Silicon-coated iron for oxidation prevention, silicon-coated nickel for oxidation prevention, and their manufacturing method
A silicon-coated anti-oxidation method forms silicon-oxygen-iron or silicon-oxygen-nickel composite layers through deposition, addressing the limitations of existing oxidation prevention methods by providing efficient, economical, and high-temperature-resistant coatings for iron and nickel.
Patent Information
- Application Number
- JP2024563662
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2022-04-28
- Filing Date
- 2023-04-28
- Publication Date
- 2026-01-27
AI Technical Summary
Existing methods for preventing metal oxidation, particularly at high temperatures, are limited in their effectiveness and efficiency, and there is a need for a simpler and more economical process that maintains the metal's electrical properties.
A silicon-coated anti-oxidation method is developed by forming a silicon-oxygen-iron or silicon-oxygen-nickel composite layer through silicon deposition, which is performed in a single sputtering step in an argon atmosphere at room temperature to 350°C for 1 to 5 minutes.
The method provides oxidation-resistant iron and nickel coatings that maintain electrical properties, are economically valuable, and can be used semi-permanently at room temperature, with significantly increased resistance to oxidation even at high temperatures.
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Abstract
Description
[Technical Field]
[0001] The present invention relates to silicon-coated anti-oxidation iron and silicon-coated anti-oxidation nickel, and methods for manufacturing the same. More particularly, the present invention relates to anti-oxidation iron including a silicon (Si)-coated surface that has oxidation resistance while maintaining electrical properties by forming a protective film of a silicon (Si)-oxygen (O)-iron (Fe) composite layer by depositing silicon (Si), and anti-oxidation nickel including a silicon (Si)-coated surface that has oxidation resistance while maintaining electrical properties by depositing silicon (Si) and forming a protective film of a silicon (Si)-oxygen (O)-nickel (Ni) composite layer, and methods for manufacturing the same. [Background technology]
[0002] Generally, metal materials are oxidized through interaction with the surrounding environment, causing corrosion and reducing the durability of the metal itself. Conventional methods for preventing corrosion of metals include a method of adding other elements to the metal itself to produce a chemically stable alloy, and a method of treating the metal surface through coating, etc.
[0003] The surface coating method has the advantage that the coating material can be selected and used depending on the metal properties, application, and surrounding environment, and that corrosion resistance can be improved, but has the disadvantage that use at high temperatures is limited.
[0004] Therefore, in order to solve the above problems, there is a need for a metal surface coating method that can simplify the process and solve the problem of oxidation. Summary of the Invention [Problem to be solved by the invention]
[0005] The present invention has been devised to solve the above-mentioned problems, and an object of the present invention is to provide a method for forming an Si-O-Fe protective layer by Si deposition to prevent oxidation and to produce an anti-oxidation iron thin film that is stable against oxidation even at high temperatures.
[0006] The present invention has been devised to solve the above-mentioned problems, and an object of the present invention is to provide a method for forming an oxidation-resistant nickel thin film by forming a Si-O-Ni protective layer by Si deposition, which prevents oxidation and is stable against oxidation even at high temperatures.
[0007] The technical problems that the invention aims to solve are not limited to the technical problems mentioned above, and other technical problems not mentioned will be clearly understood by those skilled in the art to which the invention pertains from the following description. [Means for solving the problem]
[0008] The present invention relates to silicon-coated iron for oxidation prevention, in which silicon (Si) is vapor-deposited to form a silicon (Si)-oxygen (O)-iron (Fe) mixed layer.
[0009] The silicon-coated iron is characterized by comprising an iron layer 10, an iron oxide (Fe3O4) layer 20 formed on the iron layer 10, a SiFeX layer 30 formed on the iron oxide layer 20 by mixing silicon (Si), oxygen (O), and iron (Fe), and a silicon (Si)-oxygen (O) mixed layer 40 formed on the SiFeX layer 30.
[0010] The iron oxide (Fe3O4) layer 20 is characterized by having a thickness of 3 to 7 nm.
[0011] The SiFeX layer 30, which is a mixture of silicon (Si), oxygen (O), and iron (Fe), is characterized by having a thickness of 0.8 to 1.2 nm.
[0012] The silicon (Si)-oxygen (O) mixed layer 40 is characterized by having a thickness of 5 to 30 nm.
[0013] The present invention relates to a method for producing silicon-coated iron for oxidation prevention, in which silicon (Si) is deposited on iron (Fe) in a single sputtering step.
[0014] The sputtering is performed in an argon atmosphere.
[0015] The sputtering is performed at room temperature to 350° C. for 1 to 5 minutes.
[0016] The present invention relates to a silicon-coated anti-oxidation nickel, in which silicon (Si) is vapor-deposited to form a SiNiX layer 200, which is a silicon (Si)-oxygen (O)-nickel (Ni) mixed layer.
