JPH101729A - Method for refining tantalum - Google Patents
Method for refining tantalumInfo
- Publication number
- JPH101729A JPH101729A JP17424296A JP17424296A JPH101729A JP H101729 A JPH101729 A JP H101729A JP 17424296 A JP17424296 A JP 17424296A JP 17424296 A JP17424296 A JP 17424296A JP H101729 A JPH101729 A JP H101729A
- Authority
- JP
- Japan
- Prior art keywords
- tantalum
- powder
- sintered body
- carbon
- tantalum powder
- 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.)
- Pending
Links
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims description 8
- 238000007670 refining Methods 0.000 title 1
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims abstract description 40
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 34
- 239000001569 carbon dioxide Substances 0.000 abstract description 17
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 17
- 239000000843 powder Substances 0.000 abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052799 carbon Inorganic materials 0.000 abstract description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 8
- 239000011734 sodium Substances 0.000 abstract description 8
- 229910052708 sodium Inorganic materials 0.000 abstract description 8
- 238000010438 heat treatment Methods 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 abstract description 4
- 238000011282 treatment Methods 0.000 abstract description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011591 potassium Substances 0.000 abstract description 3
- 229910052700 potassium Inorganic materials 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 26
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 9
- 239000003990 capacitor Substances 0.000 description 7
- 239000001488 sodium phosphate Substances 0.000 description 7
- 229910000162 sodium phosphate Inorganic materials 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 235000003270 potassium fluoride Nutrition 0.000 description 6
- 239000011698 potassium fluoride Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ROSDCCJGGBNDNL-UHFFFAOYSA-N [Ta].[Pb] Chemical compound [Ta].[Pb] ROSDCCJGGBNDNL-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000001721 transfer moulding Methods 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明はタンタルの精製方法
に関する。[0001] The present invention relates to a method for purifying tantalum.
【０００２】[0002]
【従来の技術】固体電解コンデンサ等に用いるタンタル
粉末は、例えばフッ化タンタル酸カリウム等のフッ化物
を原料として製造している。すなわち、先ず、フッ化タ
ンタル酸カリウム等を高温下でナトリウムと還元反応さ
せて金属タンタルを析出させ、酸と水とにより順次洗浄
し、乾燥する。その後、リン酸ナトリウムやホウ酸を少
量、均一に混合し、０．１Ｐａ以下程度の真空中で約１
５００℃に加熱し、次に冷却し、さらに凝集塊を細かく
くだく。この処理により、その後に熱処理をしても微粉
末が粒成長したり、比表面積が低下するのを防止する。
そして凝集塊を細かくくだいた後、水洗したり、あるい
はフッ酸と硝酸の混酸及び水により洗浄し、その後に乾
燥して、粉末表面に付着した物質を除去する。2. Description of the Related Art Tantalum powder used for a solid electrolytic capacitor and the like is manufactured using a fluoride such as potassium fluoride tantalate as a raw material. That is, first, potassium fluoride tantalate or the like is subjected to a reduction reaction with sodium at a high temperature to precipitate metal tantalum, which is sequentially washed with an acid and water, and dried. Thereafter, a small amount of sodium phosphate or boric acid is uniformly mixed, and about 1 Pa or less in a vacuum of about 0.1 Pa or less.
Heat to 500 ° C., then cool, and break up clumps. This treatment prevents the fine powder from growing as a grain and reducing the specific surface area even after the heat treatment.
Then, the aggregates are finely crushed, washed with water, or washed with a mixed acid of hydrofluoric acid and nitric acid and water, and then dried to remove a substance attached to the powder surface.
