Cobalt-iron-boron target material and preparation method and application thereof

Abstract

The invention relates to a cobalt-iron-boron target material and a preparation method and application thereof.The preparation method comprises the following steps that after raw materials are mixed, cold isostatic pressing forming, alloying, crushing and sintering are conducted in sequence, and the cobalt-iron-boron target material is obtained; the alloying comprises first-stage calcination, second-stage calcination and third-stage calcination; the temperature rise final temperature of the first-stage calcination is 150-250 DEG C; the temperature rise final temperature of the second-stage calcination is 400-600 DEG C; and the temperature rise final temperature of the third-stage calcination is 750-900 DEG C. According to the method, the raw materials are directly mixed and formed, then the raw materials are converted into the alloyed cobalt-iron-boron green body through three-section calcination of alloying, the alloyed cobalt-iron-boron green body is sequentially crushed and sintered, and the uniformity and compactness of cobalt-iron-boron are further improved. Therefore, the cobalt-iron-boron target material obtained through the preparation method is uniform in component and high in density, the requirement of magnetron sputtering for the target material is met, meanwhile, the yield is increased, and the production cost is reduced.

Description

Technical Field

[0001] The invention relates to the technical field of sputtering target materials, and relates to a target material and a preparation method and application thereof, and in particular to a cobalt iron boron target material and a preparation method and application thereof. Background Art

[0002] Currently, the progress of magnetic storage technology is very significant. Perpendicular magnetic recording, as a high-density data storage technology, allows data to be stored in a direction perpendicular to the surface of the medium, which helps to increase the storage capacity of hard disk drives.

[0003] Cobalt-iron-boron alloy plays a key role in perpendicular magnetic recording technology due to its excellent magnetic properties. Due to its high magnetic permeability and high correction force, it can provide faster data transmission rate and greater storage density, and has been widely used in storage devices such as magnetic tapes, hard disk drives and magnetic random access memory (MRAM).

[0004] Common cobalt iron boron materials have three main preparation methods: the first is a roasting method, in which the raw materials of iron, cobalt and boron are heated and melted, and then cast, cooled and crushed in sequence to obtain a cobalt iron boron magnet. This preparation method has high energy consumption and the prepared cobalt iron boron magnet has poor performance; the second is a chemical precipitation method, in which a salt solution of iron, cobalt and boron is subjected to a coprecipitation reaction to generate a precursor precipitate, and then the cobalt iron boron magnet is prepared through dehydration, sintering and heat treatment in sequence. This preparation method is complex and has high cost; the third is a powder metallurgy method. CN117431510A discloses a method for preparing a cobalt iron boron target material for magnetic rotation storage, in which the cobalt iron boron target material is prepared by weighing an intermediate alloy powder for high-energy ball milling activation, cobalt plating, vacuum preheating, hot isostatic pressing and hot pressing sintering, back plate welding and other steps. This method has high raw material cost, and in the preparation process, cobalt is coated on the surface of the Fe-B alloy powder, which will lead to a decrease in the uniformity of the cobalt iron boron component.

[0005] In view of the defects of the existing technology, how to reduce the preparation cost and prepare a cobalt-iron-boron target with uniform composition and high density has become a problem that needs to be solved urgently. Summary of the invention

[0006] In order to solve the above technical problems, the present invention provides a cobalt iron boron target material and a preparation method and application thereof. The present invention directly mixes and shapes the raw materials, and then converts the raw materials into alloyed cobalt iron boron blanks through three-stage calcination of alloying, and the alloyed cobalt iron boron blanks are crushed and sintered in sequence, thereby further improving the uniformity and density of cobalt iron boron. Therefore, the cobalt iron boron target material obtained by the preparation method of the present invention has uniform composition and high density, which meets the requirements of magnetron sputtering for target materials, while improving the yield rate and reducing production costs.

[0007] To achieve this object, the present invention adopts the following technical solutions:

[0008] In a first aspect, the present invention provides a method for preparing a cobalt iron boron target material, the preparation method comprising the following steps: after mixing the raw materials, cold isostatic pressing, alloying, crushing and sintering are performed in sequence to obtain the cobalt iron boron target material; the alloying comprises one-stage calcination, two-stage calcination and three-stage calcination; the heating end temperature of the one-stage calcination is 150°C-250°C; the heating end temperature of the two-stage calcination is 400°C-600°C; the heating end temperature of the three-stage calcination is 750°C-900°C.