[0017] The silicon-coated nickel is characterized by comprising a nickel layer 100, a SiNiX layer 200 formed on the nickel layer 100 by mixing silicon (Si)-oxygen (O)-nickel (Ni), a first silicon (Si)-oxygen (O) mixed layer 300 formed on the SiNiX layer 200, and a second silicon (Si)-oxygen (O) mixed layer 400 formed on the first silicon (Si)-oxygen (O) mixed layer 300.
[0018] The SiNiX layer 200 is characterized by having a thickness of 0.8 to 1.2 nm.
[0019] The silicon (Si)-oxygen (O) mixed layer including the first silicon (Si)-oxygen (O) mixed layer 300 and the second silicon (Si)-oxygen (O) mixed layer 400 is characterized in that it has a thickness of 5 to 30 nm.
[0020] The present invention relates to a method for producing silicon-coated nickel for oxidation prevention, in which silicon (Si) is deposited on nickel (Ni) in a single sputtering step.
[0021] The sputtering is performed in an argon atmosphere.
[0022] The sputtering is performed at room temperature to 350° C. for 1 to 5 minutes. [Effects of the Invention]
[0023] By solving the above problems, the present invention can provide iron for oxidation prevention, which is easily produced by simply depositing silicon (Si), and therefore the process is simple and the production efficiency is high, and since iron (Fe) and silicon (Si) are used, it is possible to provide iron for oxidation prevention, which is economically valuable.
[0024] In addition, the present invention provides iron (Fe) that is resistant to oxidation while maintaining electrical properties by forming a silicon (Si)-oxygen (O)-iron (Fe) protective film by depositing silicon (Si), and a manufacturing method thereof.
[0025] Furthermore, the present invention can provide an antioxidant iron product that can be produced by a very simple and inexpensive method and that can be used semi-permanently at room temperature.
[0026] Furthermore, the present invention can provide anti-oxidation iron with significantly increased oxidation resistance at high temperatures.
[0027] Furthermore, the present invention produces nickel, which is susceptible to oxidation, by simply depositing silicon (Si), which simplifies the process and increases production efficiency. Furthermore, the use of nickel (Ni) and silicon (Si) makes it possible to provide economically valuable anti-oxidation nickel.
[0028] In addition, the present invention provides nickel (Ni) that is resistant to oxidation while maintaining electrical properties by forming a silicon (Si)-oxygen (O)-nickel (Ni) protective film through silicon (Si) deposition, and a manufacturing method thereof.
[0029] Furthermore, the present invention can provide nickel that can be produced by a very simple and inexpensive method and that can be used semi-permanently at room temperature.
[0030] The present invention also provides anti-oxidant nickel with significantly increased oxidation resistance at high temperatures.
[0031] The effects of the present invention are not limited to those mentioned above, and other effects not mentioned will be clearly understood by those skilled in the art from the description of the claims. [Brief explanation of the drawings]
[0032] [Figure 1] 1 is a photograph of a pure iron plate and a silicon (Si) coated iron plate according to the present invention before and after heat treatment. [Figure 2] 1 is a graph showing the results of XRD measurements of a pure iron plate and a silicon-coated iron plate before and after heat treatment according to the present invention. [Figure 3] 3 is a photograph showing the results of SEM measurement of a pure iron plate and a silicon-coated iron plate according to the present invention before and after heat treatment. [Figure 4] 1A is a photograph and a graph showing the results of a cross-sectional measurement by TEM of a silicon-coated iron plate according to the present invention, and (b) and (c) are photographs and a graph showing the results of a component analysis by TEM of the sample surface. [Figure 5] 1 is a graph showing the results of measuring the sheet resistance of a pure iron plate and a silicon-coated iron plate before and after heat treatment according to the present invention. [Figure 6] 1A and 1B are photographs showing the predicted distribution of O (red) and Si (blue) on a thin Fe (gold) film of a silicon-coated iron plate according to the present invention, in which (a) is a side view and (b) is a plan view. [Figure 7] 1 is a graph showing predicted ΔE and atomic distribution based on penetration depth for pure iron and silicon coated iron plates according to the present invention. [Figure 8] 1 is a photograph of a pure nickel plate and a silicon (Si) coated nickel plate according to the present invention before and after heat treatment. [Figure 9] 1 is a graph showing the results of XRD measurements of a pure nickel plate and a silicon-coated nickel plate according to the present invention before and after heat treatment. [Figure 10] 3 is a photograph showing the results of SEM measurement of a pure nickel plate and a silicon-coated nickel plate according to the present invention before and after heat treatment. [Figure 11] 1A is a photograph and a graph showing the results of cross-sectional measurement by TEM of a silicon-coated nickel plate according to the present invention, and (b) and (c) are photographs and a graph showing the results of component analysis by TEM of the sample surface. [Figure 12] 1 is a graph showing the results of measuring the sheet resistance of a pure nickel plate and a silicon-coated nickel plate according to the present invention before and after heat treatment. [Figure 13] 1A and 1B are photographs showing the predicted distribution of O (red) and Si (gray) on a thin Ni (green) film of a silicon-coated nickel plate according to the present invention, in which (a) is a side view and (b) is a plan view. [Figure 14] 1 is a graph showing predicted ΔE and atomic distribution based on penetration depth for pure nickel plates and silicon coated nickel plates according to the present invention. DETAILED DESCRIPTION OF THE INVENTION
[0033] The terms used in this specification are generally used and widely used in consideration of the functions of the present invention, but these may change depending on the intentions of those skilled in the art, precedents, the emergence of new technologies, etc. In addition, in certain cases, the applicant may arbitrarily select terms, and in such cases, the meanings thereof will be described in detail in the description of the invention. Therefore, the terms used in this specification should be defined based on the meanings of the terms and the overall content of the present invention, rather than simply by their names.
