CN112059195B - Preparation method of ferrotantalum alloy powder, ferrotantalum alloy powder and application - Google Patents
Preparation method of ferrotantalum alloy powder, ferrotantalum alloy powder and application Download PDFInfo
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- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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Abstract
The invention relates to a preparation method of ferrotantalum alloy powder, the ferrotantalum alloy powder and application, wherein the preparation method of the ferrotantalum alloy powder comprises the following steps: firstly, preparing an iron material and a tantalum material according to a target atomic ratio and mixing; then melting completely 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 1542-1600 ℃, optimizes atomization conditions, ensures 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, and utilizes the iron-tantalum alloy powder with granularity less than 150 meshes obtained by screening, thereby being beneficial to 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 is used as the tantalum material to be prepared, 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, iron-tantalum alloy powder and application thereof.
Background
With the rapid development of society and the rapid increase of people's demands for information storage, recording media such as hard disks and optical disks using magnetic information storage technology are getting more and more attention, and the important positions are occupied in the information storage field by virtue of the advantages of high storage density, large capacity, low price and the like. Magnetic recording is a method of recording information by utilizing the magnetic properties, and can input and read information by a special method during storage and use, thereby achieving the purpose of storing information and reading information. Magnetic recording includes both horizontal magnetic recording and vertical magnetic recording, depending on the positional relationship of the magnetization direction of the medium and the surface of the medium.
Currently, in the magnetic recording market, the perpendicular magnetic recording technology has comprehensively replaced the horizontal magnetic recording technology. Because perpendicular magnetic recording technology has made the areal density and capacity of magnetic recording media rapidly increasing, common magnetic recording media are hard disks, magnetic disks, optical disks, and the like. The magnetic recording medium generally adopts a multilayer vertical structure design, taking a hard disk as an example, and specifically comprises a lubricating layer, a protective layer, a magnetic recording layer, an intermediate layer, a soft magnetic substrate layer, a substrate layer and a base layer. Among them, the soft magnetic underlayer mainly plays a role in recording and storing data, and plays a vital role in magnetic recording media. Currently, iron-cobalt-tantalum alloy films obtained by sputtering processes are the most commonly used soft magnetic substrate layers.
Sputtering is one of the main techniques for preparing thin film materials, and it uses ions generated by an ion source to form high-speed energy ion beam through accelerating aggregation in vacuum, bombard the solid surface, and the ions and atoms on the solid surface undergo kinetic energy exchange, so that the atoms on the solid surface leave the solid and are deposited on the surface of the substrate, and the bombarded solid is a raw material for preparing thin film deposited by sputtering, and the solid is generally called as sputtering target.
The iron-cobalt-tantalum alloy sputtering target material for preparing the soft magnetic substrate layer by sputtering needs to have high compactness, high bending strength and high magnetic flux: the high density can ensure that the thin film obtained by sputtering is relatively uniform, and abnormal phenomena such as 'discharge' and the like are not easy to occur; the bending strength can influence the coercive force of the magnetic material and has a critical influence on the storage of information of the magnetic material, so that the high bending strength can ensure that the target is not easy to crack and other abnormal problems during use; target flux is a very important parameter in magnetic recording targets, and in general, the higher the target flux, the more data recording and storing capabilities. Therefore, the quality of the iron-cobalt-tantalum alloy sputtering target material relates to the development of a soft magnetic substrate layer and even the whole magnetic recording industry.
