JPS62247001A - Refining method for metallic tantalum powder - Google Patents
Refining method for metallic tantalum powderInfo
- Publication number
- JPS62247001A JPS62247001A JP61089646A JP8964686A JPS62247001A JP S62247001 A JPS62247001 A JP S62247001A JP 61089646 A JP61089646 A JP 61089646A JP 8964686 A JP8964686 A JP 8964686A JP S62247001 A JPS62247001 A JP S62247001A
- Authority
- JP
- Japan
- Prior art keywords
- acid
- tantalum
- powder
- metal powder
- mixed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims description 20
- 238000007670 refining Methods 0.000 title claims description 10
- 239000000843 powder Substances 0.000 claims abstract description 48
- 239000002253 acid Substances 0.000 claims abstract description 42
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000010306 acid treatment Methods 0.000 claims abstract description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 16
- 238000000746 purification Methods 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 14
- 239000001301 oxygen Substances 0.000 abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052715 tantalum Inorganic materials 0.000 abstract description 11
- 239000003990 capacitor Substances 0.000 abstract description 8
- 238000011282 treatment Methods 0.000 abstract description 4
- 150000007513 acids Chemical class 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 229910052749 magnesium Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 239000011777 magnesium Substances 0.000 description 7
- 230000001590 oxidative effect Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- -1 hydrogen ions Chemical class 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- YZCKVEUIGOORGS-UHFFFAOYSA-N Hydrogen atom Chemical compound [H] YZCKVEUIGOORGS-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- ZIRLXLUNCURZTP-UHFFFAOYSA-I tantalum(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Ta+5] ZIRLXLUNCURZTP-UHFFFAOYSA-I 0.000 description 2
- 241000219198 Brassica Species 0.000 description 1
- 235000003351 Brassica cretica Nutrition 0.000 description 1
- 235000003343 Brassica rupestris Nutrition 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910019440 Mg(OH) Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- QKSKPIVNLNLAAV-UHFFFAOYSA-N bis(2-chloroethyl) sulfide Chemical compound ClCCSCCCl QKSKPIVNLNLAAV-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 235000010460 mustard Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Powder Metallurgy (AREA)
Abstract
Description
【発明の詳細な説明】
「産業上の利用分野」
本発明は、金属タンタル粉末の精製方法に係り、より詳
しくは、金属タンタル粉末中の酸化物、水素および過剰
に存在する金属還元剤等を効率的に除去するための金属
タンタル粉末の改善された精製方法に関するものである
。DETAILED DESCRIPTION OF THE INVENTION "Industrial Application Field" The present invention relates to a method for refining tantalum metal powder, and more specifically, the present invention relates to a method for refining tantalum metal powder. The present invention relates to an improved method for purifying tantalum metal powder for efficient removal.
「従来の技術」
周知のように、金属タンタルは、主としてそのフッ化カ
リウム塩ＫｔＴａＰ、のＮａ還元によって製造され、得
られたスポンジ状タンタルは、いくつかの化学処理およ
び熱処理を経て精製される。この金属タンタルの主たる
用途は、電解コンデンサ−原料である。この電解コンデ
ンサー用タンタル粉末の特性として、特に低い漏洩電流
係数が望まれており、この低漏洩電流係数の電解コンデ
ンサー用タンタル粉末を得るためには、生成タンタル粉
末は適当な物理的形状と粒径を持ち、かつ高純度である
ことが要求される。"Prior Art" As is well known, tantalum metal is mainly produced by Na reduction of its potassium fluoride salt KtTaP, and the obtained spongy tantalum is purified through several chemical and heat treatments. The main use of this metal tantalum is as a raw material for electrolytic capacitors. As a characteristic of this tantalum powder for electrolytic capacitors, a particularly low leakage current coefficient is desired. and high purity.
最近、電解コンデンサーにおいては、より一層の高容量
化が指向され、それに伴って、原料である金属タンタル
粉末粒子の微細化が求められている。しかし、微細化に
よる粉末構成粒子表面積の増大に伴って、酸化物が急増
する傾向にあり、金属タンタル粉末中の酸素濃度は３０
００ｐｐｍを越えるようになっている。このような高酸
素濃度はコンデンサーの性能を低下させるため、従来の
金属タンタル粉末の精製方法においては、酸素濃度低下
対策が必須となっている。Recently, electrolytic capacitors are becoming more capacitive, and as a result, the metal tantalum powder particles used as raw materials are required to be made finer. However, as the surface area of powder constituent particles increases due to refinement, oxides tend to increase rapidly, and the oxygen concentration in tantalum metal powder is 30%.