[0034] Unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by a person of ordinary skill in the art to which this invention pertains. Terms as defined in commonly used dictionaries should be interpreted to have a meaning consistent with the meaning they have in the context of the relevant art, and should not be interpreted in an idealized or overly formal sense unless expressly defined in this application.
[0035] Numerical ranges are inclusive of the numerical values defined in the range. Every maximum numerical limitation given throughout this specification should be understood to include every lower numerical limitation, as if such lower numerical limitations were expressly written herein. Every minimum numerical limitation given throughout this specification should include every higher numerical limitation, as if such higher numerical limitations were expressly written herein. Every numerical range given throughout this specification should include every narrower numerical range that falls within such broader numerical range, as if such narrower numerical ranges were all expressly written herein.
[0036] Silicon-coated iron for oxidation protection
[0037] The present invention relates to silicon-coated iron for oxidation prevention, and relates to iron for oxidation prevention in which silicon (Si)-oxygen (O)-iron (Fe) mixed layer is formed by vapor deposition of silicon.
[0038] The anti-oxidation iron having the mixed layer formed thereon may be resistant to oxidation while maintaining its electrical properties.
[0039] The mixed layer may be formed to prevent further oxidation of the iron oxide layer and exhibit oxidation resistance at high temperatures. The silicon may bond with the oxygen on the surface of the iron to fix it on the surface of the iron, and the most basic structure may be as shown in Figure 6. As shown in the side view of Figure 6(a) and the plan view of Figure 6(b), once the oxygen covers the surface of the iron and is fixed by the silicon, other oxygen cannot enter the interior of the iron, thereby exhibiting oxidation resistance.
[0040] In the present invention, the silicon-coated iron may have an electrical resistance between that of iron on which silicon (Si) is not deposited and that of gold (Au).
[0041] In the present invention, the silicon-coated iron may be in the form of a polycrystalline thin film, foil, or bulk.
[0042] In the present invention, when the silicon-coated iron is in the form of a polycrystalline thin film, foil, or lump, it may be one that is resistant to oxidation even when heated at 200 to 400° C. for 20 to 40 minutes. In the case of the polycrystalline thin film, foil, or lump, it may be one that is resistant to oxidation and does not show any visible changes in color or in the results of XRD or SEM measurement even when the heat treatment is carried out as described above.
[0043] The present invention relates to an anti-oxidation iron coated with silicon, in which a SiFeX layer, which is a silicon (Si)-oxygen (O)-iron (Fe) mixed layer, is formed by depositing silicon.
[0044] The SiFeX-coated iron for oxidation prevention may be resistant to oxidation while maintaining its electrical and magnetic properties.
[0045] The SiFeX layer may be formed to prevent further oxidation of the iron oxide layer and exhibit oxidation resistance at high temperatures. The silicon may bond with the oxygen on the surface of the iron to fix it on the surface of the iron, and the most basic structure may be configured as shown in Figure 6. As shown in the side view of Figure 6(a) and the plan view of Figure 6(b), once the oxygen covers the surface of the iron and is fixed by the silicon, other oxygen cannot enter the interior of the iron, thereby exhibiting oxidation resistance.
[0046] In the present invention, the silicon-coated iron may have the same electrical resistance as iron on which silicon (Si) is not deposited.
[0047] In the present invention, the silicon-coated iron may be in the form of a thin film, foil, or block.
[0048] In the present invention, when the silicon-coated iron is in the form of a thin film, foil, or lump, it may be one that is prevented from oxidizing even when heated at 200 to 350° C. for 20 to 40 minutes. In the case of the thin film, foil, or lump, it may be one that is prevented from oxidizing and does not show any visible changes in color or in the results of XRD or SEM measurement even when the heat treatment is carried out as described above.
[0049] In the present invention, the silicon-coated iron has a surface resistance of 9.2 × 10 -4 ~9.6×10 -4 The silicon-coated iron may have a sheet resistance similar to that of iron that is not coated with silicon, and the sheet resistance may not show a rapid increase even after heat treatment.
[0050] In the present invention, the silicon-coated iron may be composed of an iron layer 10, an iron oxide (Fe3O4) layer 20 formed on the iron layer 10, a SiFeX layer 30 formed on the iron oxide layer 20 by mixing silicon (Si), oxygen (O), and iron (Fe), and a silicon (Si)-oxygen (O) mixed layer 40 formed on the SiFeX layer 30.
