KR20170064618A - Metal thin plate with excellent corrosion resistance and etching ability and method for manufacturing the same - Google Patents
Metal thin plate with excellent corrosion resistance and etching ability and method for manufacturing the same Download PDFInfo
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- KR20170064618A KR20170064618A KR1020150170024A KR20150170024A KR20170064618A KR 20170064618 A KR20170064618 A KR 20170064618A KR 1020150170024 A KR1020150170024 A KR 1020150170024A KR 20150170024 A KR20150170024 A KR 20150170024A KR 20170064618 A KR20170064618 A KR 20170064618A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/42—Silicides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
- C23C16/0245—Pretreatment of the material to be coated by cleaning or etching by etching with a plasma
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
- C23C16/45536—Use of plasma, radiation or electromagnetic fields
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Abstract
The present invention relates to a metal thin plate having a thickness of 5 to 50 탆 and a coating layer formed on at least one side of the thin metal plate, wherein the coating layer comprises a metal thin plate containing a silicon-containing compound having an amine group, Wherein the coating composition comprises a siloxane precursor having an amine group and is coated with an atmospheric plasma to form a coating layer, the coating composition can replace a conventional chromate treatment technique by providing a method of manufacturing a metal thin plate having excellent corrosion resistance and excellent etchability It is possible to prevent the environmental pollution caused by chromium and to significantly improve the corrosion resistance and the etching property of the metal thin plate.
Description
The present invention relates to a metal thin plate having excellent corrosion resistance and etching property, and a method of manufacturing the same.
Metal foil is mainly applied to OLED lighting and displays, and iron (Fe) and nickel (Ni) alloys are mainly used in consideration of thermal expansion. Though the metal thin plate is usually manufactured by electrolytic casting technology, the metal thin plate produced by electrolytic casting is extremely liable to cause corrosion compared with the rolling material, and rusting occurs even if left in the atmosphere for several days.
Conventionally, in order to impart corrosion resistance to the thin metal plate, a surface treatment method in which a chromate film containing chromium as a main component is coated on the surface of the thin metal plate is generally performed. The main chromate treatment includes an electrolytic chromate and a coating type chromate. Of these electrolytic chromate treatments, a treatment liquid containing hexavalent chromium as a main component and various anions such as sulfuric acid, phosphoric acid, boric acid and halogen is used Thereby processing the metal thin plate. On the other hand, in the coating-type chromate treatment, inorganic colloid and inorganic ions are added to a solution in which a part of hexavalent chromium is reduced in advance in advance, and then the mixture is mixed to prepare a treatment liquid. The metal thin plate is immersed in the treatment liquid, It is a method of spraying on a thin metal plate.
However, due to the toxicity of the hexavalent chromium contained in the chromate treatment liquid, the above-mentioned chromate film-coating surface treatment method requires various measures in the working environment and in the drainage treatment, etc., and recycling and disposal of household electrical appliances and building materials using the surface- In the processing, human health and environment pollution problems are also caused. In addition, when trivalent chromium is applied, a part of trivalent chromium is converted to hexavalent chromium by the surrounding environment such as temperature and microorganisms.
Furthermore, since the chromate film coating surface treatment method forms the thickness of the plating layer to a level of micrometer (占 퐉), there is a limit that the etching property becomes disadvantageous when the chromate treated metal thin plate is processed.
The present invention provides a method of treating a surface of a thin metal plate which can replace the conventional chromate treatment technique.
The present invention also provides a thin metal plate excellent in corrosion resistance and etching property and a method for producing the same.
According to an embodiment of the present invention, there is provided a metal thin plate excellent in corrosion resistance and etching property, comprising a metal thin plate having a thickness of 5 to 50 탆 and a coating layer comprising a silicon compound having an amine group formed on at least one side of the metal thin plate do.
The silica-based compound having an amine group may be at least one selected from the group consisting of a siloxane having an amine group, a siloxane precursor having an amine group, and silicon oxide having an amine group.
The coating layer may further include at least one selected from the group consisting of silicon oxide and amine.
The coating layer may have a thickness of 10 to 500 nm.
