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WO2025036039A1 - Poudre de tantale à haute tension et son procédé de préparation, et anode de condensateur - Google Patents

Poudre de tantale à haute tension et son procédé de préparation, et anode de condensateur Download PDF

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Publication number
WO2025036039A1
WO2025036039A1 PCT/CN2024/104984 CN2024104984W WO2025036039A1 WO 2025036039 A1 WO2025036039 A1 WO 2025036039A1 CN 2024104984 W CN2024104984 W CN 2024104984W WO 2025036039 A1 WO2025036039 A1 WO 2025036039A1
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Prior art keywords
tantalum powder
tantalum
voltage
powder
treatment
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Chinese (zh)
Inventor
李仲香
陈学清
李慧
张洪刚
师德军
李霞
刘继
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Ningxia Orient Tantalum Industry Co Ltd
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Ningxia Orient Tantalum Industry Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/142—Thermal or thermo-mechanical treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/145—Chemical treatment, e.g. passivation or decarburisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/04—Electrodes or formation of dielectric layers thereon
    • H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material

Definitions

  • the present application relates to the technical field of rare metals, and in particular to a high-voltage tantalum powder, a preparation method thereof, and a capacitor anode.
  • High-voltage tantalum powder (including high-reliability tantalum powder, with an operating voltage of more than 35V) is the key raw material for solid tantalum capacitors and liquid tantalum capacitors with an operating voltage of 63V or higher.
  • the production of this kind of high-voltage tantalum powder at home and abroad adopts the method of refining and purification, that is, the process of electron bombardment-hydrogenation powder making is used to improve the purity of tantalum powder to improve the quality of tantalum powder.
  • the process of electron bombardment-hydrogenation powder making is used to improve the purity of tantalum powder to improve the quality of tantalum powder.
  • the specific capacitance and breakdown voltage of electron bombardment high-voltage powder People have tried to study the influence of particle size and particle shape on the quality of high-voltage tantalum powder from the physical properties of tantalum powder.
  • US Patent No. 5,580,367 discloses an improved flaky tantalum powder and a method for producing flaky tantalum powder.
  • the method for producing flaky tantalum powder is to use tantalum ingot hydrogenated powder or sodium reduced powder as raw materials to obtain large flakes by the above-mentioned traditional method, and then the large flakes are subjected to hydrogenation treatment and mechanical crushing to reduce the size of the flakes.
  • the flaky tantalum powder has a specific diameter-to-thickness ratio. This characteristic makes the powder after agglomeration have good process properties: such as fluidity, compact strength and formability, and capacitors with low leakage current and high breakdown voltage can be produced.
  • the process of this method is complicated and the process route is long. At the same time, due to repeated mechanical crushing, it is inevitable that metal impurities will increase. A large amount of acid washing will cause the loss of tantalum powder, which greatly increases the production cost.
  • US Patent No. 4,017,302 discloses a method for preparing high-pressure tantalum metal powder.
  • the specific process is tantalum ingot hydrogenation, grinding, grading and screening, dehydrogenation preheating, crushing through 80 mesh sieve, agglomeration, crushing, 35 mesh, 250 mesh, then -250 mesh and -35/+25 mesh powder mixing and agglomeration, testing, and product.
  • the tantalum powder prepared by this method is more suitable for high-voltage and low-capacity tantalum powder (63V).
  • US Patent No. 4141719 discloses a method for preparing high-voltage tantalum metal powder. Tantalum ingots are hydrogenated, ground, graded, degassed (1200°C), screened, 35 mesh, and mixed. Tantalum powder has a large bulk density, low oxygen content, high green block strength, and low leakage current of the sintered anode.
  • the tantalum powder prepared by this method is more suitable for high-voltage and low-capacity tantalum powder (63V).
  • US Patent No. 4555268 relates to a flaky tantalum powder with improved processing performance.
  • the powder contains 20-40% flaky tantalum powder and 70% granular tantalum powder, which is heat treated at 1250°C to 1550°C for 5 to 120 minutes before mixing.
  • the mixed tantalum powder is secondary agglomerated, which improves the processing performance.
  • the tantalum powder prepared by this method is more suitable for medium working voltage (20V to 35V).
  • U.S. Patent No. 4,740,238 relates to a tantalum powder containing flaky powder.
  • the specific process of the tantalum powder includes: tantalum powder degassing, flaking (ball milling, wet milling), pickling, screening, phosphorus doping, primary heat treatment, grinding and screening, phosphorus doping, secondary heat treatment, grinding and screening, and Mg reduction.
  • the tantalum powder prepared by this method is more suitable for medium working voltage (20V to 35V).
  • Citride application CN1004614A relates to a method and product of spherical tantalum powder. Tantalum powder is sent into a plasma reaction zone with a carrier gas, sprayed into a vacuum tank for cooling, and made into spherical tantalum powder, pickled, and heat treated at 1000-1250°C.
  • the tantalum powder withstands a pressure of 300-450V.
  • the specific capacitance of the tantalum powder prepared by this method is only 500-800 ⁇ FV/g, and the formability is extremely poor.
  • the present application provides a high-voltage tantalum powder, a preparation method thereof, and a capacitor anode, so as to further improve the specific capacitance and breakdown voltage of a capacitor made of tantalum powder.