[0051] In the present invention, the thickness of the iron oxide (Fe3O4) layer 20 may be 3 to 7 nm, and preferably 3 to 5 nm. The iron oxide layer may be formed so thin that it has almost no effect on the corrosion resistance of iron.
[0052] In the present invention, the SiFeX layer 30 made of a mixture of silicon (Si), oxygen (O), and iron (Fe) may have a thickness of 0.8 to 1.2 nm.
[0053] In the present invention, the silicon (Si)-oxygen (O) mixed layer 40 may have a thickness of 5 to 30 nm, preferably 8 to 20 nm.
[0054] Manufacturing method of silicon-coated iron for oxidation prevention
[0055] The present invention relates to a method for producing silicon-coated iron for oxidation prevention.
[0056] The silicon-coated iron for oxidation prevention of the present invention relates to iron for oxidation prevention in which a SiFeX layer, which is a silicon (Si)-oxygen (O)-iron (Fe) mixed layer, is formed by depositing silicon.
[0057] The oxidation-resistant iron on which the SiFeX layer is formed may be resistant to oxidation while maintaining its electrical properties.
[0058] The SiFeX layer may be formed to prevent further oxidation of the iron oxide layer and exhibit oxidation resistance at high temperatures. The silicon may bond with the oxygen on the surface of the iron to fix it on the surface of the iron, and the most basic structure may be configured as shown in Figure 6. As shown in the side view of Figure 6(a) and the plan view of Figure 6(b), once the oxygen covers the surface of the iron and is fixed by the silicon, other oxygen cannot enter the interior of the iron, thereby exhibiting oxidation resistance.
[0059] In the present invention, the silicon-coated iron may have the same electrical resistance as iron on which silicon (Si) is not deposited.
[0060] In the present invention, the silicon-coated iron may be in the form of a thin film, foil, or block.
[0061] In the present invention, when the silicon-coated iron is in the form of a thin film, foil, or lump, it may be one that is prevented from oxidizing even when heated at 200 to 350° C. for 20 to 40 minutes. In the case of the thin film, foil, or lump, it may be one that is prevented from oxidizing and does not show any visible changes in color or in the results of XRD or SEM measurement even when the heat treatment is carried out as described above.
[0062] In the present invention, the silicon-coated iron has a surface resistance of 9.2 × 10 -4 ~9.6×10 -4 The silicon-coated iron may have a sheet resistance value similar to that of iron not coated with silicon, and the sheet resistance value may not show a rapid increase even after heat treatment.
[0063] In the present invention, the silicon-coated iron may be composed of an iron layer 10, an iron oxide (Fe3O4) layer 20 formed on the iron layer 10, a SiFeX layer 30 formed on the iron oxide layer 20 by mixing silicon (Si), oxygen (O), and iron (Fe), and a silicon (Si)-oxygen (O) mixed layer 40 formed on the SiFeX layer 30.
[0064] In the present invention, the thickness of the iron oxide (Fe3O4) layer 20 may be 3 to 7 nm, and preferably 3 to 5 nm. The iron oxide layer may be formed so thin that it has almost no effect on the corrosion resistance of iron.
[0065] In the present invention, the SiFeX layer 30 made of a mixture of silicon (Si), oxygen (O), and iron (Fe) may have a thickness of 0.8 to 1.2 nm.
[0066] In the present invention, the silicon (Si)-oxygen (O) mixed layer 40 may have a thickness of 5 to 30 nm, preferably 8 to 20 nm.
[0067] The present invention relates to a method for manufacturing silicon-coated iron for oxidation prevention, which involves depositing silicon (Si) on iron (Fe) in a single sputtering process. Because the manufacturing process is carried out in a single process, it is very simple and economical.
[0068] In the present invention, the sputtering may be carried out in an argon atmosphere.
[0069] In the present invention, the sputtering may be performed at room temperature to 350° C. for 1 to 5 minutes, and preferably at 180 to 200° C. for 70 to 350 seconds. If the sputtering temperature and duration are higher or lower than the ranges, crystal grain boundaries and potentials are formed, resulting in a decrease in crystallinity. Therefore, it is preferable to perform the sputtering within the above temperature and duration ranges.
[0070] Silicone coated nickel for oxidation protection
[0071] The present invention relates to silicon-coated anti-oxidation nickel, which is formed by depositing silicon to form a SiNiX layer 200, which is a silicon (Si)-oxygen (O)-nickel (Ni) mixed layer.
[0072] The oxidation-resistant nickel on which the SiNiX layer 200 is formed may be resistant to oxidation while maintaining electrical properties.
[0073] The SiNiX layer 200 is formed to prevent oxidation and exhibit oxidation resistance at high temperatures. The silicon may bond with the oxygen on the surface of the nickel to fix it on the surface of the nickel, and the most basic structure may be configured as shown in Figure 6. As shown in the side view of Figure 6(a) and the plan view of Figure 6(b), when the oxygen covers the surface of the nickel and is fixed by the silicon, other oxygen cannot enter the interior of the nickel, thereby exhibiting oxidation resistance.
