Sputtering target and method of manufacturing the same

A sputtering target with a high amorphous phase ratio, manufactured via thermal spraying, addresses brittleness and crystallization issues, ensuring stable and efficient production of amorphous alloy thin films.

JP7716481B2Active Publication Date: 2025-07-31KOLON INDUSTRIES INC
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Patent Information

Application Number
JP2023539112
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Priority Date
2022-01-25
Filing Date
2022-01-26
Publication Date
2025-07-31
Estimated Expiration
2042-01-26

AI Technical Summary

Technical Problem

Sputtering targets with an amorphous phase are prone to local crystallization and brittleness due to temperature rises during the sputtering process, leading to potential breakage and product defects.

Method used

A sputtering target with a substrate and an alloy target layer having an amorphous phase ratio of 98.0% or more, manufactured using iron-based amorphous alloy powder through a thermal spraying coating process, which maintains high amorphous fraction and allows for easy adjustment of size and thickness, and can be used as a single target to form alloy thin films.

Benefits of technology

The target maintains high amorphous fraction, reduces brittleness, and minimizes cracking, enabling efficient and cost-effective production of amorphous alloy thin films with improved corrosion resistance and reduced manufacturing time.

✦ Generated by Eureka AI based on patent content.

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Abstract

A sputtering target according to one aspect of the present invention may include a substrate, and an alloy target layer provided on the substrate, the alloy target layer having an amorphous phase ratio of 98.0% or more.
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Description

Technical Field

[0001] One aspect of the present invention relates to a sputtering target and a method for manufacturing the sputtering target.

Background Art

[0002] Sputtering is a type of vacuum deposition method. In a low vacuum, a gas such as argon ionized by plasma is accelerated and made to collide with a target, ejecting atoms to form a thin film on a substrate or base material such as a wafer or glass. Sputtering has the characteristics of being superior in deposition ability compared to general distillation methods, being excellent in the ability to maintain an alloy when using a complex alloy as a sputtering target, and being excellent in the deposition ability of metals with heat resistance at high temperatures.

[0003] For the sputtering target used to form a thin film in the sputtering process, various types of sputtering targets can be used according to the composition of the thin film or coating to be formed, and generally, metal, alloy, and compound materials with a purity of 99.99% or more can be utilized. Titanium, nickel, cobalt, molybdenum, tungsten, tantalum, niobium, niobium pentoxide, aluminum, molybdenum-niobium alloy, stainless steel, nickel alloy, cobalt alloy, ITO (Indium Tin Oxide), etc. are mainly used as targets.

[0004] On the other hand, when a columnar crystal structure or a structure containing grain boundaries is formed in the thin film formed by the sputtering method, the etching solution penetrates along the grain boundaries, etc., accelerating corrosion, resulting in extremely poor corrosion resistance and a decrease in strength. Therefore, technologies for forming an amorphous thin film containing an amorphous phase and having no crystal structure have been studied.

[0005] However, in the case of an amorphous sputtering target, the temperature rises due to ion collisions during the sputtering process, and such a temperature rise is likely to change the structure near the surface of the sputtering target. That is, due to the characteristics of the thermally unstable amorphous phase, when the temperature of the sputtering target rises, local crystallization occurs on the surface of the sputtering target, which may increase the brittleness of the target and result in the sputtering target being easily broken during the sputtering process. If the sputtering target is broken during the process, it may cause a fatal problem in the production of the product. Therefore, it is necessary to ensure the stability of the sputtering target.

Prior Art Documents

Patent Documents

[0006]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0007] An object of the present invention is to provide a sputtering target having a high proportion of an amorphous phase while consisting of a desired alloy composition for forming an amorphous alloy thin film on a workpiece, and a method for manufacturing the same.

[0008] Another object of the present invention is to provide a sputtering target that can perform sputtering by utilizing a single-substrate target without using two or more substrates in order to form an alloy thin film having a desired composition by sputtering.