At present, the prior art discloses a preparation method of iron-cobalt-tantalum alloy sputtering targets, for example, CN108004515a discloses a preparation method of iron-cobalt-tantalum alloy sputtering targets, 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 carried out to obtain the iron-cobalt-tantalum alloy sputtering targets. However, the preparation method directly uses the mixed powder obtained by mixing the iron powder, the cobalt powder and the tantalum powder according to the required proportion, so that only a small amount or no compound is formed on three metals before hot pressing sintering, thereby the elemental iron or the elemental cobalt shows magnetism, and finally the magnetic flux of the iron-cobalt-tantalum alloy sputtering target is lower;
CN105473759a discloses an Fe-Co alloy sputtering target, a soft magnetic thin film layer, and a perpendicular magnetic recording medium using the same, wherein the manufacturing method includes a step of preparing Fe-Co alloy powder and pressure sintering the powder. The Fe-Co alloy powder obtained by the preparation method directly uses a 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, a pipeline is very easy to be blocked, the gas atomization method fails, and the Fe-Co alloy powder with the target proportion requirement is purchased in no place in the market, so that the preparation and 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 difficult preparation of the iron-cobalt-tantalum alloy powder can be avoided. Therefore, the invention provides a preparation method of the iron-tantalum alloy powder, the iron-tantalum alloy powder and application thereof.
Disclosure of Invention
In view of the problems existing in the prior art, the invention provides a preparation method of iron-tantalum alloy powder, iron-tantalum alloy powder and application, wherein the preparation method controls the melting temperature of iron-tantalum mixture to 1542-1600 ℃, optimizes atomization conditions, ensures 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, and is beneficial to preparing the iron-cobalt-tantalum alloy sputtering target material with high purity, high compactness, high bending strength and qualified magnetic flux by utilizing the iron-tantalum alloy powder with granularity less than 150 meshes obtained by sieving.
To achieve the purpose, the invention adopts the following technical scheme:
the invention aims 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 in the step (1) at 1542-1600 ℃ to obtain iron-tantalum melt;
(3) Atomizing the iron-tantalum melt in the step (2) under the action of inert gas to obtain the iron-tantalum alloy powder.
According to the preparation method disclosed by the invention, the melting temperature of the iron-tantalum mixture is controlled to 1542-1600 ℃, the atomization condition is optimized, the problem of pipeline blockage caused by viscosity of the iron-tantalum mixture is avoided, the iron-tantalum alloy powder with the purity of more than or equal to 99.95% and the oxygen content of less than or equal to 600ppm can be prepared, and the iron-tantalum alloy powder with the granularity of less than 150 meshes obtained by sieving is used for preparing the iron-cobalt-tantalum alloy sputtering target material with high purity, high compactness, high bending strength and qualified magnetic flux.
The melting temperature of the iron-tantalum mixture of the present invention is 1542-1600 ℃, for example 1542 ℃, 1550 ℃, 1560 ℃, 1570 ℃, 1580 ℃, 1590 ℃, 1600 ℃, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
As a preferred technical scheme of the invention, the atomic ratio of tantalum in the target atomic ratio in the step (1) is 7.5-8.5%, and the balance is iron and unavoidable impurities.
The atomic ratio of tantalum according to the present invention is 7.5-8.5%, such as 7.5%, 7.7%, 8%, 8.2% or 8.5%, etc., but is not limited to the recited values, and other non-recited values within this range are equally applicable.
The total content of the unavoidable impurities is less than 0.05%, and the purity of the prepared iron-tantalum alloy powder is more than or equal to 99.95%.
According to the invention, 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 the lowest under the atomic proportion, and the bearing pressure of smelting equipment is the lowest; on the other hand, the atomic ratio of the Fe-Ta alloy powder can ensure that the ratio of Fe is far higher than that of Ta, so that the Fe-Co-Ta alloy powder with the target atomic ratio can be obtained by subsequent combination and proportioning with the Co-Ta alloy powder, and further the Fe-Co-Ta alloy sputtering target is 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 electrolytic iron material.
Preferably, the purity of the tantalum material in the step (1) is more than or equal to 99.95%.
Preferably, the tantalum material in the step (1) is tantalum rim charge of a tantalum target.
The tantalum target material disclosed by the invention can be a tantalum target material disclosed by 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 assembly.
As a preferable technical scheme of the invention, before preparing the iron material and the tantalum material according to the target atomic ratio in the step (1), the method further comprises respectively preprocessing the iron material and the tantalum material.
Preferably, the pretreatment comprises degreasing, pickling, drying and vacuum packaging in sequence.