  • the first aspect of the present application provides a method for preparing high-pressure tantalum powder, which comprises: selecting a tantalum metal billet, wherein the impurity C content in the tantalum metal billet is ⁇ 30ppm, the total content of metal impurities Fe, Ni and Cr is ⁇ 30ppm, and the grain size is 1 ⁇ m-900 ⁇ m; performing hydrogenation treatment on the tantalum metal billet to obtain a hydrogenated material; performing pulverization treatment on the hydrogenated material to obtain hydrogen-containing tantalum powder; performing acid washing and impurity removal on the hydrogen-containing tantalum powder to obtain hydrogenated impurity-removed tantalum powder; performing subsequent treatment on the hydrogenated impurity-removed tantalum powder to obtain high-pressure tantalum powder, wherein the subsequent treatment comprises a combination of one or more of dehydrogenation treatment, high-temperature and high-vacuum heat treatment, and reduction and oxygen reduction treatment.
  • the grain size of the tantalum metal billet is 1 ⁇ m-450 ⁇ m, preferably 1 ⁇ m-350 ⁇ m, and more preferably 10 ⁇ m-150 ⁇ m.
  • the mass content of hydrogen in the hydrogenation material is greater than or equal to 0.3%, preferably greater than or equal to 0.5%.
  • the hydrogen-containing tantalum powder has a 1 ⁇ m ⁇ D V 50 ⁇ 15 ⁇ m, preferably Select hydrogen-containing tantalum powder with 1 ⁇ m ⁇ D V 50 ⁇ 10 ⁇ m.
  • the pulverization treatment includes one or more of ball milling, impact treatment and extrusion treatment; the ball milling treatment satisfies any one or more of the following conditions: 1) zirconia balls are used as ball milling media, preferably the diameter of the zirconia balls is 1mm-5mm, and more preferably 2mm-4mm; 2) wet agitated ball milling is used, and preferably water or an organic solvent is used as a dispersion medium in the wet agitated ball milling; 3) a surfactant is used as a grinding aid; preferably the grinding aid is butanone and/or isopropanol; preferably, the amount of the grinding aid added is 0.5%-5% of the weight of the hydrogenated material, preferably 1%-4%, and more preferably 1.8%-3.6%.
  • the acid used for pickling and impurity removal includes a mixed acid formed by one or more of sulfuric acid, hydrochloric acid, and nitric acid, hydrogen peroxide, and hydrofluoric acid.
  • a second aspect of the present application provides a high-pressure tantalum powder, in which the total content of metal impurities Fe, Ni and Cr is ⁇ 30 ppm, and the C content is ⁇ 30 ppm; and the high-pressure tantalum powder satisfies at least one of the following conditions: 1) the bulk density is 1.8 g/cm 3 -4.0 g/cm 3 , preferably 1.95 g/cm 3 -3.55 g/cm 3 , and further preferably 2.2 g/cm 3 -3.5 g/cm 3 ; 2) the BET specific surface area is 0.1 m 2 /g-1.0 m 2 /g, preferably 0.2 m 2 /g-0.7 m 2 /g, and further preferably 0.2 m 2 /g-0.6 m 2 /g; 3) the fluidity is ⁇ 50 s/50 g, preferably the fluidity is ⁇ 40 s/50 g, more preferably the fluidity is ⁇ 35 s/
  • the electrolytic capacitor anode made of high-voltage tantalum powder has a specific capacitance of 6500 ⁇ F ⁇ V/g-23000 ⁇ F ⁇ V/g and a breakdown voltage of 200V-300V when the enabling voltage is 150V-300V, and preferably a breakdown voltage of 200V-285V.
  • a third aspect of the present application provides a high-pressure tantalum powder, which is prepared by any one of the preparation methods of the first aspect.
  • a fourth aspect of the present application provides a capacitor anode made of tantalum powder, wherein the tantalum powder is the high-voltage tantalum powder provided in any embodiment of the second aspect or the third aspect.
  • FIG1 is a schematic diagram showing a process flow of a method for preparing high-voltage tantalum powder provided in one embodiment of the present application.
  • FIG. 2 shows a metallographic structure photograph of the tantalum metal billet of Example 1 of the present application.
  • FIG3 shows a metallographic structure photograph of the tantalum metal billet of Example 2 of the present application.
  • FIG. 4 shows a metallographic structure photograph of the tantalum metal billet of Example 3 of the present application.
  • FIG5 shows a metallographic structure photograph of the tantalum metal billet of Example 4 of the present application.
  • FIG. 6 shows a metallographic structure photograph of the tantalum metal billet of Example 5 of the present application.
  • FIG. 7 shows a metallographic structure photograph of the tantalum metal billet of Example 6 of the present application.
  • FIG8 shows a metallographic structure photograph of the tantalum metal billet of Example 7 of the present application.
  • FIG. 9 shows a metallographic structure photograph of the tantalum metal billet of Comparative Example 1 of the present application.
  • tantalum powder for high voltage use, but among the numerous preparation methods, most use electron-bombarded tantalum ingots as raw materials to improve the purity of tantalum powder; in order to further improve the specific volume and breakdown voltage of electron-bombarded high-voltage powder, the particle size and shape of tantalum powder are controlled by hydrogenation of tantalum ingots. Facts show that this method of controlling the particle size and shape of electron-bombarded powder and performing agglomeration treatment is effective in improving specific volume and breakdown voltage, but the effect is limited.