[0009] Furthermore, when a sputtering target having an amorphous alloy is used to form an amorphous alloy thin film on a workpiece, it was devised to solve the problems of local crystallization and brittleness of the amorphous alloy generated on the surface of the sputtering target. Even when there is a local temperature rise on the surface due to the sputtering process, it minimizes the increase in brittleness of the sputtering target due to crystallization and provides a sputtering target that is less likely to break during the process.

Means for Solving the Problems

[0010] The sputtering target according to one aspect of the present invention can include a substrate and an alloy target layer provided on the substrate and having an amorphous phase ratio of 98.0% or more.

[0011] The method for manufacturing a sputtering target according to one aspect of the present invention can include preparing a substrate and forming a target layer having an amorphous phase ratio of 98.0% or more by cold spraying iron (Fe)-based amorphous alloy powder or iron (Fe)-based alloy powder having a composition capable of forming an amorphous phase on the substrate.

Effects of the Invention

[0012] The sputtering target according to one aspect of the present invention can be manufactured by spraying an alloy powder having a high fraction of amorphous phase or an alloy powder having excellent amorphous forming ability onto a substrate. When using amorphous powder during the manufacture of the sputtering target, the high amorphous fraction of the amorphous alloy powder can be maintained in the target layer of the sputtering target, the ratio of the amorphous phase of the sputtering target becomes high, and the thin film manufactured using the sputtering target can also have a high amorphous fraction.

[0013] Also, when the alloy powder during the manufacture of the sputtering target is an alloy powder having excellent amorphous forming ability, its composition can be maintained in the target layer, and the thin film manufactured using the sputtering target can be composed of an amorphous material.

[0014] In addition, when manufacturing by a thermal spraying coating process using amorphous alloy powder, it is easy to adjust the size (increase in area), thickness, etc. of the sputtering target layer, and the back plate (Back plate or backing plate) can also be freely selected.

[0015] In addition, since the manufacturing process of the sputtering target is relatively simple, the production of the sputtering target is easy, and after sputtering, repair of the damaged area is also possible, so it has an excellent effect of reducing manufacturing costs.

[0016] In addition, when manufacturing an alloy thin film using a sputtering process, the sputtering targets of these constituent elements must be installed in the vacuum chamber at the same time. However, when manufacturing a sputtering target by a thermal spraying coating process using amorphous alloy powder, only a single sputtering target provided on a single substrate can be used, so miniaturization of the apparatus and reduction of manufacturing time can be achieved.

[0017] In addition, when manufacturing a sputtering target by a thermal spraying coating process, there is an advantage that a sputtering layer (coating layer) having a high density of 99.99% can be easily formed, and a cylinder-type sputtering target can be manufactured.

Brief Description of the Drawings

[0018]

Figure 1

Figure 2

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Figure 7

Embodiments for Carrying Out the Invention

[0019] Before explaining the present invention in detail below, it should be understood that the terms used in this specification are for the purpose of describing specific embodiments only and do not limit the scope of the present invention, which is limited only by the appended claims. All technical terms and scientific terms used in this specification have the same meaning as those generally understood by those having ordinary skill in the art, unless otherwise specified.

[0020] Throughout this specification and the claims, unless otherwise specified, the term "comprise (comprises, comprising)" means including the recited item, step, or group of items and steps, and is not used in a sense that excludes any other item, step, or group of items or group of steps.

[0021] On the other hand, various embodiments of the present invention can be combined with any other embodiments as long as there is no explicit indication to the contrary. In particular, a certain feature indicated as preferable or advantageous can be combined with any other feature indicated as preferable or advantageous.

[0022] In the drawings, the width, length, thickness, etc. of components may be exaggerated for convenience. Overall, the drawings are described from the perspective of an observer when explaining the drawings. When one component is said to be "above / below" another component, this includes not only the case where it is "directly above / below" the other component, but also the case where there are other components in between.

[0023] One aspect of the present invention is a sputtering target, which includes a substrate 200 and a target layer 100 provided on the substrate 200.

[0024] The substrate 200 is a back plate for forming the target layer 100 of the sputtering target, provides a surface on which the target layer 100 can be formed, and determines the size of the sputtering target. The material of the substrate 200 is not limited, and a substrate 200 made of a metal or alloy material can be used. It is often preferable to use a metal or alloy or metal oxide material with excellent electrical conductivity and thermal conductivity. For example, a substrate 200 made of copper metal, indium tin oxide (ITO), indium gallium oxide (IZO), or indium gallium zinc oxide (IGZO) can be used.