As is well known to those skilled in the art, the preparation of the powder-making material is completed, and the process of transportation, storage and the like is carried out in the middle, so that the pretreated powder-making material is required to be vacuum packed, thereby being beneficial to isolating dust and air, reducing the oxygen absorption reaction of the powder-making material, and further 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 degreasing includes ultrasonic cleaning of the iron and tantalum materials in cleaning liquid, respectively, followed by rinsing with pure water and wiping clean.
Preferably, the cleaning liquid is an aqueous solution containing a detergent.
The aqueous solution containing the liquid detergent is not limited in concentration, and a person skilled in the art can reasonably select the type and the concentration of the liquid detergent according to actual conditions, so long as the greasy dirt can be cleaned.
Preferably, the time of the ultrasonic cleaning is 50-70min, for example, 50min, 52min, 55min, 57min, 60min, 63min, 65min, 68min or 70min, etc., but not limited to the recited values, and other non-recited values within the range of values are equally 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 non-recited values within the range of the recited values are equally applicable.
Preferably, the pickling comprises ultrasonic cleaning in a pickling solution, followed by rinsing with pure water and wiping clean.
Preferably, the pickling solution is an aqueous solution of nitric acid and hydrofluoric acid.
Preferably, the nitric acid in the pickling solution is 38.5% and the hydrofluoric acid in the pickling solution is 7.1% by mass.
Preferably, the pickling time is 10-30min, for example 10min, 13min, 15min, 17min, 20min, 23min, 25min, 27min or 30min, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the drying is performed in a vacuum drying oven.
Preferably, the drying time is 60-90min, such as 60min, 65min, 70min, 75min, 80min, 85min or 90min, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the drying temperature is 65-75deg.C, such as 65deg.C, 67 deg.C, 69 deg.C, 70deg.C, 72 deg.C, 74 deg.C or 75deg.C, etc., but is not limited to the values recited, and other values not recited in the range are equally applicable.
The pretreatment of the method sequentially comprises degreasing, acid washing, drying and vacuum packaging, so that not only can the impurities such as greasy dirt, dust, water stain 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 smelting crucible in a layered superposition mode, and specifically comprises the following steps:
firstly paving the iron material at the bottom of the smelting crucible, then paving the tantalum material on the iron material to form an iron-tantalum paving unit, and then repeating the operation according to the iron-tantalum paving unit until the charging is completed.
According to the invention, the tantalum-iron-based spreading units are mixed in a layered and overlapped mode, so that local aggregation of tantalum materials with higher melting points and higher viscosity can be avoided, and the problems of uneven components of the subsequently obtained iron-tantalum melt and pipeline blockage caused by overlarge local viscosity can be prevented.
As a preferable technical scheme of the invention, the absolute vacuum degree of melting in the step (2) is less than or equal to 10Pa.
Preferably, the melting of step (2) is performed in a vacuum melting chamber, and then the iron tantalum melt is poured into a tundish, the temperature of which is controlled to 1550-1650 ℃, such as 1550 ℃, 1560 ℃, 1580 ℃, 1600 ℃, 1610 ℃, 1630 ℃, 1650 ℃ or the like, but not limited to the recited values, other non-recited values within the range of values are equally applicable.
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 an atomizing nozzle, and the temperature of the tundish is controlled to 1550-1650 ℃, so that the iron-tantalum melt can be effectively prevented from blocking the tundish, and the iron-tantalum melt can be effectively prevented from blocking a flow guide pipe between the tundish and the atomizing nozzle.
As a preferable technical scheme of the invention, 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 in step (3) is 3-4MPa, for example 3MPa, 3.2MPa, 3.4MPa, 3.5MPa, 3.7MPa, 3.9MPa or 4MPa, etc., but is not limited to the values recited, and other values not recited in this range are equally applicable.
The atomization pressure is set based on the characteristic of larger viscosity of the iron tantalum melt, and needs to be strictly controlled within a range of 3-4MPa, so that the iron tantalum melt is prevented from being blocked from flowing downwards by larger atomization pressure, and the average particle size of the iron tantalum alloy powder is prevented from being larger due to smaller atomization pressure.