【０００３】[0003]
【発明が解決しようとする課題】しかし、従来の方法で
製造したタンタル粉末は表面に酸化物等の不純物が除去
されずに付着している欠点がある。また、タンタル粉末
を形成した後に、空気中の酸素によりさらにタンタル粉
末の表面に酸化物等が付着する欠点がある。さらに、こ
のようなタンタル粉末を用いて形成した燒結体にも酸化
物等の不純物が残る欠点がある。そしてタンタル粉末や
その燒結体に酸化物等の状態で酸素を含んでいると、そ
の酸素量が多いほど固体電解コンデンサの漏れ電流等が
増加する。However, the tantalum powder produced by the conventional method has a disadvantage that impurities such as oxides are adhered to the surface without being removed. Further, there is a disadvantage that after the tantalum powder is formed, oxides and the like further adhere to the surface of the tantalum powder due to oxygen in the air. Further, the sintered body formed by using such a tantalum powder has a disadvantage that impurities such as oxides remain. If tantalum powder or its sintered body contains oxygen in the form of an oxide or the like, the greater the amount of oxygen, the greater the leakage current of the solid electrolytic capacitor.
【０００４】本発明は、以上の欠点を改良し、酸化物等
の不純物を除去できるタンタルの精製方法を提供するこ
とを課題とするものである。An object of the present invention is to provide a method for purifying tantalum which can improve the above disadvantages and remove impurities such as oxides.
【０００５】[0005]
【課題を解決するための手段】本発明は、以上の課題を
解決するために、タンタルの粉末又はその焼結体を四塩
化炭素を含む雰囲気中に晒すことを特徴とするタンタル
の精製方法を提供するものである。In order to solve the above problems, the present invention provides a method for purifying tantalum, comprising exposing a tantalum powder or a sintered body thereof to an atmosphere containing carbon tetrachloride. To provide.
【０００６】本発明によれば、タンタル粉末やこのタン
タル粉末を焼結して焼結体を形成した後に、四塩化炭素
を含む雰囲気中に晒しているため、タンタル粉末やその
焼結体の表面等に付着している酸化物や酸素が、四塩化
炭素と反応し、酸素を炭素ガスや一酸化炭素として分離
する。これにより、タンタル粉末等の表面等に付着して
いる酸化物や酸素を除去できる。According to the present invention, since the tantalum powder and the sintered tantalum powder are sintered to form a sintered body and then exposed to an atmosphere containing carbon tetrachloride, the surface of the tantalum powder and the sintered body thereof is Oxide and oxygen adhering to the like react with carbon tetrachloride and separate oxygen as carbon gas or carbon monoxide. Thereby, oxides and oxygen adhering to the surface of the tantalum powder or the like can be removed.
【０００７】[0007]
【発明の実施の形態】以下、本発明の実施の形態を説明
する。先ず、フッ化タンタル酸カリウム等のフッ化物等
を高温下でナトリウムと還元反応させ、必要に応じてさ
らに、リン酸ナトリウムやホウ酸を均一に混合する等の
処理をしてタンタル粉末を製造する。Embodiments of the present invention will be described below. First, a fluoride or the like such as potassium fluoride tantalate is subjected to a reduction reaction with sodium at a high temperature, and if necessary, a treatment such as uniformly mixing sodium phosphate or boric acid is performed to produce a tantalum powder. .
【０００８】そしてこのタンタル粉末やその焼結体を四
塩化炭素を含む雰囲気中に晒す。この処理は、例えば、
次の通りに行なう。すなわち、真空加熱炉中にタンタル
粉末やその焼結体を配置する。そしてこの炉の内部を減
圧状態にした後、炉内に炭素ガスを注入しながら四塩化
炭素のガスを炉内に注入する。その後、炭酸ガスや一酸
化炭素を含む炭酸ガスを炉内に注入し、所定時間後にそ
の状態で冷却する。これ等の処理によりタンタル粉末や
その焼結体の表面等の付着している酸化物等を除去す
る。なお、タンタル粉末等の表面等に付着している酸化
物等を除去するには、四塩化炭素と反応させればよい
が、炭酸ガス等を併せて用いることにより、効率的に酸
化物等を除去できる。[0008] The tantalum powder and its sintered body are exposed to an atmosphere containing carbon tetrachloride. This process, for example,
Perform as follows. That is, tantalum powder and its sintered body are arranged in a vacuum heating furnace. Then, after the inside of the furnace is depressurized, carbon tetrachloride gas is injected into the furnace while carbon gas is injected into the furnace. Thereafter, carbon dioxide gas including carbon dioxide gas or carbon monoxide is injected into the furnace, and after a predetermined period of time, cooled in that state. By these treatments, attached oxides and the like on the surface of the tantalum powder and the sintered body thereof are removed. In addition, in order to remove oxides and the like adhering to the surface and the like of tantalum powder and the like, it is sufficient to react with carbon tetrachloride. Can be removed.
