CN115194161A - Production process of high-purity tantalum powder - Google Patents
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- CN115194161A CN115194161A CN202210941268.XA CN202210941268A CN115194161A CN 115194161 A CN115194161 A CN 115194161A CN 202210941268 A CN202210941268 A CN 202210941268A CN 115194161 A CN115194161 A CN 115194161A
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Abstract
The invention provides a production process of high-purity tantalum powder, which comprises the following steps: high-temperature sintering, rapid quenching, pressurized hydrogenation, vacuum crushing, screening, dehydrogenation and oxygen reduction, acid washing for impurity removal and spheroidization, and the obtained low-oxygen niobium powder meets the following conditions: the oxygen content is less than or equal to 50ppm, the iron content is less than or equal to 3ppm, the magnesium content is less than or equal to 3ppm, the aluminum content is less than or equal to 3ppm, and the D50 is 10 to 40 mu m. According to the method, the tantalum ingot block sequentially passes through the working procedures of high-temperature sintering, rapid quenching, pressure hydrogenation, vacuum crushing, screening, dehydrogenation and oxygen reduction, acid washing and impurity removal and spheroidizing, so that the prepared tantalum powder is low in impurity content, low in oxygen content and high in purity.
Description
Technical Field
The invention relates to the technical field of tantalum powder, in particular to a production process of high-purity tantalum powder.
Background
In the field of industrial technology, along with the development of semiconductor technology, the integration degree of computer chips is higher and higher, when the line width of a chip enters the field of 90-45 nm, cu in a Cu coating film can carry out atomic diffusion to a Si sheet, in order to change the phenomenon, the chip coating process adopts Ta as a barrier layer material for preventing Cu from diffusing to Si, a sputtering target material is developed from an Al/Ti system to a Cu/Ta system, and the demand of a tantalum sputtering target is greatly increased. The tantalum sputtering target can be machined from a high-purity tantalum ingot, and can also be prepared from tantalum powder by hot-pressing sintering. The sputtering target prepared by hot pressing of tantalum powder can not only reduce the machining difficulty, but also eliminate the inherent texture belt of tantalum, and generate a film with higher uniformity in sputtering. Tantalum powders for tantalum sputtering targets are typically produced by the hydriding comminution of high purity tantalum ingots. The tantalum ingot hydrogenated powder also occupies a place in the preparation of tantalum capacitors, another important application field of tantalum, and is particularly used in large quantity in the preparation of medium and high voltage tantalum capacitors.
In the hydrogenation processing process of the high-purity tantalum ingot, the tantalum ingot needs to be subjected to the working procedures of sintering, hydrogenation, crushing, dehydrogenation for oxygen reduction, acid washing and the like. By adopting the conventional process, because the hardness of the tantalum ingot is high, the granularity of the tantalum powder generated after crushing is high, the hydrogenation degree is low and the oxygen reduction rate is low in the subsequent hydrogenation process, and the prepared tantalum powder generally has the problems of high impurity content and high oxygen content, so that the purity of the tantalum powder is low, and the application requirement in the field of semiconductors is not met. Therefore, there is a need for a process for producing tantalum powder, which can produce high-purity tantalum powder to meet the above requirements.
Disclosure of Invention
Aiming at the technical defects in the background art, the invention provides a production process of high-purity tantalum powder, which solves the technical problems and meets the actual requirements, and the specific technical scheme is as follows:
a production process of high-purity tantalum powder comprises the following steps:
s1, high-temperature sintering: placing the tantalum ingot block in a vacuum sintering furnace, filling inert protective gas, keeping the pressure in the furnace at 0.08-0.10MPa, and carrying out heat treatment at the temperature of 600-750 ℃ for 30-60min;
s2, rapid quenching: rapidly cooling the tantalum ingot to below 60 ℃;
s3, pressure hydrogenation: filling hydrogen into the vacuum sintering furnace, increasing the pressure in the vacuum sintering furnace to 1-2MPa, and hydrogenating by using the hydrogen to obtain a tantalum hydride ingot;
s4, vacuum crushing: crushing the tantalum hydride ingot in a vacuum environment to obtain tantalum hydride powder;
s5, screening: sieving by using a standard sieve of 400-800 meshes to obtain tantalum hydride powder which can pass through the standard sieve of 400-800 meshes;
s6, dehydrogenation and oxygen reduction: carrying out dehydrogenation and oxygen reduction on the tantalum hydride powder to obtain tantalum powder subjected to dehydrogenation and oxygen reduction;
s7, acid washing and impurity removal: carrying out acid washing treatment on the tantalum powder subjected to dehydrogenation and deoxidation to obtain high-purity tantalum powder;
s8, spheroidizing: and placing the high-purity tantalum powder in a ball mill to obtain the high-purity tantalum powder with the particle shape close to a sphere.