The metal thin plate may be formed of at least one selected from the group consisting of Ni, Fe, Cu, Mn, Ti, V, Co, Zn, Cr, 0.0 > (Al) < / RTI > and stainless steel.
According to another embodiment of the present invention, there is provided a method for forming a coating layer, comprising coating a coating composition on at least one side of a metal foil with an atmospheric plasma to form a coating layer, wherein the coating composition comprises a siloxane precursor having an amine group, And provides a method for manufacturing an excellent thin metal plate.
The atmospheric pressure plasma may have a temperature of 100 DEG C or less.
The atmospheric pressure plasma may have an output of 200 to 300 W in the plasma apparatus.
The amine group-containing siloxane precursor may be selected from the group consisting of aminopropyl triethoxysilane, trimethoxysilylpropyl ethylenediamine, trimethoxysilylpropyl allylamine, and trimethoxysilylpropyl butyl Amines (trimethoxysilylpropyl butylamine).
The method may further include pre-treating the thin metal plate with an atmospheric plasma.
And curing the coating layer.
The curing may be at least one selected from the group consisting of near-infrared light (NIR), infrared light (IR), and hot air.
The curing may be carried out at a temperature ranging from 100 to 200 ° C.
The metal thin plate may be formed of at least one selected from the group consisting of Ni, Fe, Cu, Mn, Ti, V, Co, Zn, Cr, 0.0 > (Al) < / RTI > and stainless steel.
The present invention provides a surface treatment method of a thin metal plate which can replace the conventional chromate treatment technique, thereby preventing environmental pollution caused by chromium and greatly improving the corrosion resistance and etching property of the thin metal plate.
Fig. 1 is a photograph of the results obtained after the corrosion resistance evaluation in Examples 1 and 2. Fig.
Fig. 2 is a photograph of the results of corrosion resistance evaluation of Comparative Examples 3 to 5; Fig.
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings. However, the embodiments of the present invention can be modified into various other forms, and the scope of the present invention is not limited to the embodiments described below.
Conventionally, a surface treatment method in which a chromate film containing chromium as a main component is coated is mainly used for imparting corrosion resistance to a thin metal plate. However, toxicity of hexavalent chromium causes human and environmental pollution. Therefore, the inventors of the present invention have conducted research to secure a technique for surface treatment of a metal thin plate that can replace a conventional chromate treatment technique. As a result, they have found that a composition containing a siloxane precursor having an amine group is coated on a metal thin plate surface by an atmospheric pressure plasma It has been recognized that the metal thin plate is excellent in the corrosion resistance and the etching property, leading to the present invention.
According to an embodiment of the present invention, there is provided a thin metal plate comprising a metal thin plate having a thickness of 5 to 50 탆 and a coating layer formed on at least one side of the thin metal plate, wherein the coating layer comprises a silicon- have.
The metal thin plate is mainly manufactured by an electrolytic casting process and has a problem of being extremely corrosive. However, the coating layer containing the silicon-containing compound having an amine group may be formed on the surface of the metal thin plate to impart corrosion resistance. When the corrosion resistance of the thin metal plate is imparted by the conventional chromate treatment method, the corrosion resistance can be imparted by forming the plating layer thickness of 100 nm or more. However, the coating layer containing the silica-based compound having the amine group of the present invention is formed with a thickness of less than 100 nm It is possible to impart excellent corrosion resistance.
Further, when the thin metal plate is surface-treated by the chromate treatment method, when the thickness of the plating layer is controlled to 100 nm or more in order to impart corrosion resistance to the chromate plating layer, there is a problem that the material is deformed and the etching property is poor. However, in the present invention, the coating layer can provide excellent corrosion resistance even if the thickness of the coating layer is controlled to be less than 100 nm, and the material thickness and etching property of the thin metal plate are excellent due to the thin thickness of the coating layer.
Furthermore, the amine group contained in the silicon-containing compound having an amine group may cause a neutralization reaction with an acid used for acid etching. The coating layer is not etched when the coating layer is not dissolved in the acidic etching solution. However, since the alkaline coating layer is formed on the metal thin plate and the neutralization reaction of the alkaline coating layer and the acidic etching solution is performed, The coating layer is melted and thus the etching can be made easier. That is, the metal thin plate of the present invention has an excellent etching property.