【０００９】[0009]
【実施例】以下、本発明の実施例を説明する。 実施例１：タンタル粉末は、フッ化タンタル酸カリウム
をナトリウムにより還元して得た、ＣＶ値５０ｍＦＶ／
ｇのものを用いる。そしてこのタンタル粉末を管状真空
加熱炉中に設置し、炉内を０．１１Ｐａに減圧する。減
圧後、炉内に炭酸ガスを注入し、大気圧にして加熱す
る。さらに、炭酸ガスを温度７５℃の四塩化炭素の液中
に通し、出てきた炭酸ガスと四塩化炭素のガスとの混合
ガスを炉内に注入する。この状態で温度７００℃で３０
分間保持する。この後、炭酸ガスのみを炉内に注入し、
常温まで冷却してタンタル粉末を精製する。Embodiments of the present invention will be described below. Example 1: Tantalum powder was obtained by reducing potassium fluoride tantalate with sodium, and had a CV value of 50 mFV /
g. Then, the tantalum powder is placed in a tubular vacuum heating furnace, and the pressure in the furnace is reduced to 0.11 Pa. After the pressure reduction, carbon dioxide gas is injected into the furnace, and the furnace is heated to atmospheric pressure. Further, carbon dioxide gas is passed through a liquid of carbon tetrachloride at a temperature of 75 ° C., and a mixed gas of the carbon dioxide gas and the carbon tetrachloride gas is injected into the furnace. In this state, it is 30
Hold for a minute. After this, only carbon dioxide gas is injected into the furnace,
Cool to room temperature to purify the tantalum powder.
【００１０】実施例２：フッ化タンタル酸カリウムをナ
トリウムにより還元して得た、ＣＶ値が５０ｍＦＶ／ｇ
の粉末に、約７０ｐｐｍのリンに相当するリン酸ナトリ
ウムを添加して均一に混合する。混合した後、０．１Ｐ
ａの真空中において温度１３５０℃にした雰囲気中にこ
のリン酸ナトリウムを添加したタンタル粉末を１時間放
置する。放置後、温度７５℃の四塩化炭素の液中に炭素
ガスを通して生成した炭酸ガスと四塩化炭素のガスとの
混合ガスを炉内に注入しながら、温度７００℃で３０分
間保持する。保持後、炭酸ガスのみを流しながら常温ま
で冷却する。冷却後、得られたタンタル粉末の凝集塊を
こまかくし、６０メッシュのふるいにかけて通過するも
のを選択する。次に、マグネシウムをゲッターとして
０．１Ｐａ以下の真空中で、温度７５０℃にした雰囲気
中に、この６０メッシュのふるいを通した粉末を１時間
放置する。放置後、常温まで冷却する。冷却後、酸と水
とにより洗浄し、乾燥して、タンタル粉末を精製する。Example 2 CV value obtained by reducing potassium fluorotantalate with sodium was 50 mFV / g.
, A sodium phosphate corresponding to about 70 ppm of phosphorus is added and uniformly mixed. After mixing, 0.1P
The tantalum powder to which the sodium phosphate has been added is left for 1 hour in an atmosphere at a temperature of 1350 ° C. in the vacuum of a. After the standing, the mixture is maintained at a temperature of 700 ° C. for 30 minutes while a mixed gas of carbon dioxide and carbon tetrachloride gas generated by passing carbon gas through a liquid of carbon tetrachloride at a temperature of 75 ° C. is injected into the furnace. After the holding, the mixture is cooled to room temperature while flowing only carbon dioxide gas. After cooling, the resulting agglomerates of tantalum powder are finely ground and those that pass through a 60 mesh sieve are selected. Next, the powder passed through the 60-mesh sieve is left for 1 hour in an atmosphere of 750 ° C. in a vacuum of 0.1 Pa or less using magnesium as a getter. After standing, cool to room temperature. After cooling, it is washed with an acid and water and dried to purify the tantalum powder.