As a preferable technical scheme of the invention, the preparation method comprises the following steps:
(1) Preparing pretreated iron materials and tantalum materials according to a target atomic ratio, and then mixing in a smelting crucible in a layered superposition mode, wherein the method specifically comprises the following steps: firstly paving the iron material at the bottom of the smelting crucible, paving the tantalum material on the iron material to form an iron-tantalum paving unit, and repeating the operation according to the iron-tantalum paving unit until the charging is completed to obtain an iron-tantalum mixture;
wherein, the atomic proportion of tantalum in the target atomic proportion 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 degreasing, pickling, drying and vacuum packaging;
(2) Putting the iron-tantalum mixture in the step (1) into a vacuum smelting chamber, controlling the absolute vacuum degree to be less than or equal to 10Pa, and completely smelting at 1542-1600 ℃ to obtain iron-tantalum melt;
(3) Pouring the iron-tantalum melt in the step (2) into a tundish, controlling the temperature of the tundish to 1550-1650 ℃, atomizing under the action of argon with the purity of more than or equal to 5N, and controlling the pressure to 3-4MPa to obtain the iron-tantalum alloy powder.
The preparation method of the invention belongs to an aerosol powder preparation method, and is a powder preparation method which takes fast-moving high-pressure gas as an atomizing medium, breaks metal liquid or alloy liquid into fine liquid drops through impact action and condenses the fine liquid drops into solid powder. The gas atomization method is the best method for producing fully alloyed powders, and the particles of each alloy powder obtained not only have the same uniform chemical composition as the given molten alloy, but also refine the crystalline structure due to the rapid solidification, eliminating macrosegregation of the second phase.
The second purpose of the invention is to provide iron tantalum alloy powder which is prepared by the preparation method of one purpose.
The invention further provides an application of the iron-tantalum alloy powder, wherein two iron-tantalum alloy powders are screened, and the iron-tantalum alloy powder with granularity less than 150 meshes is used for preparing iron-cobalt-tantalum alloy sputtering targets, in particular to a process for preparing the iron-cobalt-tantalum alloy sputtering targets by using a hot isostatic pressing process.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) According to the preparation method, the melting temperature of the iron-tantalum mixture is controlled to be 1542-1600 ℃, and atomization conditions are optimized, 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, and the iron-tantalum alloy powder with the granularity less than 150 meshes obtained by screening is utilized, so that the preparation of the iron-cobalt-tantalum alloy sputtering target material with high purity, high compactness, high bending strength and qualified magnetic flux is facilitated;
(2) According to the preparation method disclosed by the invention, the tantalum rim charge of the tantalum target is used as the tantalum charge for preparation, so that the problem of treatment of the tantalum rim charge generated in the machining process of the tantalum target is solved, and the iron-tantalum alloy powder with extremely high application value can be prepared, thereby realizing waste recycling.
Drawings
FIG. 1 is a scanning electron microscope image of the iron tantalum alloy powder of example 1 of the present invention;
fig. 2 is an EDS spectrum of the iron tantalum alloy powder of example 1 of the present invention.
