TWI798580B - Fe-Si-B-Nb system target - Google Patents

Abstract

The present invention provides a Fe-Si-B-Nb based target material, which can suppress the wear or damage of the blade of the cutting tool, suppress the generation of cracks or gaps in the target material body, and can also suppress the target material in the machining of the target material. Occurrence of unevenness on the surface. In the Fe-Si-B-Nb based target material of the present invention, the composition formula of the atomic ratio is Fe _100-XYZa Si _X B _Y Nb _{Z Ma} , 15≦X+Y≦35, 0.3≦X/Y≦2.0, 1≦Z≦20, 0<a≦20 means that M is one or more elements selected from the group consisting of Al, Ti, V, Cr, Mn, Cu, Zr, Mo, W, and C, and the rest Inevitable impurities are included, and the average value of the Vickers hardness measured at 5 measurement points is 300 HV to 1100 HV, and the Vickers hardness is preferably in the range of 500 HV to 1000 HV.

Description

Fe-Si-B-Nb system target

The present invention relates to, for example, an Fe-Si-B-Nb-based target used for forming a soft magnetic film.

The miniaturization and weight reduction of various products including electronic equipment are progressing, and functional films are being applied. For example, in Patent Document 1, as a soft magnetic film suitable for a core material such as a magnetic head, a soft magnetic film containing Fe as a main component and containing a metal element selected from the group consisting of Nb, Nb-Ta, and Ta is proposed. A soft magnetic film of semi-metal elements in the group consisting of B (boron) and B-Si, and N (nitrogen). The soft magnetic film composed of Fe-Si-B-Nb-N has low coercive force, low magnetostriction and high saturation magnetic flux compared with the conventional soft magnetic film containing Co-Nb-Zr alloy. It is a useful technology because it has excellent soft magnetic properties such as density and good thermal stability, and is also excellent in corrosion resistance and wear resistance.

Furthermore, the soft magnetic film composed of Fe-Si-B-Nb-N can be formed by sputtering, for example. Specifically, the following method is proposed: using Fe as the main component and containing a metal element selected from the group consisting of Nb, Nb-Ta and Ta, a metal element selected from the group consisting of B and B-Si The Fe-Si-B-Nb alloy of the half-metal element is used as the target, and nitrogen gas is periodically mixed in an inert sputtering gas such as Ar to form a film whose composition is modulated in the film thickness direction, and then Carry out heat treatment. [Prior art literature] [Patent Document]

[Patent Document 1] Japanese Patent Laid-Open No. 2-163911

[Problems to be Solved by the Invention] The Fe-Si-B-Nb-based alloy target disclosed in Patent Document 1 is a so-called difficult-to-cut material with a high possibility of cracks, chipping, and falling off of the target body during machining to the shape and size of the target. . Therefore, during machining, the blade of the cutting tool may be worn or damaged, and unevenness may be induced on the surface of the obtained target material, or the target material body may be damaged in some cases.

The object of the present invention is to provide a Fe-Si-B-Nb-based target material, which can suppress the blade of the cutting tool in the machining of the Fe-Si-B-Nb-based target material (hereinafter also referred to as "target material"). Wear or breakage of the target material can be suppressed, cracks or gaps in the target body can be suppressed, and unevenness on the target surface can also be suppressed. [Means to solve the problem]

Regarding the target material of the present invention, the atomic ratio composition formula is Fe _100-XYZa Si _X B _Y Nb _Z M _a , 15≦X+Y≦35, 0.3≦X/Y≦2.0, 1≦Z≦20, 0< a≦20 means that M is one or more elements selected from the group consisting of Al, Ti, V, Cr, Mn, Cu, Zr, Mo, W, and C, and the remainder contains unavoidable impurities, and in The average value of the Vickers hardness (Vickers hardness) measured at five measurement points was 300 HV to 1100 HV.

The average value of the Vickers hardness measured at five measurement points of the target material of the present invention is preferably 500 HV to 1000 HV. [Effect of the invention]

In the machining of the target, the present invention can suppress the abrasion or breakage of the blade of the cutting tool, suppress the generation of cracks or notches in the target body, and can also suppress the generation of unevenness on the surface of the target. Therefore, it becomes a technique useful for manufacturing parts excellent in the above-mentioned soft magnetic properties, thermal stability, corrosion resistance, wear resistance, and the like.