【００１１】実施例３：フッ化タンタル酸カリウムをナ
トリウムにより還元して得た、ＣＶ値５０ｍＦＶ／ｇの
粉末に、約７０ｐｐｍのリンに相当するリン酸ナトリウ
ムを添加して均一に混合する。混合した後、０．１Ｐａ
の真空中において温度１３５０℃にした雰囲気中に１時
間放置する。放置後、得られたタンタル粉末の凝集塊を
こまかくし、６０メッシュのふるいにかけて通過するも
のを選択する。次に、硝酸と、フッ酸と、水との混合液
（容積比４０：５：５５）中に入れて、十分攪拌する。
攪拌後、濾過水洗し、乾燥する。乾燥後、管状真空加熱
炉中に設置し０．１１Ｐａに減圧する。減圧後、炉内に
炭酸ガスを注入し、大気圧にして加熱する。さらに温度
７５℃の四塩化炭素の液中に炭素ガスを通して生成した
炭酸ガスと四塩化炭素のガスとの混合ガスを炉内に注入
しながら、温度７００℃で３０分間保持する。保持後、
炭酸ガスのみを流しながら常温まで冷却して、タンタル
粉末を精製する。Example 3 To a powder having a CV value of 50 mFV / g obtained by reducing potassium fluoride tantalate with sodium, about 70 ppm of sodium phosphate corresponding to phosphorus is added and uniformly mixed. After mixing, 0.1 Pa
Is left for 1 hour in an atmosphere of 1350 ° C. in a vacuum. After standing, the obtained agglomerates of the tantalum powder are finely ground, and those that pass through a 60-mesh sieve are selected. Next, the mixture is placed in a mixed solution of nitric acid, hydrofluoric acid and water (volume ratio 40: 5: 55) and stirred sufficiently.
After stirring, the mixture is filtered, washed with water, and dried. After drying, it is placed in a tubular vacuum heating furnace and the pressure is reduced to 0.11 Pa. After the pressure reduction, carbon dioxide gas is injected into the furnace, and the furnace is heated to atmospheric pressure. Furthermore, the mixture is maintained at a temperature of 700 ° C. for 30 minutes while a mixed gas of carbon dioxide gas and carbon tetrachloride gas generated by passing carbon gas into a liquid of carbon tetrachloride at a temperature of 75 ° C. is injected into the furnace. After holding,
Cool to room temperature while flowing only carbon dioxide gas to purify the tantalum powder.
【００１２】実施例４：フッ化タンタル酸カリウムをナ
トリウムにより還元して得たＣＶ値５０ｍＦＶ／ｇの粉
末を、管状真空加熱炉中に設置し０．１１Ｐａに減圧す
る。減圧後、炉内に炭酸ガスを注入し、大気圧にして加
熱する。加熱後、さらに温度７５℃の四塩化炭素の液中
に炭素ガスを通して生成した炭酸ガスと四塩化炭素のガ
スとの混合ガスを炉内に注入しながら、温度７５０℃で
３０分間保持する。保持後、１０％の一酸化炭素を含む
炭酸ガスのみを炉内に流しながら常温まで冷却して、タ
ンタル粉末を精製する。Example 4 A powder having a CV value of 50 mFV / g obtained by reducing potassium fluorotantalate with sodium is placed in a tubular vacuum heating furnace, and the pressure is reduced to 0.11 Pa. After the pressure reduction, carbon dioxide gas is injected into the furnace, and the furnace is heated to atmospheric pressure. After the heating, the mixture is maintained at a temperature of 750 ° C. for 30 minutes while a mixed gas of a carbon dioxide gas and a carbon tetrachloride gas generated by passing a carbon gas into a liquid of carbon tetrachloride at a temperature of 75 ° C. is injected into the furnace. After the holding, the tantalum powder is purified by cooling to room temperature while flowing only carbon dioxide containing 10% of carbon monoxide into the furnace.