Specifically, in step S1, the inert shielding gas is selected from one of helium, neon and argon.
Specifically, in the step S1, the vacuum sintering furnace is a microwave heating vacuum sintering furnace, and the microwave heating power is 5kw to 6kw.
Specifically, in step S2, normal-temperature or low-temperature nitrogen is filled into the inner cavity of the vacuum sintering furnace by using a nitrogen filling device, and the tantalum ingot is rapidly cooled to below 60 ℃ within 10min through nitrogen heat exchange.
Specifically, in step S3, hydrogen is introduced into the vacuum sintering furnace, the pressure in the furnace is increased to 0.5 to 2MPa, the temperature is kept at 700 to 900 ℃ for 1 to 2h, and the niobium hydride ingot is obtained after cooling.
Specifically, in step S4, crushing the tantalum hydride ingot by using a vacuum crusher to obtain tantalum hydride powder.
Specifically, in step S6, tantalum hydride powder and 3-6% of metal reducing agent are mixed and then added into a dehydrogenation oxygen reduction furnace, the mixture is heated to 900-950 ℃ and is kept warm for 4-10h, then the pressure in the furnace is released, the mixture is kept warm for 3-4h at 900-950 ℃, finally the temperature is reduced to 25-30 ℃, and the mixture is discharged after passivation, so that the tantalum powder for dehydrogenation oxygen reduction is obtained.
Specifically, in step S7, the tantalum powder after dehydrogenation and deoxidation is subjected to acid washing by using a 20% hydrochloric acid solution, so as to remove impurities such as magnesium ions, iron ions, aluminum ions and the like, and is filtered and washed by pure water and dried in a vacuum drying oven at 80 ℃ to obtain the high-purity tantalum powder.
Specifically, the high-purity tantalum powder obtained in the step S7 has an oxygen content of less than or equal to 50ppm, an iron content of less than or equal to 3ppm, a magnesium content of less than or equal to 3ppm, and an aluminum content of less than or equal to 3ppm.
Specifically, the D50 of the high-purity tantalum powder obtained in the step S8 is 10 to 40 μm.
The invention has the beneficial effects that:
1. according to the production process, tantalum ingot blocks are sequentially subjected to high-temperature sintering, rapid quenching, pressure hydrogenation, vacuum crushing, screening, dehydrogenation and oxygen reduction, acid pickling and impurity removal and spheroidization, so that the prepared tantalum powder is low in impurity content, low in oxygen content and high in purity;
2. before hydrogenation, a rapid quenching process is added, the tantalum ingot is rapidly cooled to below 60 ℃, cold and hot changes can cause thermal expansion and cold contraction of the tantalum ingot, due to the action of internal stress and the rapid cooling, the temperature difference between the inside and the outside of the tantalum ingot is further increased, so that the thermal expansion and cold contraction of each part of the tantalum ingot are uneven, the tantalum ingot is easier to break, the granularity of powder obtained by breaking is more uniform, the particle size is smaller, and in the subsequent hydrogenation and dehydrogenation oxygen reduction processes, the hydrogenation rate is high and the deoxidation rate is high;
3. the vacuum sintering furnace is adopted for heating by microwaves, the heating speed is high, the penetrability is better, the temperature inside and outside the niobium ingot is more uniform in the heating process, the vacuum sintering furnace is adopted for sintering, a vacuum crusher is adopted for crushing, and inert gas is filled for protection, so that the oxygen content of tantalum powder is reduced, and high-purity tantalum powder is obtained;
4. the spheroidizing process is added, the specific surface area of the obtained tantalum powder is larger, and the particle uniformity of the powder is better.