[0025] The size of the substrate 200 is not limited, but when it is used as a target in the sputtering process of the sputtering target, it can vary according to the sputtering process time, speed, and workload, and can be determined according to the method and conditions for manufacturing the sputtering target.

[0026] A bonding layer can be provided between the substrate 200 and the target layer 100 described later. If the bonding between the target layer 100 provided on the substrate 200 and the substrate 200 is not good at the interface, there may be a problem that the target layer 100 peels off. However, in order to supplement the bonding characteristics between the substrate 200 and the target layer 100, for example, a bonding layer such as an elastomer can be provided. If excellent bonding between the substrate 200 and the bonding layer is not required, the target layer 100 may be directly formed on the substrate 200 without a separate bonding layer.

[0027] The target layer 100 is an alloy layer provided on the substrate 200 and can be provided on the surface of the substrate 200 or the bonding layer. The target layer 100 preferably consists of an alloy composition excellent in glass-forming ability and is an amorphous alloy layer containing an amorphous phase.

[0028] Specifically, the alloy contained in the target layer 100 is preferably an iron-based alloy having a composition containing iron (Fe) as a main component, and more preferably an iron-based amorphous alloy containing elements capable of improving the glass-forming ability. As the amorphous sputtering target material, it can partially contain large atoms such as K, Sr, Eu, Ca, Y, Pb, Er, In, Zr, etc., which can improve the glass-forming ability. It can contain intermediate atoms such as Ni, Cr, Co, Cu, V, Mo, W, Pt, Nb, Ta, Au, Ag, Ti, etc., and small atoms such as P, S, B, C elements can be added.

[0029] The iron-based alloy according to an embodiment of the present invention contains Fe, Cr, and Mo, and further contains at least one or more elements selected from the group consisting of Ni, Co, Cu, V, W, Pt, Nb, Ta, Au, Ag, Ti, P, S, B, and C, and preferably contains two or more elements selected from the above element group.

[0030] On the other hand, at least one element selected from the group consisting of Ni, Co, Cu, V, W, Pt, Nb, Ta, Au, Ag, Ti, P, S, B, and C, which is further contained, is preferably contained within 10 wt% each in the entire alloy.

[0031] When at least one selected element exceeds 10 wt.%, due to the decrease in the amorphous forming ability of the alloy and the decrease in the glass transition temperature (Tg) and crystallization temperature (Tx), the proportion of the amorphous phase may become low or crystallization may easily occur. Also, for this reason, crystallization may occur in the target layer 100 due to the heat generated during sputtering, and cracks may occur in the target, or compositional unevenness of the alloy thin film 300 produced by sputtering may be caused.

[0032] When the alloy forming the target layer 100 has the above composition, an iron-based alloy target layer 100 excellent in the amorphous forming ability of the alloy can be provided. Here, a high proportion of the amorphous phase can be contained in the target layer 100, and even if the target layer 100 does not contain the amorphous phase or contains it in a low proportion, a high proportion of the amorphous phase can be obtained in the finally obtained thin film.

[0033] The proportion of the amorphous phase contained in the target layer 100 is 80 to 100%, preferably 90 to 100%, more preferably 95 to 100%.

[0034] When the proportion of the amorphous phase is lower than the said range, the proportion of the crystal phase becomes high, and due to the non-uniform distribution of the elements forming the crystal phase in the alloy, the compositional uniformity of the sputtered thin film may decrease. Also, with the increase in the proportion of the crystal phase, the brittleness of the target layer 100 increases, or the amorphous forming ability decreases due to the decrease in the glass transition temperature (Tg) and crystallization temperature (Tx) of the alloy in the part of the target layer 100 where the crystal phase is formed, so that further crystallization may locally occur due to the temperature rise during sputtering, which may cause cracks in the target layer 100.