【００１３】次に、実施例１〜実施例４のタンタル粉末
について、従来例とともに、不純物含有量及び比容量を
測定し、表１に示した。Next, the tantalum powders of Examples 1 to 4 were measured for impurity content and specific capacity together with the conventional example, and the results are shown in Table 1.
【００１４】なお、従来例のタンタル粉末は、フッ化タ
ンタル酸カリウムをナトリウムにより還元して得た、Ｃ
Ｖ値が５０ｍＦＶ／ｇのタンタル粉末をそのまま用い
る。The tantalum powder of the conventional example is obtained by reducing potassium fluoride tantalate with sodium.
A tantalum powder having a V value of 50 mFV / g is used as it is.
【００１５】[0015]
【表１】 [Table 1]
【００１６】この表１から明らかな通り、実施例１〜実
施例４の方が従来例に比べて、酸素含有量が約５７．８
％〜７０．０％、リンがほぼ同量そしてマグネシウムが
５０％未満〜７０％となる。すなわち、特に、酸素及び
マグネシウムの含有量が少なくなっている。なお、予じ
めリン酸ナトリウムを添加したタンタル粉末を処理した
実施例２及び実施例３の方が、リン酸ナトリウムを添加
しないタンタル粉末を処理した実施例１及び実施例４に
比較して、タンタル粉末中の酸素含有量が少なく、約８
２．５％〜９９．３％になっている。As is apparent from Table 1, the oxygen content of Examples 1 to 4 is about 57.8 compared to the conventional example.
% To 70.0%, about the same amount of phosphorus and less than 50% to 70% of magnesium. That is, the contents of oxygen and magnesium are particularly low. In addition, Examples 2 and 3 in which the tantalum powder to which sodium phosphate was added were treated in advance were compared with Examples 1 and 4 in which the tantalum powder to which sodium phosphate was not added was treated. Low oxygen content in tantalum powder, about 8
2.5% to 99.3%.
【００１７】また、実施例１〜実施例４及び従来例のタ
ンタル粉末を用いて製造した定格１０Ｖ、１０μＦのタ
ンタル固体電解コンデンサについて漏れ電流を測定した
ところ、表２に示す通りの結果が得られた。なお、試料
数は各々５００個とする。そして各タンタル固体電解コ
ンデンサは、タンタル粉末として実施例１〜実施例４及
び従来例のものを用いる以外は同一の条件として、次の
通りに製造する。すなわち、タンタル粉末を、上下パン
チを有する圧粉成形金型のキャビティにタンタル粉末を
１３．５mg充填し、その中に直径０．２５mmのタンタル
製のリード線の一端を入れ、圧縮して、１．０×１．７
×１．１mm角の成形体を形成する。成形後、真空中にお
いて、温度１４３０℃で燒結し、燒結体を形成する。そ
の後、０．１％の硝酸溶液中に燒結体を浸漬し、電圧４
２Ｖで陽極酸化して酸化皮膜を形成する。酸化皮膜を形
成後、硝酸マンガン溶液中に燒結体を浸漬する。浸漬
後、加熱し、さらに再化成する。そして浸漬から再化成
までの工程を繰り返して行い二酸化マンガン層を形成す
る。二酸化マンガン層を形成後、コロイダルカーボン中
に燒結体を浸漬してカーボン層を形成する。カーボン層
を形成後、銀ペースト中に燒結体を浸漬して、銀層を形
成する。銀層を形成後、陽極リード線をリードフレーム
に溶接するとともに、銀層を銀導電性ペーストによりリ
ードフレームに接続する。その後、トランスファーモル
ド法によりエポキシ樹脂からなる外装を形成して、タン
タル固体電解コンデンサとする。The leakage current was measured for the tantalum solid electrolytic capacitors having a rated voltage of 10 V and 10 μF manufactured using the tantalum powders of Examples 1 to 4 and the conventional example. The results shown in Table 2 were obtained. Was. The number of samples is 500 each. Each tantalum solid electrolytic capacitor is manufactured as follows under the same conditions except that the tantalum powder used in Examples 1 to 4 and the conventional example are used. That is, 13.5 mg of tantalum powder is filled into a cavity of a compacting mold having upper and lower punches, and one end of a tantalum lead wire having a diameter of 0.25 mm is put into the cavity and compressed. 0.0 × 1.7
A molded body having a size of 1.1 mm square is formed. After the forming, sintering is performed at a temperature of 1430 ° C. in a vacuum to form a sintered body. Thereafter, the sintered body was immersed in a 0.1% nitric acid solution, and a voltage of 4% was applied.