It exceeds 00 ppm. Since such a high oxygen concentration deteriorates the performance of the capacitor, it is essential to take measures to reduce the oxygen concentration in conventional methods for refining tantalum metal powder.
これに対し、特開昭５８−２７９０３号公報に開示され
るように、金属タンタル粉末と、Ｍｇ、Ｃａ、 Ｂｅ。On the other hand, as disclosed in Japanese Unexamined Patent Publication No. 58-27903, metallic tantalum powder and Mg, Ca, Be.
Ｌｉ、Ａ（等の還元用金属粉末の混合物とを不活性雰囲
気中または真空中において加熱し、生成した前記還元用
金属粉末の酸化物を酸によって溶解除去することにより
、金属タンタル粉末中の酸化物を織少さ仕る方法が探ら
れている。そして、この溶解除去に適用される酸として
は、例えば、前記公報に示されるように、一般に塩酸が
使用されている。A mixture of reducing metal powders such as Li and A (etc.) is heated in an inert atmosphere or in a vacuum, and the generated oxide of the reducing metal powder is dissolved and removed with an acid, thereby reducing the oxidation in the tantalum metal powder. A method of reducing the weave of the material is being sought.As the acid used for this dissolution and removal, for example, as shown in the above-mentioned publication, hydrochloric acid is generally used.
［発明が解決しようとする問題点」
前記した金属タンタル粉末中の酸化物の溶解除去におい
て、本発明者らの実験によれば、周知の塩酸処理では水
素含有量の低減は期待できず、むしろ増加する場合らあ
るという事実が認められた。[Problems to be Solved by the Invention] According to experiments conducted by the present inventors, the well-known hydrochloric acid treatment cannot be expected to reduce the hydrogen content in dissolving and removing oxides from the metal tantalum powder, but rather reduces the hydrogen content. It was acknowledged that there are cases where the number of cases increases.
つまり、従来技術によると脱酸素処理において、還元剤
であるＭ ｇｑ Ｃａｓ Ａ Ｑｓ Ｂ ｅと酸素との
間で生じた還元生成物を塩酸で処理する際、タンタル粒
子表面付近に存在する過剰の還元剤が酸と反応する。こ
れを、Ｍｇを例に挙げて示すと、次のような反応となる
。In other words, according to the conventional technology, when the reduction product generated between the reducing agent M gq Cas A Qs B e and oxygen is treated with hydrochloric acid in the deoxidation treatment, the excessive reduction existing near the surface of the tantalum particles The agent reacts with the acid. If this is illustrated using Mg as an example, the following reaction will occur.
Ｍｇ＋ ２ＨＣＱ−ＭｇＣＱｔ＋ ２Ｈ・・・・■この
０式に示した反応の結果生じた発生期の水素は、容易に
Ｔａと結合し、タンタル中の水素濃度が高まる。Mg+ 2HCQ-MgCQt+ 2H...■ The nascent hydrogen generated as a result of the reaction shown in equation 0 easily combines with Ta, increasing the hydrogen concentration in tantalum.
そして、この水素濃度の増加は、次のような問題を招来
することが判明した。すなわち、コンデンサー用タンク
ルベレットは、金属タンタルの圧粉成形体を焼結して得
られるが、この圧粉成形体の圧縮強度は、一般に５．５
ｋｇ／ａｘ”以上が求められている。これに対し、本発
明者らの実験によると、第１図に示すように金属タンタ
ル粉末中の水素濃度は、圧粉成形体の強度と密接な関係
があり、前記の成形体強度（グリーン強度）を得るには
、金属タンタル粉末中の水素濃度は１１００ｐｐ以下で
あることが必要条件であることが確かめられた。It has been found that this increase in hydrogen concentration brings about the following problems. In other words, tanker berets for capacitors are obtained by sintering a powder compact of tantalum metal, and the compressive strength of this powder compact is generally 5.5.
kg/ax" or more. On the other hand, according to the experiments conducted by the present inventors, the hydrogen concentration in the tantalum metal powder has a close relationship with the strength of the powder compact, as shown in Figure 1. It was confirmed that in order to obtain the above-mentioned compact strength (green strength), the hydrogen concentration in the tantalum metal powder must be 1100 pp or less.