The target material of the present invention has a Vickers hardness specified by Japanese industrial standard (JIS) Z 2244 in the range of 300 HV to 1100 HV. The target of the present invention makes the average value of the Vickers hardness measured at 5 measurement points within a specific range of 300 HV to 1100 HV, and is used for machining such as cutting or grinding to form the shape and size of the target. During processing, in addition to suppressing the occurrence of cracks or notches in the target body, it is also possible to suppress the occurrence of unevenness on the surface. Therefore, the target material of the present invention has a smooth surface, and it is possible to suppress induction of abnormal discharge or scattering of nodules and adhesion to the target material. It is preferable to set all the Vickers hardnesses measured at the above-mentioned five measurement points to a specific range of 300 HV to 1100 HV.

In addition, the target material of the present invention can suppress the generation of built-up edge (built-up edge) on inserts such as milling machines and lathes, for example, by setting the Vickers hardness to 300 HV or more. That is, the target material of the present invention can suppress the cutting amount of the blade accompanying the growth of the built-up edge from gradually increasing as the cutting process progresses, and can reduce the size difference of the target material at the start of cutting and the end of cutting, and It is also possible to suppress the breakage of the blade accompanying the peeling of the built-up edge.

In addition, if there is a low-hardness part in the eroded region of the target, for example, in the Fe-based alloy matrix phase, only the low-hardness part will remain or fall off, and the surface of the eroded region of the target will become rough. It is easy to become the starting point of abnormal discharge. Therefore, the target material of the present invention has a Vickers hardness of 300 HV or more. And, from the same reason as above, the target material according to the embodiment of the present invention preferably has a Vickers hardness of 500 HV or higher, more preferably 550 HV or higher.

The target material of this invention can suppress the abrasion amount of the insert, such as a milling machine or a lathe, for example, by making a Vickers hardness 1100 HV or less. That is, as the target material of the present invention is cut, the cutting amount of the blade accompanying the wear of the blade gradually decreases, and in addition to being able to suppress the dimensional difference between the target material at the start of cutting and the end of cutting from becoming large, Breakage of the blade can also be suppressed. And, from the same reason as above, the target material according to the embodiment of the present invention preferably has a Vickers hardness of 1000 HV or less, more preferably 950 HV or less.

The Vickers hardness mentioned in the present invention means that, in addition to suppressing the above-mentioned generation of cracks or cracks in the main body of the target, from the viewpoint of suppressing the generation of abnormal discharge during film formation, the hardness on any 5 points of the eroded surface of the target is The average value of the Vickers hardness measured at each measurement point is in the range of 300 HV to 1100 HV. In addition, the Vickers hardness was measured at a total of 5 positions corresponding to arbitrary four positions on the outer peripheral portion and positions corresponding to the center portion in the planar direction of the eroded surface of the target. At this time, the load was 9.8 N, and the pressing time was 10 seconds. In addition, the target material according to the embodiment of the present invention preferably does not have a Fe-Si-B-Nb-based composite compound phase in the metal structure from the viewpoint of a Vickers hardness of 300 HV to 1100 HV.

Regarding the target material of the present invention, the atomic ratio composition formula is Fe _100-XYZa Si _X B _Y Nb _Z M _a , 15≦X+Y≦35, 0.3≦X/Y≦2.0, 1≦Z≦20, 0< a≦20 indicates that M is one or more elements selected from the group consisting of Al, Ti, V, Cr, Mn, Cu, Zr, Mo, W, and C, and the remainder contains unavoidable impurities. The contents of Si, B, Nb, and M elements can be appropriately adjusted within a range that does not greatly impair soft magnetic properties, thermal stability, corrosion resistance, and wear resistance. In the target material of the present invention, a soft magnetic film having a low coercive force can be obtained by setting the total amount of Si and B, that is, X+Y in the composition formula to 15 or more. Moreover, it is preferable that X+Y should be 20 or more in the target material which concerns on embodiment of this invention from the same reason as above. Moreover, the target material of this invention can obtain the soft magnetic film which has a high saturation magnetic flux density by making X+Y into 35 or less. Moreover, it is preferable that X+Y is 33 or less in the target material which concerns on embodiment of this invention from the same reason as above.

