Iron-silicon-boron target material as well as preparation method and application thereof

Abstract

The invention provides an iron-silicon-boron target material as well as a preparation method and application thereof, and relates to the technical field of target material preparation. The preparation method of the iron-silicon-boron target material comprises the following steps that S1, raw materials including, by weight, 75%-85% of iron, 10%-15% of silicon and 5%-10% of boron are mixed and smelted, an iron-silicon-boron alloy blank is obtained, and the iron-silicon-boron alloy blank is prepared from, by weight, 75%-85% of iron, 10%-15% of silicon and 5%-10% of boron; s2, refining the iron-silicon-boron alloy blank to obtain alloy powder with a particle size range of 15-45 [mu] m; and S3, the alloy powder is subjected to compression molding, and the iron-silicon-boron target material is obtained. According to the preparation method disclosed by the invention, the density and the purity of the iron-silicon-boron target material are synergistically improved by regulating and controlling the ratio of the raw materials of iron, silicon and boron and combining the whole preparation process. The iron-silicon-boron target material prepared by the method is uniform and fine in grain, the density can reach 99% or above, the purity is 99.9% or above, and the problem that a traditional target material is insufficient in density and purity is solved.

Description

Technical Field

[0001] This invention relates to the field of target preparation technology, and in particular to an iron-silicon-boron target, its preparation method, and its application. Background Technology

[0002] Iron-silicon-boron alloys are widely used in the preparation of amorphous and nanocrystalline thin films due to their excellent magnetic properties. Iron-silicon-boron sputtering targets are the core raw materials for sputtering these films, and their performance directly determines the quality of the film. However, current techniques for preparing iron-silicon-boron sputtering targets often suffer from complex processes and difficulties in industrial production. Furthermore, the prepared targets are prone to defects such as coarse grains, low density, and low purity.

[0003] These defects lead to frequent arcing discharges on the target during sputtering, affecting not only sputtering efficiency but also resulting in numerous surface defects and insufficient density in the prepared film. This, in turn, impacts the magnetic properties of the film, increases magnetic loss, and makes it difficult to meet the high-quality preparation requirements of amorphous or nanocrystalline thin films. Therefore, developing a simple, industrially feasible method for preparing high-performance iron-silicon-boron targets is of great significance. Summary of the Invention

[0004] This invention addresses the shortcomings of current iron-silicon-boron (FeSiB) sputtering targets, such as coarse grains, low density, and low purity. It provides a method for preparing FeSiB sputtering targets, which significantly improves the density and purity of the FeSiB sputtering targets by using a specific ratio of iron, silicon, and boron raw materials combined with a specific preparation process.

[0005] Another object of the present invention is to provide an iron-silicon-boron target.

[0006] Another object of the present invention is to provide an application of iron-silicon-boron target material in the preparation of amorphous and nanocrystalline thin films.

[0007] Another object of the present invention is to provide a composite thin film material.

[0008] In a first aspect, the present invention protects a method for preparing an iron-silicon-boron target material, comprising the following steps: S1. Iron, silicon, and boron are mixed according to their weight percentages and smelted to obtain an iron-silicon-boron alloy billet. The weight percentages of iron, silicon, and boron are: iron 75-85%, silicon 10-15%, and boron 5-10%. S2. The iron-silicon-boron alloy billet is refined to obtain alloy powder with a particle size range of 15-45μm; S3. Press the alloy powder into shape to obtain the iron-silicon-boron target material. The pressing pressure is 300-500MPa, the holding time is 10-20min, and the forming temperature is 200-300℃.

[0009] According to the method for preparing an iron-silicon-boron target material protected by the present invention, preferably, the refining treatment in S2 is a process of ball milling followed by sieving with hydrogen gas flow, preferably with a ball-to-material ratio of 10-15:1, a ball milling speed of 300-400 r / min, and a ball milling time of 2-4 h. According to the method for preparing an iron-silicon-boron target material protected by the present invention, preferably, the hydrogen flow rate in S2 is 1~3 L / min.