Detailed Description
The technical scheme of the invention is further described below by the specific embodiments with reference to the accompanying drawings. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a preparation method of iron-tantalum alloy powder, which comprises the following steps:
(1) Sequentially degreasing, pickling, drying and vacuum packaging the electrolytic iron material with the purity of more than or equal to 99.95% and tantalum rim charge (with the purity of more than or equal to 99.95%) of the tantalum target material disclosed in CN 102517531A:
respectively placing the electrolytic iron material and tantalum rim charge into an aqueous solution containing a detergent, performing ultrasonic cleaning at 60 ℃ for 60min for degreasing treatment, and then washing with pure water and wiping cleanly; then ultrasonic cleaning is carried out in acid pickling solution for 20min, the nitric acid in the acid pickling solution is 38.5 percent and the hydrofluoric acid in the acid pickling solution is 7.1 percent according to the mass percent, and then the acid pickling solution is washed and wiped clean by pure water; then respectively placing the electrolytic iron material and tantalum rim charge obtained by acid washing into a vacuum drying oven, and drying for 80 minutes at 70 ℃; finally, vacuum packaging is carried out for standby;
according to the atomic proportion of tantalum being 8%, the balance being iron and unavoidable impurities as target atomic proportions, preparing pretreated electrolytic iron material and tantalum rim charge, and then mixing in a smelting crucible in a layered superposition mode, wherein the method specifically comprises the following steps: firstly paving the iron material at the bottom of the smelting crucible, paving the tantalum material on the iron material to form an iron-tantalum paving unit, and repeating the operation according to the iron-tantalum paving unit until the charging is completed to obtain an iron-tantalum mixture;
(2) Putting the iron-tantalum mixture in the step (1) into a vacuum smelting chamber, controlling the absolute vacuum degree to be less than or equal to 10Pa, and completely smelting at 1570 ℃ to obtain iron-tantalum melt;
(3) Pouring the iron-tantalum melt in the step (2) into a tundish, controlling the temperature of the tundish to 1600 ℃, atomizing under the action of argon with the purity of more than or equal to 5N, and controlling the pressure to 3.5MPa to obtain the iron-tantalum alloy powder.
SEM-EDS detection is carried out on the iron tantalum alloy powder, a scanning electron microscope image is shown in fig. 1, an EDS energy spectrum is shown in fig. 2, and EDS energy spectrum measurement results are summarized in Table 1; among them, 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
The present example provides a method for producing an iron tantalum alloy powder, and the other conditions are exactly the same as in example 1 except that the "control absolute vacuum degree is 10Pa or less" in step (2) is replaced by "control absolute vacuum degree fluctuates between 12 and 15 Pa".
Example 3
This example provides a method for producing an iron tantalum alloy powder, and the conditions are exactly the same as in example 1 except that the "pressure of 3.5MPa" in step (3) is replaced with "pressure of 2.5 MPa".
Example 4
This example provides a method for producing an iron tantalum alloy powder, and the conditions are exactly the same as in example 1 except that the "pressure of 3.5MPa" in step (3) is replaced with "pressure of 4.5 MPa".
Example 5
The embodiment provides a preparation method of iron-tantalum alloy powder, which comprises the following steps:
(1) Sequentially degreasing, pickling, drying and vacuum packaging the electrolytic iron material with the purity of more than or equal to 99.95% and tantalum rim charge (with the purity of more than or equal to 99.95%) of the tantalum target material disclosed in CN 102517531A:
firstly, respectively placing the electrolytic iron material and tantalum rim charge into an aqueous solution containing a detergent, carrying out ultrasonic cleaning at 50 ℃ for 70min for degreasing treatment, and then washing with pure water and wiping cleanly; then ultrasonic cleaning is carried out in acid pickling solution for 10min, wherein the nitric acid in the acid pickling solution is 38.5 percent and the hydrofluoric acid in the acid pickling solution is 7.1 percent by mass percent, and then the acid pickling solution is washed and wiped clean by pure water; then respectively placing the electrolytic iron material and tantalum rim charge obtained by acid washing into a vacuum drying oven, and drying for 90min at 65 ℃; finally, vacuum packaging is carried out for standby;
according to the atomic proportion of tantalum being 7.5%, the balance being iron and unavoidable impurities as target atomic proportions, preparing pretreated electrolytic iron material and tantalum rim charge, and then mixing in a smelting crucible in a layered superposition mode, wherein the method specifically comprises the following steps: firstly paving the iron material at the bottom of the smelting crucible, paving the tantalum material on the iron material to form an iron-tantalum paving unit, and repeating the operation according to the iron-tantalum paving unit until the charging is completed to obtain an iron-tantalum mixture;
(2) Putting the iron-tantalum mixture in the step (1) into a vacuum smelting chamber, controlling the absolute vacuum degree to be less than or equal to 10Pa, and completely smelting at 1542 ℃ to obtain iron-tantalum melt;