Detailed Description
The following description will be given of embodiments of the present invention with reference to the following examples, which are not intended to limit the present invention to the following examples, and the present invention relates to the related essential parts in the technical field, and it should be considered that the known technology in the technical field is known and understood by those skilled in the art.
Example 1: preparing a tantalum ingot with the purity of more than or equal to 99.95%, placing the tantalum ingot in a vacuum sintering furnace heated by microwave, introducing argon as protective gas, keeping the pressure in the furnace at 0.10MPa, starting the vacuum sintering furnace, setting the power of microwave heating to 5KW, raising the temperature in the vacuum sintering furnace to 600 ℃, and carrying out heat treatment for 60min at the temperature of 600 ℃; normal-temperature nitrogen is filled into an inner cavity of the vacuum sintering furnace by using a nitrogen filling device, the tantalum ingot is rapidly cooled to below 60 ℃ within 10min through nitrogen heat exchange, the temperature change can cause the thermal expansion and cold contraction of the tantalum ingot, and the temperature difference between the inside and the outside of the tantalum ingot is further increased due to the action of internal stress and the rapid cooling means, so that the thermal expansion and cold contraction of each part of the tantalum ingot are not uniform, and the tantalum ingot is more easily crushed; filling hydrogen into the vacuum sintering furnace, increasing the pressure in the furnace to 2MPa, preserving the heat at 900 ℃ for 2h, and cooling to obtain tantalum hydride ingots; crushing the tantalum hydride ingot by a vacuum crusher to obtain tantalum hydride powder; sieving by using a 800-mesh standard sieve to obtain tantalum hydride powder capable of passing through the 800-mesh standard sieve; mixing tantalum hydride powder and 5% of magnesium powder, adding the mixture into a dehydrogenation and oxygen reduction furnace, heating the mixture to 900 ℃, preserving heat for 5 hours, releasing the pressure in the furnace, preserving heat for 3 hours at 900 ℃, finally cooling the mixture to 25-30 ℃, and discharging the mixture after passivation to obtain the dehydrogenation and oxygen reduction tantalum powder; carrying out acid washing on the tantalum powder subjected to dehydrogenation and oxygen reduction by using a 20% hydrochloric acid solution so as to remove impurities such as magnesium ions, iron ions, aluminum ions and the like, filtering and washing by using pure water, and drying in a vacuum drying oven at 80 ℃ to obtain high-purity tantalum powder; and (3) placing the high-purity tantalum powder in a ball mill to obtain the high-purity tantalum powder with a particle shape close to a sphere, wherein the main impurity content and the particle size distribution of the high-purity tantalum powder are shown in table 1.
Comparative example 1: preparing a tantalum ingot with the purity of more than or equal to 99.95 percent, placing the tantalum ingot in a vacuum sintering furnace heated by microwave, introducing argon as protective gas, keeping the pressure in the furnace at 0.10MPa, starting the vacuum sintering furnace, setting the microwave heating power to be 5KW, raising the temperature in the vacuum sintering furnace to 600 ℃, and carrying out heat treatment for 60min at the temperature of 600 ℃; cooling the tantalum ingot to below 60 ℃ by a natural cooling means; filling hydrogen into the vacuum sintering furnace, increasing the pressure in the furnace to 2MPa, preserving the heat at 900 ℃ for 2h, and cooling to obtain tantalum hydride ingots; crushing the tantalum hydride ingot by a vacuum crusher to obtain tantalum hydride powder; sieving by using a 500-mesh standard sieve to obtain tantalum hydride powder capable of passing through the 500-mesh standard sieve; mixing tantalum hydride powder and 5% magnesium powder, adding the mixture into a dehydrogenation and oxygen reduction furnace, heating the mixture to 900 ℃, preserving heat for 5 hours, releasing the pressure in the furnace, preserving heat for 3 hours at 900 ℃, finally cooling the mixture to 25-30 ℃, and discharging the mixture after passivation to obtain the dehydrogenation and oxygen reduction tantalum powder; carrying out acid washing on the tantalum powder subjected to dehydrogenation and oxygen reduction by using a 20% hydrochloric acid solution so as to remove impurities such as magnesium ions, iron ions, aluminum ions and the like, filtering and washing by using pure water, and drying in a vacuum drying box at the temperature of 80 ℃ so as to obtain high-purity tantalum powder; and (3) putting the high-purity tantalum powder into a ball mill to obtain the high-purity tantalum powder with the particle shape close to a sphere, wherein the main impurity content and the particle size distribution of the high-purity tantalum powder are shown in the table 1.
