CN112059195A - Preparation method of iron-tantalum alloy powder, iron-tantalum alloy powder and application - Google Patents
Preparation method of iron-tantalum alloy powder, iron-tantalum alloy powder and application Download PDFInfo
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Abstract
The invention relates to a preparation method of iron-tantalum alloy powder, the iron-tantalum alloy powder and application thereof, wherein the preparation method of the iron-tantalum alloy powder comprises the following steps: firstly, preparing an iron material and a tantalum material according to a target atomic ratio and mixing; then completely melting at 1542-1600 ℃; and then atomizing under the action of inert gas to obtain the iron-tantalum alloy powder. The preparation method controls the melting temperature of the iron-tantalum mixture to be 1542-1600 ℃, and optimizes the atomization condition, so that the purity of the prepared iron-tantalum alloy powder is more than or equal to 99.95 percent, the oxygen content is less than or equal to 600ppm, the iron-tantalum alloy powder with the granularity less than 150 meshes is obtained by screening, and the preparation method is favorable for preparing the iron-cobalt-tantalum alloy sputtering target material with high purity, high compactness, high bending strength and qualified magnetic flux; the tantalum rim charge of the tantalum target material is used as the tantalum material for preparation, so that waste is changed into valuable.
Description
Technical Field
The invention relates to the technical field of alloy powder preparation, in particular to a preparation method of iron-tantalum alloy powder, the iron-tantalum alloy powder and application.
Background
With the rapid development of society and the rapid increase of information storage demand of people, recording media such as hard disks and optical disks using magnetic information storage technology are receiving more and more attention, and have occupied a significant position in the information storage field by virtue of their advantages such as high storage density, large capacity, low price, and the like. Magnetic recording is a method of recording information by using magnetic properties, and can input and read information by a special method during storage and use, thereby achieving the purposes of storing information and reading information. Magnetic recording includes both horizontal magnetic recording and vertical magnetic recording, depending on the positional relationship of the medium magnetization direction to the medium surface.
At present, perpendicular magnetic recording technology has comprehensively replaced horizontal magnetic recording technology in the magnetic recording market. Because perpendicular magnetic recording technology has brought about a rapid increase in areal density and capacity of magnetic recording media, there are common magnetic recording media such as hard disks, magnetic disks, and optical disks. Magnetic recording media are generally designed in a multilayer perpendicular structure, taking a hard disk as an example, and specifically comprise a lubricating layer, a protective layer, a magnetic recording layer, an intermediate layer, a soft magnetic substrate layer, a substrate layer and a substrate layer. Among them, the soft magnetic underlayer mainly functions to record and store data, and the role in the magnetic recording medium is important. Currently, the thin film of fe-co-ta alloy obtained by the sputtering process is the most commonly used soft magnetic substrate layer.
Sputtering is one of the main techniques for preparing thin film materials, which utilizes ions generated by an ion source to form ion beam flow with high speed energy through accelerated aggregation in vacuum, bombards the surface of a solid, and the ions and atoms on the surface of the solid generate kinetic energy exchange, so that the atoms on the surface of the solid leave the solid and are deposited on the surface of a substrate, and the bombarded solid is a raw material for preparing a thin film deposited by a sputtering method, and the solid is generally called as a sputtering target material.
The iron-cobalt-tantalum alloy sputtering target material for preparing the soft magnetic substrate layer by sputtering needs to have high density, high bending strength and high magnetic flux: the high density can ensure that the film obtained by sputtering is relatively uniform and is not easy to generate abnormal phenomena such as 'discharge' and the like; the bending strength can influence the coercive force of the magnetic material and has a crucial influence on the information storage of the magnetic material, so that the high bending strength can ensure that the target material is not easy to crack and other abnormal problems when in use; target magnetic flux is a very important parameter in magnetic recording targets, and generally the higher the target magnetic flux, the greater the ability to record and store data. Therefore, the quality of the iron-cobalt-tantalum alloy sputtering target material is related to the soft magnetic substrate layer and even the development of the whole magnetic recording industry.