[0010] According to the preparation method of the iron-silicon-boron target material protected by the present invention, preferably, the smelting temperature in S1 is 1500~1600℃ and the holding time is 30~60min.

[0011] According to the preparation method of the iron-silicon-boron target material protected by the present invention, preferably, electromagnetic stirring is added during the smelting process described in S1, and preferably the rotation speed of the electromagnetic stirring is 200~300 r / min.

[0012] According to the method for preparing an iron-silicon-boron target material protected by the present invention, preferably, the smelting temperature in step S1 is 1600℃ and the holding time is 30 minutes; the pressing pressure in step S3 is 500 MPa, the holding time is 10 minutes, and the forming temperature is 300℃. Secondly, the present invention also specifically protects an iron-silicon-boron target material prepared by a method for preparing an iron-silicon-boron target material.

[0013] According to the iron-silicon-boron target material protected by the present invention, preferably, the iron-silicon-boron target material has a density greater than or equal to 99.0% and a purity greater than or equal to 99.90%.

[0014] Thirdly, the present invention also specifically protects the application of an iron-silicon-boron target material in the preparation of amorphous and nanocrystalline thin films.

[0015] Fourthly, the present invention also specifically protects a composite thin film material, which is prepared by magnetron sputtering of the iron-silicon-boron target material protected by the present invention on the substrate surface.

[0016] Beneficial effects: This invention provides a method for preparing iron-silicon-boron (FeSiB) sputtering targets. By controlling the ratio of iron, silicon, and boron elements in the raw materials and combining this method with the overall preparation process, the density and purity of the FeSiB sputtering targets are synergistically improved. The FeSiB sputtering targets prepared by this invention have uniform and fine grains, with a density of over 99% and a purity of over 99.9%, thus solving the problems of insufficient density and purity of traditional sputtering targets.

[0017] The iron-silicon-boron target of the present invention has excellent target performance, effectively improves the arc discharge phenomenon in the sputtering process, and makes the prepared film layer with fewer surface defects and a denser coating. It can be used efficiently to prepare amorphous or nanocrystalline thin films and significantly reduces the magnetic loss of the film. Detailed Implementation

[0018] The following examples are for illustrative purposes only and are not intended to limit the scope of the invention. Where specific techniques or conditions are not specified in the examples, they should be performed according to the techniques or conditions described in the literature in this field, or according to the product instructions. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased from legitimate channels.

[0019] In a specific embodiment, the present invention provides a method for preparing an iron-silicon-boron target material, comprising the following steps: S1. Iron, silicon, and boron are mixed according to their weight percentages and smelted to obtain an iron-silicon-boron alloy billet. The weight percentages of iron, silicon, and boron are: iron 75-85%, silicon 10-15%, and boron 5-10%. S2. The iron-silicon-boron alloy billet is refined to obtain alloy powder with a particle size range of 15~45μm; S3. Press the alloy powder into shape to obtain an iron-silicon-boron target material. The pressing pressure is 300~500MPa, the holding time is 10~20min, and the forming temperature is 200~300℃.

[0020] It should be noted that: In the preparation process of this invention, the proportion of smelting raw materials can be controlled to prepare a high-purity iron-silicon-boron alloy billet with uniform composition. Further refining treatment is combined to refine the silicon-boron alloy billet to alloy powder with a particle size range of 15~45μm. Combined with a pressing and molding process that matches the particle size, a high-purity, high-density iron-silicon-boron target material is prepared.

[0021] In some specific embodiments, in order to further control impurities and improve purity, the smelting mentioned in this invention is preferably carried out in an induction melting furnace, where a vacuum / inert atmosphere is more conducive to reducing impurity content.

[0022] In some specific embodiments, the weight percentage of iron in the ratio of raw materials iron, silicon, and boron mentioned in S1 of this invention can be, for example, 75%, 78%, 80%, 82%, 85%, or any other arbitrary range; the weight percentage of silicon can be, for example, 10%, 11%, 12%, 13%, 14%, 15%, or any other arbitrary range; and the weight percentage of boron can be, for example, 5%, 6%, 7%, 8%, 9%, 10%, or any other arbitrary range. The three components can be combined in any ratio within the above ranges, with a total of 100%.