  • the first embodiment of the present application provides a method for preparing high-voltage tantalum powder, as shown in Figure 1, the preparation method comprises: selecting a tantalum metal blank, the impurity C content in the tantalum metal blank is ⁇ 30ppm (preferably ⁇ 20ppm), the total content of metal impurities Fe, Ni and Cr is ⁇ 30ppm (preferably ⁇ 20ppm), and the grain size is 1 ⁇ m-900 ⁇ m; hydrogenating the tantalum metal blank to obtain a hydrogenated material; pulverizing the hydrogenated material to obtain hydrogen-containing tantalum powder; pickling and removing impurities from the hydrogen-containing tantalum powder to obtain hydrogenated impurity-removed tantalum powder; performing subsequent treatment on the hydrogenated impurity-removed tantalum powder to obtain high-voltage tantalum powder, and the subsequent treatment comprises one or more combinations of dehydrogenation treatment, high-temperature and high-vacu
  • the grain size of the tantalum metal blank is too large, and the BET specific surface area of the hydrogen-containing tantalum powder obtained after pulverization is too small, so the specific volume of the tantalum powder finally obtained is low; the purity of the tantalum metal blank, such as carbon, iron, nickel, chromium and other metal impurities, is high, the leakage current of the product increases, and the reliability is reduced.
  • This application uses tantalum metal blanks with an impurity C content of ⁇ 30ppm, a total content of metal impurities Fe, Ni and Cr of ⁇ 30ppm, and a grain size of 1 ⁇ m-900 ⁇ m as raw materials for hydrogenation, pulverization and post-treatment, which effectively improves the breakdown voltage and CV value (specific volume) of the capacitor made of tantalum powder, and reduces its leakage current.
  • the above-mentioned hydrogenation, impurity removal and post-treatment improve the fluidity and electrical properties of the tantalum metal blank, so the high-voltage tantalum powder prepared thereby is easier to make into a capacitor, and the breakdown voltage and CV value of the capacitor are fully improved, and the leakage current is effectively controlled.
  • the preparation method of the present application can be carried out by referring to conventional processes for hydrogenation, impurity removal and post-treatment. Therefore, the process is simple and controllable, the production process has low safety risks and wide applicability.
  • the high-voltage tantalum powder that passes 50 mesh is selected as the raw material for subsequent electrode production.
  • the grain size of tantalum metal billet is determined by the comparison method in GB/T6394 "Method for determination of average grain size of metals".
  • the tantalum metal blank used in the present application may be a tantalum ingot, a tantalum rod, a tantalum wire and/or other tantalum materials.
  • the tantalum metal blank may be prepared by a known method or may be derived from a known product. There are many methods for preparing the tantalum metal blank.
  • any chemical substance that is conducive to grain refinement may be added as a refiner in the required proportion during the treatment of the tantalum metal blank, such as one or more of phosphorus, nitrogen, boron, silicon, yttrium, etc.; the grain size may also be controlled by adjusting the tantalum material treatment process, such as: sintering temperature and/or holding time; the purpose of grain refinement may also be achieved by reprocessing the tantalum material, such as: heat treatment and processing technology. Alternatively, the purpose of grain refinement may be achieved by combining the above treatment methods.
  • the grain size of the tantalum metal blank is 1 ⁇ m-450 ⁇ m, preferably 1 ⁇ m-350 ⁇ m, and more preferably 10 ⁇ m-150 ⁇ m.
  • Hydrogenation treatment can be implemented with reference to conventional processes. Hydrogenation treatment uses the characteristic that the maximum hydrogen absorption of metal tantalum and tantalum alloys at different temperatures is different, and the hydrogen content of metal tantalum is controlled by adjusting the hydrogenation process. Since the maximum hydrogen absorption of metal tantalum and tantalum alloys increases with decreasing temperature, the higher the temperature at which hydrogen is stopped, the lower the hydrogen content, and the lower the temperature at which hydrogen is stopped, the higher the hydrogen content; generally, after the temperature drops to the temperature at which hydrogen is stopped, hydrogen is continued to be passed for a period of time, and the holding time varies according to the size of the metal tantalum and tantalum alloy loaded into the hydrogenation container (the larger the block, the longer the time required), and then hydrogen is stopped to allow the metal tantalum and tantalum alloy to absorb hydrogen fully and evenly.
  • the mass content of hydrogen in the hydride material is greater than or equal to 0.3%, preferably greater than or equal to 0.5%. This is to avoid the hydrogen content being too low, the hydrogen embrittlement of the hydride material being not good enough, and it being difficult to perform fine crushing during the pulverization process.
  • the above hydrogen content can enable the metal tantalum hydride block material to maintain good hydrogen embrittlement, so that the tantalum hydride block can be fully crushed to the desired particle size, thereby improving production efficiency and yield. It should be noted here that there will be hydrogen saturation in the hydride material, and the actual hydrogen content will not exceed this saturation.
  • the temperature for stopping hydrogen flow during hydrogenation treatment is any temperature ⁇ 200°C, and may be any temperature between 150°C and 200°C; may be any temperature between 100°C and 200°C, may be any temperature between 50°C and 100°C, and preferably any temperature between 50°C and 150°C. This effectively controls the mass content of hydrogen in the hydrogenation material and avoids its content being too low.
  • the above-mentioned pulverization treatment refers to the mechanical crushing of the hydrogenated material (such as tantalum block) with good hydrogen embrittlement resistance obtained by hydrogenation treatment. There is no restriction on the pulverization method, and it can be crushed by air flow.