At present, the prior art discloses preparation methods of some iron-cobalt-tantalum alloy sputtering targets, for example, CN108004515A discloses a preparation method of an iron-cobalt-tantalum alloy sputtering target, an iron-cobalt-tantalum alloy sputtering target and an application thereof, in the preparation method, iron powder, cobalt powder and tantalum powder are mixed under the protection of inert gas to obtain iron-cobalt-tantalum mixed powder, and then cold pressing, vacuum degassing, primary hot pressing sintering and secondary hot pressing sintering are sequentially performed to obtain the iron-cobalt-tantalum alloy sputtering target. However, according to the preparation method, the iron powder, the cobalt powder and the tantalum powder are directly mixed according to a required proportion to obtain mixed powder, so that the three metals only have a small amount or basically do not form a compound before hot-pressing sintering, so that the simple substance iron or the simple substance cobalt presents magnetism, and finally the magnetic flux of the iron-cobalt-tantalum alloy sputtering target is low;
CN105473759A discloses a sputtering target material of Fe-Co alloy, a soft magnetic thin film layer, and a perpendicular magnetic recording medium using the same, wherein the manufacturing method comprises the steps of preparing Fe-Co alloy powder, and pressure sintering the powder. The preparation method directly uses the Fe-Co alloy powder obtained by the gas atomization method, and the prepared Fe-Co alloy sputtering target material can meet the performances of high purity, high compactness, high bending strength, magnetic flux and the like and meet the requirement of magnetron sputtering. However, the molten liquid of the Fe-Co alloy is very viscous, so that pipelines are easily blocked, and the gas atomization method fails, and Fe-Co alloy powder with target proportion requirements is purchased everywhere in the market, so that the preparation and the research and development of the Fe-Co alloy sputtering target material are greatly hindered.
In summary, if the iron-tantalum alloy powder and the cobalt-tantalum alloy powder are prepared first, and then the iron-tantalum alloy powder, the cobalt-tantalum alloy powder and the tantalum powder are uniformly mixed according to the target atomic ratio for preparing the iron-cobalt-tantalum alloy sputtering target, the problem of difficulty in preparing the iron-cobalt-tantalum alloy powder can be solved. Therefore, the invention provides a preparation method of iron-tantalum alloy powder, the iron-tantalum alloy powder and application.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a preparation method of iron-tantalum alloy powder, the iron-tantalum alloy powder and application thereof, the preparation method controls the melting temperature of an iron-tantalum mixture to be 1542-1600 ℃, and optimizes atomization conditions, so that the purity of the prepared iron-tantalum alloy powder is more than or equal to 99.95%, the oxygen content is less than or equal to 600ppm, the iron-tantalum alloy powder with the granularity of less than 150 meshes is obtained by screening, and the preparation method is favorable for preparing the iron-cobalt-tantalum alloy sputtering target material with high purity, high compactness, high bending strength and qualified magnetic flux.
In order to achieve the purpose, the invention adopts the following technical scheme:
one of the purposes of the invention is to provide a preparation method of iron-tantalum alloy powder, which comprises the following steps:
(1) preparing and mixing an iron material and a tantalum material according to a target atomic ratio to obtain an iron-tantalum mixture;
(2) completely melting the iron-tantalum mixture obtained in the step (1) at 1542-1600 ℃ to obtain an iron-tantalum molten mass;
(3) and (3) atomizing the iron-tantalum fused mass obtained in the step (2) under the action of inert gas to obtain iron-tantalum alloy powder.
The preparation method controls the melting temperature of the iron-tantalum mixture to be 1542-1600 ℃, optimizes the atomization condition, avoids the problem of pipeline blockage caused by the viscosity of iron-tantalum melt, can prepare iron-tantalum alloy powder with the purity of more than or equal to 99.95 percent and the oxygen content of less than or equal to 600ppm, and is beneficial to preparing the iron-cobalt-tantalum alloy sputtering target with high purity, high compactness, high bending strength and qualified magnetic flux by screening the iron-tantalum alloy powder with the granularity of less than 150 meshes.
The melting temperature of the iron-tantalum mixture of the present invention is 1542-1600 ℃, such as 1542 ℃, 1550 ℃, 1560 ℃, 1570 ℃, 1580 ℃, 1590 ℃ or 1600 ℃, but not limited to the values listed, and other values not listed in the numerical range are also applicable.