Comparative example 2: preparing a tantalum ingot with the purity of more than or equal to 99.95 percent, putting the tantalum ingot into a common sintering furnace, raising the temperature in the sintering furnace to 600 ℃, and carrying out heat treatment for 60min at the temperature of 600 ℃; filling air into the inner cavity of the sintering furnace by using a ventilation device, and rapidly cooling the tantalum ingot to below 60 ℃ within 10min through air heat exchange; filling hydrogen into the sintering furnace, increasing the pressure in the sintering furnace to 2MPa, preserving heat for 2 hours at 900 ℃, and cooling to obtain tantalum hydride ingots; crushing the tantalum hydride ingot by a common crusher to obtain tantalum hydride powder; sieving by using a 800-mesh standard sieve to obtain tantalum hydride powder capable of passing through the 800-mesh standard sieve; mixing tantalum hydride powder and 5% magnesium powder, adding the mixture into a dehydrogenation and oxygen reduction furnace, heating the mixture to 900 ℃, preserving heat for 5 hours, releasing the pressure in the furnace, preserving heat for 3 hours at 900 ℃, finally cooling the mixture to 25-30 ℃, and discharging the mixture after passivation to obtain the dehydrogenation and oxygen reduction tantalum powder; carrying out acid washing on the tantalum powder subjected to dehydrogenation and oxygen reduction by using a 20% hydrochloric acid solution so as to remove impurities such as magnesium ions, iron ions, aluminum ions and the like, filtering and washing by using pure water, and drying in a vacuum drying box at the temperature of 80 ℃ so as to obtain high-purity tantalum powder; and (3) putting the high-purity tantalum powder into a ball mill to obtain the high-purity tantalum powder with the particle shape close to a sphere, wherein the main impurity content and the particle size distribution of the high-purity tantalum powder are shown in the table 1.
TABLE 1 comparison of Properties
| Item | O content (ppm) | Fe content (ppm) | Mg content (ppm) | Al content (ppm) | Particle size D50 (μm) |
| Niobium ingot | 320 | ﹤5 | ﹤5 | ﹤5 | -- |
| Example 1 | 49 | 2.53 | 2.77 | 2.98 | 15.2 |
| Comparative example 1 | 106 | 3.03 | 2.63 | 2.95 | 35.7 |
| Comparative example 2 | 297 | 2.61 | 2.87 | 2.74 | 16.7 |
In example 1, high-temperature sintering, rapid quenching, pressure hydrogenation, vacuum crushing, screening, dehydrogenation and oxygen reduction, acid washing for impurity removal, and spheroidizing were sequentially performed. The comparative example 1 sequentially carries out the working procedures of high-temperature sintering, natural cooling, pressure hydrogenation, vacuum crushing, screening, dehydrogenation and oxygen reduction, acid cleaning and impurity removal and spheroidization. Compared with the comparative example 1, the working procedure of rapid quenching is adopted in the embodiment 1, the tantalum ingot block is rapidly cooled to below 60 ℃, the thermal expansion and cold contraction of the tantalum ingot block can be caused by the change of cold and heat, the internal stress effect is realized, and the rapid cooling is matched, so that the temperature difference between the inside and the outside of the tantalum ingot block is further increased, the thermal expansion and cold contraction effect of all parts of the tantalum ingot block is uneven, the tantalum block is easier to break, and the data in the table 1 show that the granularity of the powder obtained by breaking in the embodiment 1 is more uniform and smaller.