[0074] In the present invention, when the silicon-coated nickel is a single crystal thin film, it may be one that is prevented from being oxidized even when heated at 300 to 500° C. for 20 to 50 minutes.
[0075] In the present invention, when the silicon-coated nickel is in the form of a polycrystalline thin film, foil, or lump, it may be one that is resistant to oxidation even when heated at 200 to 400° C. for 20 to 40 minutes. In the case of the polycrystalline thin film, foil, or lump, it may be one that is resistant to oxidation and does not show any visible changes in color or in the results of XRD or SEM measurement even when the heat treatment is carried out as described above.
[0076] In the present invention, the silicon-coated nickel has a surface resistance of 6.2 × 10-4 ~6.8×10 -4 The silicon-coated nickel may have a sheet resistance value similar to that of nickel that is not coated with silicon, and the sheet resistance value may not show a rapid increase even after heat treatment.
[0077] In the present invention, the silicon-coated nickel may be composed of a nickel layer 100, a SiNiX layer 200 formed on the nickel 100 and containing a mixture of silicon (Si)-oxygen (O)-nickel (Ni), a first silicon (Si)-oxygen (O) mixed layer 300 formed on the SiNiX layer 200, and a second silicon (Si)-oxygen (O) mixed layer 400 formed on the first silicon (Si)-oxygen (O) mixed layer 300.
[0078] In the present invention, the SiNiX layer 200 may have a thickness of 0.8 to 1.2 nm.
[0079] In the present invention, the silicon (Si)-oxygen (O) composite layer including the first silicon (Si)-oxygen (O) composite layer 300 and the second silicon (Si)-oxygen (O) composite layer 400 may have a thickness of 5 to 30 nm, preferably 8 to 20 nm. The first silicon (Si)-oxygen (O) composite layer 300 may have a higher oxygen content than a nickel content, and the second silicon (Si)-oxygen (O) composite layer 400 may have a higher nickel content than an oxygen content.
[0080] Manufacturing method for silicon-coated anti-oxidation nickel
[0081] The present invention relates to a method for producing silicon-coated nickel for oxidation protection.
[0082] The silicon-coated anti-oxidation nickel of the present invention relates to an anti-oxidation nickel in which silicon is deposited to form a SiNiX layer 200, which is a silicon (Si)-oxygen (O)-nickel (Ni) mixed layer. The present invention also relates to a method for manufacturing the silicon-coated anti-oxidation nickel.
[0083] The oxidation-resistant nickel on which the SiNiX layer is formed may be resistant to oxidation while maintaining its electrical properties.
[0084] The SiNiX layer is formed to prevent oxidation and exhibit oxidation resistance at high temperatures. The silicon may bond with the oxygen on the surface of the nickel to fix it on the surface of the nickel, and the most basic structure may be configured as shown in Figure 6. As shown in the side view of Figure 6(a) and the plan view of Figure 6(b), when the oxygen covers the surface of the nickel and is fixed by the silicon, other oxygen cannot enter the interior of the nickel, thereby exhibiting oxidation resistance.
[0085] In the present invention, the silicon-coated nickel may have the same electrical resistance as nickel without silicon (Si) deposition.
[0086] In the present invention, the silicon-coated nickel may be in the form of a single crystal thin film, a polycrystalline thin film, a foil, or a lump.
[0087] In the present invention, when the silicon-coated nickel is a single crystal thin film, it may be one that is prevented from being oxidized even when heated at 300 to 500° C. for 20 to 50 minutes.
[0088] In the present invention, when the silicon-coated nickel is in the form of a polycrystalline thin film, foil, or lump, it may be one that is resistant to oxidation even when heated at 200 to 400° C. for 20 to 40 minutes. In the case of the polycrystalline thin film, foil, or lump, it may be one that is resistant to oxidation and does not show any visible changes in color or in the results of XRD or SEM measurement even when the heat treatment is carried out as described above.
[0089] In the present invention, the silicon-coated nickel has a surface resistance of 6.2 × 10 -4 ~6.8×10 -4 The silicon-coated nickel may have a sheet resistance value similar to that of nickel that is not coated with silicon, and the sheet resistance value may not show a rapid increase even after heat treatment.
[0090] In the present invention, the silicon-coated nickel may be composed of a nickel layer 100, a SiNiX layer 200 formed by mixing silicon (Si)-oxygen (O)-nickel (Ni) on the nickel 100, a first silicon (Si)-oxygen (O) mixed layer 300 formed on the SiNiX layer 200, and a second silicon (Si)-oxygen (O) mixed layer 400 formed on the first silicon (Si)-oxygen (O) mixed layer 300.
[0091] In the present invention, the SiNiX layer 200 may have a thickness of 0.8 to 1.2 nm.
[0092] In the present invention, the silicon (Si)-oxygen (O) composite layer including the first silicon (Si)-oxygen (O) composite layer 300 and the second silicon (Si)-oxygen (O) composite layer 400 may have a thickness of 5 to 30 nm, preferably 8 to 20 nm. The first silicon (Si)-oxygen (O) composite layer 300 may have a higher oxygen content than a nickel content, and the second silicon (Si)-oxygen (O) composite layer 400 may have a higher nickel content than an oxygen content.