In a preferred embodiment of the present invention, the target atomic ratio in step (1) is 7.5 to 8.5 atomic% of tantalum, and the balance is iron and unavoidable impurities.
The atomic ratio of tantalum in the present invention is 7.5 to 8.5%, for example, 7.5%, 7.7%, 8%, 8.2%, or 8.5%, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
The total content of the inevitable impurities is less than 0.05 percent, and the purity of the prepared iron-tantalum alloy powder is ensured to be more than or equal to 99.95 percent.
The atomic proportion of tantalum in the target atomic proportion is 7.5-8.5%, on one hand, according to a phase diagram, the Fe-Ta eutectic temperature is lowest and the bearing pressure of smelting equipment is lowest under the atomic proportion; on the other hand, the iron-tantalum alloy powder with the atomic ratio can ensure that the iron ratio is far higher than that of tantalum, so that the iron-cobalt-tantalum alloy powder with the target atomic ratio can be conveniently obtained by combining and proportioning the iron-tantalum alloy powder with cobalt-tantalum alloy powder and tantalum powder, and the iron-cobalt-tantalum alloy sputtering target material is further prepared.
As a preferable technical scheme of the invention, the purity of the iron material in the step (1) is more than or equal to 99.95 percent.
Preferably, the iron material in the step (1) is an electrolytic iron material.
Preferably, the purity of the tantalum material obtained in the step (1) is more than or equal to 99.95%.
Preferably, the tantalum material in the step (1) is a tantalum rim charge of a tantalum target material.
The tantalum target material can be a tantalum target material disclosed in CN102517531A, CN103572223A or CN103572225A, and a large amount of tantalum rim charge of the tantalum target material can be generated in the process of machining the tantalum target material to prepare a target material component.
As a preferable technical scheme of the invention, before the iron material and the tantalum material are prepared according to the target atomic ratio in the step (1), the iron material and the tantalum material are respectively pretreated.
Preferably, the pretreatment comprises deoiling, pickling, drying and vacuum packaging in sequence.
As is well known to those skilled in the art, the preparation of the powder material is completed and then the powder process is carried out, and the processes of transportation, storage and the like are also carried out in the middle, so that the pretreated powder material needs to be subjected to vacuum packaging, which is beneficial to isolating dust and air and reducing the oxygen absorption reaction of the powder material, thereby ensuring that the finally prepared iron-tantalum alloy powder meets the requirement that the oxygen content is less than or equal to 600 ppm; in addition, when the powder is formally prepared, the vacuum package is disassembled.
Preferably, the deoiling comprises putting the iron material and the tantalum material into cleaning liquid respectively for ultrasonic cleaning, and then washing and wiping the materials by pure water.
Preferably, the cleaning liquid is an aqueous solution containing a detergent.
The concentration of the aqueous solution containing the detergent is not limited, and the type and the concentration of the detergent can be reasonably selected by a person skilled in the art according to actual conditions as long as the oil stain can be cleaned.
Preferably, the ultrasonic cleaning is performed for 50-70min, such as 50min, 52min, 55min, 57min, 60min, 63min, 65min, 68min or 70min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the temperature of the ultrasonic cleaning is 50 to 70 ℃, for example, 50 ℃, 52 ℃, 55 ℃, 57 ℃, 60 ℃, 63 ℃, 65 ℃, 68 ℃ or 70 ℃, etc., but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the acid washing comprises ultrasonic cleaning in an acid washing solution, followed by rinsing with pure water and wiping clean.
Preferably, the acid wash is an aqueous solution of nitric acid and hydrofluoric acid.
Preferably, the acid washing solution contains 38.5% of nitric acid and 7.1% of hydrofluoric acid by mass percentage.
Preferably, the time for the acid washing is 10-30min, such as 10min, 13min, 15min, 17min, 20min, 23min, 25min, 27min or 30min, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the drying is carried out in a vacuum drying oven.
Preferably, the drying time is 60-90min, such as 60min, 65min, 70min, 75min, 80min, 85min or 90min, but not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the drying temperature is 65-75 deg.C, such as 65 deg.C, 67 deg.C, 69 deg.C, 70 deg.C, 72 deg.C, 74 deg.C or 75 deg.C, but is not limited to the recited values, and other values not recited within the range of values are equally applicable.