また、良好な電解コンデンサーを構成するためには、金
属タンタル粉末中の酸化物は、酸素濃度で２０００ｐｐ
ｍ以下であることが要請され、さらに還元用金属の残留
量も５ｐｐＩ１１未満である必要も判明している。In addition, in order to construct a good electrolytic capacitor, the oxide in the metal tantalum powder must have an oxygen concentration of 2000pp.
m or less, and it has also been found that the residual amount of the reducing metal must also be less than 5 ppI11.
本発明は、前記事情に鑑みてなされたもので、その目的
は、金属タンタル粉末中の酸化物に基づく酸素濃度を２
０００ｐｐｍ以下、水素６庁をＬＯＯＤＤＩＩＩ以下、
かつ還元用金属の残留量を５ ｐｐｍ未満とすることが
できる金属タンタル粉末の精製方法を提供することにあ
る。The present invention has been made in view of the above circumstances, and its purpose is to reduce the oxygen concentration based on oxides in tantalum metal powder by 2.
000 ppm or less, Hydrogen 6 Agency is below LOOD DIII,
Another object of the present invention is to provide a method for purifying metallic tantalum powder that can reduce the residual amount of reducing metal to less than 5 ppm.
「問題点を解決するための手段」
本願の第１の発明は、金属タンタル粉末と還元用金属粉
末の混合物を不活性雰囲気中または真空中において加熱
処理し、次いで生成物を酸処理する工程を含む金属タン
タル粉末の精製方法において、前記酸処理を塩酸と硝酸
との混酸により行なうことを特徴とするものであり、こ
の場合、混酸の全酸濃度が１０，１ＩＯｅ／１２以上で
、しかも混酸中の組成割合が塩酸５ｔｏ（１／Ｑ以上、
硝酸０．１３〜６．５ｉｏ（／Ｑである必要がある。"Means for Solving the Problems" The first invention of the present application includes a step of heat-treating a mixture of tantalum metal powder and reducing metal powder in an inert atmosphere or vacuum, and then treating the product with an acid. A method for purifying a metal tantalum powder containing tantalum powder, characterized in that the acid treatment is performed with a mixed acid of hydrochloric acid and nitric acid, and in this case, the total acid concentration of the mixed acid is 10,1 IOe/12 or more, and The composition ratio is 5 to of hydrochloric acid (1/Q or more,
Nitric acid needs to be 0.13 to 6.5 io(/Q).
また、本願の第２の発明は、前記酸処理を塩酸と硝酸と
フッ酸との混酸により行なうことを特徴とするものであ
り、この場合、混酸の全酸濃度がＬＯｘｏＱ／（１以上
で、しから混酸中の組成割合が塩酸５ｍｏｌ／ｌ以上、
硝酸０．１３〜６．５３ＩＯｆ２／ （２、フッ酸３．
０ｚｏ（１／Ｑ以下である必要がある。Further, the second invention of the present application is characterized in that the acid treatment is performed with a mixed acid of hydrochloric acid, nitric acid, and hydrofluoric acid, and in this case, the total acid concentration of the mixed acid is LOxoQ/(1 or more, The composition ratio in the mustard mixed acid is 5 mol/l or more of hydrochloric acid,
Nitric acid 0.13-6.53 IOf2/ (2, hydrofluoric acid 3.
0zo (needs to be 1/Q or less.
「作用 」
前記本発明は、種々実験検討の結果、求められたしので
、この構成における酸の作用と、その必要とする濃度は
、下記のようである。"Effect" The present invention was obtained as a result of various experimental studies, and the action of the acid in this configuration and its required concentration are as follows.
ａ、塩酸；還元用金属粉末の残分および同金属粉末酸化
物の溶解に役立つ。この作用効果を確実にするためには
、混酸中の塩酸濃度が５ ｒｔｔｏ（１／ Ｑ以上であ
ることを必要とし、この下限以下の濃度では水酸化タン
タルを化成しやすくなり、酸素濃度が低下しにくい。a. Hydrochloric acid; useful for dissolving the residue of the reducing metal powder and the oxide of the same metal powder. In order to ensure this effect, the concentration of hydrochloric acid in the mixed acid must be 5 rtto (1/Q or more), and if the concentration is below this lower limit, tantalum hydroxide will be easily formed and the oxygen concentration will decrease. It's hard to do.