[0009] Among them, the heating end temperature of the first stage calcination can be 150°C, 180°C, 200°C, 220°C or 250°C, the heating end temperature of the second stage calcination can be 400°C, 450°C, 500°C, 550°C or 600°C, and the heating end temperature of the third stage calcination can be 750°C, 780°C, 800°C, 850°C, 880°C or 900°C, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0010] The present invention directly mixes and shapes the raw materials, and then converts the raw materials into alloyed cobalt iron boron blanks through three-stage calcination of alloying, and the alloyed cobalt iron boron blanks are crushed and sintered in sequence, thereby further improving the uniformity and density of cobalt iron boron. Therefore, the cobalt iron boron target material obtained by the preparation method of the present invention has uniform composition and high density, meets the requirements of magnetron sputtering for target materials, and at the same time improves the yield rate and reduces the production cost.

[0011] Preferably, the raw materials include an iron source, a boron source and a cobalt source.

[0012] Preferably, the iron source comprises iron powder.

[0013] Preferably, the boron source comprises boron powder.

[0014] Preferably, the cobalt source comprises cobalt powder.

[0015] Preferably, the molar ratio of the iron source, the boron source and the cobalt source is (15-20):(60-65):(15-25), for example, it can be 15:60:15, 15:65:15, 15:60:25, 15:65:25, 20:60:15, 20:60:25, 20:65:15 or 20:65:25, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0016] Preferably, the particle size D50 of the raw material is 10 μm-45 μm, for example, 10 μm, 20 μm, 30 μm, 40 μm or 45 μm, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0017] Preferably, the purity of the raw material is ≥99.99%, for example, it can be 99.99%, 99.992%, 99.995%, 99.998% or 99.999%, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0018] Preferably, the mixing method comprises ball milling.

[0019] Preferably, the ball-to-material ratio of the ball mill is (3-6):1, for example, 3:1, 4:1, 5:1, 5.5:1 or 6:1, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0020] Preferably, the ball milling comprises dry ball milling.

[0021] Preferably, the mixed atmosphere is an inert gas atmosphere.

[0022] Preferably, the inert gas atmosphere includes a nitrogen atmosphere and / or an argon atmosphere.

[0023] Preferably, the mixing time is 12h-24h, for example, 12h, 16h, 18h, 20h or 24h, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0024] Preferably, the cold isostatic pressing pressure is 150 MPa-280 MPa, for example, 150 MPa, 180 MPa, 200 MPa, 220 MPa or 250 MPa, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0025] Preferably, the holding time of the cold isostatic pressing is 5 min-10 min, for example, it can be 5 min, 6 min, 7 min, 8 min, 9 min or 10 min, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0026] Preferably, the alloying atmosphere is a vacuum atmosphere.

[0027] Preferably, the vacuum degree of the vacuum atmosphere is less than 1×10 -4 Pa, for example, can be 1×10 -5 Pa, 3×10 -5 Pa, 5×10 -5Pa, 7×10 -5 Pa or 9×10 -5 Pa, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0028] Preferably, the heating rate of the first-stage calcination is 2°C / min-5°C / min, for example, 2°C / min, 3°C / min, 4°C / min, 4.5°C / min or 5°C / min, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0029] Preferably, the holding time of the first calcination stage is 2h-4h, for example, 2h, 2.5h, 3h, 3.5h or 4h, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0030] Preferably, the heating rate of the second-stage calcination is 2°C / min-5°C / min, for example, 2°C / min, 3°C / min, 4°C / min, 4.5°C / min or 5°C / min, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0031] Preferably, the holding time of the second-stage calcination is 3h-6h, for example, 3h, 3.5h, 4h, 4.5h, 5h or 6h, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0032] Preferably, the heating rate of the three-stage calcination is 1°C / min-3°C / min, for example, it can be 1°C / min, 1.5°C / min, 2°C / min, 2.5°C / min or 3°C / min, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0033] Preferably, the holding time of the three-stage calcination is 2h-5h, for example, 2h, 2.5h, 3h, 3.5h, 4h or 5h, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0034] The present invention improves the density and uniformity of the cobalt iron boron target material through alloying by three-stage calcination. Among them, regulating the insulation temperature and insulation time of the first stage calcination in the alloying process is conducive to removing substances with low volatility points such as water vapor in the raw material powder, reducing the influence of these substances on the density of the cobalt iron boron target material in subsequent reactions; regulating the insulation temperature and insulation time of the second stage calcination in the alloying process makes the temperature field in the environment more uniform, which is conducive to the full contact of the powder in the raw material, and is also conducive to the reaction of the raw material powder in a more uniform temperature field, thereby further improving the uniformity of the cobalt iron boron target material; regulating the insulation temperature and insulation time of the three-stage calcination in the alloying process is conducive to the alloying reaction to proceed uniformly and stably, further improving the density and uniformity of the cobalt iron boron target material.