[0035] On the one hand, the thickness of the target layer 100 is not particularly limited and can be easily controlled according to the technical field to which it is applied and the required values of the product. However, a range of 50 μm to 4000 μm, preferably 100 μm to 4000 μm, may be preferable.

[0036] As a method for manufacturing the target layer 100 made of an alloy containing an amorphous phase, after powderizing the alloy, a method of forming the target layer 100 in a thermal spraying coating process, a method of vapor deposition or sputtering of the alloy, a method of manufacturing into ribbons or flakes and then forming or sintering at a high temperature, a method of casting, pressing or crimping, etc. can be used, and it is preferable to use a method of forming the target layer 100 by thermal spraying coating of alloy powder.

[0037] When manufacturing a sputtering target in a thermal spraying coating process using amorphous alloy powder, after completely melting the alloy powder, a step of rapidly cooling at a high cooling rate (~10 6 K / s) can be included. Since the target layer 100 can be formed while maintaining the amorphous phase of the powder through control of the spraying temperature, there is an advantage that it is easy to control the thickness, size, etc.

[0038] On the contrary, in the case of methods such as forming or sintering at a high temperature, casting, pressing or crimping, vapor deposition or sputtering, etc., it is difficult to apply a high cooling rate (~10 6 K / s), so it is difficult to form an amorphous structure (short range ordered structure), and an additional bonding process with a back plate or backing plate is added, which may cause a decrease in productivity and economy.

[0039] More specifically, the target layer 100 can be manufactured by various spraying methods. Among them, it is preferable to utilize thermal spraying methods including high-velocity oxy-fuel (HVOF), plasma spraying, flame spraying, arc spraying, twin wire arc spraying (TWAS), and cold spraying.

[0040] When using a thermal spraying method to form the target layer 100, an alloy powder with a desired alloy composition can be used, which has the advantage of being easy to control the coating method and conditions. Also, when using an alloy powder containing an amorphous phase as a feedstock, the target layer 100 can be formed while maintaining a high proportion of the amorphous phase contained in the powder, which is advantageous for forming an amorphous target layer 100 having a high fraction of the amorphous phase.

[0041] One embodiment of the present invention discloses a sputtering target including a target layer 100 formed by a thermal spraying method, and discloses a sputtering target provided with a target layer 100 by a cold spraying method among thermal spraying methods.

[0042] In the case of a spraying coating process involving high temperatures such as atmospheric plasma spraying (APS), arc spraying, and high-velocity oxy-fuel (HVOF) spray, since the powder is deposited in a temperature range higher than the glass transition temperature (Tg) or the crystallization temperature (Tx), oxidation of the powder due to in-flight oxidation occurs, where the powder is oxidized by a high heat source during flight, and depletion of metal elements occurs thereby. Such depletion of additive elements locally reduces the amorphous forming ability of the coating layer, and crystallization of the alloy may occur in the depleted region.

[0043] However, when using the low-temperature spraying coating process, such problems do not occur, and it has the advantages that the overall amorphous fraction of the target is higher than that of the materials manufactured by other spraying coating processes, a uniform proportion of the amorphous phase can be obtained, and the purity and density are also higher.

[0044] Low-temperature spraying is a technology that uses high-pressure compressed gas, such as helium, nitrogen, argon or mixed gas, to accelerate metal or composite material powder to supersonic speed of about 500 - 1200 m / s to induce plastic deformation of the powder, and laminates the powder on the base material to form a dense sprayed layer. Since the powder is laminated in a solid state without melting at a low temperature to cause plastic deformation by kinetic energy, it is applied to copper and titanium materials with high reactivity with oxygen at high temperatures, or utilized as a method for spraying amorphous and nanocrystalline materials with low phase stability, and has the advantage that the characteristics (purity, composition, etc.) of the initial powder are maintained as they are.

[0045] Also, when forming the target layer 100 by a spraying method using amorphous alloy powder, since the formed sprayed layer is provided on the substrate 200 or the base material, there is an advantage that the bonding bonding process conventionally required for bonding the target layer 100 to the substrate 200 can be omitted.

[0046] Furthermore, the method of manufacturing a sputtering target by laminating powder through a spraying coating process is also preferably utilized for the maintenance (repair) of waste sputtering targets.