ｂ、硝酸；還元用金属粉末の残分と酸との反応によって
生じた発生期の水素（水素イオン）を酸化する作用を有
し、タンタル中への水素の移動を防ぐ。混酸中の硝酸濃
度が０．１３ＩＯρ／ρ未満では酸化力が弱く、水素除
去作用が不充分である。b. Nitric acid; has the effect of oxidizing nascent hydrogen (hydrogen ions) produced by the reaction between the residue of the reducing metal powder and the acid, and prevents hydrogen from moving into tantalum. If the nitric acid concentration in the mixed acid is less than 0.13IOρ/ρ, the oxidizing power is weak and the hydrogen removal effect is insufficient.
本発明の実験によれば、ＮＯ，の発生
が確認されているところから、次の反応■、■の生起が
確実と考えられる。According to the experiments of the present invention, since the generation of NO was confirmed, it is considered that the following reactions (1) and (2) occur with certainty.
Ｍｇ＋ ２ ＨＣＱ−ＭｇＣｉ２ｔ＋ ２ Ｈ・・・・
■Ｊ−１＋ ＩＩ Ｎ Ｏ、→ 夏−１ｖ Ｏ
＋ Ｎ Ｏｔ ・ ・ ・ ・ ・ ・■また、逆
に混酸中の硝酸濃度か６．５肋ρ／１２を越えろと、酸
化力が強くなり、金属を酸化してタンタル中の酸素濃度
を高め、脱酸効果が低下するので好ましくない。Mg+ 2 HCQ-MgCi2t+ 2 H...
■J-1+ II N O, → Summer-1v O
＋ NOt ・ ・ ・ ・ ・ ・■On the other hand, if the nitric acid concentration in the mixed acid exceeds 6.5 ρ/12, the oxidizing power becomes stronger, oxidizing the metal and increasing the oxygen concentration in tantalum. This is not preferred because the deoxidizing effect decreases.
Ｃ、フッ酸；タンタル粒子表面の酸化タンタル層を溶解
除去してタンタル粉末の酸素濃度の低下に貢献する。し
かし、このフッ酸は、混酸中のの濃度が３．Ｏｉ＋ｏ１
２／（２を越えると、タンタル粉末中の水素濃度が増大
するので、３゜０ｘｏＱ／Ｑ以下で混合する必要がある
。C, hydrofluoric acid; dissolves and removes the tantalum oxide layer on the surface of the tantalum particles, contributing to lowering the oxygen concentration of the tantalum powder. However, this hydrofluoric acid has a concentration of 3. Oi+o1
2/(If it exceeds 2, the hydrogen concentration in the tantalum powder will increase, so it is necessary to mix at 3°0xoQ/Q or less.
そして、前記各酸からなる混酸中の全酸濃度は１０ｘｏ
１２／ｇ以上であることが望ましい。というのは、全酸
濃度が１Ｏｘｏ１２／（２より低下すると、下記反応が
平行して生起し、水酸イオンが化成しやすくなるからで
ある。The total acid concentration in the mixed acid consisting of each of the above acids is 10xo
It is desirable that it is 12/g or more. This is because when the total acid concentration is lower than 1Oxo12/(2), the following reactions occur in parallel, and hydroxyl ions are easily formed.
ＭｇＯ＋２Ｈ（ｄ！−４ＭｇＣ（ｌｔ＋ＨｔＯ−−−−
■ＭｇＯ＋Ｈｔｏ−Ｍｇ（ＯＨ）ｔ・・・・・自・・・
■つまり、反応■の終了前に塩酸濃度が不足すると、反
応■が生起し、水酸イオンがＴａと反応して水酸化タン
タルを化成し、酸素を取り込む結果となる。■の反応を
確実に抑制するには混酸の全酸濃度は１０ｍｏｆ２／Ｑ
以上であることが好ましい。MgO+2H(d!-4MgC(lt+HtO----
■MgO+Hto-Mg(OH)t...Self...
(2) That is, if the concentration of hydrochloric acid is insufficient before the completion of reaction (2), reaction (2) occurs, and hydroxide ions react with Ta to form tantalum hydroxide, resulting in the uptake of oxygen. To reliably suppress the reaction (①), the total acid concentration of the mixed acid is 10mof2/Q.
It is preferable that it is above.
