A cobalt iron boron target material, a preparation method thereof and application thereof

Abstract

The present application relates to a kind of cobalt iron boron target material and its preparation method and application, the preparation method includes the following steps: after mixing raw material, sequentially carry out cold isostatic pressing forming, alloying, crushing and sintering, obtain the cobalt iron boron target material;The alloying includes one-stage calcination, two-stage calcination and three-stage calcination;The temperature rising end point temperature of one-stage calcination is 150-250 DEG C;The temperature rising end point temperature of two-stage calcination is 400-600 DEG C;The temperature rising end point temperature of three-stage calcination is 750-900 DEG C.The raw material is directly mixed into shape in the present application, then by the three-stage calcination of alloying, raw material is converted into alloyed cobalt iron boron blank, alloyed cobalt iron boron blank is sequentially crushed and sintered, further improve the uniformity and density of cobalt iron boron.Therefore, the cobalt iron boron target material obtained by the preparation method of the present application is uniform in composition, high in density, meets the requirements of magnetron sputtering for target material, simultaneously improves the material yield, reduces production cost.

Description

Technical Field

[0001] This invention relates to the field of sputtering target technology, to a target material and its preparation method and application, and particularly to a cobalt iron boron target material and its preparation method and application. Background Technology

[0002] Currently, magnetic storage technology has made significant progress. 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 alloys play a crucial role in perpendicular magnetic recording technology due to their excellent magnetic properties. Their high permeability and high coercivity enable faster data transfer rates and greater storage density, leading to their widespread use in storage devices such as magnetic tape, hard disk drives, and magnetic random access memory (MRAM).

[0004] Common cobalt-iron-boron (CFeB) materials are prepared using three main methods: The first is the roasting method, which involves heating and melting raw materials of iron, cobalt, and boron, followed by casting, cooling, and crushing to obtain a CFeB magnet. This method is energy-intensive and produces CFeB magnets with poor performance. The second is the chemical precipitation method, which involves co-precipitating iron, cobalt, and boron salt solutions to generate precursor precipitates, followed by dehydration, sintering, and heat treatment to obtain the CFeB magnet. This method is complex and costly. The third is the powder metallurgy method. CN117431510A discloses a method for preparing a CFeB target for magnetic gyratory storage, which involves weighing intermediate alloy powder, high-energy ball milling activation, cobalt plating, vacuum preheating pressing, hot isostatic pressing sintering, and backplate welding to obtain the CFeB target. This method has high raw material costs, and the process of coating the Fe-B alloy powder with cobalt during preparation leads to reduced uniformity of the CFeB composition.

[0005] Given the shortcomings of existing technologies, how to reduce preparation costs and produce cobalt-iron-boron targets with uniform composition and high density has become an urgent problem to be solved. Summary of the Invention

[0006] To address the aforementioned technical problems, this invention provides a cobalt-iron-boron (CFeB) sputtering target, its preparation method, and its applications. This invention directly mixes and shapes the raw materials, then transforms them into an alloyed CFeB billet through a three-stage alloying calcination process. The alloyed CFeB billet is then sequentially crushed and sintered, further improving the uniformity and density of the CFeB. Therefore, the CFeB target obtained by the preparation method of this invention has uniform composition and high density, meeting the requirements of magnetron sputtering, while simultaneously improving the yield and reducing production costs.

[0007] To achieve this objective, the present invention adopts the following technical solution:

[0008] In a first aspect, the present invention provides a method for preparing a cobalt-iron-boron target material, the method comprising the following steps: after mixing raw materials, performing cold isostatic pressing, alloying, crushing and sintering sequentially to obtain the cobalt-iron-boron target material; the alloying includes a first-stage calcination, a second-stage calcination and a third-stage calcination; the final temperature of the first-stage calcination is 150℃-250℃; the final temperature of the second-stage calcination is 400℃-600℃; and the final temperature of the third-stage calcination is 750℃-900℃.

[0009] The final temperature of the first stage of calcination can be 150℃, 180℃, 200℃, 220℃ or 250℃; the final temperature of the second stage of calcination can be 400℃, 450℃, 500℃, 550℃ or 600℃; and the final temperature of the third stage of calcination can be 750℃, 780℃, 800℃, 850℃, 880℃ or 900℃, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0010] This invention directly mixes and shapes the raw materials, then transforms them into alloyed cobalt-iron-boron (CFeB) billets through a three-stage alloying calcination process. The alloyed CFeB billets are then sequentially crushed and sintered, further improving the uniformity and density of the CFeB. Therefore, the CFeB target material obtained by the preparation method of this invention has uniform composition and high density, meeting the requirements of magnetron sputtering, while simultaneously improving the yield and reducing production costs.