  • the hydrogen-containing tantalum powder has a particle size of 1 ⁇ m ⁇ D V 50 ⁇ 15 ⁇ m, preferably 1 ⁇ m ⁇ D V 50 ⁇ 10 ⁇ m.
  • the pulverization treatment includes one or more of ball milling, impact treatment and extrusion treatment; the ball milling treatment satisfies any one or more of the following conditions: 1) using zirconium oxide balls as ball milling media, preferably the diameter of the zirconium oxide balls is 1mm-5mm, and more preferably 2mm-4mm; 2) wet stirring ball milling is used, preferably water or an organic solvent is used as a dispersion medium in the wet stirring ball milling; 3) a surfactant is used as a grinding aid; preferably the grinding aid is butanone and/or isopropanol; preferably, the amount of the grinding aid added is 0.5%-5% of the weight of the hydrogenated material, preferably 1%-4%, and more preferably 1.8%-3.6%.
  • the above-mentioned pulverization treatment is first mechanically crushed to a size that can pass through a 100-mesh sieve, and then wet-mixed ball milling is used, for example, zirconium oxide balls are used as ball milling media, and water or an organic solvent is used as a dispersion medium, and continuous ball milling is performed until D V 50 ⁇ 15 ⁇ m, preferably D V 50 ⁇ 10 ⁇ m.
  • tantalum hydride powder has a high hardness, grinding with ordinary stainless steel balls will cause severe wear of the stainless steel balls, causing a large amount of metal impurities to mix into the material, resulting in a high impurity content.
  • zirconium oxide balls with a higher hardness rather than stainless steel balls for grinding.
  • grinding balls with a diameter of 1mm-5mm preferably 2mm-4mm.
  • the reason is that the filling amount of grinding media with a small diameter in the grinding chamber is large, which increases the impact and friction of the grinding media and increases the contact area of the grinding media. The increase in grinding area also helps to finely grind. It was unexpectedly found that generally, grinding balls with a diameter of 1mm-5mm, preferably 2mm-4mm, can achieve better grinding effects.
  • Ultrafine powders with a particle size of less than 0.1 ⁇ m may be difficult to avoid during ball milling. They are often easily oxidized or even self-ignited. At the same time, the finer the powder particle size, the larger its surface area and the greater the surface free energy, which leads to the re-agglomeration of fine particles, which is not conducive to micronization.
  • a surfactant is preferably added to the dispersion medium as a grinding aid.
  • the surfactant can adhere to the surface of the tantalum powder particles to form a protective layer, the surface of the material particles is passivated while the micronized ball ultrafine grinding is carried out, which can effectively inhibit the oxidation of ultrafine powders during ball milling and subsequent treatment, thereby improving product quality.
  • the preferred grinding aid is butanone and/or isopropanol. More preferably, the amount of grinding aid added is 0.5%-5% of the weight of the hydrogenated material, preferably 1%-4%, and more preferably 1.8%-3.6%.
  • the hydrogen-containing tantalum powder is pickled and impurities are removed.
  • the pickling and impurities removal can reduce impurities such as oxygen, carbon, iron, nickel, chromium, etc. in the tantalum powder.
  • the implementation of the pickling and impurities removal can refer to the conventional pickling and impurity removal process of tantalum powder.
  • the acid used for pickling and impurities removal includes a mixed acid formed by one or more of sulfuric acid, hydrochloric acid, nitric acid, hydrogen peroxide and hydrofluoric acid.
  • the hydrogenated de-impurity tantalum powder has a high content of impurities such as oxygen, H, and F.
  • the increase in the content of these impurities will affect the electrical properties of the capacitor, especially the increase in leakage current, because the impurities in the tantalum powder become the center of crystallization nucleation of the anodic oxide film during the anodic oxidation process, which is the cause of defects in the oxide film, and will eventually cause the leakage current to increase and the flash voltage to decrease.
  • the problems caused by poor powder fluidity, the presence of fine powder particles, and high content of impurities such as oxygen, hydrogen and fluorine can be effectively overcome by treating with any one or more of the above-mentioned process combinations of pelletizing, high temperature and high vacuum heat treatment, and magnesium reduction and oxygen reduction treatment.
  • Dehydrogenation treatment, high temperature and high vacuum heat treatment, and reduction and oxygen reduction treatment are all common processes in tantalum powder processing. Therefore, the above-mentioned treatment processes of this application can refer to conventional processes. In some embodiments, the above-mentioned treatments can be performed in sequence. In some embodiments, the dehydrogenation treatment is to place the hydrogen-containing tantalum powder in a closed furnace filled with argon and heated to 700-900°C for 60-200 minutes, and then cool it out of the furnace and sieve it.
  • any chemical substance that is beneficial to inhibiting the shrinkage of tantalum powder and reducing the loss of specific surface area during high-temperature sintering can be added as a sintering inhibitor in the required proportion during high-temperature and high-vacuum heat treatment, such as one or more of phosphorus, nitrogen, and boron.
  • the temperature of high-temperature and high-vacuum heat treatment is generally controlled at 1000°C-1600°C, and the heat preservation time is 15min-200min. After high-temperature and high-vacuum heat treatment, the tantalum powder is pelletized and granulated.
  • the magnesium reduction and oxygen reduction treatment can be a conventional oxygen reduction.
  • a reducing agent whose affinity with oxygen is greater than the affinity of tantalum with oxygen, such as alkaline earth metals, rare earth metals and their hydrides, is mixed into the material to be treated.