The silica-based compound having an amine group may be at least one selected from the group consisting of a siloxane having an amine group, a siloxane precursor having an amine group, and silicon oxide having an amine group. The coating layer may further include at least one selected from the group consisting of silicon oxide and amine, in addition to the silicon-containing compound having an amine group.
It is preferable that the metal thin plate has a thickness of 5 to 50 탆. When the thin metal thin plate is manufactured to a thickness of less than 5 탆, the strength is very weak. Therefore, Which is unsuitable for use as a flexible metal thin plate.
The thickness of the coating layer is preferably 10 to 500 nm, more preferably 50 to 300 nm. If the thickness of the coating layer is less than 10 nm, sufficient corrosion resistance can not be provided. If the thickness is more than 500 nm, etchability may be reduced.
The kind of the metal thin plate is not particularly limited, but may be, for example, silver, nickel, iron, copper, manganese, titanium, vanadium, cobalt, , Zinc (Zn), chromium (Cr), aluminum (Al), and stainless steel.
According to another embodiment of the present invention, there is provided a method of manufacturing a metal foil, which comprises coating a coating composition with atmospheric pressure plasma on at least one side of a metal foil to form a coating layer, wherein the coating composition comprises a siloxane precursor having an amine group desirable.
Before forming the coating layer on the surface of the metal thin plate, the metal thin plate may be pretreated with the atmospheric plasma to impart the activity to the surface of the metal thin plate.
Since the atmospheric pressure plasma is formed at atmospheric pressure, it does not require a high-cost vacuum system as in the case of forming a low-pressure (or vacuum) plasma plasma, Can be improved. Therefore, in the present invention, it is possible to pretreat a thin metal plate after plasma is generated using a microwave under atmospheric pressure.
The pretreatment may be performed in an atmospheric environment. Since the plasma pretreatment is performed in the atmospheric environment, it is possible to remove chemical contaminants which are very efficient in removing organic substances on the metal thin plate surface and can occur on the surface. In addition, the activity of the thin plate surface can be enhanced, so that the adhesion between the thin metal plate and the coating layer to be formed in the subsequent step can be enhanced.
If the output of the plasma apparatus is less than 200 W, plasma generation may be difficult. If the output of the plasma apparatus is more than 300 W, plasma oxidation may occur.
A coating layer may be formed by coating at least one surface of the metal thin plate having the activity by pretreatment with an atmospheric plasma with a coating composition with an atmospheric pressure plasma.
The coating composition may include a siloxane precursor having an amine group and a solvent. The kind of the solvent is not particularly limited as long as it is a volatile substance, but is preferably at least one selected from the group consisting of alcohol, methanol and distilled water.
The method of forming a coating layer using atmospheric plasma may be performed by applying a current to a pair of electrodes opposing each other at a constant interval to generate a DC or AC atmospheric plasma between the electrodes. A coating layer may be formed on the surface of the thin metal plate by passing a thin metal plate together with a composition including a siloxane precursor having an amine group between the two electrodes on which the atmospheric pressure plasma is generated.
The siloxane precursor having the amine group passing between the electrodes in which the atmospheric pressure plasma is generated may undergo the radical polymerization reaction due to the energy of the atmospheric plasma. Therefore, the siloxane precursor having an amine group can generate a silicon-based compound having an amine group due to the radical polymerization reaction, and the coating layer can be formed while the silicon-based compound having the amine group collides against the surface of the metal thin plate.
The silicon-containing compound having an amine group generated by the radical polymerization reaction due to the atmospheric plasma may be at least one selected from the group consisting of a siloxane having an amine group, a siloxane precursor having an amine group, and silicon oxide having an amine group. In addition to the generation of the silicon-containing compound having the amine group, the radical polymerization may include at least one selected from the group consisting of silicon oxide and amine.
