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Method and device for surface passivation of tantalum metal

A metal surface and metal technology, which is applied in the field of passivation of tantalum powder or porous tantalum metal surface for the production of electrolytic capacitors, can solve the problems of low productivity, unsuitable, long passivation time, etc., achieve low oxygen content, save time, Good electrical performance

Active Publication Date: 2011-09-14
NINGXIA ORIENT TANTALUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The prior art including patent documents US 6927967B2, US 6432161B1, US 6238456B1, CN 1919508A, CN101404213A, US 6992881B2, US 7485256B2 and CN 1899728A has disclosed the passivation of tantalum powder, but these prior art are the passivation of tantalum powder at room temperature. Oxygen gas is passed into a vacuum furnace equipped with heat treatment and cooled to room temperature or higher temperature and stays in the reaction chamber, and the heat generated by the reaction of oxygen-containing gas and tantalum powder is also kept in it; such passivation treatment Long time, and often cause intense oxidation of tantalum powder
The Chinese patent with the publication number CN101348891A discloses a method for reducing oxygen through the controlled passivation of tantalum powder, in which pure oxygen is used for passivation treatment; the problem with this method is that it is not suitable for passivating tantalum powder after heat treatment change
In the prior art, the passivation of tantalum powder after heat treatment is to fill the reactor with oxygen-containing gas and keep it still. Due to the heat generated by passivation, the temperature of tantalum powder will increase, and the high temperature will accelerate oxidation, and a vicious cycle will occur. Control oxidation rate
This has the problem of long passivation time and low productivity.

Method used

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  • Method and device for surface passivation of tantalum metal
  • Method and device for surface passivation of tantalum metal
  • Method and device for surface passivation of tantalum metal

Examples

Experimental program
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Effect test

Embodiment 1

[0068] With a specific surface area of ​​1.79m 2 / g, bulk density is 0.50g / cm 3 , the porosity is 97.0% and the oxygen content is 6200ppm The original powder prepared by reducing potassium fluorotantalate with sodium is mixed with 120ppm of phosphorus according to the weight of tantalum powder, and then spheroidized and granulated to obtain a bulk density of 1.01 g / cm 3 Particles with a porosity of 93.9%. Pour the above spheroidized and granulated tantalum powder into a tantalum crucible, the porosity of which is 96.8% of that of the original powder, and put the crucible into figure 2 In the tantalum powder heat treatment passivation device shown, the thickness of the tantalum powder in the tantalum crucible is about 45 mm. In the multiple tantalum crucibles on the same horizontal plane, there is a gap of about 1 cm between the tantalum crucibles. There is a 3cm gap, so put it into the vacuum heat treatment furnace, under the pressure of 1.33×10 -1Heat to 1200°C in a vacuu...

Embodiment 2

[0071] Carry out granulation equally with the same tantalum powder of embodiment 1, pour granulation tantalum powder in the tantalum crucible, crucible is packed into such as image 3 In the tantalum powder heat treatment passivation device shown, the thickness of the tantalum powder in the tantalum crucible is about 45 mm. In the multiple tantalum crucibles on the same horizontal plane, there is a gap of about 1 cm between the tantalum crucibles, so that the vacuum In the heat treatment furnace, at a pressure of 1.33×10 -1 Heating to 1200°C in a vacuum below Pa for 30 minutes, then stop heating, and after cooling down to 120°C, close 322, feed argon gas from 321 into the reaction chamber, close 321 and start cycle 309 after the pressure reaches about 0.1MPa, Argon gas enters the lower part of the reaction chamber from the gas inlet 340, and the argon gas extracted from the upper gas outlet 307 is cooled by the cooling pipe 308 through which cooling water with a temperature of...

Embodiment 3

[0077] For the passivation of tantalum powder after deoxidation heat treatment, the S-2h tantalum powder after the heat treatment in Example 2 is calculated as tantalum powder and mixed with 2 wt% magnesium powder to form a mixed powder, and the above mixed powder is loaded into such as Figure 5 In the shown tantalum powder deoxidation reaction chamber, there is a gap of about 6 cm between the crucibles of each layer, and a gap of about 8 cm between the crucible and the side wall of the reaction chamber; the above-mentioned tantalum powder is deoxidized at 850 ° C for 3 hours, and the heating is stopped. , cooling down, doping nitrogen at 250°C, and then lowering the temperature to 32°C in argon according to the same method as in Example 1, then performing passivation treatment in the same way as in Example 1, and performing the passivation treatment for the first to eighth times as follows Table 4 is evacuated and filled with air, and the temperature of the gas entering the r...

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Abstract

The invention relates to a method for surface passivation of tantalum metal after heat treatment. The method comprises the following steps of: introducing a low-temperature oxygen-containing gas into the lower part of a reaction chamber to passivate the surface of the tantalum metal after the heat treatment; and simultaneously, extracting out the high-temperature oxygen-containing gas on the upper part of the reaction chamber to form a flowing oxygen-containing gas to passivate the surface of the tantalum metal. The invention also provides a device for the surface passivation of the tantalum metal to implement the method. To prepare the tantalum metal according to the method, the passivation time of the tantalum metal can be greatly shortened, the passivation process is safe and reliable, the productivity is high, and the obtained tantalum powder and tantalum anode are low in oxygen content and high in electrical properties.

Description

Technical field [0001] The present invention relates to the field of tantalum metal production, and in particular to a passivation method and device for producing tantalum powder or porous tantalum metal surface for electrolytic capacitors. Background technique [0002] The largest use of tantalum metal is in the manufacture of tantalum electrolytic capacitors. The manufacturing process of tantalum electrolytic capacitors usually involves pressing tantalum powder to form a compact, which is then sintered in a vacuum furnace into a porous body with interconnected particles. The porous sintered body is then anodized in a suitable electrolyte to make it porous. A uniform interconnected dielectric oxide film is formed on the surface of the bulk particles, which forms an anode. The surface of the oxide film is then coated with cathode material to form a cathode, and then the capacitor anode and cathode are encapsulated and formed. The main parameters for evaluating tantalum elec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C8/12H01G9/042H01G9/052B22F1/00
Inventor 潘伦桃
Owner NINGXIA ORIENT TANTALUM IND
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