  • the most commonly used method is to mix into the material to be treated 0.2%-6.0% of the weight of the material to be treated with metallic magnesium powder, and then heat it under vacuum or under the protection of an inert gas (preferably an inert gas), keep it warm at 800°C-900°C for 1 hour-3 hours, then evacuate the vacuum, and keep it warm for another 2 hours-6 hours under vacuum conditions; then cool it, passivate it, and remove magnesium to obtain high-pressure tantalum powder.
  • an inert gas preferably an inert gas
  • a high-pressure tantalum powder in which the total content of metal impurities Fe, Ni and Cr is ⁇ 30 ppm (preferably ⁇ 20 ppm), and the C content is ⁇ 30 ppm (preferably ⁇ 20 ppm); and the high-pressure tantalum powder satisfies at least one of the following conditions: 1) bulk density is 1.8 g/cm 3 -4.0 g/cm 3 , preferably 1.95 g/cm 3 -3.55 g/cm 3 , and more preferably 2.2 g/cm 3 -3.5 g/cm 3 ; 2) BET specific surface area is 0.1 m 2 /g-1.0 m 2 /g, preferably 0.2 m 2 /g-0.7 m 2 /g, and more preferably 0.2 m 2 /g-0.6 m 2 /g; 3) fluidity is ⁇ 50 s/50 g, preferably fluidity is ⁇ 40 s/50
  • the electrolytic capacitor anode made of the above high-voltage tantalum powder has a specific capacitance of 6500 ⁇ F ⁇ V/g-23000 ⁇ F ⁇ V/g, preferably a specific capacitance of 7000 ⁇ F ⁇ V/g-20000 ⁇ F ⁇ V/g, and a breakdown voltage of 200V-300V, preferably a breakdown voltage of 200V-285V, when the energizing voltage is 150V-270V.
  • a high-voltage tantalum powder is provided, which is prepared by the preparation method of any one of the above embodiments of the present application.
  • the high-voltage tantalum powder prepared in the present application has a high CV value and breakdown voltage, and has a low leakage current, meeting the use requirements of high-reliability and high-specific capacitance electrolytic capacitors.
  • a capacitor anode is provided.
  • the capacitor anode is made of tantalum powder.
  • the tantalum powder is any high-voltage tantalum powder provided in the second embodiment or the third embodiment of the present application.
  • the bulk density is determined according to the funnel method of GB/T1479.1, Part 1: Funnel method; the fluidity (Flow) is determined according to the Hall flowmeter of GB/T1482; the specific surface area of metal powder is determined according to GB/T13390: Nitrogen adsorption method; the grain size is determined according to the comparison method in the determination method of average grain size of metals of GB/T6394.
  • the chemical impurity content is shown in Table 2, and the metallographic structure photograph is shown in Figure 2.
  • Step 2 the tantalum metal billet is loaded into the hydrogenation container of the hydrogenation furnace and heated to 800°C for insulation, high-purity hydrogen is introduced and the hydrogen pressure is maintained at 1.3-1.5MPa, and the heat is maintained for 15 hours, and then the temperature is reduced and the hydrogen pressure is maintained at 1.3-1.5MPa, so that the tantalum ingot can fully absorb hydrogen and react with hydrogen.
  • the hydrogen is stopped, and when the temperature is lower than 40°C, it is taken out of the furnace to obtain a hydrogenated material with good hydrogen embrittlement.
  • Step 3 the hydrogenated material is coarsely crushed into tantalum powder that can completely pass through an 80-mesh sieve using a jaw crusher.
  • the above tantalum powder is ball-milled with anhydrous ethanol as a ball-milling medium, butanone and isopropanol as grinding aids (the amount of butanone added is 1.0% of the weight of the hydrogenated material, and the amount of isopropanol added is 3.0% of the weight of the hydrogenated material), and a 3mm diameter zirconium oxide ball is used as a ball-milling medium.
  • Wet stirring ball milling is performed for 1.5 hours to obtain hydrogen-containing tantalum powder with Dv50 ⁇ 15 ⁇ m. After screening, hydrogen-containing tantalum powder with 1 ⁇ m ⁇ DV50 ⁇ 15 ⁇ m and a hydrogen content of 0.497% is obtained.
  • Step 4 the sieved hydrogenated tantalum powder is washed with a mixed acid of HNO 3 and HF (the volume ratio of HNO 3 , HF and water is 4:1:20) to remove metal impurities, dried and sieved to obtain hydrogenated impurity-removed tantalum powder.
  • a mixed acid of HNO 3 and HF the volume ratio of HNO 3 , HF and water is 4:1:20
  • Step 5 the above hydrogenated impurity-removed tantalum powder is placed in a closed furnace filled with argon and heated to 900°C for 180 minutes for dehydrogenation treatment, then cooled and sieved after being taken out of the furnace.
  • the above dehydrogenated tantalum powder is subjected to high-temperature high-vacuum heat treatment and deoxidation treatment, which is specifically implemented by heating to 1300°C and keeping it for 60 minutes under a vacuum of 10-3 Pa, and then crushing it to less than 50 mesh.
  • 2% magnesium chips are added to the above tantalum powder, heated to 900°C in an argon atmosphere in a closed furnace and kept warm for 2 hours, and then vacuumed, and kept warm for another 3 hours under vacuum conditions, then cooled, passivated, taken out of the furnace, and finally washed with 20% HNO3 to remove magnesium oxide and excess magnesium, dried and sieved to make it completely pass through a 50-mesh sieve to obtain high-pressure tantalum powder A.