[0093] The present invention relates to a method for manufacturing silicon-coated nickel for oxidation prevention, which involves depositing silicon (Si) on nickel (Ni) in a single sputtering process. Because the manufacturing process is carried out in a single process, it is very simple and economical.
[0094] In the present invention, the sputtering may be carried out in an argon atmosphere.
[0095] In the present invention, the sputtering may be performed at room temperature to 350° C. for 1 to 5 minutes, and preferably at 180 to 200° C. for 70 to 350 seconds. If the sputtering temperature and duration are higher or lower than the ranges, crystal grain boundaries and potentials are formed, resulting in a decrease in crystallinity. Therefore, it is preferable to perform the sputtering within the above temperature and duration ranges.
[0096] Example
[0097] EXAMPLES Hereinafter, examples of the present invention will be described in detail, but it is obvious that the present invention is not limited to the following examples.
[0098] The advantages and features of the present invention, as well as methods for achieving them, will become clearer with reference to the following examples. However, the present invention is not limited to the examples disclosed below, and can be embodied in various different forms. These examples are provided merely to complete the disclosure of the present invention and to fully convey the scope of the invention to those skilled in the art. The present invention is defined only by the scope of the claims.
[0099] <Example 1> Silicon-coated iron plate
[0100] Silicon (Si) was deposited to a thickness of 20 nm on an iron (Fe) plate by sputtering at 190° C. for 5 minutes in an argon atmosphere to prepare a silicon-coated iron plate.
[0101] <Comparative Example 1> Iron plate without silicone coating
[0102] An iron plate without silicone coating was prepared.
[0103] <Example 2> Silicon-coated nickel plate
[0104] Silicon (Si) was deposited to a thickness of 20 nm on a nickel (Ni) plate by sputtering at 190° C. for 5 minutes in an argon atmosphere to prepare a silicon-coated nickel plate.
[0105] <Comparative Example 2> Nickel plate without silicon coating
[0106] A nickel plate without any silicon coating was prepared.
[0107] <Experimental Example 1> Observation of the degree of oxidation after heat treatment
[0108] The iron plates manufactured in Example 1 and Comparative Example 1 were heat-treated at 300° C. for 30 minutes, and were observed before and after the heat treatment. The results are shown in FIG.
[0109] As shown in FIG. 1, the iron plate of Comparative Example 1 was oxidized and turned black after heat treatment, whereas the silicon-coated iron plate prepared in Example 1 maintained its original color even after heat treatment, confirming that no oxidation occurred.
[0110] From the above results, it was confirmed that the silicon-coated iron according to the present invention exhibits resistance to oxidation.
[0111] In addition, the nickel plates manufactured in Example 2 and Comparative Example 2 were heat-treated at 400° C. for 30 minutes, and were observed before and after the heat treatment. The results are shown in FIG.
[0112] As shown in FIG. 8, the nickel plate of Comparative Example 2 was oxidized and turned black after the heat treatment, whereas the silicon-coated nickel plate prepared in Example 2 maintained its original color even after the heat treatment, confirming that no oxidation occurred.
[0113] From the above results, it was confirmed that the silicon-coated nickel according to the present invention exhibits resistance to oxidation.
[0114] <Experimental Example 2> XRD measurement
[0115] The iron plates manufactured in Example 1 and Comparative Example 1 were heat-treated at 300° C. for 30 minutes, and were measured by XRD before and after the heat treatment. The results are shown in FIG.
[0116] As shown in Figure 2, the silicon-coated iron plate produced in Example 1 showed no peaks other than Fe before or after heat treatment. Furthermore, the crystal structure remained unchanged. This confirmed that the silicon-coated iron plate did not oxidize after heat treatment. On the other hand, in the case of the iron plate in Comparative Example 1, iron oxide peaks were observed after heat treatment, confirming that oxidation had occurred. It is believed that iron oxide (Fe3O4) was also produced in Example 1, but this was not apparent in the XRD results because the oxidation reaction was minimal and the iron oxide was produced very thinly.
[0117] From the above results, it was confirmed that the silicon-coated iron according to the present invention exhibits resistance to oxidation.
[0118] In addition, the nickel plates manufactured in Example 2 and Comparative Example 2 were heat-treated at 400° C. for 30 minutes, and were measured by XRD before and after the heat treatment. The results are shown in FIG.
[0119] As shown in Figure 9, the silicon-coated nickel plate prepared in Example 2 showed no peaks other than Ni before or after heat treatment. Furthermore, the crystal structure remained unchanged. This confirmed that the silicon-coated nickel plate did not oxidize after heat treatment. On the other hand, the nickel plate prepared in Comparative Example 2 showed a nickel oxide peak after heat treatment, confirming that oxidation had occurred.
[0120] From the above results, it was confirmed that the silicon-coated nickel according to the present invention exhibits resistance to oxidation.