[0023] In some specific embodiments, the particle size range of the alloy powder mentioned in S1 of this invention is 15~45μm, meaning that all particles in the alloy powder have a particle size within this range, with the maximum particle size not exceeding 45μm and the minimum particle size being 15μm. By combining particles of this size range, a significant increase in the density of the iron-silicon-boron target material after pressing can be achieved.

[0024] In some specific embodiments, the pressing pressure mentioned in S3 of the present invention can be a point value such as 300 MPa, 350 MPa, 400 MPa, 450 MPa, 500 MPa or any range of values; the holding time can be a point value such as 10 min, 15 min, 20 min; and the molding temperature can be a point value such as 200, 250°C, 300°C.

[0025] In order to achieve the refining effect of the present invention, in some specific exemplary embodiments, the refining treatment in S2 is a sieving treatment after ball milling with hydrogen gas flow. Preferably, the ball-to-material ratio of the ball milling process is 10~15:1, the ball milling speed is 300~400 r / min, and the ball milling time is 2~4 h.

[0026] By optimizing the ball-to-material ratio, milling speed, and milling time, both sufficient impact and shearing of the material can be ensured, while excessive compression and agglomeration can be avoided, thus achieving an ideal refining effect. The ball-to-material ratio mentioned in this invention can be, for example, a point value such as 10:1, 11:1, 12:1, 13:1, 14:1, 15:1, or any range thereof; the milling speed can be, for example, a point value such as 300 r / min, 350 r / min, 400 r / min, or any range thereof; and the milling time can be, for example, 2 h, 3 h, 4 h, etc.

[0027] Hydrogen gas not only plays a protective role in ball milling, preventing powder oxidation, but also assists in breaking down the crystal structure of the alloy through unique reactions such as hydrogenation and disproportionation, further promoting particle and grain refinement. The preferred hydrogen flow rate for ball milling mentioned in this invention is 1~3 L / min, for example, values ​​such as 1 L / min, 2 L / min, and 3 L / min.

[0028] In some specific embodiments, in order to further obtain a high-purity iron-silicon-boron alloy billet with uniform and fine grains, so that the components of the raw materials form an iron-silicon-boron alloy billet with uniformly distributed crystal phases, the smelting temperature mentioned in S1 of this invention is 1500~1600℃, and the holding time is 30~60min.

[0029] In a specific embodiment, in order to further improve the uniformity and density of the crystalline phase of the iron-silicon-boron alloy billet, electromagnetic stirring is added during the smelting process described in S1 of the present invention, preferably at a speed of 200~300 r / min.

[0030] In some specific exemplary embodiments, the present invention preferably provides a method for preparing iron-silicon-boron target material, wherein the smelting temperature in S1 is 1600℃ and the holding time is 30 minutes; the pressing pressure in S3 is 500 MPa, the holding time is 10 minutes, and the forming temperature is 300℃.

[0031] In a specific embodiment, the present invention also specifically protects an iron-silicon-boron target material prepared by a method for preparing the iron-silicon-boron target material.

[0032] In some specific embodiments, the iron-silicon-boron target material prepared by the method of the present invention has a density greater than or equal to 99.0% and a purity greater than or equal to 99.90%.

[0033] In a specific embodiment, the present invention also specifically protects the application of an iron-silicon-boron target material in the preparation of amorphous and nanocrystalline thin films.

[0034] In a specific embodiment, the present invention also specifically protects a composite thin film material, which is prepared by magnetron sputtering of the iron-silicon-boron target on the substrate surface.

[0035] The iron-silicon-boron target material prepared by this invention has high purity and high density, and the target material grains are uniform and fine. When this target material is used to sputter to prepare composite thin film materials such as amorphous thin films and nanocrystalline thin films, there is no obvious arc discharge phenomenon during the sputtering process, the film surface is smooth without obvious defects, the density is high, and the magnetic loss is reduced by 12% or more compared with the thin film prepared by traditional target materials.