  • the chemical impurity content is shown in Table 3.
  • High-voltage tantalum powder A was pressed into a shape with a pressed density of 6.5 g/cm 3 and a core powder weight of 1 g, and tested according to the standard. Sintered for 30 minutes in a vacuum furnace at 10 -3 Pa according to the sintering conditions in Table 4. A sintered block was obtained. The sintered block was energized in a 0.01% volume phosphoric acid solution at the energizing voltage in Table 4 to obtain a capacitor anode. The electrical performance indicators thereof were measured and listed in Table 4.
  • the powder is loaded into an elastic mold, sealed and placed into an isostatic press high-pressure cylinder, and pressed and formed at a pressure of 180Mpa.
  • the formed tantalum rod is sintered in a graphite furnace at a sintering temperature of 2200°C and a holding time of 240min to obtain a tantalum metal blank B.
  • the chemical impurity content is shown in Table 2, and the metallographic structure photograph is shown in Figure 3.
  • Step 2 the tantalum metal billet is loaded into the hydrogenation container of the hydrogenation furnace and heated to 800°C for insulation, high-purity hydrogen is introduced and the hydrogen pressure is maintained at 1.3-1.5MPa, and the heat is maintained for 15 hours, and then the temperature is reduced and the hydrogen pressure is maintained at 1.3-1.5MPa, so that the tantalum ingot can fully absorb hydrogen and react with hydrogen.
  • the hydrogen is stopped, and when the temperature is lower than 40°C, it is taken out of the furnace to obtain a hydrogenated material with good hydrogen embrittlement.
  • step 3 of Example 1 to obtain a particle size of 1 ⁇ m ⁇ DV50 ⁇ 15 ⁇ m and a hydrogen content of It is 0.517% hydrogen-containing tantalum powder.
  • Example 1 Repeat step 4) of Example 1 to obtain hydrogenated impurity-removed tantalum powder.
  • the chemical impurity content thereof is shown in Table 3.
  • High-pressure tantalum powder B was pressed into a shape with a pressed density of 6.5 g/cm 3 and a core powder weight of 1 g, and tested according to the standard. Sintered for 30 minutes in a vacuum furnace at 10 -3 Pa according to the sintering conditions in Table 4. A sintered block was obtained. The sintered block was energized in a 0.01% volume phosphoric acid solution at the energizing voltage in Table 4 to obtain a capacitor anode. The electrical performance indicators thereof were measured and listed in Table 4.
  • the powder is loaded into an elastic mold, sealed and placed into an isostatic press high-pressure cylinder, and pressed and formed at a pressure of 180Mpa.
  • the formed tantalum rod is sintered in a vertical melting furnace at a sintering temperature of 2400°C and a holding time of 240min to obtain a tantalum metal blank C, the chemical impurity content of which is shown in Table 2, and the metallographic structure photograph is shown in Figure 4.
  • Step 2 the tantalum metal billet is loaded into the hydrogenation container of the hydrogenation furnace and heated to 800°C for insulation, high-purity hydrogen is introduced and the hydrogen pressure is maintained at 1.3-1.5MPa, and the heat is maintained for 15 hours, and then the temperature is reduced and the hydrogen pressure is maintained at 1.3-1.5MPa, so that the tantalum ingot can fully absorb hydrogen and react with hydrogen.
  • the hydrogen is stopped, and when the temperature is lower than 40°C, it is taken out of the furnace to obtain a hydrogenated material with good hydrogen embrittlement.
  • step 4) of Example 1 to obtain hydrogenated impurity-removed tantalum powder.
  • Step 5) of Example 1 was repeated to obtain high-pressure tantalum powder C.
  • the chemical impurity content thereof is shown in Table 3.
  • the high-voltage tantalum powder C was pressed into a shape with a pressed density of 6.5 g/cm 3 and a core powder weight of 1 g, and tested according to the standard. Sintered for 30 minutes in a vacuum furnace at 10 -3 Pa according to the sintering conditions in Table 4. A sintered block was obtained. The sintered block was energized in a 0.01% volume phosphoric acid solution at the energizing voltage in Table 4 to obtain a capacitor anode. The electrical performance indicators thereof were measured and listed in Table 4.
  • Step 1) The tantalum metal blank is a commercially available high-purity tantalum rod with the grade Ta1.
  • the chemical impurity content and grain size are shown in Table 2, and the metallographic structure photo is shown in Figure 5.
  • Step 2 the tantalum metal billet is loaded into the hydrogenation container of the hydrogenation furnace and heated to 800°C for insulation, high-purity hydrogen is introduced and the hydrogen pressure is maintained at 1.3-1.5MPa, and the heat is maintained for 15 hours, and then the temperature is reduced and the hydrogen pressure is maintained at 1.3-1.5MPa, so that the tantalum ingot can fully absorb hydrogen and react with hydrogen.
  • the hydrogen is stopped, and when the temperature is lower than 40°C, it is taken out of the furnace to obtain a hydrogenated material with good hydrogen embrittlement.
  • step 4) of Example 1 to obtain hydrogenated impurity-removed tantalum powder.
  • Step 5) of Example 1 was repeated to obtain high-voltage tantalum powder D.
  • the chemical impurity content thereof is shown in Table 3.