[0035] Preferably, the crushing method includes ball milling.

[0036] The present invention can effectively avoid the element segregation phenomenon generated by the raw materials in the alloying process by crushing the alloyed CoFeB blank, and can destroy the pore structure in the CoFeB blank by crushing. At the same time, the small-particle CoFeB blank obtained by crushing can reduce the energy consumption in the reaction process in the subsequent sintering process, thereby reducing the manufacturing cost and being beneficial to improving the density and uniformity of the CoFeB target material.

[0037] Preferably, the powder particle size D50 obtained after the crushing is 5 μm-20 μm, for example, 5 μm, 10 μm, 15 μm, 18 μm or 20 μm, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0038] Preferably, after the crushing and before the sintering, a jacket degassing treatment is performed.

[0039] Preferably, the temperature of the sheath degassing treatment is 200°C-350°C, for example, it can be 200°C, 230°C, 250°C, 280°C, 300°C or 350°C, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0040] Preferably, the vacuum degree of the package after degassing is less than 1×10 -3 Pa, for example, can be 1×10 -4 Pa, 3×10 -4 Pa, 5×10 -4 Pa, 7×10 -4 Pa or 9×10 -4 Pa, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0041] Preferably, the sintering comprises hot isostatic pressing.

[0042] Preferably, the hot isostatic pressing sintering pressure is 100 MPa-130 MPa, for example, 100 MPa, 105 MPa, 110 MPa, 120 MPa, 125 MPa or 130 MPa, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0043] Preferably, the terminal temperature of the sintering is 600°C-850°C, for example, it can be 600°C, 650°C, 700°C, 750°C, 800°C or 850°C, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0044] Preferably, the sintering holding time is 1 h-3 h, for example, 1 h, 1.5 h, 2 h, 2.5 h or 3 h, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0045] The present invention prepares the cobalt iron boron target material by sintering, and further improves the density and uniformity of the target material by reasonably controlling the sintering temperature and time. Within the preferred sintering temperature and sintering time range, not only can a target material with uniform composition and high density that meets the requirements of magnetron sputtering be obtained, but also the yield rate can be improved and the production cost can be reduced.

[0046] As a preferred technical solution of the present invention, the preparation method comprises the following steps:

[0047] (1) ball-milling an iron source, a boron source and a cobalt source in proportion to obtain a mixture, wherein the mixing atmosphere is an inert gas atmosphere and the mixing time is 12 hours to 24 hours.

[0048] (2) The mixed material is subjected to cold isostatic pressing to obtain a formed body, wherein the pressure of the cold isostatic pressing is 150 MPa-280 MPa, and the holding time of the cold isostatic pressing is 5 min-10 min.

[0049] (3) placing the formed body into a vacuum sintering furnace for alloying to obtain an alloyed cobalt iron boron body, wherein the alloying vacuum degree is less than 1×10 -4 Pa, the alloying includes one-stage calcination, two-stage calcination and three-stage calcination, the heating rate of the one-stage calcination is 2°C / min-5°C / min, the heating end temperature is 150°C-250°C, and the holding time is 2h-4h, the heating rate of the two-stage calcination is 2°C / min-5°C / min, the heating end temperature is 400°C-600°C, and the holding time is 3h-6h, the heating rate of the three-stage calcination is 1°C / min-3°C / min, the heating end temperature is 750°C-900°C, and the holding time is 2h-5h.