[0036] Example 1 A method for preparing an iron-silicon-boron target material includes the following steps: S1. Weigh 80% iron, 12% silicon, and 8% boron by weight percentage, place the raw materials in an induction melting furnace, and smelt at 1550℃ for 45 minutes. During the smelting process, perform electromagnetic stirring at a speed of 250r / min to obtain a uniform iron-silicon-boron alloy billet. S2. Place the alloy billet in a ball mill, introduce a hydrogen flow of 2L / min, and ball mill for 3 hours at a ball-to-material ratio of 12:1 and a rotation speed of 350r / min. Then, sieve the crushed powder to obtain alloy powder with a particle size distribution of 15~45μm. S3.3. The alloy powder is pressed into shape under a pressure of 400MPa and a temperature of 250℃ for 15 minutes. Then the formed blank is machined to obtain the iron-silicon-boron target material that meets the requirements of the drawing.

[0037] The iron-silicon-boron target material prepared in this embodiment has uniform and fine grains. When this target material is used to prepare amorphous thin films by sputtering, there is no obvious arc discharge phenomenon during the sputtering process, the film surface is smooth without obvious defects, the density is high, and the magnetic loss is reduced by 15% compared with the thin films prepared by traditional target materials.

[0038] Example 2 A method for preparing an iron-silicon-boron target material includes the following steps: S1. Weigh 75% iron, 15% silicon, and 10% boron by weight percentage, place the raw materials in an induction melting furnace, and smelt at 1500℃ for 60 minutes. During the smelting process, perform electromagnetic stirring at a speed of 200r / min to obtain a uniform iron-silicon-boron alloy billet. S2. Place the alloy billet in a ball mill, introduce a hydrogen flow of 1L / min, and ball mill for 4 hours with a ball-to-material ratio of 10:1 and a rotation speed of 300r / min. Then, sieve the crushed powder to obtain alloy powder with a particle size distribution of 15~45μm. S3. The alloy powder is pressed into shape under a pressure of 300MPa and a temperature of 200℃ for 20 minutes. The formed blank is then machined to obtain an iron-silicon-boron target material that meets the requirements of the drawing.

[0039] The iron-silicon-boron target material prepared in this embodiment has uniform and fine grains. When this target material is used to prepare amorphous thin films by sputtering, there is no obvious arc discharge phenomenon during the sputtering process, the film surface has few defects, the density is better, and the magnetic loss is reduced by 12% compared with the film prepared by traditional target materials.

[0040] Example 3 A method for preparing an iron-silicon-boron target material includes the following steps: S1. Weigh 85% iron, 10% silicon, and 5% boron by weight percentage, place the raw materials in an induction melting furnace, and smelt at 1600℃ for 30 minutes. During the smelting process, perform electromagnetic stirring at a speed of 300 r / min to obtain a uniform iron-silicon-boron alloy billet. S2. Place the alloy billet in a ball mill, introduce a hydrogen flow of 3L / min, and ball mill for 2 hours with a ball-to-material ratio of 15:1 and a rotation speed of 400r / min. Then, sieve the crushed powder to obtain alloy powder with a particle size distribution of 15~45μm. S3. The alloy powder is pressed into shape under a pressure of 500MPa and a temperature of 300℃ for 10 minutes. The formed blank is then machined to obtain an iron-silicon-boron target material that meets the requirements of the drawing.

[0041] The iron-silicon-boron target material prepared in this embodiment has uniform and fine grains. When this target material is used to sputter and prepare amorphous thin films, there is no obvious arc discharge phenomenon during the sputtering process. It has good density, smooth surface, and magnetic loss is reduced by 18% compared with thin films prepared by traditional target materials.