[0121] <Experimental Example 3> SEM observation
[0122] The iron plates manufactured in Example 1 and Comparative Example 1 were heat-treated at 300° C. for 30 minutes, and were observed before and after the heat treatment using an SEM at 10,000 times magnification. The results are shown in FIG.
[0123] As shown in Figure 3, the iron plate of Comparative Example 1 showed changes on the surface after heat treatment, whereas the silicon-coated iron plate produced in Example 1 showed no changes on the surface after heat treatment. This confirmed that no oxidation occurred in the silicon-coated anti-oxidation iron plate produced in Example 1.
[0124] From the above results, it was confirmed that the silicon-coated iron according to the present invention exhibits resistance to oxidation.
[0125] In addition, the nickel plates manufactured in Example 2 and Comparative Example 2 were heat-treated at 400° C. for 30 minutes, and were observed before and after the heat treatment using an SEM at 10,000 times magnification. The results are shown in FIG.
[0126] 10, the nickel plate of Comparative Example 2 showed a change in the surface after heat treatment, whereas the silicon-coated nickel plate prepared in Example 2 showed no change in the surface after heat treatment. This confirmed that no oxidation occurred in the silicon-coated anti-oxidation nickel plate prepared in Example 2.
[0127] From the above results, it was confirmed that the silicon-coated nickel according to the present invention exhibits resistance to oxidation.
[0128] <Experimental Example 4> TEM analysis
[0129] The iron plate manufactured in Example 1 was analyzed by TEM, and the results are shown in FIG.
[0130] As shown in Figure 4, it was confirmed that the silicon-coated iron plate has a thin film surface formed in the following order: an iron layer, an iron oxide (Fe3O4) layer formed on the iron layer, a SiFeX layer formed on the iron oxide layer by mixing silicon (Si), oxygen (O) and iron (Fe), and a silicon (Si)-oxygen (O) mixed layer formed on the SiFeX layer.
[0131] When the iron plate was exposed to air, a natural oxide film formed, revealing iron oxide (Fe3O4). However, the natural oxide film was so thin that it was not visible to the naked eye or in XRD results. By depositing silicon on the natural oxide film, silicon atoms fixed the oxygen atoms, which were free to move on the silicon surface, to their optimal sites, resulting in the appearance of the SiFeX layer, which was determined to play a crucial role in preventing oxidation. It was confirmed that Si-O-Fe bonds were formed.
[0132] From the above results, it was confirmed that the silicon-coated iron according to the present invention can exhibit oxidation resistance at high temperatures by forming a Si-O-Fe mixed layer on the iron layer, thereby preventing oxidation.
[0133] In addition, the silicon-coated nickel plate prepared in Example 2 was analyzed by TEM, and the results are shown in FIG.
[0134] As shown in FIG. 11, it was confirmed that the silicon-coated nickel plate had a thin film surface formed in the following order: a nickel layer, a SiNiX layer formed on the nickel layer by mixing silicon (Si)-oxygen (O)-nickel (Ni), a first silicon (Si)-oxygen (O) mixed layer formed on the SiNiX layer, and a second silicon (Si)-oxygen (O) mixed layer formed on the first silicon (Si)-oxygen (O) mixed layer.
[0135] By depositing silicon on the nickel layer, silicon atoms fix the oxygen atoms that move freely on the surface of the nickel layer at the optimal site, forming Si-O-Ni bonds. The SiNiX layer formed as a result was determined to play an important role in preventing oxidation.
[0136] From the above results, it was confirmed that the silicon-coated nickel according to the present invention can exhibit oxidation resistance at high temperatures by forming a Si-O-Ni mixed layer on the nickel layer, thereby preventing oxidation.
[0137] <Experimental Example 5> Measurement of surface resistance
[0138] The iron plates manufactured in Example 1 and Comparative Example 1 were heat treated at 300° C. for 30 minutes, and the sheet resistance was measured before and after the heat treatment. The results are shown in FIG.
[0139] As shown in FIG. 5, the sheet resistance of the iron plate of Comparative Example 1 increased sharply after heat treatment, whereas the silicon-coated iron plate of Example 1 did not show any significant change after heat treatment.
[0140] From the above results, it was confirmed that the silicon-coated iron according to the present invention exhibits resistance to oxidation while maintaining electrical properties.
[0141] In addition, the nickel plates manufactured in Example 2 and Comparative Example 2 were heat treated at 400° C. for 30 minutes, and the sheet resistance was measured before and after the heat treatment. The results are shown in FIG.
[0142] As shown in FIG. 12, the sheet resistance of the nickel plate of Comparative Example 2 increased sharply after heat treatment, whereas the silicon-coated nickel plate of Example 2 did not show any significant change after heat treatment.
[0143] From the above results, it was confirmed that the silicon-coated nickel according to the present invention exhibits resistance to oxidation while maintaining electrical properties.