The target material of the present invention can obtain a soft magnetic film having thermal stability by setting the ratio of Si to B, that is, X/Y of the composition formula, to be 0.3 to 2.0. Moreover, it is preferable that X/Y shall be 0.7 or more and 1.6 or less for the target material which concerns on embodiment of this invention from the same reason as above.

In the target material of the present invention, a soft magnetic film having corrosion resistance can be obtained by setting the Nb content, that is, Z in the composition formula to 1 or more. Moreover, it is preferable that Z is 3 or more in the target material which concerns on embodiment of this invention from the same reason as above. Moreover, the target material of this invention can obtain the soft magnetic film which has a high saturation magnetic flux density by making Z into 20 or less. Moreover, it is preferable that Z is 10 or less in the target material which concerns on embodiment of this invention from the same reason as above. In addition, the target material of this invention can also acquire the same effect as above by substituting a part or all of Nb with Ta.

The target of the present invention contains more than 0 one or more elements selected from the group consisting of Al, Ti, V, Cr, Mn, Cu, Zr, Mo, W, and C, that is, a in the composition formula exceeds 0. Thereby, when the target material of the present invention heat-treats an amorphous film formed by sputtering or the like, it has the effect of precipitation of fine nuclei, and can form a microcrystalline film starting from the nuclei, thereby obtaining a low-distortion film. Coercive soft magnetic film. Moreover, it is preferable that a is 0.5 or more in the target material which concerns on embodiment of this invention from the same reason as above. Moreover, the target material of this invention can obtain the soft magnetic film which has a high saturation magnetic flux density by making a into 20 or less. Moreover, it is preferable that a is 10 or less in the target material which concerns on embodiment of this invention from the same reason as above. Moreover, it is preferable that a is set to 5 or less in the target material which concerns on embodiment of this invention from the same reason as above.

The target material of the present invention can be obtained, for example, by a powder sintering method. Specifically, it can be obtained by pressurizing and sintering a mixed powder obtained by mixing pure metal powder or alloy powder so as to obtain the above component composition. As the alloy powder, in order not to form a Fe-Si-B-Nb complex compound phase in the metal structure of the target as much as possible, it is preferable to use Fe-Si alloy powder, Fe-B alloy powder, Fe-Nb alloy powder, Fe- Si-B alloy powder, Fe-Si-Nb alloy powder, Fe-B-Nb alloy powder, Fe-Si-M alloy powder, Fe-B-M alloy powder, Fe-Nb-M alloy powder, Fe-Si-B-M alloy Powder, Fe-Si-Nb-M alloy powder, Fe-B-Nb-M alloy powder. In addition, as pressure sintering, for example, a hot isostatic pressing (HIP) method, a hot pressing method, an electrical sintering method, or the like can be applied.

The pressurized sintering is preferably carried out under conditions of a sintering temperature of 700° C. to 1300° C., a pressurized pressure of 30 MPa to 200 MPa, and 1 hour to 10 hours. By setting the sintering temperature to 700° C. or higher, the powder can be sintered and the generation of voids can be suppressed. In addition, melting of the powder can be suppressed by setting the sintering temperature to 1300° C. or lower. The target material of the present invention is preferable in terms of suppressing the formation of Fe-Si-B-Nb composite compound phase and suppressing the generation of voids when HIP sintering the mixed powder obtained by mixing pure metal powder. Sintering is carried out under the condition that the sintering temperature is 700°C to 900°C. In addition, by setting the applied pressure to 30 MPa or more, the progress of sintering can be promoted and the generation of voids can be suppressed. In addition, by setting the applied pressure to 200 MPa or less, it is possible to suppress the introduction of residual stress into the target during sintering, thereby suppressing the occurrence of cracks after sintering. In addition, by setting the sintering time to 1 hour or more, the progress of sintering can be accelerated, and generation of voids can be suppressed. In addition, by setting the sintering time to 10 hours or less, it is possible to suppress a decrease in production efficiency. [Example]