[0047] The formed target layer 100 can have somewhat different characteristics depending on the composition of the alloy contained in the alloy powder, the proportion of the amorphous phase, the spraying method, and the spraying conditions. Since there is no oxide present at the particle boundary of the target layer 100, the purity of the coating layer is similar to the purity of the powder (low impurity content), the porosity is extremely low, and the proportion of the amorphous phase is obtained at a level similar to that of the feedstock.

[0048] Specifically, the content of impurities contained in the target layer 100 can be 0.05 wt.% or less, preferably 0.001 to 0.04 wt.%, and more preferably 0.001 to 0.005 wt.%. When the content of impurities is higher than this range, the composition of the thin film may differ from that of the powder, which may cause a decrease in the expected properties (such as wear resistance and corrosion resistance).

[0049] Here, the impurities include not only impurities taken in from the outside, but also elements such as nitrogen and oxygen that are present in trace amounts at grain boundaries during the process of forming the target layer 100, metal oxides formed by in-flight oxidation, ceramic phases in which metal atoms are chemically bonded to non-metal atoms, intermetallic compounds, etc. It includes not only foreign substances, but also new compounds and crystal phases that are not contained in the amorphous alloy powder.

[0050] Also, the porosity of the target layer 100 can be 0.1% or less. A more preferable porosity can be 0.01 to 0.1%. When the porosity of the target layer 100 is higher than this range, there is a problem that the peeling of the target layer 100 and the roughness of the thin film increase during sputtering, resulting in a lower quality of the final product.

[0051] Also, the proportion of the amorphous phase contained in the target layer 100 is preferably 98.0% or more, preferably 99.0% or more, and more preferably 99.5% or more. It is preferably in the range of 0.96 to 1 times, preferably 0.98 to 1 times, compared to the proportion of the amorphous phase contained in the amorphous alloy powder used for coating. When the proportion of the amorphous phase contained in the target layer 100 is lower than this range or contains a lower proportion of the amorphous phase than the amorphous alloy powder, local compositional differences may occur in the thin film, which may cause a decrease in properties.

[0052] Also, the strength or Vickers hardness (HV) of the sputtering target layer 100 0.3) is often in the range of 900 - 1100 Hv, similar to the initial powder, preferably 1000 - 1100 Hv. When the strength or Vickers hardness is low, there may be a compositional difference in the coating layer depending on the position, and it can be understood that the bonding force at the grain boundaries of the powder is low. In such a case, as sputtering progresses, the composition of the thin film may be different from that of the target layer 100, or a part of the target layer 100 may peel off and fall onto the thin film, which may cause product defects.

[0053] On the other hand, the size and shape of the amorphous alloy powder used in the thermal spraying process for forming the target layer 100 are not restricted, but it is preferably a powder close to spherical shape. The average particle size of the alloy powder is 40 μm or less, preferably 30 μm or less.

[0054] When the particle size is smaller than the said range, the kinetic energy of the powder becomes low and the lamination efficiency decreases, and the economy during the production of the sputtering target becomes low. Also, metal oxides may be formed by inflight oxidation due to the increase in the specific surface area per unit g. When it is larger than the said range, there is a problem that the porosity of the target layer 100 becomes high because the powder is not induced to deform.

[0055] One embodiment of the present invention provides a sputtering target obtained by thermally spraying an amorphous alloy powder onto a substrate 200 to form a target layer, or by heat treatment when necessary. When heat treatment is performed after low-temperature thermal spraying coating, the heat treatment can be performed within a range where oxides are not formed or within a temperature range where crystallization does not occur. During the heat treatment, the alloy of the target layer 100 can maintain the amorphous phase while reducing the porosity and improving the density of the target layer 100.

[0056] Here, as the heat treatment atmosphere, heat treatment in a vacuum atmosphere or an Ar atmosphere is appropriate, and it is preferably performed at 550 to 570°C, more preferably at 560 to 570°C. When the heat treatment temperature is lower than this range, since the effect of improving pores cannot be obtained, it is difficult to improve the density of the coating layer. When the temperature is higher than this range, crystallization may occur, and there may be a problem that the amorphous fraction decreases.