The pretreatment sequentially comprises degreasing, pickling, drying and vacuum packaging, so that not only can impurities such as oil stains, dust, water stains and the like on the surfaces of the iron material and the tantalum material be removed, but also the iron material and the tantalum material can be effectively prevented from being oxidized by air, and further the purity requirement of the prepared iron-tantalum alloy powder is ensured.
As a preferable technical scheme of the invention, the mixing in the step (1) is carried out in a layered superposition mode in a melting crucible, and the method specifically comprises the following steps:
firstly, the iron material is laid at the bottom of the smelting crucible, then the tantalum material is laid on the iron material to form an iron-tantalum paving unit, and then the operations are repeated according to the iron-tantalum paving unit until the loading is finished.
According to the invention, the tantalum-iron-based paving units are mixed in a layered and superposed manner, so that local aggregation of tantalum materials with higher melting points and higher viscosity can be avoided, and the problems of non-uniform components of iron-tantalum melts obtained subsequently and pipeline blockage caused by overlarge local viscosity are prevented.
As a preferable technical scheme of the invention, the absolute vacuum degree of the melting in the step (2) is less than or equal to 10 Pa.
Preferably, the melting in step (2) is performed in a vacuum melting chamber, and then the iron tantalum melt is poured into a tundish, and the temperature of the tundish is controlled to 1550-.
According to the invention, the melting temperature is controlled to be 1542-1600 ℃ and the absolute vacuum degree is less than or equal to 10Pa, so that the iron-tantalum mixture can be fully melted and uniformly mixed; further, the obtained iron tantalum melt is poured into a tundish connected with the atomizing nozzle, the temperature of the iron tantalum melt is controlled to be 1550-.
In a preferred embodiment of the present invention, the inert gas in step (3) is argon.
Preferably, the purity of the argon gas is more than or equal to 5N.
Preferably, the atomization pressure in step (3) is 3-4MPa, such as 3MPa, 3.2MPa, 3.4MPa, 3.5MPa, 3.7MPa, 3.9MPa or 4MPa, but not limited to the recited values, and other values not recited in the range of values are also applicable.
The atomization pressure is set based on the characteristic that the iron-tantalum melt has high viscosity, and needs to be strictly controlled within the range of 3-4MPa, so that the iron-tantalum melt can be prevented from flowing downwards due to high atomization pressure, and the iron-tantalum alloy powder can be prevented from having large average particles due to low atomization pressure.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) preparing pretreated iron material and tantalum material according to a target atomic ratio, and then mixing the pretreated iron material and the pretreated tantalum material in a melting crucible in a layered superposition mode, wherein the method specifically comprises the following steps: firstly, laying the iron material at the bottom of the smelting crucible, then laying the tantalum material on the iron material to form an iron-tantalum laying unit, and then repeating the operation according to the iron-tantalum laying unit until the loading is finished to obtain an iron-tantalum mixture;
wherein the atomic ratio of tantalum in the target atomic ratio is 7.5-8.5%, and the balance is iron and unavoidable impurities;
the purity of the iron material is more than or equal to 99.95 percent, and the purity of the tantalum material is more than or equal to 99.95 percent;
the pretreatment sequentially comprises deoiling, pickling, drying and vacuum packaging;
(2) putting the iron-tantalum mixture obtained in the step (1) into a vacuum melting chamber, controlling the absolute vacuum degree to be less than or equal to 10Pa, and completely melting at 1542-1600 ℃ to obtain an iron-tantalum melt;
(3) pouring the iron tantalum fused mass obtained in the step (2) into a tundish, controlling the temperature of the tundish to be 1550-.
The invention relates to a preparation method, belonging to a gas atomization powder preparation method, which is a powder preparation method that takes high-pressure gas which moves rapidly as an atomization medium, breaks metal liquid or alloy liquid into fine liquid drops through the impact action and condenses the fine liquid drops into solid powder. The gas atomization method is the best method for producing completely alloyed powder, and the obtained particles of each alloy powder not only have the same uniform chemical composition as that of a given molten alloy, but also have a refined crystalline structure due to a rapid solidification effect, so that the macrosegregation of a second phase is eliminated.