[0050] (4) The alloyed cobalt-iron-boron blank is crushed to obtain a crushed material with a powder particle size D50 of 5 μm-20 μm.

[0051] (5) Put the crushed material into the metal sheath and degas the sheath at a temperature of 200℃-350℃, with a vacuum degree of <1×10 -3 After Pa, the package is sealed; the sealed package is placed in a hot isostatic pressing furnace for sintering, the sintering temperature is 600°C-850°C, and the insulation time is 1h-3h to obtain a sintered cobalt-iron-boron blank.

[0052] (6) Processing and welding the sintered CoFeB blank in sequence according to the required size to obtain the CoFeB target material.

[0053] In a second aspect, the present invention provides a cobalt iron boron target material, which is prepared by the preparation method described in the first aspect.

[0054] In a third aspect, the present invention provides an application of the cobalt iron boron target material as described in the second aspect, wherein the cobalt iron boron target material is applied as a magnetron sputtering target material.

[0055] Compared with the prior art, the present invention has at least the following beneficial effects:

[0056] (1) The present invention directly mixes the raw materials into a mold, and then converts the raw materials into an alloyed CoFeB blank through a three-stage calcination process. The alloyed CoFeB blank is then crushed and sintered in sequence, thereby further improving the uniformity and density of CoFeB.

[0057] (2) The cobalt iron boron target material obtained by the preparation method of the present invention has uniform composition and high density, which meets the requirements of magnetron sputtering for target materials, while improving the yield rate and reducing the production cost. DETAILED DESCRIPTION

[0058] For the convenience of understanding the present invention, the present invention lists the following embodiments. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0059] Example 1

[0060] This embodiment provides a method for preparing a cobalt iron boron target, the preparation method comprising the following steps:

[0061] (1) ball milling and mixing iron powder with a D50 of 20 μm and a purity of 99.99%, boron powder with a D50 of 20 μm and a purity of 99.99%, and cobalt powder with a D50 of 20 μm and a purity of 99.99% to obtain a mixture, wherein the molar ratio of the iron powder, the boron powder and the cobalt powder is 20:60:20, the ball-to-material ratio is 4:1, the mixing atmosphere is a nitrogen gas atmosphere, and the mixing time is 18 hours;

[0062] (2) cold isostatic pressing the mixed material to obtain a formed body, wherein the pressure of the cold isostatic pressing is 200 MPa and the holding time of the cold isostatic pressing is 8 min;

[0063] (3) The formed body is placed in a vacuum sintering furnace for alloying to obtain an alloyed cobalt iron boron body, wherein the alloying vacuum degree is 5×10 -5 Pa, the alloying includes one-stage calcination, two-stage calcination and three-stage calcination, the heating rate of the one-stage calcination is 3°C / min, the heating end temperature is 200°C, and the holding time is 3h, the heating rate of the two-stage calcination is 3°C / min, the heating end temperature is 500°C, and the holding time is 4h, the heating rate of the three-stage calcination is 2°C / min, the heating end temperature is 800°C, and the holding time is 3h;

[0064] (4) crushing the cobalt iron boron blank to obtain a crushed material with a powder particle size D50 of 10 μm;

[0065] (5) The crushed material is placed in a metal sheath and degassed at 300°C with a vacuum degree of 5×10 -4 The package is sealed at Pa; the sealed package is placed in a hot isostatic pressing furnace for sintering at a sintering temperature of 700°C and a holding time of 2 hours to obtain a sintered cobalt-iron-boron blank;

[0066] (6) Processing and welding the sintered CoFeB blank in sequence according to the required size to obtain the CoFeB target material.