The atmospheric pressure plasma preferably has a temperature of 100 ° C or lower, and when the temperature exceeds 100 ° C, thermal deformation is applied to the metal thin plate, which may be a problem due to structural deformation or electrochemical characteristics. The lower limit of the plasma temperature is not particularly limited, but it is preferably carried out at a temperature of from room temperature to 100 ° C for ease of work.
If the output of the plasma apparatus is less than 200 W, plasma generation may be difficult. If the output of the plasma apparatus is more than 300 W, plasma oxidation may occur.
The type of siloxane precursor having an amine group includes, but is not limited to, aminoproyl triethoxysilane, trimethoxysilylpropyl ethylenediamine, trimethoxysilylpropyl allylamine, And trimethoxysilylpropyl butylamine. ≪ Desc / Clms Page number 7 >
After the coating composition is coated on at least one side of the metal thin plate with an atmospheric pressure plasma to form a coating layer, the coating layer can be cured and stabilized.
The curing may be accomplished, for example, by one or more methods selected from the group consisting of near-infrared light (NIR), infrared light (NIR), and hot air, Most preferred.
If the temperature is less than 100 ° C., the coating layer may be uncured to insufficient corrosion resistance. If the temperature is higher than 200 ° C., the metal thin plate may be oxidized or thermally deformed and may be bent have.
The metal thin plate may be formed of at least one selected from the group consisting of Ni, Fe, Cu, Mn, Ti, V, Co, Zn, Cr, And at least one metal or alloy selected from the group consisting of aluminum (Al) and stainless steel.
Hereinafter, the present invention will be described more specifically by way of specific examples. The following examples are provided to aid understanding of the present invention, and the scope of the present invention is not limited thereto.
Example
[Example 1]
A thin plate of iron and nickel alloy having a thickness of 20 占 퐉 was prepared, and the alloy thin plate was activated by pretreatment with atmospheric plasma in an atmospheric atmosphere. 20% by weight of aminopropyltriethoxysilane and 80% by weight of methanol were mixed to prepare a coating composition, and an activated alloy thin plate was passed through the atmospheric pressure plasma equipment together with the coating composition to form a coating layer having a thickness of 30 nm on the thin plate surface / RTI > The atmospheric pressure plasma was formed by a device with a temperature of 100 DEG C and an output of 200W. The coating layer was cured at a temperature of 100 캜 using near infrared light to prepare a stabilized coating layer.
[Example 2]
An alloy thin plate having a coating layer formed thereon was prepared in the same manner as in Example 1, except that a coating layer having a thickness of 100 nm was formed.
[Comparative Example 1]
An alloy thin plate having a coating layer was prepared in the same manner as in Example 1, except that a coating layer was formed using a siloxane precursor not containing an amine group.
[Comparative Example 2]
A coating layer was formed in the same manner as in Example 1, except that a coating layer was formed using a vacuum plasma
[Comparative Example 3]
Anhydrous chromic acid was dissolved in ion-exchanged water to prepare a chromic acid solution having a chromium concentration of 0.6 g / L, and a chromate treatment solution having a pH of 5.7 was prepared using caustic soda. The alloy thin plate was immersed in a chromate treatment solution for 3 seconds, and then the solution was removed to form a coating layer. The alloy thin plate on which the coating layer was formed was heated at a temperature of 70 DEG C for 3 Lt; / RTI >
[Comparative Example 4]
A coating layer was formed in the same manner as in Comparative Example 3, except that the pH of the chromate treatment solution was controlled at 4.5.
[Comparative Example 5]
A coating layer was formed in the same manner as in Comparative Example 3 except that the pH of the chromate treatment solution was controlled at 3.0.
The components contained in the coating layers of Examples 1 to 2 and Comparative Examples 1 to 5 were examined by ICP mass spectrometry and the corrosion resistance and the etching properties of Examples 1 to 2 and Comparative Examples 1 to 5 were evaluated by the evaluation methods described below The results are shown in Table 1. < tb > < TABLE >
≪ Evaluation of corrosion resistance &
The corrosion resistance was evaluated by the occurrence area of the red rust on the surface of the metal foil after 48 hours at a salt pressure of 5% and a spray pressure of 35 to 1 kg / cm 2 .