The second purpose of the invention is to provide iron-tantalum alloy powder prepared by the preparation method of the first purpose.
The third purpose of the invention is to provide the application of the iron-tantalum alloy powder, wherein the iron-tantalum alloy powder of the second purpose is screened, and the iron-tantalum alloy powder with the granularity smaller than 150 meshes is used for preparing an iron-cobalt-tantalum alloy sputtering target material, in particular to the process for preparing the iron-cobalt-tantalum alloy sputtering target material by utilizing a hot isostatic pressing process.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the preparation method controls the melting temperature of the iron-tantalum mixture to be 1542-1600 ℃, and optimizes the atomization condition, so that the purity of the prepared iron-tantalum alloy powder is more than or equal to 99.95 percent, the oxygen content is less than or equal to 600ppm, the iron-tantalum alloy powder with the granularity of less than 150 meshes is obtained by screening, and the preparation method is favorable for preparing the iron-cobalt-tantalum alloy sputtering target material with high purity, high compactness, high bending strength and qualified magnetic flux;
(2) the preparation method of the invention prepares the tantalum rim charge of the tantalum target material as the tantalum material, which not only solves the problem of processing the tantalum rim charge generated in the machining process of the tantalum target material, but also can prepare the iron-tantalum alloy powder with extremely high application value, thereby changing waste into valuable.
Drawings
FIG. 1 is a scanning electron microscope image of FeTa alloy powder according to example 1 of the present invention;
FIG. 2 is an EDS energy spectrum of the iron-tantalum alloy powder according to example 1 of the present invention.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a preparation method of iron-tantalum alloy powder, which comprises the following steps:
(1) sequentially carrying out pretreatment of deoiling, pickling, drying and vacuum packaging on an electrolytic iron material with the purity of more than or equal to 99.95 percent and a tantalum rim charge (with the purity of more than or equal to 99.95 percent) of the tantalum target material disclosed by CN 102517531A:
respectively putting the electrolytic iron material and the tantalum rim charge into an aqueous solution containing a detergent, ultrasonically cleaning for 60min at 60 ℃ for deoiling treatment, and then washing and wiping the materials by pure water; then ultrasonically cleaning the steel plate for 20min in a pickling solution for pickling, wherein the pickling solution contains 38.5% of nitric acid and 7.1% of hydrofluoric acid by mass percent, and then washing the steel plate by pure water and wiping the steel plate clean; then, respectively putting the electrolytic iron material and the tantalum rim charge obtained by acid cleaning into a vacuum drying oven, and drying for 80min at 70 ℃; finally, vacuum packaging is carried out for standby;
preparing pretreated electrolytic iron material and tantalum rim charge according to the target atomic ratio of tantalum of 8%, the balance of iron and inevitable impurities, and then mixing in a melting crucible in a layered superposition mode, wherein the method specifically comprises the following steps: firstly, laying the iron material at the bottom of the smelting crucible, then laying the tantalum material on the iron material to form an iron-tantalum laying unit, and then repeating the operation according to the iron-tantalum laying unit until the loading is finished to obtain an iron-tantalum mixture;
(2) putting the iron-tantalum mixture obtained in the step (1) into a vacuum melting chamber, controlling the absolute vacuum degree to be less than or equal to 10Pa, and completely melting at 1570 ℃ to obtain an iron-tantalum melt;
(3) pouring the iron-tantalum fused mass obtained in the step (2) into a tundish, controlling the temperature of the tundish to be 1600 ℃, atomizing under the action of argon with the purity of more than or equal to 5N, and controlling the pressure to be 3.5MPa to obtain the iron-tantalum alloy powder.
Performing SEM-EDS detection on the iron-tantalum alloy powder, wherein a scanning electron micrograph is shown in figure 1, an EDS energy spectrum is shown in figure 2, and EDS energy spectrum measurement results are summarized in Table 1; as can be seen from fig. 1, the sphericity of the iron-tantalum alloy powder is high, and as can be seen from table 1, the composition of the iron-tantalum alloy powder satisfies the target atomic ratio.