[0067] Example 2

[0068] This embodiment provides a method for preparing a cobalt iron boron target, the preparation method comprising the following steps:

[0069] (1) ball milling and mixing iron powder with a D50 of 10 μm and a purity of 99.995%, boron powder with a D50 of 10 μm and a purity of 99.995%, and cobalt powder with a D50 of 10 μm and a purity of 99.995% to obtain a mixture, wherein the molar ratio of the iron powder, the boron powder and the cobalt powder is 15:60:15, the ball-to-material ratio is 6:1, the mixing atmosphere is a nitrogen gas atmosphere, and the mixing time is 12 hours;

[0070] (2) cold isostatic pressing the mixed material to obtain a formed body, wherein the pressure of the cold isostatic pressing is 280 MPa and the holding time of the cold isostatic pressing is 5 min;

[0071] (3) The formed blank is placed in a vacuum sintering furnace for alloying to obtain an alloyed cobalt iron boron blank, wherein the alloying vacuum degree is 9×10 -5 Pa, the alloying includes one-stage calcination, two-stage calcination and three-stage calcination, the heating rate of the one-stage calcination is 2°C / min, the heating end temperature is 150°C, and the holding time is 4h, the heating rate of the two-stage calcination is 2°C / min, the heating end temperature is 400°C, and the holding time is 6h, the heating rate of the three-stage calcination is 1°C / min, the heating end temperature is 750°C, and the holding time is 5h;

[0072] (4) crushing the cobalt iron boron blank to obtain a crushed material with a powder particle size D50 of 5 μm;

[0073] (5) The crushed material is placed in a metal sheath and degassed at 200°C with a vacuum degree of 9×10 -4 After Pa, the package is sealed; the sealed package is placed in a hot isostatic pressing furnace for sintering at a sintering temperature of 600°C and a holding time of 3 hours to obtain a sintered cobalt-iron-boron blank;

[0074] (6) Processing and welding the sintered CoFeB blank in sequence according to the required size to obtain the CoFeB target material.

[0075] Example 3

[0076] This embodiment provides a method for preparing a cobalt iron boron target, the preparation method comprising the following steps:

[0077] (1) ball milling and mixing iron powder with a D50 of 45 μm and a purity of 99.999%, boron powder with a D50 of 45 μm and a purity of 99.999%, and cobalt powder with a D50 of 45 μm and a purity of 99.999% to obtain a mixture, wherein the molar ratio of the iron powder, the boron powder and the cobalt powder is 20:65:25, the ball-to-material ratio is 3:1, the mixing atmosphere is an argon gas atmosphere, and the mixing time is 24 hours;

[0078] (2) cold isostatic pressing the mixed material to obtain a formed body, wherein the pressure of the cold isostatic pressing is 150 MPa and the holding time of the cold isostatic pressing is 10 min;

[0079] (3) The formed blank is placed in a vacuum sintering furnace for alloying to obtain an alloyed cobalt iron boron blank, wherein the alloying vacuum degree is 1×10 -5Pa, the alloying includes one-stage calcination, two-stage calcination and three-stage calcination, the heating rate of the one-stage calcination is 5°C / min, the heating end temperature is 250°C, and the holding time is 2h, the heating rate of the two-stage calcination is 5°C / min, the heating end temperature is 600°C, and the holding time is 3h, the heating rate of the three-stage calcination is 3°C / min, the heating end temperature is 900°C, and the holding time is 2h;

[0080] (4) crushing the cobalt iron boron blank to obtain a crushed material with a powder particle size D50 of 20 μm;

[0081] (5) The crushed material is placed in a metal sheath and degassed at 350°C with a vacuum degree of 1×10 -4 After Pa, the package is sealed; the sealed package is placed in a hot isostatic pressing furnace for sintering at a sintering temperature of 850°C and a holding time of 1 hour to obtain a sintered cobalt-iron-boron blank;

[0082] (6) Processing and welding the sintered CoFeB blank in sequence according to the required size to obtain the CoFeB target material.

[0083] Example 4

[0084] The only difference between this embodiment and embodiment 1 is that, except for the temperature of the third calcination in step (2) being 700° C., the rest is the same as embodiment 1.

[0085] Example 5

[0086] The difference between this embodiment and embodiment 1 is that, except that the temperature of the third-stage calcination in step (2) is 950° C., the rest is the same as embodiment 1.

[0087] Example 6

[0088] The only difference between this embodiment and embodiment 1 is that, except for the time of the three-stage calcination in step (2) being 1.5 h, the rest is the same as embodiment 1.