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

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

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

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

[0015] Preferably, the molar ratio of the iron source, boron source, and 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. Other unlisted values ​​within the range are also applicable.

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

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

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

[0020] Preferably, the ball milling includes 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, it can be 12h, 16h, 18h, 20h or 24h, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0024] Preferably, the pressure of the cold isostatic pressing is 150MPa-280MPa, for example, it can be 150MPa, 180MPa, 200MPa, 220MPa or 250MPa, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0025] Preferably, the holding time for cold isostatic pressing is 5 min to 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. Other unlisted values ​​within the range are also applicable.

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

[0027] Preferably, the vacuum degree of the vacuum atmosphere is <1×10⁻⁶. -4 Pa, for example, could be 1×10 -5 Pa, 3×10 -5 Pa, 5×10 -5Pa, 7×10 -5 Pa or 9×10 -5 Pa, but not limited to the listed values, applies to other unlisted values ​​within the range as well.

[0028] Preferably, the heating rate of the calcination stage is 2℃ / min-5℃ / min, for example, it can be 2℃ / min, 3℃ / min, 4℃ / min, 4.5℃ / min or 5℃ / min, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0029] Preferably, the holding time for the calcination is 2h-4h, for example, it can be 2h, 2.5h, 3h, 3.5h or 4h, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0030] Preferably, the heating rate of the two-stage calcination is 2℃ / min-5℃ / min, for example, it can be 2℃ / min, 3℃ / min, 4℃ / min, 4.5℃ / min or 5℃ / min, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

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

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

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

[0034] This invention improves the density and uniformity of cobalt-iron-boron (CFeB) sputtering targets through a three-stage calcination alloying process. Specifically, controlling the holding temperature and time during the first calcination stage helps remove low-volatility substances such as water vapor from the raw material powder, reducing their impact on the density of the CFeB sputtering target in subsequent reactions. Controlling the holding temperature and time during the second calcination stage creates a more uniform temperature field, facilitating sufficient contact between the powder and the raw material powder and promoting a more uniform reaction, thus further improving the uniformity of the CFeB sputtering target. Controlling the holding temperature and time during the third calcination stage ensures a uniform and stable alloying reaction, further enhancing the density and uniformity of the CFeB sputtering target.

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

[0036] This invention effectively avoids elemental segregation during the alloying process by crushing the alloyed cobalt-iron-boron billet. Crushing also disrupts the porous structure of the cobalt-iron-boron billet. Furthermore, the smaller cobalt-iron-boron billet particles obtained from the crushing process reduce energy consumption during subsequent sintering, thereby lowering manufacturing costs and improving the density and uniformity of the cobalt-iron-boron target material.

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

[0038] Preferably, after crushing and before sintering, a degassing treatment is performed using a cladding system.

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

[0040] Preferably, the vacuum degree after the degassing treatment is <1×10⁻⁶. -3 Pa, for example, could be 1×10 -4 Pa, 3×10 -4 Pa, 5×10 -4 Pa, 7×10 -4 Pa or 9×10 -4 Pa, but not limited to the listed values, applies to other unlisted values ​​within the range as well.

[0041] Preferably, the sintering includes hot isostatic pressing (HIP).

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

[0043] Preferably, the final sintering temperature is 600℃-850℃, for example, it can be 600℃, 650℃, 700℃, 750℃, 800℃ or 850℃, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

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

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

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

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

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

[0049] (3) The formed billet is placed in a vacuum sintering furnace for alloying to obtain an alloyed cobalt-iron-boron billet, wherein the vacuum degree of alloying is <1×10 -4 Pa, the alloying includes a first-stage calcination, a second-stage calcination, and a third-stage calcination. The heating rate of the first-stage calcination is 2℃ / min-5℃ / min, the final temperature is 150℃-250℃, and the holding time is 2h-4h. The heating rate of the second-stage calcination is 2℃ / min-5℃ / min, the final temperature is 400℃-600℃, and the holding time is 3h-6h. The heating rate of the third-stage calcination is 1℃ / min-3℃ / min, the final temperature is 750℃-900℃, and the holding time is 2h-5h.