[0057] The sputtering target according to this aspect of the present invention is preferably utilized as a single target capable of forming an alloy thin film 300 having the same composition as the target layer 100 on the surface of the workpiece 400 when gas atoms ionized during sputtering collide with the surface. Utilizing it as a single target means that, in the sputtering process, a sputtering target having a target layer 100 made of an alloy of a single composition formed on a single substrate 200 (single plate) is used as the only one.

[0058] The alloy of a single composition means that, except when it contains completely different elements or the contents of the contained elements are different from each other, even if some impurities are contained during the process of forming the target layer 100, or the content difference or the ratio of the contained amorphous phase that can be ignored changes, it is usually regarded as an alloy of the same composition.

[0059] The alloy contained in the target layer 100 is an iron-based amorphous alloy excellent in amorphous forming ability, having a high ratio of amorphous phase, glass transition temperature (Tg), and crystallization temperature (Tx), and being less likely to crystallize even due to a local temperature rise of the target during the sputtering process. Therefore, the brittle characteristics are good, and almost no cracks occur in the sputtering target.

[0060] In addition, when the sputtering target formed in the thermal spraying coating process is used as a single target in the sputtering process, due to the excellent properties (high amorphous forming ability) of the target layer 100 described above and the sound microstructure (extremely low porosity and powder interface defects) of the target layer 100 resulting from the thermal spraying coating process, even if the temperature of the target rises during the sputtering process, it is possible to prevent cracks from being formed in the target layer 100 due to physical property deterioration in fine structural defects (pores and powder interface defects).

[0061] Another aspect of the present invention is a method for manufacturing a sputtering target, including the steps of preparing an iron-based alloy powder and a substrate 200, and thermally spraying an iron-based amorphous alloy powder onto the substrate 200 described above to form a target layer 100.

[0062] It is preferable to use the same amorphous alloy powder as described above for the iron-based alloy powder, and even if it does not contain an amorphous phase, it is better to use an alloy powder with a composition having a high amorphous forming ability. Similar to the above-described one, the substrate 200 may be electrically connected to the cathode during the sputtering process so that the ionized gas atoms are accelerated toward the target layer 100.

[0063] Although various methods can be used for the thermal spraying method, it is most preferable to use the cold spray method.

[0064] This aspect of the present invention has the advantage that when manufacturing a thin film containing an amorphous phase through a sputtering method, in terms of being able to utilize a single sputtering target compared to a method of performing sputtering using two or more targets calculated by the ratio of the alloy composition in order to provide an alloy with an excellent amorphous forming ability composition as a target, the composition of the manufactured thin film can be homogenized and the sputtering process can be simplified, and there is an advantage of solving the problem that it is difficult to manufacture a target of an amorphous alloy composition by sintering or casting.

[0065] The target substrate 200 of the sputtering target described above can be directly utilized as a backplate during the sputtering process. It is often a single plate and can be connected to a DC or AC power source to serve as a cathode (- electrode). The target layer 100 provided on the substrate 200 provides a surface for sputtering. During the progress of the sputtering process, the alloy contained in the target layer 100 of the sputtering target becomes the object of sputtering and forms an alloy thin film 300 with the same composition on a workpiece 400 such as a base material or the substrate 200 that serves as an anode (Anode, + electrode). to form an alloy thin film 300 with the same composition.

[0066] The apparatus used for sputtering and the sputtering conditions are not limited and can be carried out with apparatuses and conditions that can be adopted at the normal technical level.

[0067] Another aspect of the present invention relates to an alloy thin film formed using the above-described sputtering target as a sputtering target, and a structure including the alloy thin film.

[0068] The thin film produced by sputtering preferably contains an alloy with the same composition as the target layer 100. Although there may actually be some errors in the measurement method and sample collection, the composition of the thin film formed by the sputtering process can be expressed as having the same composition as the target layer 100 that serves as the sputtering target.