  • the high-voltage tantalum powder D was pressed into a shape with a pressed density of 6.5 g/cm 3 and a core powder weight of 1 g, and tested according to the standard. Sintered for 30 minutes in a vacuum furnace at 10 -3 Pa according to the sintering conditions in Table 4. A sintered block was obtained. The sintered block was energized in a 0.01% volume phosphoric acid solution at the energizing voltage in Table 4 to obtain a capacitor anode. The electrical performance indicators thereof were measured and listed in Table 4.
  • the tantalum metal blank is a commercially available high-purity tantalum ingot with a grade of Ta1, the chemical impurity content and grain size of which are shown in Table 2, and the metallographic structure photograph is shown in Figure 6.
  • Step 2 the tantalum metal billet is loaded into the hydrogenation container of the hydrogenation furnace and heated to 800°C for insulation, high-purity hydrogen is introduced and the hydrogen pressure is maintained at 1.3-1.5MPa, and the heat is maintained for 15 hours, and then the temperature is reduced and the hydrogen pressure is maintained at 1.3-1.5MPa, so that the tantalum ingot can fully absorb hydrogen and react with hydrogen.
  • the hydrogen is stopped, and when the temperature is lower than 40°C, it is taken out of the furnace to obtain a hydrogenated material with good hydrogen embrittlement.
  • step 4) of Example 1 to obtain hydrogenated impurity-removed tantalum powder.
  • Step 5) of Example 1 was repeated to obtain high-pressure tantalum powder E.
  • the chemical impurity content thereof is shown in Table 3.
  • the high-voltage tantalum powder E was pressed into a shape with a pressed density of 6.5 g/cm 3 and a core powder weight of 1 g, and tested according to the standard. Sintered for 30 minutes in a vacuum furnace at 10 -3 Pa according to the sintering conditions in Table 4. A sintered block was obtained. The sintered block was energized in a 0.01% volume phosphoric acid solution at the energizing voltage in Table 4 to obtain a capacitor anode. The electrical performance indicators thereof were measured and listed in Table 4.
  • the powder was loaded into an elastic mold, sealed and placed in a high-pressure cylinder of an isostatic press, and pressed and formed at a pressure of 210 MPa to obtain a tantalum rod.
  • the formed tantalum rod was sintered in a vertical melting furnace at a sintering temperature of 2800°C and a holding time of 360 min to obtain a tantalum metal billet F.
  • the chemical impurity content is shown in Table 2.
  • Example 1 The subsequent operations are the same as those in Example 1, and the obtained high-voltage tantalum powder F is used to make a capacitor anode in the manner of Example 1.
  • the powder was loaded into an elastic mold, sealed, and placed in a high-pressure cylinder of an isostatic press. A pressure of 210 MPa was used to press-form the powder to obtain a tantalum rod.
  • the formed tantalum rod was sintered in a vertical melting furnace at a sintering temperature of 2800°C and a holding time of 480 min to obtain a tantalum metal billet G.
  • the chemical impurity content is shown in Table 2.
  • Example 1 The subsequent operations are the same as those in Example 1, and the obtained high-voltage tantalum powder G is used to make a capacitor anode in the manner of Example 1.
  • the tantalum metal blank (comparison blank 1) is a commercially available high-purity tantalum ingot with the grade Ta1, the chemical impurity content of which is shown in Table 2, and the metallographic structure photograph is shown in Figure 8.
  • step 2) of Example 1 Repeat step 2) of Example 1 to obtain a hydrogenated material with good hydrogen embrittlement resistance.
  • step 4) of Example 1 to obtain hydrogenated impurity-removed tantalum powder.
  • Step 5) of Example 1 was repeated to obtain Comparative Sample 1.
  • the chemical impurity content thereof is shown in Table 3.
  • Comparative sample 1 was pressed into a shape with a pressed density of 6.5 g/cm 3 and a core powder weight of 1 g, and tested according to the standard. Sintered for 30 minutes in a vacuum furnace at 10 -3 Pa according to the sintering conditions in Table 4. A sintered block was obtained. The sintered block was energized in a 0.01% volume phosphoric acid solution at the energizing voltage in Table 4 to obtain a capacitor anode. The electrical performance indicators thereof were measured and listed in Table 4.
  • the tantalum metal billet is a high-purity tantalum ingot with a commercial grade of Ta1 (comparative billet 2), and its chemical impurity content is shown in Table 2.
  • the tantalum metal billet is loaded into the hydrogenation container of the hydrogenation furnace and heated to 800°C for insulation. High-purity hydrogen is introduced and the hydrogen pressure is maintained at 1.3-1.5MPa for 15 hours. The temperature is then lowered and the hydrogen pressure is maintained at 1.3-1.5MPa to allow the tantalum ingot to fully absorb hydrogen and react with hydrogen. After the temperature drops to 100°C, the hydrogen is stopped. When the temperature is lower than 40°C, the billet is taken out of the furnace to obtain a hydrogenated material with good hydrogen embrittlement.
  • the hydride material is then crushed into tantalum hydride powder with Dv50 ⁇ 15 ⁇ m.
  • the crushed tantalum hydride powder is pickled with a mixed acid of HNO 3 and HF (the volume ratio of HNO 3 , HF and water is 4:1:20) to remove metal impurities, dried and sieved to obtain tantalum hydride powder without impurities.
  • a mixed acid of HNO 3 and HF the volume ratio of HNO 3 , HF and water is 4:1:20
  • the above hydrogenated impurity-removed tantalum powder is placed in a closed furnace filled with argon and heated to 900°C for 180 minutes for dehydrogenation treatment, then cooled out of the furnace and sieved.
