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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 low efficiency, complex process, and many reducing agents.

Inactive Publication Date: 2004-10-06
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

[0036] 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 into a crucible, add 1 kg of metallic sodium, place it in a closed reactor, put in argon gas after vacuuming, heat it to 800 °C with an electric furnace, and keep it warm for 30 minutes. Reheat to 900°C and keep warm for 30 minutes.

[0037] The second step (separation of tantalum powder): after the reduction material in the first step is cooled, the reaction material is stripped from the crucible and broken, and the soluble salt and alkali metal are washed away with deionized water, washed with hydrochloric acid solution, and then Wash with deionized water until neutral to obtain tantalum powder, dry the tantalum powder, and sieve 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), Fischer average particle size (FSSS), specific surface area...

Embodiment 2

[0071] The first step (reduction of tantalum oxide): use 10 kg of tantalum oxide and 15 kg of CaCl 2 , 22 kilograms of KCl, 10 kilograms of NaCl, put them into the reaction vessel, put argon and nitrogen into it after vacuuming, heat to 850°C with an electric furnace, when CaCl 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 speed of 640 g / min to reduce the tantalum oxide to tantalum powder, and then Heat to 900°C and keep it warm for 60 minutes to make the reduction reaction fully proceed.

[0072] 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, broken, washed with deionized water to remove soluble salts and alkali metals, and then washed with hydrochloric acid. Wash with deionized water until neutral to obtain tantalum powder, dry the tantalu...

Embodiment 3

[0106] The first step (reduction of tantalum oxide): use 10 kg of tantalum oxide and 15 kg of CaCl 2 , 22 kilograms of KCl, 10 kilograms of NaCl, put into the reaction vessel, after vacuuming, argon and nitrogen are introduced, heated to 1050 °C with an electric furnace, stirred with a stirrer, so that tantalum oxide is dispersed in the melt, and the reactor Cool and inject 5510 grams of liquid metal sodium at a rate of 1020 g / min to reduce the tantalum oxide to tantalum powder, and keep the temperature at 1050° C. for 20 minutes to fully carry out the reduction reaction.

[0107] 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, broken, washed with deionized water to remove soluble salts and alkali metals, and then washed with hydrochloric acid. Wash with deionized water to neutral to obtain tantalum powder, dry this tantalum powder, sieve with 80 mesh sieves, obt...

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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

technical field [0001] The invention relates to a preparation method of tantalum powder and / or niobium powder with high specific surface area. Background technique [0002] An important use of tantalum and niobium powders is in the production of 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 pressed into shape, and then sintered into a porous body, followed by anodic oxidation to form a continuous dielectric on the surface of the porous body. The surface of the oxide film is coated with a solid electrolyte cathode material and then encapsulated to make a tantalum or niobium solid electrolyte capacitor. The weight specific capacitance or volume specific capacitance of this kind of capacitor is related to the specific surface area of ​​tantalum and niobium powder. High specific surface area tantalum and niobium powder can make anode with high sp...

Claims

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Application Information

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Patent Type & Authority Patents(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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