[0144] <Experimental Example 6> Measurement of oxygen energy difference based on penetration depth
[0145] The energy of oxygen penetrating into the iron was calculated based on the depth from the surface, using the energy of the silicon-coated iron plate manufactured in Example 1 when it was present outside the surface. The difference between this and the energy calculated when oxygen was present on the surface of the sample is shown in FIG. 7.
[0146] As shown in FIG. 7, in the case of the silicon-coated iron plate manufactured in Example 1, oxygen must overcome an energy barrier to pass through the Si—O—Fe mixed layer from the surface, and the energy barrier represents resistance to oxidation.
[0147] From the above results, it was confirmed that the silicon-coated iron according to the present invention exhibits resistance to oxidation.
[0148] In addition, the energy of oxygen penetrating into nickel was calculated based on the depth from the surface, using the energy of the silicon-coated nickel plate produced in Example 2 when it was present outside the surface as a reference, and the difference between this and the energy calculated when oxygen was present on the surface of the sample is shown in FIG. 14.
[0149] As shown in FIG. 14, in the case of the silicon-coated nickel plate manufactured in Example 2, oxygen must overcome an energy barrier to pass through the Si-O-Ni mixed layer from the surface, and the energy barrier represents resistance to oxidation.
[0150] From the above results, it was confirmed that the silicon-coated nickel according to the present invention exhibits resistance to oxidation.
[0151] This invention was supported by the Samsung Research Funding & Incubation Center of Samsung Electronics under project number SRFC-MA2202-02. [Explanation of symbols]
[0152] 10 Iron Layer 20 Iron oxide (Fe3O4) layer 30 SiFeX layers 40 Silicon (Si)-oxygen (O) mixed layer 100 Nickel (Ni) layer 200 SiNiX layers 300 First silicon (Si)-oxygen (O) mixed layer 400 Second silicon (Si)-oxygen (O) mixed layer
Claims
1. Silicon (Si) is deposited to form a SiFeX layer (30), which is a silicon (Si)-oxygen (O)-iron (Fe) mixed layer, for oxidation prevention.
2. The silicon-coated iron is an iron layer (10); The iron oxide (Fe) formed on the iron layer (10) ３ O ４ ) layer (20); a SiFeX layer (30) formed on the iron oxide layer (20) by mixing silicon (Si)-oxygen (O)-iron (Fe); 2. The silicon-coated iron for oxidation prevention according to claim 1, characterized in that it is composed of a silicon (Si)-oxygen (O) mixed layer (40) formed on the SiFeX layer (30).
3. The iron oxide (Fe ３ O ４ ) layer (20) is The silicon-coated iron for oxidation prevention according to claim 2, characterized in that the thickness is 3 to 7 nm.
4. The SiFeX layer (30) is a mixture of silicon (Si), oxygen (O), and iron (Fe). The silicon-coated iron for oxidation prevention according to claim 2, characterized in that the thickness is 0.8 to 1.2 nm.
5. The silicon (Si)-oxygen (O) mixed layer (40) is The silicon-coated iron for oxidation prevention according to claim 2, characterized in that the thickness is 5 to 30 nm.
6. A method for manufacturing silicon-coated iron for oxidation prevention, in which silicon (Si) is deposited on iron (Fe) in a single sputtering process.
7. The sputtering is 6. A method for producing silicon-coated iron for oxidation prevention, characterized in that the method is carried out in an argon atmosphere.
8. The sputtering is 6. A method for producing silicon-coated iron for oxidation prevention according to claim 6, characterized in that the treatment is carried out at room temperature to 350°C for 1 to 5 minutes.
9. Silicon (Si) is deposited to form a SiNiX layer (200), which is a silicon (Si)-oxygen (O)-nickel (Ni) mixed layer, on the silicon-coated nickel for oxidation prevention.
10. The silicon-coated nickel is a nickel layer (100); A SiNiX layer (200) formed on the nickel layer (100) by mixing silicon (Si)-oxygen (O)-nickel (Ni), a first silicon (Si)-oxygen (O) mixed layer (300) formed on the SiNiX layer (200); and a second silicon (Si)-oxygen (O) mixed layer (400) formed on the first silicon (Si)-oxygen (O) mixed layer (300). The silicon-coated nickel for oxidation prevention according to claim 9,
11. The SiNiX layer (200) is The silicon-coated nickel for oxidation prevention according to claim 10, characterized in that the thickness is 0.8 to 1.2 nm.
12. The silicon (Si)-oxygen (O) mixed layer including the first silicon (Si)-oxygen (O) mixed layer (300) and the second silicon (Si)-oxygen (O) mixed layer (400) is The silicon-coated anti-oxidation nickel according to claim 10, characterized in that the thickness is 5 to 30 nm.
13. A method for manufacturing silicon-coated anti-oxidation nickel by depositing silicon (Si) on nickel (Ni) in a single sputtering process.
14. The sputtering is The method for producing silicon-coated nickel for oxidation prevention according to claim 13, characterized in that it is carried out under an argon atmosphere.
15. The sputtering is The method for producing silicon-coated nickel for oxidation prevention according to claim 14, characterized in that the process is carried out at room temperature to 350°C for 1 to 5 minutes.