First, Fe powder, Si powder, B powder, Nb powder, and Cu powder are prepared. Moreover, in order to obtain the target material as Example 1 of the present invention, the composition formula in atomic ratio is Fe ₆₆ Si _13.5 B _14.5 Nb ₅ Cu ₁ , (X+Y=28, X/Y=0.9, Z=5, a= In the method 1), each powder prepared above is weighed and mixed in a V-type mixer to obtain a mixed powder. Then, the mixed powder was filled into a capsule made of soft iron, and degassed and sealed at 450° C. for 4 hours. Then, under the conditions of 750° C., 122 MPa, and 1 hour, the capsule was pressurized and sintered by HIP to produce a sintered body.

In order to obtain the target material as Example 2 of the present invention, gas atomized powder and Nb powder composed of an alloy having the composition formula of Fe _69.5 Si _14.2 B _15.3 Cu ₁ in atomic ratio were prepared, and the composition formula of atomic ratio was Fe ₆₆ Si _13.5 B _14.5 Nb ₅ Cu ₁ , (X+Y=28, X/Y=0.9, Z=5, a=1), weigh the powders prepared above and mix them in a V-type mixer to obtain a mixed powder. Then, the mixed powder was filled into a mold of a hot press device, and pressurized and sintered under the conditions of 1000° C., 30 MPa, and 2 hours to produce a sintered body.

In order to obtain the target material as Example 3 of the present invention, Fe powder, Si powder, B powder, Nb powder and Ti powder were prepared, and the composition formula in terms of atomic ratio was Fe ₆₀ Si _4.5 B _14.5 Nb ₁ Ti ₂₀ , (X+Y= 19. X/Y=0.3, Z=1, a=20), after weighing the powders prepared above, mix them in a V-type mixer to obtain mixed powders. Then, the mixed powder was filled into a capsule made of soft iron, and degassed and sealed at 450° C. for 4 hours. Then, under the conditions of 950° C., 122 MPa, and 1 hour, the capsule was pressurized and sintered by HIP to produce a sintered body.

In order to obtain the target material as Example 4 of the present invention, Fe powder, Si powder, B powder, Nb powder and V powder were prepared, and the composition formula in terms of atomic ratio was Fe _44.9 Si _23.3 B _11.7 Nb ₂₀ V _0.1 , (X+Y= 35. X/Y=2.0, Z=20, a=0.1), after weighing the powders prepared above, mix them in a V-type mixer to obtain mixed powders. Then, the mixed powder was filled into a capsule made of soft iron, and degassed and sealed at 450° C. for 4 hours. Then, under the conditions of 950° C., 122 MPa, and 1 hour, the capsule was pressurized and sintered by HIP to produce a sintered body.

In order to obtain the target material as Example 5 of the present invention, Fe powder, Si powder, B powder, Nb powder and Cr powder were prepared, and the composition formula in terms of atomic ratio was Fe ₅₆ Si ₈ B ₁₇ Nb ₉ Cr ₁₀ , (X+Y= 25. X/Y=0.5, Z=9, a=10), after weighing the powders prepared above, mix them in a V-type mixer to obtain mixed powders. Then, the mixed powder was filled into a capsule made of soft iron, and degassed and sealed at 450° C. for 4 hours. Then, under the conditions of 950° C., 122 MPa, and 1 hour, the capsule was pressurized and sintered by HIP to produce a sintered body.

In order to obtain the target material as Example 6 of the present invention, Fe powder, Si powder, B powder, Nb powder and Mo powder were prepared, and the composition formula in terms of atomic ratio was Fe ₆₅ Si ₉ B ₆ Nb ₁₅ Mo ₅ , (X+Y= 15. X/Y=1.5, Z=15, a=5), after weighing the powders prepared above, mix them in a V-type mixer to obtain mixed powders. Then, the mixed powder was filled into a capsule made of soft iron, and degassed and sealed at 450° C. for 4 hours. Then, under the conditions of 950° C., 122 MPa, and 1 hour, the capsule was pressurized and sintered by HIP to produce a sintered body.