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

[0051] (5) Load the crushed material into a metal sheath and degas the sheath at a temperature of 200℃-350℃, with a vacuum degree <1×10⁻⁶. -3 After Pa, the package is sealed; the sealed package is then placed in a hot isostatic pressing furnace for sintering at a temperature of 600℃-850℃ for 1-3 hours to obtain the sintered cobalt-iron-boron billet.

[0052] (6) The sintered cobalt iron boron blank is processed and welded in sequence according to the required dimensions to obtain the cobalt iron boron 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] Thirdly, the present invention provides an application of the cobalt-iron-boron target as described in the second aspect, wherein the cobalt-iron-boron target is used as a magnetron sputtering target.

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

[0056] (1) The present invention directly mixes and shapes the raw materials, and then transforms the raw materials into alloyed cobalt iron boron blanks through three-stage calcination of alloying. The alloyed cobalt iron boron blanks are then crushed and sintered in sequence, which further improves the uniformity and density of cobalt iron boron.

[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 material, while improving the yield and reducing the production cost. Detailed Implementation

[0058] To facilitate understanding of the present invention, the following embodiments are provided. Those skilled in the art should understand that these embodiments are merely illustrative and should not be construed as limiting the scope of the invention.

[0059] Example 1

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

[0061] (1) 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% were ball-milled to obtain a mixture in which the molar ratio of iron powder, boron powder and cobalt powder was 20:60:20, the ball-to-material ratio was 4:1, the mixing atmosphere was a nitrogen atmosphere, and the mixing time was 18 h.

[0062] (2) The mixture is subjected to cold isostatic pressing to obtain a molded blank, 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 billet is placed in a vacuum sintering furnace for alloying to obtain an alloyed cobalt-iron-boron billet, wherein the vacuum degree of alloying is 5×10 -5 Pa, the alloying includes a first-stage calcination, a second-stage calcination, and a third-stage calcination. The first-stage calcination has a heating rate of 3℃ / min, a final heating temperature of 200℃, and a holding time of 3h. The second-stage calcination has a heating rate of 3℃ / min, a final heating temperature of 500℃, and a holding time of 4h. The third-stage calcination has a heating rate of 2℃ / min, a final heating temperature of 800℃, and a holding time of 3h.

[0064] (4) The cobalt iron boron billet is crushed to obtain crushed material with a powder particle size D50 of 10μm;

[0065] (5) The crushed material is loaded into a metal sheath and degassed at 300°C with a vacuum degree of 5×10⁻⁶. -4 The package is sealed at Pa; the sealed package is then placed in a hot isostatic pressing furnace for sintering at a temperature of 700℃ for 2 hours to obtain a sintered cobalt-iron-boron billet.

[0066] (6) The sintered cobalt iron boron blank is processed and welded in sequence according to the required dimensions to obtain the cobalt iron boron target material.

[0067] Example 2

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

[0069] (1) 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% are ball-milled to obtain a mixture, wherein the molar ratio of iron powder, boron powder and 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 12h;

[0070] (2) The mixture is subjected to cold isostatic pressing to obtain a molded blank, 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 billet is placed in a vacuum sintering furnace for alloying to obtain an alloyed cobalt-iron-boron billet, wherein the vacuum degree of alloying is 9×10 -5 Pa, the alloying includes a first-stage calcination, a second-stage calcination, and a third-stage calcination. The first-stage calcination has a heating rate of 2℃ / min, a final heating temperature of 150℃, and a holding time of 4h. The second-stage calcination has a heating rate of 2℃ / min, a final heating temperature of 400℃, and a holding time of 6h. The third-stage calcination has a heating rate of 1℃ / min, a final heating temperature of 750℃, and a holding time of 5h.

[0072] (4) The cobalt iron boron billet is crushed to obtain crushed material with a powder particle size D50 of 5μm;

[0073] (5) The crushed material is loaded into a metal sheath and degassed at 200°C with a vacuum degree of 9×10⁻⁶. -4 After Pa, the package is sealed; the sealed package is placed in a hot isostatic pressing furnace for sintering at a temperature of 600℃ for 3 hours to obtain a sintered cobalt-iron-boron billet.

[0074] (6) The sintered cobalt iron boron blank is processed and welded in sequence according to the required dimensions to obtain the cobalt iron boron target material.