[0089] Example 7

[0090] The only difference between this embodiment and embodiment 1 is that, except for the time of the three-stage calcination in step (2) being 5.5 hours, the rest is the same as embodiment 1.

[0091] Example 8

[0092] The only difference between this embodiment and embodiment 1 is that, except for the sintering temperature of step (5) being 550° C., the rest is the same as embodiment 1.

[0093] Example 9

[0094] The only difference between this embodiment and embodiment 1 is that, except for the sintering temperature of step (5) being 900° C., the rest is the same as embodiment 1.

[0095] Example 10

[0096] The only difference between this embodiment and embodiment 1 is that, except for the sintering time in step (5) being 0.5 h, the rest is the same as embodiment 1.

[0097] Embodiment 11

[0098] The only difference between this embodiment and embodiment 1 is that, except for the sintering time of step (5) being 3.5 hours, the rest is the same as embodiment 1.

[0099] Comparative Example 1

[0100] The difference between this comparative example and Example 1 is that, except for not performing step (3), the rest is the same as Example 1.

[0101] Comparative Example 2

[0102] The difference between this comparative example and Example 1 is that, except that the first calcination in step (3) is not performed, the rest is the same as Example 1.

[0103] Comparative Example 3

[0104] The difference between this comparative example and Example 1 is that, except that the second-stage calcination in step (3) is not performed, the rest is the same as Example 1.

[0105] Comparative Example 4

[0106] The difference between this comparative example and Example 1 is that, except that the three-stage calcination in step (3) is not performed, the rest is the same as Example 1.

[0107] Comparative Example 5

[0108] The difference between this comparative example and Example 1 is that, except for not performing step (4), the rest is the same as Example 1.

[0109] Comparative Example 6

[0110] This comparative example provides a method for preparing a cobalt iron boron target, and the preparation method comprises the following steps:

[0111] (1) ball milling and mixing iron powder with a D50 of 20 μm and a purity of 99.99%, boron powder with a D50 of 20 μm and a purity of 99.99%, and cobalt powder with a D50 of 20 μm and a purity of 99.99% to obtain a mixture, wherein the molar ratio of the iron powder, the boron powder and the cobalt powder is 20:60:20, the ball-to-material ratio is 4:1, the mixing atmosphere is a nitrogen gas atmosphere, and the mixing time is 18 hours;

[0112] (2) evacuating the atomizing furnace and filling it with argon to 0.8 MPa, adding the prepared mixed material into the smelting crucible in the smelting chamber inside the atomizing furnace, heating the smelting crucible to 1600° C., and keeping the melt after the material in the smelting crucible is completely melted for 7 minutes, and then cooling the melt to 1350° C. to obtain an alloy melt;

[0113] (3) heating the tundish of the atomizing furnace to 1300° C., transferring the alloy melt in the smelting crucible to the tundish and starting atomization, the aperture of the atomizing nozzle is 5 mm, the pressure of the smelting chamber is 20 KPa, the pressure of the atomizing chamber is 0 Pa, and the atomizing pressure is 1 MPa; passing the powder obtained after the atomization through a 100 mesh sieve, and selecting the alloy powder with a D50 of 10 μm for subsequent sintering;

[0114] (4) The alloy powder was placed in a metal sheath and degassed at 300°C with a vacuum degree of 5×10 -4 The package is sealed at Pa; the sealed package is placed in a hot isostatic pressing furnace for sintering at a sintering temperature of 700°C and a holding time of 2h to obtain a sintered cobalt-iron-boron blank;

[0115] (5) The sintered CoFeB blank is processed and welded in sequence according to the required size to obtain the CoFeB target.

[0116] Test Method

[0117] The actual density of the cobalt iron boron targets prepared in Examples 1-11 and Comparative Examples 1-6 was measured by the water displacement method, and the density was calculated by comparing with the theoretical density and recorded in Table 1.