In example 1, a vacuum sintering furnace and a vacuum crusher were used for processing, and in comparative example 2, a common sintering furnace and a common crusher were used for processing. As can be seen from the data in table 1, in example 1, the oxygen content of the tantalum powder can be significantly reduced by performing oxidation protection with an inert gas, thereby obtaining a high-purity tantalum powder.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The production process of the high-purity tantalum powder is characterized by comprising the following steps of:
s1, high-temperature sintering: placing the tantalum ingot block in a vacuum sintering furnace, filling inert protective gas, keeping the pressure in the furnace at 0.08-0.10MPa, and carrying out heat treatment at the temperature of 600-750 ℃ for 30-60min;
s2, rapid quenching: rapidly cooling the tantalum ingot to below 60 ℃;
s3, pressure hydrogenation: filling hydrogen into the vacuum sintering furnace, increasing the pressure in the vacuum sintering furnace to 1-2MPa, and hydrogenating by using the hydrogen to obtain a tantalum hydride ingot;
s4, vacuum crushing: crushing tantalum hydride ingots in a vacuum environment to obtain tantalum hydride powder;
s5, screening: sieving the tantalum powder by using a standard sieve of 400 to 800 meshes to obtain tantalum hydride powder which can pass through the standard sieve of 400 to 800 meshes;
s6, dehydrogenation and oxygen reduction: carrying out dehydrogenation and oxygen reduction on the tantalum hydride powder to obtain tantalum powder subjected to dehydrogenation and oxygen reduction;
s7, acid washing and impurity removal: carrying out acid washing treatment on the tantalum powder subjected to dehydrogenation and deoxidation to obtain high-purity tantalum powder;
s8, spheroidizing: and placing the high-purity tantalum powder in a ball mill to obtain the high-purity tantalum powder with a particle shape close to a sphere.
2. The process of claim 1, wherein in step S1, the inert shielding gas is selected from helium, neon, and argon.
3. The production process of high-purity tantalum powder according to claim 1, wherein in the step S1, the adopted vacuum sintering furnace is a microwave heating vacuum sintering furnace, and the microwave heating power is 5KW to 6KW.
4. The production process of high-purity tantalum powder according to claim 1, wherein in the step S2, normal-temperature or low-temperature nitrogen is filled into the inner cavity of the vacuum sintering furnace by using a nitrogen filling device, and the tantalum ingot is rapidly cooled to below 60 ℃ within 10min through nitrogen heat exchange.
5. The production process of the high-purity tantalum powder as claimed in claim 1, wherein in the step S3, hydrogen is introduced into a vacuum sintering furnace, the pressure in the furnace is increased to 0.5-2MPa, the temperature is kept at 700-900 ℃ for 1-2h, and a niobium hydride ingot is obtained after cooling.
6. The production process of high-purity tantalum powder according to claim 1, wherein in the step S4, a vacuum crusher is used for crushing tantalum hydride ingots to obtain tantalum hydride powder.
7. The production process of high-purity tantalum powder according to claim 1, wherein in step S6, tantalum hydride powder is mixed with 3-6% of metal reducing agent and then added into a dehydrogenation oxygen reduction furnace, the mixture is heated to 900-950 ℃ and is kept warm for 4-10h, then the pressure in the furnace is released, the mixture is kept warm for 3-4h at 900-950 ℃, finally the temperature is reduced to 25-30 ℃, and the mixture is taken out of the furnace after passivation to obtain the dehydrogenation oxygen reduction tantalum powder.
8. The production process of high-purity tantalum powder according to claim 1, wherein in step S7, the tantalum powder after dehydrogenation and oxygen reduction is subjected to acid washing by using a 20% hydrochloric acid solution so as to remove impurities such as magnesium ions, iron ions, aluminum ions and the like, and the tantalum powder is filtered and washed by pure water and dried in a vacuum drying oven at 80 ℃ so as to obtain the high-purity tantalum powder.
9. The production process of high-purity tantalum powder according to claim 1, wherein the oxygen content of the high-purity tantalum powder obtained in step S7 is less than or equal to 50ppm, the iron content is less than or equal to 3ppm, the magnesium content is less than or equal to 3ppm, and the aluminum content is less than or equal to 3ppm.
10. The production process of the high-purity tantalum powder as claimed in claim 1, wherein the D50 of the high-purity tantalum powder obtained in the step S8 is 10-40 μm.
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| CN115889794A (en) * | 2022-11-14 | 2023-04-04 | 北京兴荣源科技有限公司 | Preparation method of low-cost spherical cobalt-chromium-molybdenum 3D printing powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115889794A (en) * | 2022-11-14 | 2023-04-04 | 北京兴荣源科技有限公司 | Preparation method of low-cost spherical cobalt-chromium-molybdenum 3D printing powder |
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Application publication date: 20221018 |