[0075] Example 3

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

[0077] (1) 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% are ball-milled to obtain a mixture, wherein the molar ratio of iron powder, boron powder and cobalt powder is 20:65:25, the ball-to-material ratio is 3:1, the mixing atmosphere is argon gas atmosphere, and the mixing time is 24 h;

[0078] (2) The mixture is subjected to cold isostatic pressing to obtain a molded blank, 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 billet is placed in a vacuum sintering furnace for alloying to obtain an alloyed cobalt-iron-boron billet, wherein the vacuum degree of alloying is 1×10 -5Pa, the alloying includes a first-stage calcination, a second-stage calcination, and a third-stage calcination. The first-stage calcination has a heating rate of 5℃ / min, a final heating temperature of 250℃, and a holding time of 2h. The second-stage calcination has a heating rate of 5℃ / min, a final heating temperature of 600℃, and a holding time of 3h. The third-stage calcination has a heating rate of 3℃ / min, a final heating temperature of 900℃, and a holding time of 2h.

[0080] (4) The cobalt iron boron billet is crushed to obtain crushed material with a powder particle size D50 of 20μm;

[0081] (5) The crushed material is loaded into a metal sheath and degassed at 350°C with a vacuum degree of 1×10⁻⁶. -4 After Pa, the package is sealed; the sealed package is placed in a hot isostatic pressing furnace for sintering at a temperature of 850℃ and a holding time of 1h to obtain the sintered cobalt-iron-boron billet.

[0082] (6) The sintered cobalt iron boron blank is processed and welded in sequence according to the required dimensions to obtain the cobalt iron boron target material.

[0083] Example 4

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

[0085] Example 5

[0086] The only difference between this embodiment and embodiment 1 is that, except that the calcination temperature in step (2) is 950°C, everything else is the same as in embodiment 1.

[0087] Example 6

[0088] The only difference between this embodiment and embodiment 1 is that, except that the calcination time for the three stages in step (2) is 1.5 hours, everything else is the same as in embodiment 1.

[0089] Example 7

[0090] The only difference between this embodiment and embodiment 1 is that, except that the calcination time for the three stages in step (2) is 5.5 hours, everything else is the same as in embodiment 1.

[0091] Example 8

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

[0093] Example 9

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

[0095] Example 10

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

[0097] Example 11

[0098] The only difference between this embodiment and embodiment 1 is that, except that the sintering time in step (5) is 3.5 hours, everything else is the same as in embodiment 1.

[0099] Comparative Example 1

[0100] The only difference between this comparative example and Example 1 is that, except for step (3) not being performed, everything else is the same as in Example 1.

[0101] Comparative Example 2

[0102] The only difference between this comparative example and Example 1 is that, except for the absence of a calcination step (3), the rest is the same as Example 1.

[0103] Comparative Example 3

[0104] The only difference between this comparative example and Example 1 is that, except for the absence of the two-stage calcination in step (3), everything else is the same as in Example 1.

[0105] Comparative Example 4

[0106] The only difference between this comparative example and Example 1 is that, except for the absence of the three-stage calcination in step (3), everything else is the same as in Example 1.

[0107] Comparative Example 5

[0108] The only difference between this comparative example and Example 1 is that, except for step (4) not being performed, everything else is the same as in Example 1.

[0109] Comparative Example 6

[0110] This comparative example provides a method for preparing a cobalt-iron-boron target material, the method comprising the following steps:

[0111] (1) 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% were ball-milled to obtain a mixture in which the molar ratio of iron powder, boron powder and cobalt powder was 20:60:20, the ball-to-material ratio was 4:1, the mixing atmosphere was a nitrogen atmosphere, and the mixing time was 18 h.

[0112] (2) Evacuate the atomizing furnace and fill it with argon gas to 0.8 MPa. Add the prepared mixture into the melting crucible in the melting chamber inside the atomizing furnace. Heat the melting crucible to 1600°C. After the material in the melting crucible has completely melted, keep the melt at 7 minutes. Then cool the melt to 1350°C to obtain the alloy melt.

[0113] (3) Heat the tundish of the atomizing furnace to 1300°C, transfer the alloy melt in the melting crucible to the tundish to start atomization, the atomizing nozzle diameter is 5 mm, the pressure in the melting chamber is 20 kPa, the pressure in the atomizing chamber is 0 Pa, and the atomization pressure is 1 MPa; after atomization, pass the powder obtained through a 100-mesh sieve, and select alloy powder with D50 of 10 μm for subsequent sintering;

[0114] (4) The alloy powder is packed into a metal cladding, and the cladding is degassed at 300°C with a vacuum degree of 5×10⁻⁶. -4 The package is sealed at Pa; the sealed package is then placed in a hot isostatic pressing furnace for sintering at a temperature of 700℃ for 2 hours to obtain the sintered cobalt-iron-boron billet.