[0069] In particular, when the target layer 100 used as a sputtering target contains an amorphous phase, the thin film produced by sputtering can be provided to also contain the amorphous phase of the target layer 100. The difference between the ratio of the amorphous phase contained in the thin film and the ratio of the amorphous phase contained in the target layer 100 is ideally 0%, but can be within 5%, preferably obtained within 0.1 - 5%.

[0070] In addition, the structure of the powder laminated form of the target layer 100 formed by the thermal spraying method has the advantage that an alloy of a desired composition can be directly applied to a thin film because chemical reactions and impurity formation between or inside the alloy powders can be minimized during the sputtering process.

Example

[0071] Hereinafter, the present invention will be described more specifically through examples.

[0072] (Example) Manufacture of Sputtering Target As an Fe-based amorphous alloy powder, it contains medium-sized atoms such as Cr and Mo, and small-sized atoms such as B and C. The content of each component is Cr: 15.8 wt.%, Mo: 27.0 wt.%, B: 1.2 wt.%, C: 3.7 wt.%, and the balance is Fe. An Fe-based amorphous alloy powder having the average particle size shown in Table 1 was prepared. Then, each alloy powder was used to form a target layer having the thickness shown in Table 1 on a stainless steel substrate by a cold spray method, a high-velocity oxy-fuel (HVOF) spraying method, and an atmospheric plasma spraying (APS) method.

[0073]

Table 1

[0074] (Experimental Example) Experimental Example 1 - Microstructure Analysis of Fe-based Amorphous Powder The cross-sectional microstructure of the Fe-based amorphous alloy powder in Table 1 was observed with an electron microscope, and X-Ray diffraction analysis of the Fe-based amorphous alloy powder was performed. The results are shown in Figure 2.

[0075] Figure 2(a) is a photograph of the cross-sectional microstructure of the powder. It can be confirmed that the powder is observed to be spherical overall, and the average particle size is 29.5 μm. From the results of Figure 2(b), no crystalline peak has been detected, only a broad halo peak has been detected, and it is judged that the powders all maintain an amorphous phase.

[0076] Experimental Example 2 - Structural Property Analysis of the Target Layer For the alloy coating layers and alloy powders of Test Specimens 1 to 6, the alloy composition and the presence or absence of impurities or foreign substances were confirmed through ICP analysis, the crystal structure was analyzed using X-ray diffraction (XRD) analysis, and the microstructure (porosity and elemental distribution) of the coating layer was confirmed using a field emission scanning electron microscope and a field emission electron probe micro analyzer.

[0077] Figure 3 is a photograph taken after manufacturing a sputtering target using the iron-based amorphous powder of Test Specimen 1 in a region on the base material with a horizontal and vertical length of 8 cm each.

[0078] Figures 4 and 5 are photographs of the cross-section and microstructure of the iron-based amorphous alloy target layers manufactured by a low-temperature spraying coating process and a high-velocity oxy-fuel spraying process, using the powders of Test Specimen 1 and Test Specimen 2 respectively.

[0079] In Figure 4(a), the thickness of the target layer was measured to be 420 μm, and no defects or impurities were observed in the interior of the target layer and in the interface region between the target layer and the base material.

[0080] Figure 4(b) shows the microstructure of the target layer observed at a high magnification. From the fact that no oxides were detected at the grain boundaries in the portion marked (1), it can be seen that the target layer contains impurities at the same level as the initial powder.

[0081] In Fig. 5(a), although no bonding was observed inside the target layer and at the interface between the target layer and the base material, it was observed that there were some pores at the grain boundaries. In Fig. 5(b), the spaces between the grain boundaries were clearly observed. Since it is analyzed that an Fe-Cr-based composite oxide exists in the portion marked (2), it is expected that the impurity content in the target layer is higher than that in the target layer of the low-temperature spraying process shown in Fig. 4, and higher than the impurity content contained in the iron-based amorphous alloy powder used in the production.

[0082] Fig. 6 shows the XRD analysis results for the target layer produced in the low-temperature spraying coating process of Specimen 1. As a result of the analysis, when forming the target layer by the low-temperature spraying method using the iron-based amorphous alloy powder of Specimen 1, as shown in Fig. 2(b), no peaks of the crystalline phase were detected, and only a broad halo peak was detected. Thus, it was shown that the amorphous phase was maintained as in the powder.

