electron beam apparatus used in a post-process of a functional coating film according to an embodiment of the present invention.

3A, when the DC voltage of the electron beam generating apparatus 110 of the electron beam apparatus 100 is fixed at 3 (keV) and the RF power is changed to 100 to 300 (W), the electron beam is irradiated Surface temperature.

3B, when the RF power of the electron beam generating apparatus 110 of the electron beam apparatus 100 is fixed at 200 (W) and the DC voltage is changed in the range of 1 to 5 (keV), the electron beam irradiation Lt; / RTI >

3A and 3B, as the energy of the electron beam increases, the temperature of the surface irradiated with the electron beam increases. Therefore, the RF power and the DC voltage can be adjusted to adjust the temperature of the metal surface necessary for the post-treatment.

FIG. 4A is a photograph of a functional coating film according to an embodiment of the present invention after electron beam irradiation for 15 minutes. FIG. FIG. 4B is a photograph of the functional coating film according to an embodiment of the present invention when the electron beam is irradiated for 10 minutes in the post-treatment. FIG. 4C is a photograph of the functional coating film according to another embodiment of the present invention after electron beam irradiation for 5 minutes. FIG. FIG. 4D is a photograph of an electron beam irradiated for 5 minutes during the post-treatment of the functional coating film on the metal surface according to another embodiment of the present invention.

The flow rate of argon (Ar) was set to 25 (sccm), and the RF power and the DC voltage were set to 200 (W) and 1.5 (keV), respectively. However, the irradiation time of the electron beam coating solution coated surface was changed to 15 minutes, 10 minutes, and 5 minutes, respectively.

Referring to FIG. 4A, when a coating film on the surface of a material was irradiated with an electron beam under the above conditions for 15 minutes, a functional coating film having properties such as abrasion resistance and corrosion resistance was formed. Referring to FIG. 4B, when a coating film on the surface of the material was irradiated with an electron beam under the above conditions for 10 minutes, a functional coating film having properties such as abrasion resistance and corrosion resistance was formed. Referring to FIG. 4C, when a coating film on the surface of the material was irradiated with an electron beam under the above conditions for 5 minutes, a functional coating film having properties such as abrasion resistance and corrosion resistance was formed. Therefore, when the electron beam is irradiated for a predetermined time or longer, the functional coating film can be formed on the surface of the material.

Referring to FIG. 4D, when a coating film of a metal surface was irradiated with an electron beam under the above conditions for 5 minutes, a functional coating film having properties such as abrasion resistance and corrosion resistance was formed. Therefore, if the electron beam is irradiated for a predetermined time or longer, the functional coating film may be formed on the metal surface.

On the other hand, if the pressure inside the chamber 120 is high, the coating layer may not be constant due to colloidal particle aggregation of the coating liquid. Therefore, it is most preferable to make the inside of the chamber 120 a vacuum state.

Therefore, it is possible to shorten the processing time and improve the quality and production yield of the functional coating film by irradiating the electron beam in the post-treatment process of the functional coating film on the metal surface, as compared with the case using the electric furnace.

As described above, the present invention is not limited to the above-described embodiments, but may be applied to other methods, such as a method of manufacturing a functional coating film according to the present invention, It will be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.

100; Electron beam apparatus 110; Electron beam generating device
120; Chamber 130; quid pro quo

Claims (12)

Synthesizing a ceramic precursor;
Gel is prepared by dissolving the ceramic precursor in a dispersion medium to prepare a sol, which is a colloid-like coating solution, and applying the sol to a metal surface to form a thin film, followed by sol- ) Spray coating a metal surface by a method;
Drying and pre-treating the surface of the spray-coated metal; And
Treating the surface of the coated metal with an electron beam for 5 to 15 minutes in a chamber in which the electron beam is irradiated to the metal surface in a vacuum state to strengthen the bonding of the metal and the ceramic,
(Ar) plasma discharge, the flow rate of the argon (Ar) is 25 (sccm) at the time of the argon (Ar) plasma discharge, and the electron beam Wherein the apparatus has an RF power of 200 (W) and a DC voltage of 1.5 (keV). The method according to claim 1,
Wherein the ceramic precursor is an inorganic polymer. 3. The method of claim 2,
Wherein the inorganic polymer is one of Polycarbosilane (PCS), Polymethylsilane (PMS), Polytitanomethylsilane (PTMS), Dimethylaluminum isopropoxide (DMAI) or Trimethylaluminum (TMA). delete delete delete delete delete delete delete A functional coating film produced by the manufacturing method of any one of claims 1, 2, and 3. 12. The method of claim 11,
Wherein the coating film formed by the manufacturing method is a SiO 2 , Al 2 O 3 , TiO 2 or metal-ceramic hetero-bonding material.
KR1020150144309A 2015-10-15 2015-10-15 Functional Coating Film Manufacturing Method and Functional Coating Film KR101766970B1 (en)

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Publication number Priority date Publication date Assignee Title
JP2007254890A (en) * 2006-03-22 2007-10-04 General Electric Co <Ge> Method of forming strain-proof coating by sol-gel method
KR100824274B1 (en) * 2006-11-17 2008-04-24 주식회사 티씨케이 Metal coated with ceramic and manufacturing method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007254890A (en) * 2006-03-22 2007-10-04 General Electric Co <Ge> Method of forming strain-proof coating by sol-gel method
KR100824274B1 (en) * 2006-11-17 2008-04-24 주식회사 티씨케이 Metal coated with ceramic and manufacturing method thereof
JP2008126227A (en) 2006-11-17 2008-06-05 Tokai Carbon Korea Co Ltd Metal coated with ceramic on the surface, and its manufacturing method

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