  • the above dehydrogenated tantalum powder is subjected to high temperature and high vacuum heat treatment and deoxidation treatment, specifically, the treatment is carried out at 1300°C under vacuum for 60 minutes, then crushed to -50 mesh, and then subjected to 900°C deoxidation treatment, and finally 20% HNO3
  • the magnesium oxide and excess magnesium were removed by pickling, and the powder was dried and sieved to make it completely pass through a 50-mesh sieve to obtain comparative sample 2.
  • the chemical impurity content is shown in Table 3.
  • Comparative sample 2 was pressed into a shape with a pressed density of 6.5 g/cm 3 and a core powder weight of 1 g, and tested according to the standard. Sintered for 30 minutes in a vacuum furnace at 10 -3 Pa according to the sintering conditions in Table 4. A sintered block was obtained. The sintered block was energized in a 0.01% volume phosphoric acid solution at the energizing voltage in Table 4 to obtain a capacitor anode. The electrical performance indicators thereof were measured and listed in Table 4.
  • the tantalum metal blank is a commercially available tantalum rod with a grade of Ta3 (comparative blank 3), and the chemical impurity content thereof is shown in Table 2.
  • the tantalum metal billet is loaded into the hydrogenation container of the hydrogenation furnace and heated to 800°C for insulation. High-purity hydrogen is introduced and the hydrogen pressure is maintained at 1.3-1.5MPa for 15 hours. The temperature is then lowered and the hydrogen pressure is maintained at 1.3-1.5MPa to allow the tantalum ingot to fully absorb hydrogen and react with hydrogen. After the temperature drops to 100°C, the hydrogen is stopped. When the temperature is lower than 40°C, the billet is taken out of the furnace to obtain a hydrogenated material with good hydrogen embrittlement.
  • step 4) of Example 1 to obtain hydrogenated impurity-removed tantalum powder.
  • Step 5) of Example 1 was repeated to obtain Comparative Sample 3.
  • the chemical impurity content thereof is shown in Table 3.
  • Comparative sample 3 was pressed into a shape with a pressed density of 6.5 g/cm 3 and a core powder weight of 1 g, and tested according to the standard. Sintered for 30 minutes in a vacuum furnace at 10 -3 Pa according to the sintering conditions in Table 4. A sintered block was obtained. The sintered block was energized in a 0.01% volume phosphoric acid solution at the energizing voltage in Table 4 to obtain a capacitor anode. The electrical performance indicators thereof were measured and listed in Table 4.
  • Table 2 Main chemical impurity content and grain size of tantalum metal blanks
  • Table 3 Main impurity content and other properties of high-voltage tantalum powder
  • Table 4 Specific capacitance and leakage current of electrolytic capacitor anodes obtained from different high voltage tantalum powders under different sintering conditions
  • the preparation method of the present application is used to obtain high-voltage tantalum powder.
  • the electrolytic capacitor anode made of the high-voltage tantalum powder has a specific capacitance of 7000 ⁇ F ⁇ V/g-25000 ⁇ F ⁇ V/g and a breakdown voltage of 200V-285V when the enabling voltage is 150V-270V, achieving a high specific capacitance and a low leakage current.
  • the CV value of the high-voltage tantalum powder it can be seen that as the grain size increases, the CV value gradually decreases; especially when comparing high-voltage tantalum powder A, high-voltage tantalum powder F and high-voltage tantalum powder G, it can be found that as the grain size increases, the CV value gradually decreases, and the leakage current gradually increases. Gradually decrease.

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Abstract

L'invention concerne une poudre de tantale à haute tension et son procédé de préparation, et une anode de condensateur. Le procédé de préparation comprend la sélection d'une ébauche de métal de tantale, la teneur en impureté C dans l'ébauche de métal de tantale étant inférieure ou égale à 30 ppm, la teneur totale en impuretés métalliques Fe, Ni et Cr étant inférieure ou égale à 30 ppm, et la taille de grain étant de 1 à 900 µm ; la soumission de l'ébauche de métal de tantale à un traitement d'hydrogénation, de façon à obtenir un matériau hydrogéné ; la soumission du matériau hydrogéné à un traitement de pulvérisation, de façon à obtenir une poudre de tantale contenant de l'hydrogène ; la soumission de la poudre de tantale contenant de l'hydrogène à un décapage acide et à une élimination d'impuretés de façon à obtenir une poudre de tantale hydrogénée et exempte d'impuretés ; et la soumission de la poudre de tantale hydrogénée et exempte d'impuretés à un traitement ultérieur, de façon à obtenir une poudre de tantale à haute pression, le traitement ultérieur comprenant l'un ou une combinaison de plusieurs parmi un traitement de déshydrogénation, un traitement thermique à haute température et sous vide poussé et un traitement de réduction et de réduction d'oxygène. La réalisation de l'hydrogénation, de la pulvérisation et des traitements ultérieurs au moyen de l'ébauche de métal de tantale en tant que matière première améliore efficacement la tension de claquage et la valeur CV d'un condensateur constitué de la poudre de tantale, et réduit le courant de fuite du condensateur.
PCT/CN2024/104984 2023-08-15 2024-07-11 Poudre de tantale à haute tension et son procédé de préparation, et anode de condensateur Pending WO2025036039A1 (fr)

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