[0083] Fig. 7 shows the results of analyzing the target layer of the sputtering target of Specimen 1 by EPMA. As a result of the analysis, it was found that Fe, Cr, Mo, and B contained in the alloy were uniformly and finely distributed, and no segregation of alloy elements due to the precipitation of phases was observed.

[0084] Experimental Example 3 - Physical Property Analysis of Sputtering Target The amorphous ratio, porosity, and hardness of the alloy powder and sputtering target layer used in Specimens 1 to 7 were measured, and the crack density after surface polishing of the target material was confirmed. Based on the analysis results of the microstructure of the target layer, it was evaluated in four grades: very excellent, excellent, good, and bad.

[0085] The results of Experimental Examples 1 and 3 are summarized and shown in Table 2 below.

[0086]

Table 2

[0087] Experimental Example 4 - Evaluation of the surface of the sputtering target after sputtering Sputtering was performed using Test Pieces 1 to 7. After sputtering, visual evaluation of the surface of the target material used and measurement of the crack density using an optical microscope were carried out, and based on the results, evaluation was made in four grades of very excellent, excellent, good, and bad, and shown in Table 3 below.

[0088]

Table 3

[0089] The features, structures, effects, etc. exemplified in the above-described embodiments can be combined or modified for other embodiments by those having ordinary knowledge in the field to which the embodiments belong. Therefore, the content related to such combinations and modifications should be construed as being included in the scope of the present invention.

Description of Reference Numerals

[0090] 100 Target layer 200 Substrate 300 Alloy thin film 400 Workpiece

Claims

1. A substrate, and an alloy target layer provided on the substrate and having a proportion of an amorphous phase of 98.0% or more, the sputtering target comprising: wherein the porosity of the target layer is 0.1% or less, the target layer contains an iron (Fe)-based alloy composed of iron (Fe), Cr, Mo, B, and C, and the contents of B and C are each 10 wt.% or less with respect to the entire iron (Fe)-based alloy. The sputtering target.

2. The sputtering target according to claim 1, wherein the thickness of the target layer is 50 to 4000 μm.

3. The sputtering target according to claim 1, wherein the substrate is a single plate, and the target layer provided on the substrate has a single composition.

4. Preparing a substrate; forming a target layer having a proportion of an amorphous phase of 98.0% or more by cold spraying an iron (Fe)-based amorphous alloy powder or an iron (Fe)-based alloy powder having a composition capable of forming an amorphous phase on the substrate, the method for manufacturing a sputtering target comprising: wherein the iron (Fe)-based alloy powder is an iron (Fe)-based alloy powder composed of iron (Fe), Cr, Mo, B, and C, the porosity of the target layer is 0.1% or less, and the contents of B and C are each 10 wt.% or less with respect to the entire iron (Fe)-based alloy powder. The method for manufacturing a sputtering target.

5. The method for manufacturing a sputtering target according to claim 4, wherein the average particle size of the iron (Fe)-based alloy powder is 40 μm or less.

6. The method for manufacturing a sputtering target according to claim 4, wherein the thickness of the target layer is 50 to 4000 μm.

7. The method for manufacturing a sputtering target according to claim 4, wherein the proportion of the amorphous phase contained in the target layer is 0.96 to 1 times the proportion of the amorphous phase contained in the iron (Fe)-based alloy powder.

8. The method for manufacturing a sputtering target according to claim 4, further comprising heat-treating the sputtering target at a temperature lower than the crystallization temperature (Tx) of the iron (Fe)-based alloy powder.

9. A method for manufacturing an alloy thin film, comprising colliding ionized gas atoms with a sputtering target manufactured according to any one of claims 4 to 8 to deposit an element contained in the target layer onto a workpiece.

Citation Information

Patent Citations

  • Hard metal materials, hard metal coatings, methods of treating metal materials and methods of forming metal coatings

    JP2005524776A

  • Sputtering target and method for production thereof

    JP2009263796A

  • Aluminum alloys for sputtering target with high corrosion resistance and lightness and method of producing the same

    KR1020190109863A