本発明は、特定濃度の塩酸と硝酸との混酸が本発明の目
的を達成するのにはなはだ有効である点に特徴があるか
、これにさらに特定濃度のフッ酸を添加することにより
その効果を一層向上させ、確実なものとするものである
。The present invention is characterized in that a mixed acid of hydrochloric acid and nitric acid at a specific concentration is extremely effective in achieving the object of the present invention, or by adding hydrofluoric acid at a specific concentration to this mixed acid, the effect can be improved. This will further improve and make it more reliable.
以下、この発明を実施例によりさらに詳しく説明する。Hereinafter, this invention will be explained in more detail with reference to Examples.
「実施例」
フッ化タンタル酸カリウムをＮａで還元して得られた金
属タンタル粉末を真空中にて熱処理してできたスボンノ
状のタンタル塊を〜２５０μし６０メツシユ）に粉砕し
た粉末で、以下の特性のものを使用した。"Example" A tantalum metal powder obtained by reducing potassium fluorotantalate with Na is heat-treated in a vacuum, and a tantalum-shaped lump of tantalum is pulverized to ~250μ and 60 meshes.The following powders are used. A material with the following characteristics was used.
・比表面積（透過法による）・・・・・１８００ｃｌｔ
／ ｇこの粉末を５重量％のＭｇ粉と混合し、不活性雰
囲気（Ａｒガス）中、８００℃で、２時間加熱してＭｇ
によりタンタル中の酸素の除去処理を行なった。・Specific surface area (by transmission method)...1800clt
/g This powder was mixed with 5% by weight Mg powder and heated at 800°C for 2 hours in an inert atmosphere (Ar gas) to convert Mg.
Oxygen in tantalum was removed using the following method.
この反応の結果、生じたタンタル表面のマグネシウム酸
化物および残留マグネシウムを各種の酸洗条件（本発明
；ｌ〜１０、比較例；１１〜１８）で溶解除去した。酸
洗後の粉末は中和処理、水洗の後、乾燥して分析した。As a result of this reaction, the resulting magnesium oxide and residual magnesium on the tantalum surface were dissolved and removed under various pickling conditions (invention; 1 to 10; comparative example; 11 to 18). The powder after pickling was neutralized, washed with water, dried, and analyzed.
酸洗条件および得られた金属タンタル粉末の分析値を表
１に示した。Table 1 shows the pickling conditions and the analytical values of the obtained tantalum metal powder.
表から明らかなように、本発明の精製法によれば、金属
タンタル粉末中の酸素濃度、水素濃度を同時に低下させ
、かつ還元用金属の除去も充分に達成し得ることが認め
られる。As is clear from the table, it is recognized that according to the refining method of the present invention, it is possible to simultaneously reduce the oxygen concentration and hydrogen concentration in the tantalum metal powder, and to sufficiently remove the reducing metal.
（以下、余白）
［表１コ
「発明の効果」
以上説明したように、この発明に係る金属タンタル粉末
の精製方法は、金属タンタル粉末と還元用金属粉末の混
合物を不活性雰囲気中または真空中において加熱処理し
、次いで生成物を酸処理する工程を含む金属タンタル粉
末の精製方法において、前記酸処理を塩酸と硝酸との混
酸により行なうことを特徴とするものであり、また前記
酸処理を塩酸と硝酸とフッ酸との混酸により行なうこと
を特徴とするものである。(Hereinafter, blank space) [Table 1 "Effects of the Invention" As explained above, the method for refining tantalum metal powder according to the present invention is to process a mixture of tantalum metal powder and reducing metal powder in an inert atmosphere or in a vacuum. A method for purifying tantalum metal powder, which includes a step of heat-treating the powder and then treating the product with an acid, characterized in that the acid treatment is carried out with a mixed acid of hydrochloric acid and nitric acid; The method is characterized in that it is carried out using a mixed acid of nitric acid and hydrofluoric acid.
そして、この発明によれば、金属タンタル粉末中の酸化
物に基づく酸素濃度を２０００ｐｐｍ以下、水素６度を
１１００ｐｐ以下、かつ還元用金属の残留量を５ ｐｐ
ｍ未満とすることができ、電解コンデンサー製造に好適
な金属タンタル粉末を容易に提供することができる。According to the present invention, the oxygen concentration based on the oxide in the metal tantalum powder is 2000 ppm or less, the hydrogen 6 degree is 1100 pp or less, and the residual amount of reducing metal is 5 ppm.
It is possible to easily provide tantalum metal powder suitable for manufacturing electrolytic capacitors.
