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Process for preparing Nb and/or Ta powder

A production method and technology of tantalum powder, applied in the production field of niobium and/or tantalum powder, can solve problems such as inability to obtain niobium powder, loss of precious metal tantalum, pollution of niobium powder, etc.

Inactive Publication Date: 2002-12-04
NINGXIA ORIENT TANTALUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Also, it is well known that alkali metals cannot reduce tantalum oxide and niobium oxide. Therefore, reducing potassium fluoroniobate containing niobium oxide and / or potassium fluorotantalate containing tantalum oxide with alkali metals cannot obtain pure niobium powder and / or or tantalum powder, and cause the loss of precious metals tantalum and niobium
[0011] In addition, the use of nickel-based alloy materials for reaction vessels and stirrers will cause pollution to niobium powder when alkali metals are used to reduce potassium fluoroniobate. Therefore, so far, there has been no industrial reduction of potassium fluoroniobate by alkali metal Successful precedent for producing capacitor grade niobium powder

Method used

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  • Process for preparing Nb and/or Ta powder
  • Process for preparing Nb and/or Ta powder
  • Process for preparing Nb and/or Ta powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 15 kg of potassium fluorooxyniobate (containing 1.02 kg of Nb 2 o 5 ) niobium raw material, with 25 kg of NaCl, 15 kg of KCl, 12 kg of CaCl 2 Put it into a closed reaction vessel with a stirring blade and a heat-resistant alloy lining inside with an inert gas inlet and outlet, heat it to 700°C under an argon atmosphere, inject 6,500 grams of liquid metal sodium, and make it undergo a reduction reaction, and then Heat up to 800°C for 1 hour. After cooling to room temperature, the reaction materials are stripped out, washed with water and pickled, and then dried to obtain 4107 grams of niobium powder. The BET specific surface area of ​​the original powder is 6.56m 2 / g, the oxygen content of the original powder of niobium powder is 9800ppm. attached figure 1 It is the scanning electron micrograph of the microstructure of this niobium powder. It can be seen that the niobium powder particles are porous aggregates with large specific surface area composed of many primary ...

Embodiment 2

[0059] The niobium raw material of 29 kg of potassium oxyfluoroniobate containing 1.03 kg of niobium oxide was mixed with 25 kg of NaCl and 2 kg of CaCl 2 , 40 kilograms of KCl are injected 11750 grams of liquid metal sodium at 800 ℃ according to the same method of embodiment 1, and other production processes are all identical with embodiment 1. Obtain 8350 grams of niobium powder, the BET specific surface area of ​​the former powder is 6.41m 2 / g, the oxygen content of the original powder of niobium powder is 11000ppm. The reduction recovery of niobium powder is shown in Table 1.

[0060] The raw niobium powder obtained above was subjected to doping, deoxidation and thermal agglomeration treatment in the same manner as in Example 1 to obtain agglomerated niobium powder.

[0061] The main chemical impurity content of niobium powder is shown in Table 2, and the physical properties are shown in Table 3. The porosity of agglomerated niobium powder is 88.99%.

[0062] Using th...

Embodiment 3

[0064] Mix the tantalum raw material containing 2.10 kg of tantalum oxide and 30 kg of potassium fluorotantalate with 65 kg of NaCl, 20 kg of KCl, and 8.0 kg of MgCl 2 Put it into a closed reaction vessel lined with a heat-resistant alloy with a stirring blade and an inert gas inlet and outlet. Heating to 800°C under an argon atmosphere, injecting 10,500 grams of liquid metal sodium to cause a reduction reaction, then raising the temperature, keeping it at 850°C for 1 hour, cooling to room temperature, stripping off the reaction material, washing with water, pickling, and then drying Dry, obtain tantalum powder 14094 grams, the BET specific surface area of ​​former powder is 3.86m 2 / g, its oxygen content is 7800ppm. The reduction recovery rate of tantalum powder is shown in Table 1.

[0065] The raw tantalum powder obtained above is doped, deoxidized and thermally agglomerated according to existing methods to obtain agglomerated tantalum powder.

[0066] The main chemical ...

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Abstract

A process for preparing Nb and / or Ta powder features that under the action of reducer chosen from alkali metal plus at least one of the halides of Mg, Ca, Sr, Ba, Li and Ce, the alkali-metal fluonidobium and / or tantalate is reduced at 300-1050 deg.C to obtain said products. Its advantages are high recovery rate for reduction, and large specific surface area, high porosity and low oxygen content of product.

Description

technical field [0001] The present invention relates to a process for the production of niobium and / or tantalum powder. Background technique [0002] Niobium and tantalum, known as valve metals, have similar properties and can be used to manufacture the anode of electrolytic capacitors, that is, niobium wire or tantalum wire is embedded in niobium powder or tantalum powder, pressed into shape, sintered into a porous sintered body, and then in the electrolyte Anodic oxidation is carried out in the solution, and a dielectric oxide film is formed on the surface of the porous sintered body. On the oxide film, manganese dioxide or a conductive organic polymer solid electrolyte is sequentially formed to form a carbon layer and a silver layer as the cathode of the capacitor. The anode terminal and the cathode terminal are then resin-encapsulated to obtain a niobium / tantalum solid electrolytic capacitor. [0003] As the niobium powder or tantalum powder of the electrolytic capacito...

Claims

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Application Information

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IPC IPC(8): B22F9/24C22B34/24
Inventor 潘伦桃何季麟袁宁峰郑爱国温晓立王丹鹏张庆生李兴邦
Owner NINGXIA ORIENT TANTALUM IND
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