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Preparation method of high specific surface area tantalum powder and/or niobium powder

A technology with high specific surface area and tantalum powder, used in electrolytic capacitors, electrical components, circuits, etc., can solve the problems of large acid content, many reducing agents, and low efficiency.

Inactive Publication Date: 2003-04-16
NINGXIA ORIENT TANTALUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantage of this method is that too many reducing agents are used, and the amount of acid that must be used in pickling is also large. In addition, since the method includes two reductions, and the first reduction requires strict control of the degree of reduction, this method The method is complicated and the efficiency is not high

Method used

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  • Preparation method of high specific surface area tantalum powder and/or niobium powder
  • Preparation method of high specific surface area tantalum powder and/or niobium powder
  • Preparation method of high specific surface area tantalum powder and/or niobium powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The first step (reduction of tantalum oxide): use 4 kg of tantalum oxide and 6 kg of MgCl 2 , 6 kg of KCl, 3 kg of NaCl, mix well, put it in a crucible, then add 1 kg of sodium metal, and place it in a closed reactor. After vacuuming, pass in argon gas, heat it to 800°C with an electric furnace, and keep it for 30 minutes. Then heat to 900°C and keep it for 30 minutes.

[0038] The second step (the separation of tantalum powder): After the reduction material of the first step is cooled, the reaction material is stripped from the crucible and broken, washed with deionized water to remove soluble salts and alkali metals, and then washed with hydrochloric acid solution, and then used The tantalum powder is obtained by washing with deionized water until it is neutral. The tantalum powder is dried and sieved with a 100-mesh sieve to obtain 2953 grams of tantalum powder (original powder). The yield of tantalum powder is 90.15%. The bulk density (SBD), Fisher average particle size...

Embodiment 2

[0072] The first step (reduction of tantalum oxide): use 10 kg of tantalum oxide and 15 kg of CaCl 2 , 22 kg of KCl, 10 kg of NaCl, put them into the reaction vessel, evacuated and then pass in argon and nitrogen, and use an electric furnace to heat to 850°C. 2 , KCl and NaCl are melted and stirred with a stirrer to disperse the tantalum oxide in the melt. Cool the reactor and inject 5250 grams of liquid metal sodium at a rate of 640 g / min to reduce the tantalum oxide to tantalum powder. Heat to 900°C and keep for 60 minutes to allow the reduction reaction to proceed fully.

[0073] The second step (separation of tantalum powder): Then, after the material obtained in the first step is cooled, the reaction material is stripped from the reactor, crushed, washed with deionized water to remove soluble salts and alkali metals, and then washed with hydrochloric acid. The tantalum powder was washed with deionized water to neutrality to obtain tantalum powder. The tantalum powder was drie...

Embodiment 3

[0107] The first step (reduction of tantalum oxide): use 10 kg of tantalum oxide and 15 kg of CaCl 2 , 22 kg of KCl, 10 kg of NaCl, put into the reaction vessel, evacuated and vented with argon and nitrogen, heated to 1050 ℃ with an electric furnace, stirred with a stirrer to disperse the tantalum oxide in the melt, After cooling, 5510 grams of liquid metal sodium was injected at a rate of 1020 g / min to reduce tantalum oxide to tantalum powder. The temperature was kept at 1050°C for 20 minutes to allow the reduction reaction to proceed fully.

[0108] The second step (separation of tantalum powder): Then, after the material obtained in the first step is cooled, the reaction material is stripped from the reactor, crushed, washed with deionized water to remove soluble salts and alkali metals, and then washed with hydrochloric acid. The tantalum powder is obtained by washing with deionized water to neutrality. The tantalum powder is dried and sieved with an 80-mesh sieve to obtain 75...

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Abstract

A tantalum powder and / or a niobium powder with high specific surface area are prepared through reaction between the oxides one of tantalum and / or niobium, alkali metal and halide of at least of Mg, Ca, Sr, Ba and Ce. Its advantages are simple preparing process, and high specific surface area, purity and flowability, and thus it is especially suitable for making the anode of capacitor.

Description

Invention field [0001] The invention relates to a method for preparing tantalum powder and / or niobium powder with high specific surface area. Background technique [0002] An important use of tantalum powder and niobium powder is to produce capacitors. In order to prepare tantalum and niobium solid electrolytic capacitors, tantalum powder and niobium powder (embedded with tantalum wire and niobium wire) are generally used to press and form, and then sintered into a porous body, followed by anodization to form a continuous dielectric on the surface of the porous body. The oxide film is coated with a solid electrolyte cathode material on the surface of the oxide film and then encapsulated to make a tantalum and niobium solid electrolyte capacitor. The weight-to-capacitance or volume-to-capacitance of this kind of capacitor is related to the specific surface area of ​​tantalum and niobium powder. High specific surface area of ​​tantalum and niobium powder can be used to make anodes ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/20B22F9/24C21B15/00C22B5/04C22B34/24H01G9/052
CPCB22F9/24C22B34/24C22B5/04C21B15/006H01G9/0525Y02P10/134B22F9/20
Inventor 何季麟潘伦桃袁宁峰温晓利李兴邦
Owner NINGXIA ORIENT TANTALUM IND
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