(3) Pouring the iron-tantalum melt in the step (2) into a tundish, controlling the temperature of the tundish to 1550 ℃, atomizing under the action of argon with the purity of more than or equal to 5N, and controlling the pressure to 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 degreasing, pickling, drying and vacuum packaging the electrolytic iron material with the purity of more than or equal to 99.95% and tantalum rim charge (with the purity of more than or equal to 99.95%) of the tantalum target material disclosed in CN 102517531A:
respectively placing the electrolytic iron material and tantalum rim charge into an aqueous solution containing a detergent, performing ultrasonic cleaning at 70 ℃ for 50min for degreasing treatment, and then washing with pure water and wiping cleanly; then ultrasonic cleaning is carried out in pickling solution for 30min, nitric acid in the pickling solution is 38.5% and hydrofluoric acid in the pickling solution is 7.1% by mass, and then the pickling solution is washed and wiped clean by pure water; then respectively placing the electrolytic iron material and tantalum rim charge obtained by acid washing into a vacuum drying oven, and drying for 60 minutes at 75 ℃; finally, vacuum packaging is carried out for standby;
according to the atomic proportion of tantalum being 8.5%, the balance being iron and unavoidable impurities as target atomic proportions, preparing pretreated electrolytic iron material and tantalum rim charge, and then mixing in a smelting crucible in a layered superposition mode, wherein the method specifically comprises the following steps: firstly paving the iron material at the bottom of the smelting crucible, paving the tantalum material on the iron material to form an iron-tantalum paving unit, and repeating the operation according to the iron-tantalum paving unit until the charging is completed to obtain an iron-tantalum mixture;
(2) Putting the iron-tantalum mixture in the step (1) into a vacuum smelting chamber, controlling the absolute vacuum degree to be less than or equal to 10Pa, and completely smelting at 1600 ℃ to obtain iron-tantalum melt;
(3) Pouring the iron-tantalum melt in the step (2) into a tundish, controlling the temperature of the tundish to be 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 iron tantalum alloy powder, and the conditions are exactly the same as in example 1 except that the "melting completion at 1570 ℃ in step (2) is replaced by" melting completion at 1500 ℃.
Comparative example 2
This comparative example provides a method for preparing iron tantalum alloy powder, and the conditions are exactly the same as in example 1 except that the "melting completion at 1570 ℃ in step (2) is replaced with" melting completion at 1650 ℃.
The iron-tantalum alloy powders prepared in the above examples and comparative examples were subjected to the following performance tests:
sphericity degree: 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 national standard GB/T14265-2017 general rules of analysis methods of hydrogen, oxygen, nitrogen, carbon and sulfur in metal materials;
yield rate: the iron-tantalum alloy powder with the granularity less than 150 meshes obtained by sieving accounts for the mass percent of the feeding amount of the iron material and the tantalum material;
the results of the tests concerning the tantalum iron alloy powders prepared in the above examples and comparative examples are shown in Table 2.
TABLE 2
The following points can be found from table 2:
(1) According to the preparation method disclosed by the invention, the melting temperature of the iron-tantalum mixture is controlled to 1542-1600 ℃, and the atomization condition is optimized, so that the prepared iron-tantalum alloy powder has good sphericity and the oxygen content is less than or equal to 600ppm, the iron-tantalum alloy powder with the granularity less than 150 meshes obtained by screening has higher corresponding yield and can reach 85% at most, 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 addition, the tantalum rim charge of the tantalum target is used as the tantalum material for preparation, so that waste is changed into valuable;
(2) As can be seen from comparative examples 1 and 2, in example 2, the absolute vacuum degree was controlled to fluctuate between 12 to 15Pa during the melting process of the iron-tantalum mixture, resulting in the oxygen content of the prepared iron-tantalum alloy powder being up to 580ppm;
(3) As can be seen from comparative examples 1 and examples 3 and 4, since the control pressure of example 3 is lower than 3-4MPa and is only 2.5MPa in the process of gas atomization, the average granularity of the prepared iron-tantalum alloy powder is larger, and the yield is reduced to 56%; because the control pressure of the embodiment 4 exceeds 3-4MPa and reaches 4.5MPa in the gas atomization process, the downward flowing resistance of the iron-tantalum melt is high, and the yield of the prepared iron-tantalum alloy powder is only 47%;
(4) As can be seen from comparative examples 1 and 2, the melting temperature of the iron-tantalum mixture corresponding to 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 comparative example 2 increased the melting temperature of the iron-tantalum mixture to 1650 deg.c, the sphericity, oxygen content, yield of the resulting iron-tantalum alloy powder were not much different from example 1, but the energy consumption and cost input were increased.