◎: Not corroded
○: Corrosion area is more than 0% and less than 5%
?: Corrosion area exceeding 5% and not more than 30%
X: corrosion area exceeds 30%
≪ Evaluation of etchability &
In the corrosion resistance evaluation, the coated metal thin plate was immersed in an etching solution (product name: TAK CL-8 made by Adeka Co., Ltd., 20% by mass solution) at 30 캜 for 1 minute to etch the etched surface, Respectively. After measuring the width and depth of the cut section, the etching factor (f) was determined to evaluate the etchability.
◎: etching factor is 1.0 or more
?: Etching factor is 0.6 to 1.0
B: etching factor was 0.3 to 0.6
X: etching factor less than or equal to 0.3
According to the results shown in Table 1, Examples 1 and 2 exhibit excellent effects of both corrosion resistance and etchability. Fig. 1 (a) is a photograph of the result of corrosion-resistance evaluation of Example 1, and Fig. 1 (b) is a photograph of the result of corrosion-resistance evaluation of Example 2. Fig. 1, it was confirmed that the metal thin plates of Examples 1 and 2 were free from corrosion.
On the other hand, since the coating layer of Comparative Example 1 does not contain an amine group, the coating layer of Comparative Example 2 exhibits the effect of heating in the etching property, and the coating layer of Comparative Example 2 does not contain an amine group. And 2, respectively.
In addition, in Comparative Examples 3 to 5, it was confirmed that the corrosion resistance and the etching property exhibited the effect of heating with the chromated metal thin plate. Fig. 2 (a) shows the result after the corrosion resistance evaluation in Comparative Example 3, Fig. 2 (b) shows the results after the corrosion resistance evaluation in Comparative Example 4, and Fig. 2 (c) shows the results after the corrosion resistance evaluation in Comparative Example 5. As shown in Fig. 2, the metal thin plates of Comparative Examples 3 to 5 were found to have corrosion resistance.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, It will be obvious to those of ordinary skill in the art.
Claims (14)
A coating layer formed on at least one side of the thin metal plate and containing a silicon-based compound having an amine group
Wherein the metal foil has excellent corrosion resistance and etching property.
Wherein the silicon-containing compound having an amine group is at least one selected from the group consisting of a siloxane having an amine group, a siloxane precursor having an amine group, and silicon oxide having an amine group, and is excellent in corrosion resistance and etchability.
Wherein the coating layer further comprises at least one selected from the group consisting of silicon oxide and amine.
Wherein the coating layer has a thickness of 10 to 500 nm and is excellent in corrosion resistance and etching property.
The metal thin plate may be formed of at least one selected from the group consisting of Ni, Fe, Cu, Mn, Ti, V, Co, Zn, Cr, And at least one metal or alloy selected from the group consisting of aluminum (Al) and stainless steel.
Wherein the coating composition comprises a siloxane precursor having an amine group.
Wherein the atmospheric pressure plasma has a temperature of 100 DEG C or less and is excellent in corrosion resistance and etching property.
Wherein the atmospheric pressure plasma has an output of 200 to 300 W, and the plasma apparatus has an excellent corrosion resistance and an excellent etching ability.
The amine group-containing siloxane precursor may be selected from the group consisting of aminopropyl triethoxysilane, trimethoxysilylpropyl ethylenediamine, trimethoxysilylpropyl allylamine and trimethoxysilylpropyl butyl (Trimethoxysilylpropyl butylamine). The method according to claim 1,
Further comprising the step of pre-treating the thin metal plate with an atmospheric pressure plasma.
Further comprising the step of curing the coating layer.
Wherein the hardening is at least one selected from the group consisting of near-infrared light (NIR), infrared light (NIR), and hot air.
Wherein the curing is carried out at a temperature ranging from 100 to 200 캜, wherein the curing is excellent in corrosion resistance and etching property.
The metal thin plate may be formed of at least one selected from the group consisting of Ni, Fe, Cu, Mn, Ti, V, Co, Zn, Cr, And at least one metal or alloy selected from the group consisting of aluminum (Al) and stainless steel.
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