[0118] Table 1

[0119]

[0120]

[0121] The test results show that:

[0122] (1) It can be seen from Examples 1-11 and Comparative Examples 1-6 that the present invention directly mixes and shapes the raw materials, and then converts the raw materials into alloyed cobalt iron boron blanks through three-stage calcination of alloying, and the alloyed cobalt iron boron blanks are crushed and sintered in sequence, thereby further improving the uniformity and density of cobalt iron boron. Therefore, the cobalt iron boron target material obtained by the preparation method of the present invention has uniform composition and high density, meets the requirements of magnetron sputtering for target materials, and at the same time improves the yield rate and reduces production costs.

[0123] (2) It can be seen from Example 1, Examples 4-7 and Comparative Examples 1-4 that the present invention can further improve the uniformity and density of the cobalt iron boron target by further controlling the temperature and time of the three-stage calcination during the alloying process.

[0124] (3) It can be seen from Example 1 and Examples 8-11 that the density of the cobalt iron boron target can be further improved by further controlling the sintering temperature and time.

[0125] (4) It can be seen from Example 1 and Comparative Examples 5-6 that the present invention directly mixes the raw materials and then converts the raw materials into an alloyed CoFeB blank through three-stage calcination, and the alloyed CoFeB blank is crushed and sintered in sequence to further improve the uniformity and density of CoFeB.

[0126] In summary, the present invention directly mixes and shapes the raw materials, and then converts the raw materials into alloyed cobalt iron boron blanks through three-stage calcination of alloying, and the alloyed cobalt iron boron blanks are crushed and sintered in sequence, thereby further improving the uniformity and density of cobalt iron boron. Therefore, the cobalt iron boron target material obtained by the preparation method of the present invention has uniform composition and high density, meets the requirements of magnetron sputtering for the target material, and at the same time improves the yield rate and reduces the production cost.

[0127] The applicant declares that the above is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention shall fall within the protection scope and disclosure scope of the present invention.

Claims

1. A method for preparing a cobalt-iron-boron target, characterized in that: The preparation method comprises the following steps: After the raw materials are mixed, cold isostatic pressing, alloying, crushing and sintering are performed in sequence to obtain the cobalt iron boron target material; The alloying comprises one-stage calcination, two-stage calcination and three-stage calcination; The heating end point temperature of the first stage calcination is 150°C-250°C; The heating end temperature of the second stage calcination is 400°C-600°C; The heating end temperature of the three-stage calcination is 750°C-900°C.

2. The preparation method according to claim 1, characterized in that: The raw materials include an iron source, a boron source and a cobalt source; Preferably, the molar ratio of the iron source, the boron source and the cobalt source is (15-20):(60-65):(15-25); Preferably, the particle size D50 of the raw material is 10 μm-45 μm.

3. The preparation method according to claim 1 or 2, characterized in that: The mixing method includes ball milling; Preferably, the ball milling comprises dry ball milling; Preferably, the mixed atmosphere is an inert gas atmosphere; Preferably, the mixing time is 12h-24h.

4. The preparation method according to any one of claims 1 to 3, characterized in that The cold isostatic pressing pressure is 150MPa-280MPa; Preferably, the holding time of the cold isostatic pressing is 5 min-10 min.

5. The preparation method according to any one of claims 1 to 4, characterized in that: The alloying atmosphere is a vacuum atmosphere; Preferably, the vacuum degree of the vacuum atmosphere is less than 1×10 -4 Pa.

6. The preparation method according to any one of claims 1 to 5, characterized in that: The holding time of the first calcination stage is 2h-4h; Preferably, the holding time of the second stage calcination is 3h-6h; Preferably, the holding time of the three-stage calcination is 2h-5h.

7. The preparation method according to any one of claims 1 to 6, characterized in that: The powder particle size D50 obtained after the crushing is 5 μm-20 μm.

8. The preparation method according to any one of claims 1 to 7, characterized in that: The sintering includes hot isostatic pressing; Preferably, the end point temperature of the sintering is 600°C-850°C; Preferably, the sintering holding time is 1h-3h.

9. A cobalt iron boron target, characterized in that: The cobalt iron boron target is prepared by the preparation method described in any one of claims 1 to 8.

10. An application of the cobalt-iron-boron target material as claimed in claim 9, characterized in that: The cobalt iron boron target material is applied to magnetron sputtering target material.

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