The applicant states that the detailed structural features of the present invention are described by the above embodiments, but the present invention is not limited to the above detailed structural features, i.e. it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be apparent to those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope of the present invention and the scope of the disclosure.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (7)
1. The preparation method of the iron-tantalum alloy powder is characterized by comprising the following steps of:
(1) Preparing and mixing an iron material and a tantalum material according to a target atomic ratio to obtain an iron-tantalum mixture; the purity of the iron material is more than or equal to 99.95%; the iron material is electrolytic iron material; the purity of the tantalum material is more than or equal to 99.95%; the tantalum material is tantalum rim charge of a tantalum target material;
wherein, the atomic proportion of tantalum in the target atomic proportion is 7.5-8.5%, and the balance is iron and unavoidable impurities;
the mixing is carried out in a smelting crucible in a layered superposition mode, and specifically comprises the following steps:
firstly paving the iron material at the bottom of the smelting crucible, paving the tantalum material on the iron material to form an iron-tantalum paving unit, and repeating the operation according to the iron-tantalum paving unit until the charging is completed;
(2) Putting the iron-tantalum mixture in the step (1) into a vacuum smelting chamber, controlling the absolute vacuum degree to be less than or equal to 10Pa, and completely smelting at 1542-1600 ℃ to obtain iron-tantalum melt;
(3) Pouring the iron-tantalum melt in the step (2) into a tundish, controlling the temperature of the tundish to 1550-1650 ℃, atomizing under the action of argon with the purity of more than or equal to 5N, and controlling the pressure to 3-4MPa to obtain the iron-tantalum alloy powder;
the purity of the iron-tantalum alloy powder is more than or equal to 99.95 percent, the oxygen content is less than or equal to 600ppm, and the yield corresponding to the iron-tantalum alloy powder with the granularity less than 150 meshes obtained by sieving can reach 85 percent at the highest.
2. The method according to claim 1, further comprising pretreating the iron and tantalum materials, respectively, before preparing the iron and tantalum materials in the target atomic ratio in step (1); the pretreatment comprises degreasing, pickling, drying and vacuum packaging in sequence.
3. The method according to claim 2, wherein the degreasing includes ultrasonic cleaning of the iron and tantalum materials in a cleaning liquid, followed by rinsing with pure water and wiping clean; the cleaning liquid is an aqueous solution containing a detergent; the ultrasonic cleaning time is 50-70min; the temperature of the ultrasonic cleaning is 50-70 ℃.
4. The method of claim 2, wherein the pickling comprises ultrasonic cleaning in a pickling solution followed by rinsing with pure water and wiping clean; the pickling solution is an aqueous solution of nitric acid and hydrofluoric acid; the pickling solution comprises 38.5 mass percent of nitric acid and 7.1 mass percent of hydrofluoric acid; the pickling time is 10-30min.
5. The method of claim 2, wherein the drying is performed in a vacuum oven; the drying time is 60-90min; the drying temperature is 65-75 ℃.
6. An iron tantalum alloy powder prepared by the method of any one of claims 1 to 5.
7. The use of the iron-tantalum alloy powder, which is characterized in that the iron-tantalum alloy powder of claim 6 is screened, and the iron-tantalum alloy powder with the granularity less than 150 meshes is used for preparing an iron-cobalt-tantalum alloy sputtering target.
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