TABLE 1
| Element(s) | Mass percent/％ | Atomic percent/%) | Error/%) |
| Fe | 78.02 | 91.99 | 1.63 |
| Ta | 21.98 | 8.01 | 2.31 |
| Total amount of | 100.00 | 100.00 | / |
Example 2
This example provides a method for producing an iron-tantalum alloy powder, which is identical to example 1 except that "controlling the absolute vacuum degree to be less than or equal to 10 Pa" in step (2) is replaced with "controlling the absolute vacuum degree to fluctuate between 12 Pa and 15 Pa".
Example 3
This example provides a method for producing an iron-tantalum alloy powder, which is identical to example 1 except that "pressure 3.5 MPa" in step (3) is replaced with "pressure 2.5 MPa".
Example 4
This example provides a method for producing an iron-tantalum alloy powder, which is identical to example 1 except that "pressure 3.5 MPa" in step (3) is replaced with "pressure 4.5 MPa".
Example 5
The embodiment provides a preparation method of iron-tantalum alloy powder, which comprises the following steps:
(1) sequentially carrying out pretreatment of deoiling, pickling, drying and vacuum packaging on an electrolytic iron material with the purity of more than or equal to 99.95 percent and a tantalum rim charge (with the purity of more than or equal to 99.95 percent) of the tantalum target material disclosed by CN 102517531A:
respectively putting the electrolytic iron material and the tantalum rim charge into an aqueous solution containing detergent, ultrasonically cleaning for 70min at 50 ℃ for deoiling treatment, and then washing and wiping the materials by pure water; then ultrasonically cleaning for 10min in a pickling solution for pickling, wherein the pickling solution contains 38.5% of nitric acid and 7.1% of hydrofluoric acid by mass percent, and then washing and wiping the pickling solution clean by pure water; then, respectively putting the electrolytic iron material and the tantalum rim charge obtained by acid cleaning into a vacuum drying oven, and drying for 90min at 65 ℃; finally, vacuum packaging is carried out for standby;
preparing pretreated electrolytic iron material and tantalum rim charge according to the target atomic ratio of 7.5% of tantalum, the balance of iron and inevitable impurities, and then mixing in a melting crucible in a layered superposition mode, wherein the method specifically comprises the following steps: firstly, laying the iron material at the bottom of the smelting crucible, then laying the tantalum material on the iron material to form an iron-tantalum laying unit, and then repeating the operation according to the iron-tantalum laying unit until the loading is finished to obtain an iron-tantalum mixture;
(2) putting the iron-tantalum mixture obtained in the step (1) into a vacuum melting chamber, controlling the absolute vacuum degree to be less than or equal to 10Pa, and completely melting at 1542 ℃ to obtain an iron-tantalum melt;
(3) pouring the iron-tantalum fused mass obtained in the step (2) into a tundish, controlling the temperature of the tundish to be 1550 ℃, atomizing under the action of argon with the purity of more than or equal to 5N, and controlling the pressure to be 4MPa to obtain the iron-tantalum alloy powder.
Example 6
The embodiment provides a preparation method of iron-tantalum alloy powder, which comprises the following steps:
(1) sequentially carrying out pretreatment of deoiling, pickling, drying and vacuum packaging on an electrolytic iron material with the purity of more than or equal to 99.95 percent and a tantalum rim charge (with the purity of more than or equal to 99.95 percent) of the tantalum target material disclosed by CN 102517531A:
respectively putting the electrolytic iron material and the tantalum rim charge into an aqueous solution containing detergent, ultrasonically cleaning for 50min at 70 ℃ for deoiling treatment, and then washing and wiping the electrolytic iron material and the tantalum rim charge clean by pure water; then ultrasonically cleaning the steel plate in a pickling solution for 30min for pickling, wherein the pickling solution contains 38.5% of nitric acid and 7.1% of hydrofluoric acid by mass percent, and then washing the steel plate with pure water and wiping the steel plate clean; then, respectively putting the electrolytic iron material and the tantalum rim charge obtained by acid cleaning into a vacuum drying oven, and drying for 60min at 75 ℃; finally, vacuum packaging is carried out for standby;
preparing pretreated electrolytic iron material and tantalum rim charge according to the target atomic ratio of tantalum of 8.5%, the balance of iron and inevitable impurities, and then mixing in a melting crucible in a layered superposition mode, wherein the method specifically comprises the following steps: firstly, laying the iron material at the bottom of the smelting crucible, then laying the tantalum material on the iron material to form an iron-tantalum laying unit, and then repeating the operation according to the iron-tantalum laying unit until the loading is finished to obtain an iron-tantalum mixture;
(2) putting the iron-tantalum mixture obtained in the step (1) into a vacuum melting chamber, controlling the absolute vacuum degree to be less than or equal to 10Pa, and completely melting at 1600 ℃ to obtain an iron-tantalum melt;
(3) pouring the iron-tantalum molten mass obtained in the step (2) into a tundish, controlling the temperature of the tundish to 1650 ℃, atomizing under the action of argon with the purity of more than or equal to 5N, and controlling the pressure to be 3MPa to obtain the iron-tantalum alloy powder.