[0115] (5) The sintered cobalt iron boron blank is processed and welded in sequence according to the required dimensions to obtain the cobalt iron boron target material.

[0116] Test methods

[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. The density was calculated by comparing it with the theoretical density and recorded in Table 1.

[0118] Table 1

[0119]

[0120]

[0121] The test results show that:

[0122] (1) As can be seen from Examples 1-11 and Comparative Examples 1-6, the present invention directly mixes and shapes the raw materials, then transforms them into alloyed cobalt-iron-boron (CFI) billets through a three-stage alloying calcination process. The CFI billets are then sequentially crushed and sintered, further improving the uniformity and density of the CFI. Therefore, the CFI target material obtained by the preparation method of the present invention has uniform composition and high density, meeting the requirements of magnetron sputtering for target materials, while simultaneously improving the yield and reducing production costs.

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

[0124] (3) As can be seen from Examples 1 and 8-11, the present invention can further improve the density of cobalt iron boron targets by further controlling the sintering temperature and time.

[0125] (4) As can be seen from Example 1 and Comparative Examples 5-6, the present invention directly mixes and shapes the raw materials, then transforms the raw materials into alloyed cobalt iron boron blanks through three-stage calcination of alloying, and then crushes and sintersects the alloyed cobalt iron boron blanks in sequence, thereby further improving the uniformity and density of cobalt iron boron.

[0126] In summary, this invention directly mixes and shapes the raw materials, then transforms them into alloyed cobalt-iron-boron (CFeB) billets through a three-stage alloying calcination process. The alloyed CFeB billets are then sequentially crushed and sintered, further improving the uniformity and density of the CFeB. Therefore, the CFeB target material obtained by the preparation method of this invention has uniform composition and high density, meeting the requirements of magnetron sputtering, while simultaneously improving the yield and reducing production costs.

[0127] The applicant declares that the above description is only a specific embodiment 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 conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. A method of producing a cobalt iron boron target material, characterized by, The preparation method comprises the following steps: After the raw materials are mixed, cold isostatic pressing, alloying, crushing and sintering are sequentially performed to obtain the cobalt-iron-boron target material; The alloying comprises one-stage calcination, two-stage calcination and three-stage calcination; The temperature at the end of the one-stage calcination is 150-250℃; The temperature at the end of the two-stage calcination is 400-600℃; The temperature at the end of the three-stage calcination is 750-900℃; The holding time of the three-stage calcination is 2-5h; The atmosphere of the alloying is a vacuum atmosphere; The raw materials comprise an iron source, a boron source and a cobalt source; The molar ratio of the iron source, the boron source and the cobalt source is (15-20):(60-65):(15-25).

2. The production method according to claim 1, characterized by, The particle size D50 of the raw materials is 10-45μm.

3. The preparation method according to claim 1, characterized in that, The mixing method comprises ball milling.

4. The preparation method according to claim 3, characterized in that, The ball milling comprises dry ball milling.

5. The preparation method according to claim 1, characterized in that, The atmosphere of the mixing is an inert gas atmosphere.

6. The preparation method according to claim 1, characterized in that, The mixing time is 12-24h.

7. The preparation method according to claim 1, characterized in that, The pressure of the cold isostatic pressing is 150-280MPa.

8. The method of claim 1, wherein, The holding time of the cold isostatic pressing is 5-10min.

9. The preparation method according to claim 1, wherein The vacuum atmosphere has a vacuum degree <1x10 -4 Pa.

10. The method of claim 1, wherein, The holding time of the one-stage calcination is 2-4h.

11. The method of claim 1, wherein, The holding time of the two-stage calcination is 3-6h.

12. The method of claim 1, wherein, The particle size D50 of the powder obtained after the crushing is 5-20μm.

13. The method of claim 1, wherein, The sintering comprises hot isostatic sintering.

14. The method of claim 1, wherein, The end temperature of the sintering is 600-850℃.

15. The method of claim 1, wherein, The holding time of the sintering is 1-3h.

16. A cobalt iron boron target material, characterized by, The cobalt-iron-boron target material is prepared by the preparation method according to any one of claims 1-15.

17. Use of a cobalt iron boron target material as claimed in claim 16, characterized in that The cobalt-iron-boron target material is applied to a magnetron sputtering target material.

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