Anodize at 2V to form an oxide film. After forming the oxide film, the sintered body is immersed in a manganese nitrate solution. After immersion, heat and re-form. Then, the steps from immersion to re-chemical formation are repeated to form a manganese dioxide layer. After forming the manganese dioxide layer, the sintered body is immersed in colloidal carbon to form a carbon layer. After forming the carbon layer, the sintered body is immersed in a silver paste to form a silver layer. After forming the silver layer, the anode lead wire is welded to the lead frame, and the silver layer is connected to the lead frame with a silver conductive paste. Thereafter, an outer package made of an epoxy resin is formed by a transfer molding method to obtain a tantalum solid electrolytic capacitor.
【００１９】[0019]
【表２】 [Table 2]
【００２０】この表２から明らかな通り、タンタル固体
電解コンデンサの漏れ電流は、実施例１〜実施例４のタ
ンタル粉末を用いた方が従来例のそれを用いた方より
も、最大値が約４１．７％〜６６．７％にそして平均値
が約２８．４％〜５１．４％に低下している。As is apparent from Table 2, the maximum value of the leakage current of the tantalum solid electrolytic capacitor is about the maximum in the case of using the tantalum powder of Examples 1 to 4 as compared with that of the conventional example. It has fallen from 41.7% to 66.7% and the average has dropped to about 28.4% to 51.4%.
【００２０】[0020]
【発明の効果】以上の通り、本発明の精製方法によれ
ば、タンタル粉末又はその焼結体を四塩化炭素を含む雰
囲気中に晒しているため、酸化物等の不純物を減少で
き、タンタル固体電解コンデンサの漏れ電流特性等を改
良できるタンタル粉末やその燒結体からなるタンタルが
得られる。As described above, according to the purification method of the present invention, since the tantalum powder or its sintered body is exposed to the atmosphere containing carbon tetrachloride, impurities such as oxides can be reduced, and the tantalum solid can be reduced. It is possible to obtain tantalum made of a tantalum powder or a sintered body thereof that can improve the leakage current characteristics and the like of the electrolytic capacitor.
Claims (1)
炭素を含む雰囲気中に晒すことを特徴とするタンタルの
精製方法。1. A method for purifying tantalum, comprising exposing a tantalum powder or a sintered body thereof to an atmosphere containing carbon tetrachloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17424296A JPH101729A (en) | 1996-06-13 | 1996-06-13 | Method for refining tantalum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17424296A JPH101729A (en) | 1996-06-13 | 1996-06-13 | Method for refining tantalum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH101729A true JPH101729A (en) | 1998-01-06 |
Family
ID=15975208
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17424296A Pending JPH101729A (en) | 1996-06-13 | 1996-06-13 | Method for refining tantalum |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH101729A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100448585B1 (en) * | 2002-01-09 | 2004-09-13 | 파츠닉(주) | Removing apparatus of binder for tantal capacitor |
-
1996
- 1996-06-13 JP JP17424296A patent/JPH101729A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100448585B1 (en) * | 2002-01-09 | 2004-09-13 | 파츠닉(주) | Removing apparatus of binder for tantal capacitor |
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