Comparative example 1
This comparative example provides a method for preparing an iron-tantalum alloy powder, which is identical to example 1 except that "complete melting at 1570" in step (2) is replaced with "complete melting at 1500 ℃.
Comparative example 2
This comparative example provides a method for preparing an iron-tantalum alloy powder, which is identical to example 1 except that "complete melting at 1570" in step (2) is replaced with "complete melting at 1650 ℃.
The iron-tantalum alloy powder prepared in the above examples and comparative examples was subjected to the following performance tests:
sphericity: judging according to a scanning electron microscope image obtained by SEM-EDS detection;
oxygen content: the determination is carried out according to a thermal conductivity method disclosed in the general rules of analytical methods for hydrogen, oxygen, nitrogen, carbon and sulfur in metal materials of the national Standard GB/T14265-2017;
yield: the iron-tantalum alloy powder with the granularity less than 150 meshes obtained by screening accounts for the mass percentage of the feeding amount of the iron material and the tantalum material;
the results of the relevant tests on the iron tantalum alloy powders prepared in the above examples and comparative examples are shown in Table 2.
TABLE 2
From table 2, the following points can be obtained:
(1) according to the preparation method, the melting temperature of the iron-tantalum mixture is controlled to be 1542-; in addition, the tantalum rim charge of the tantalum target material is used as the tantalum material for preparation, so that waste is changed into valuable;
(2) comparing examples 1 and 2, it can be seen that in example 2, in the process of melting the iron-tantalum mixture, the absolute vacuum degree is controlled to fluctuate between 12 Pa and 15Pa, so that the oxygen content of the prepared iron-tantalum alloy powder is up to 580 ppm;
(3) comparing example 1 with examples 3 and 4, it can be seen that in example 3, the average particle size of the prepared iron-tantalum alloy powder is larger and the yield is reduced to 56% because the control pressure in the gas atomization process is lower than 3-4MPa and only 2.5 MPa; in the embodiment 4, the pressure is controlled to exceed 3-4MPa and reach 4.5MPa in the gas atomization process, so that the downward flow resistance of the iron-tantalum melt is large, and the yield of the prepared iron-tantalum alloy powder is only 47%;
(4) as can be seen by comparing the example 1 with the comparative examples 1 and 2, the melting temperature of the iron-tantalum mixture corresponding to the comparative example 1 is lower than 1542-1600 ℃ and is only 1500 ℃, so that the iron-tantalum melt has the problem of uneven components, the oxygen content of the prepared iron-tantalum alloy powder is up to 572ppm, and the yield of the prepared iron-tantalum alloy powder is only 67%; although the melting temperature of the iron-tantalum mixture is increased to 1650 ℃ in the comparative example 2, the sphericity, oxygen content and yield of the obtained iron-tantalum alloy powder are not much different from those of the iron-tantalum alloy powder in the example 1, but the energy consumption and cost investment are increased.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The preparation method of the iron-tantalum alloy powder is characterized by comprising the following steps:
(1) preparing and mixing an iron material and a tantalum material according to a target atomic ratio to obtain an iron-tantalum mixture;
(2) completely melting the iron-tantalum mixture obtained in the step (1) at 1542-1600 ℃ to obtain an iron-tantalum molten mass;
(3) and (3) atomizing the iron-tantalum fused mass obtained in the step (2) under the action of inert gas to obtain iron-tantalum alloy powder.