第１図は、金属タンタル粉末中の水素濃度と、同金属タ
ンタル圧扮成形体の強度との関係を示すグラフである。FIG. 1 is a graph showing the relationship between the hydrogen concentration in the tantalum metal powder and the strength of the pressed tantalum metal powder.
Claims (4)
活性雰囲気中または真空中において加熱処理し、次いで
生成物を酸処理する工程を含む金属タンタル粉末の精製
方法において、 前記酸処理を塩酸と硝酸との混酸により行なうことを特
徴とする金属タンタル粉末の精製方法。(1) A method for purifying a tantalum metal powder, which includes a step of heat-treating a mixture of a tantalum metal powder and a reducing metal powder in an inert atmosphere or in a vacuum, and then treating the product with an acid, wherein the acid treatment is performed with hydrochloric acid. A method for refining tantalum metal powder, characterized by carrying out the purification using a mixed acid with nitric acid.
混酸中の組成割合が塩酸５ｍｏｌ／ｌ以上、硝酸０．１
３〜６．５ｍｏｌ／ｌであることを特徴とする特許請求
の範囲第１項に記載の金属タンタル粉末の精製方法。(2) The total acid concentration of the mixed acid is 10 mol/l or more, and the composition ratio in the mixed acid is 5 mol/l or more of hydrochloric acid and 0.1 nitric acid.
The method for refining tantalum metal powder according to claim 1, characterized in that the concentration is 3 to 6.5 mol/l.
不活性雰囲気中または真空中において加熱処理し、次い
で生成物を酸処理する工程を含む金属タンタル粉末の精
製方法において、 前記酸処理を塩酸と硝酸とフッ酸との混酸により行なう
ことを特徴とする金属タンタル粉末の精製方法。(3) A method for purifying a tantalum metal powder, which includes a step of heat-treating a mixture of a tantalum metal powder and a reducing metal powder in an inert atmosphere or in a vacuum, and then treating the product with an acid, wherein the acid treatment is performed with hydrochloric acid. A method for refining tantalum metal powder, characterized in that it is carried out using a mixed acid of nitric acid and hydrofluoric acid.
混酸中の組成割合が塩酸５ｍｏｌ／ｌ以上、硝酸０．１
３〜６．５ｍｏｌ／ｌ、フッ酸３．０ｍｏｌ／ｌ以下で
あることを特徴とする特許請求の範囲第３項に記載の金
属タンタル粉末の精製方法。(4) The total acid concentration of the mixed acid is 10 mol/l or more, and the composition ratio in the mixed acid is 5 mol/l or more of hydrochloric acid and 0.1 nitric acid.
The method for refining tantalum metal powder according to claim 3, characterized in that the content of tantalum powder is 3 to 6.5 mol/l, and the content of hydrofluoric acid is 3.0 mol/l or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61089646A JPS62247001A (en) | 1986-04-18 | 1986-04-18 | Refining method for metallic tantalum powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61089646A JPS62247001A (en) | 1986-04-18 | 1986-04-18 | Refining method for metallic tantalum powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62247001A true JPS62247001A (en) | 1987-10-28 |
| JPH0233761B2 JPH0233761B2 (en) | 1990-07-30 |
Family
ID=13976532
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61089646A Granted JPS62247001A (en) | 1986-04-18 | 1986-04-18 | Refining method for metallic tantalum powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62247001A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04362102A (en) * | 1991-06-06 | 1992-12-15 | Showa Kiyabotsuto Suupaa Metal Kk | Production of tantalum powder |
| JP2000038662A (en) * | 1998-07-24 | 2000-02-08 | Tosoh Corp | Sputtering target |
| JP2021001394A (en) * | 2019-06-21 | 2021-01-07 | 住友金属鉱山株式会社 | Method for producing metal cadmium |
-
1986
- 1986-04-18 JP JP61089646A patent/JPS62247001A/en active Granted
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04362102A (en) * | 1991-06-06 | 1992-12-15 | Showa Kiyabotsuto Suupaa Metal Kk | Production of tantalum powder |
| JP2000038662A (en) * | 1998-07-24 | 2000-02-08 | Tosoh Corp | Sputtering target |
| JP2021001394A (en) * | 2019-06-21 | 2021-01-07 | 住友金属鉱山株式会社 | Method for producing metal cadmium |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0233761B2 (en) | 1990-07-30 |
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