In order to obtain the target material as Example 7 of the present invention, Fe powder, Si powder, B powder, Nb powder, Mn powder, Zr powder and W powder were prepared, and the composition formula in terms of atomic ratio was Fe ₅₈ Si _13.5 B _14.5 Nb ₅ Mn ₃ Zr ₃ W ₃ , (X+Y=28, X/Y=0.9, Z=5, a=9), weigh the powders prepared above, and mix them in a V-type mixer to obtain a mixed powder . Then, the mixed powder was filled into a capsule made of soft iron, and degassed and sealed at 450° C. for 4 hours. Then, under the conditions of 950° C., 122 MPa, and 1 hour, the capsule was pressurized and sintered by HIP to produce a sintered body.

In order to obtain a target as a comparative example, a gas mist with the atomic ratio composition formula Fe ₆₆ Si _13.5 B _14.5 Nb ₅ Cu ₁ (X+Y=28, X/Y=0.9, Z=5, a=1) was prepared It was pulverized, filled into capsules made of soft iron, and degassed and sealed at 450° C. for 4 hours. Then, under the conditions of 950° C., 122 MPa, and 1 hour, the above-mentioned capsule was pressurized and sintered by HIP to produce a sintered body.

Each of the sintered compacts obtained above was machined to produce a target. At this time, it was confirmed that none of the targets of Invention Example 1 to Invention Example 7 had cracks during machining, and that the surface after finishing was smooth without unevenness. On the other hand, the target as a comparative example had cracks during machining, and could not be machined into the shape of the target.

For each of the sintered bodies obtained above, the Vickers hardness was measured at a total of 5 locations at 4 locations corresponding to the outer peripheral portion and 5 locations corresponding to the central portion in the planar direction of the surface serving as the eroded surface of the target. It should be noted that the measurement interval is measured by setting a distance between indentations that is not affected by the measurement. In addition, the Vickers hardness was measured in accordance with JIS Z 2244 using MVK-E manufactured by Akashi Seisakusho Co., Ltd., and measured at a load of 9.8 N and a pressing time of 10 seconds. The results are shown in Table 1.

[Table 1] Vickers Hardness [HV] Measuring point average value 1 2 3 4 5 Example 1 of the present invention 609 622 630 833 914 722 Example 2 of the present invention 893 903 884 896 881 891 Example 3 of the present invention 1051 258 896 556 742 701 Example 4 of the present invention 630 602 749 713 936 726 Example 5 of the present invention 991 692 498 613 1090 777 Example 6 of the present invention 463 486 373 507 341 434 Example 7 of the present invention 551 830 619 1064 1173 847 comparative example 1262 1239 1248 1239 1267 1251

The average value of the Vickers hardness of the target material which is a comparative example exceeded 1100 HV. On the other hand, it was confirmed that the average values of the Vickers hardnesses of the targets of Invention Example 1 to Invention Example 7 were all in the range of 300 HV to 1100 HV. From this, it can be confirmed that the target material of the present invention suppresses the occurrence of cracks or notches during machining, and has a smooth surface without unevenness on the surface after finishing. Thereby, the target of the present invention can be expected to be useful as a target for forming a soft magnetic film by suppressing induction of abnormal discharge or scattering of nodules and adhering to the target material.

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Claims (2)

A Fe-Si-B-Nb based target, wherein the atomic ratio composition formula is Fe _100-XYZa Si _X B _Y Nb _Z M _a , 15≦X+Y≦35, 0.3≦X/Y≦2.0, 1≦ Z≦20, 0<a≦20 means that M is one or more elements selected from the group consisting of Al, Ti, V, Cr, Mn, Zr, Mo, W, and C, and the remainder contains unavoidable impurities, and the average value of the Vickers hardness measured at 5 measurement points is 300HV~1100HV, and there is no Fe-Si-B-Nb composite compound phase in the metal structure. The Fe-Si-B-Nb based target material according to claim 1, wherein the average value of the Vickers hardness measured at 5 measurement points is 500HV~1000HV.