2. The production method according to claim 1, wherein the atomic ratio of tantalum in the target atomic ratio in step (1) is 7.5 to 8.5%, and the balance is iron and inevitable impurities.
3. The preparation method according to claim 1 or 2, wherein the purity of the iron material in the step (1) is more than or equal to 99.95 percent;
preferably, the iron material in the step (1) is an electrolytic iron material;
preferably, the purity of the tantalum material in the step (1) is more than or equal to 99.95 percent;
preferably, the tantalum material in the step (1) is a tantalum rim charge of a tantalum target material.
4. The production method according to any one of claims 1 to 3, further comprising, before the preparing of the iron material and the tantalum material in the target atomic ratio in step (1), respectively pretreating the iron material and the tantalum material;
preferably, the pretreatment sequentially comprises deoiling, pickling, drying and vacuum packaging;
preferably, the deoiling comprises respectively putting the iron material and the tantalum material into cleaning liquid for ultrasonic cleaning, and then washing and wiping the materials by pure water;
preferably, the cleaning liquid is an aqueous solution containing a detergent;
preferably, the ultrasonic cleaning time is 50-70 min;
preferably, the temperature of the ultrasonic cleaning is 50-70 ℃;
preferably, the acid washing comprises ultrasonic cleaning in acid washing solution, and then washing and wiping with pure water;
preferably, the acid washing solution is an aqueous solution of nitric acid and hydrofluoric acid;
preferably, the acid pickling solution contains 38.5% of nitric acid and 7.1% of hydrofluoric acid by mass percent;
preferably, the pickling time is 10-30 min;
preferably, the drying is carried out in a vacuum drying oven;
preferably, the drying time is 60-90 min;
preferably, the temperature of the drying is 65-75 ℃.
5. The preparation method according to any one of claims 1 to 4, wherein the mixing in step (1) is carried out in a layered superposition manner in a melting crucible, and specifically comprises the following steps:
firstly, the iron material is laid at the bottom of the smelting crucible, then the tantalum material is laid on the iron material to form an iron-tantalum paving unit, and then the operations are repeated according to the iron-tantalum paving unit until the loading is finished.
6. The production method according to any one of claims 1 to 5, wherein the absolute degree of vacuum of the melting in the step (2) is 10Pa or less;
preferably, the melting in the step (2) is performed in a vacuum melting chamber, and then the iron-tantalum molten mass is poured into a tundish, and the temperature of the tundish is controlled at 1550-.
7. The production method according to any one of claims 1 to 6, wherein the inert gas in the step (3) is argon;
preferably, the purity of the argon is more than or equal to 5N;
preferably, the atomization pressure of the step (3) is 3-4 MPa.
8. The production method according to any one of claims 1 to 7, characterized by comprising the steps of:
(1) preparing pretreated iron material and tantalum material according to a target atomic ratio, and then mixing the pretreated iron material and the pretreated tantalum material in a melting crucible in a layered superposition mode, wherein the method specifically comprises the following steps: firstly, laying the iron material at the bottom of the smelting crucible, then laying the tantalum material on the iron material to form an iron-tantalum laying unit, and then repeating the operation according to the iron-tantalum laying unit until the loading is finished to obtain an iron-tantalum mixture;
wherein the atomic ratio of tantalum in the target atomic ratio is 7.5-8.5%, and the balance is iron and unavoidable impurities;
the purity of the iron material is more than or equal to 99.95 percent, and the purity of the tantalum material is more than or equal to 99.95 percent;
the pretreatment sequentially comprises deoiling, pickling, drying and vacuum packaging;
(2) putting the iron-tantalum mixture obtained in the step (1) into a vacuum melting chamber, controlling the absolute vacuum degree to be less than or equal to 10Pa, and completely melting at 1542-1600 ℃ to obtain an iron-tantalum melt;
(3) pouring the iron tantalum fused mass obtained in the step (2) into a tundish, controlling the temperature of the tundish to be 1550-.
9. An iron-tantalum alloy powder, characterized by being produced by the production method according to any one of claims 1 to 8.
10. Use of the iron tantalum alloy powder according to claim 9 for preparing an iron cobalt tantalum alloy sputtering target by sieving the iron tantalum alloy powder with a particle size of less than 150 meshes.
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