[0042] Comparative Example 1 A method for preparing an iron-silicon-boron target material includes the following steps: S1. Batching and smelting: Weigh 73% iron, 15% silicon and 12% boron by weight percentage, place the raw materials in an induction melting furnace, and smelt at 1550℃ for 45 minutes. During the smelting process, electromagnetic stirring is performed at a speed of 250r / min to obtain iron-silicon-boron alloy billet. S2. Place the alloy billet in a ball mill, introduce a hydrogen flow of 2L / min, and ball mill for 3 hours at a ball-to-material ratio of 12:1 and a rotation speed of 350r / min. Then, sieve the crushed powder to obtain alloy powder with a particle size distribution of 15~45μm. S3. The alloy powder is pressed into shape under a pressure of 400MPa and a temperature of 250℃ for 15 minutes. The formed blank is then machined to obtain an iron-silicon-boron target material that meets the requirements of the drawing.

[0043] The target material prepared in Comparative Example 1 has an uneven grain distribution. When this target material is used to prepare amorphous thin films by sputtering, severe arcing occurs during the sputtering process, frequently interrupting the sputtering process; the prepared film surface has a large number of pinholes and protrusions, resulting in low density, and the magnetic loss is only 3% lower than that of films prepared with traditional targets.

[0044] Result detection The iron-silicon-boron targets prepared in the examples and comparative examples were subjected to relevant performance tests, specifically the tests.

[0045] The test results are shown in Table 1.

[0046] Table 1 Serial Number Target density (%) Target purity (%) Reduction in magnetic loss (%) Example 1 99.2 99.92 15 Example 2 99.0 99.90 12 Example 3 99.3 99.93 18 Comparative Example 1 96.5 99.91 3 The target density (%) represents the percentage of the actual density to the theoretical density of the target, reflecting the proportion of pores inside the target. The higher the density, the lower the porosity, and the denser the target structure. The actual density of the target is determined using the Archimedes' displacement method.

[0047] The purity (%) of the target material was determined by inductively coupled plasma optical emission spectrometry (ICP-OES).

[0048] The detection results of the embodiments and comparative examples of this invention were obtained using the same method and under the same conditions.

[0049] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing an iron-silicon-boron target, characterized in that, Includes the following steps: S1. Iron, silicon, and boron are mixed according to their weight percentages and smelted to obtain an iron-silicon-boron alloy billet. The weight percentages of iron, silicon, and boron are: iron 75-85%, silicon 10-15%, and boron 5-10%. S2. The iron-silicon-boron alloy billet is refined to obtain alloy powder with a particle size range of 15~45μm; S3. Press the alloy powder into shape to obtain an iron-silicon-boron target material. The pressing pressure is 300~500MPa, the holding time is 10~20min, and the forming temperature is 200~300℃.

2. The method for preparing the iron-silicon-boron target material according to claim 1, characterized in that, The refining process described in S2 is a process of ball milling with hydrogen gas followed by sieving. The preferred ball-to-material ratio for the ball milling process is 10-15:1, the ball milling speed is 300-400 r / min, and the ball milling time is 2-4 h.

3. The method for preparing the iron-silicon-boron target material according to claim 2, characterized in that, The hydrogen flow rate described in S2 is 1~3L / min.

4. The method for preparing the iron-silicon-boron target material according to any one of claims 1 to 3, characterized in that, The smelting temperature described in S1 is 1500~1600℃, and the holding time is 30~60min.

5. The method for preparing the iron-silicon-boron target material according to claim 3, characterized in that, Electromagnetic stirring is added during the smelting process described in S1, and the preferred speed of the electromagnetic stirring is 200~300 r / min.

6. The method for preparing the iron-silicon-boron target material according to any one of claims 1 to 5, characterized in that, The smelting temperature described in S1 is 1600℃, and the holding time is 30 minutes; the pressing pressure described in S3 is 500MPa, the holding time is 10 minutes, and the forming temperature is 300℃.

7. An iron-silicon-boron target material prepared by the method of any one of claims 1 to 6.

8. The iron-silicon-boron sputtering target according to claim 7, characterized in that, The iron-silicon-boron sputtering target has a density of ≥99.0% and a purity of ≥99.90%.

9. The application of the iron-silicon-boron target material according to claim 7 or 8 in the preparation of amorphous and nanocrystalline thin films.

10. A composite thin film material, characterized in that, It is prepared by magnetron sputtering of the iron-silicon-boron target material as described in claim 7 or 8 on the substrate surface.