JP4596541B2 - Anode body for solid electrolytic capacitor and solid electrolytic capacitor - Google Patents
Anode body for solid electrolytic capacitor and solid electrolytic capacitor Download PDFInfo
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- JP4596541B2 JP4596541B2 JP2005273823A JP2005273823A JP4596541B2 JP 4596541 B2 JP4596541 B2 JP 4596541B2 JP 2005273823 A JP2005273823 A JP 2005273823A JP 2005273823 A JP2005273823 A JP 2005273823A JP 4596541 B2 JP4596541 B2 JP 4596541B2
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- 239000003990 capacitor Substances 0.000 title claims description 37
- 239000007787 solid Substances 0.000 title claims description 34
- 239000000843 powder Substances 0.000 claims description 33
- 229910052751 metal Inorganic materials 0.000 claims description 26
- 239000002184 metal Substances 0.000 claims description 26
- 230000009471 action Effects 0.000 claims description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 9
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims description 4
- 239000007784 solid electrolyte Substances 0.000 claims description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 31
- 239000002245 particle Substances 0.000 description 8
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
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- 238000000034 method Methods 0.000 description 4
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- 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 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 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 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 230000003252 repetitive effect Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
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- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003792 electrolyte Substances 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
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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Description
本発明は、タンタル、ニオブなどの弁作用金属を用いた固体電解コンデンサ用陽極体およびこれを用いた固体電解コンデンサに関する。 The present invention relates to an anode body for a solid electrolytic capacitor using a valve metal such as tantalum and niobium, and a solid electrolytic capacitor using the same.
従来から弁作用金属として、タンタル、ニオブを用いた固体電解コンデンサは、小型で静電容量が大きく、周波数特性に優れ、ＣＰＵの電源回路などに広く使用されている。また、携帯型電子機器の発展に伴い、特にチップ型固体電解コンデンサの小型化および大容量化が進行している。この小型化および大容量化を実現するために、固体電解コンデンサ用陽極体を構成する弁作用金属粉末の粒径を小さくすることにより、陽極体を大きくすること無くコンデンサ容量の大容量化を図ってきた。 Conventionally, a solid electrolytic capacitor using tantalum or niobium as a valve metal is small, has a large capacitance, is excellent in frequency characteristics, and is widely used in a power supply circuit of a CPU. In addition, with the development of portable electronic devices, chip-type solid electrolytic capacitors have been reduced in size and capacity. In order to achieve this reduction in size and increase in capacity, the particle size of the valve metal powder constituting the anode body for a solid electrolytic capacitor is reduced to increase the capacity of the capacitor without increasing the anode body. I came.
例えば、弁作用金属粉末であるタンタル粉末は、一般に出発原料であるフッ化タンタル酸カリウムをナトリウムで還元する還元工程、還元によって生じた副生成塩や不純物を除去する酸洗・水洗工程、ガス生成不純物の除去と熱凝集を行う熱処理工程、脱酸を行う脱酸工程を経て、得ることができる。 For example, tantalum powder, which is a valve metal powder, is generally a reduction process in which potassium fluoride tantalate, the starting material, is reduced with sodium, a pickling / water washing process to remove by-product salts and impurities generated by the reduction, and gas generation. It can be obtained through a heat treatment step for removing impurities and thermal aggregation, and a deoxidation step for deoxidation.
また、近年においては、出発原料を五酸化タンタルとして、五酸化タンタルを気体状マグネシウムで還元する還元工程、酸洗・水洗工程、熱処理工程、脱酸工程を経て、得ることができるタンタル粉末が知られている。 In recent years, tantalum pentoxide is used as a starting material, and tantalum powder that can be obtained through a reduction process, a pickling / water washing process, a heat treatment process, and a deoxidation process in which tantalum pentoxide is reduced with gaseous magnesium is known. It has been.
しかし、コンデンサ容量の大容量化を実現するために、弁作用金属の粉末粒径を小さくすると、固体電解コンデンサ用陽極体の強度が低下し、例えばチップ型固体電解コンデンサを基板実装する際のリフローの熱による熱的ストレスや、リフローの熱により外装樹脂の膨張収縮によって生じる機械的ストレスや、陽極体内部の吸湿水が急激に気化することに起こる体積膨張によるストレス等により、電気的特性の劣化を引き起こす。このような問題の改善策として高ＣＶ粉末に凝集粉を添加した改善案が、例えば特許文献１に開示されている。 However, if the powder particle size of the valve action metal is reduced in order to increase the capacity of the capacitor, the strength of the anode body for the solid electrolytic capacitor is reduced. For example, reflow when mounting a chip type solid electrolytic capacitor on a substrate is performed. Deterioration of electrical characteristics due to thermal stress due to heat of the surface, mechanical stress caused by expansion and contraction of the exterior resin due to heat of reflow, and stress due to volume expansion caused by sudden vaporization of the hygroscopic water inside the anode body cause. As an improvement measure for such a problem, for example, Patent Document 1 discloses an improvement plan in which agglomerated powder is added to a high CV powder.
しかしながら、この特許文献１に記載の技術では、凝集粉、あるいは原粉よりＣＶが低い粉末を添加するため、固体電解コンデンサのコンデンサ容量が減少する。原粉が高ＣＶであればその傾向が顕著に現れるため、固体電解コンデンサの小型化および大容量化には不向きである。 However, in the technique described in Patent Document 1, aggregated powder or powder having a CV lower than that of the raw powder is added, so that the capacitance of the solid electrolytic capacitor is reduced. If the raw powder has a high CV, the tendency appears remarkably, so it is not suitable for downsizing and increasing the capacity of the solid electrolytic capacitor.
本発明は、固体電解コンデンサのコンデンサ容量を減少することなく、リフロー時に加わる熱的および機械的ストレスに対する強度に優れる固体電解コンデンサ用陽極体および固体電解コンデンサを提供することを目的とする。 An object of the present invention is to provide a solid electrolytic capacitor anode body and a solid electrolytic capacitor that are excellent in strength against thermal and mechanical stress applied during reflow without reducing the capacitance of the solid electrolytic capacitor.
上記課題を解決するために、本発明の固体電解コンデンサ用陽極体は、弁作用金属粉末を加圧成形し、陽極リード線を植立して成形体を形成し、高温・真空中で焼結した固体電解コンデンサ用陽極体において、前記弁作用金属粉末は、弁作用金属のフッ化物を還元して得られる粉末からなる第１の弁作用金属粉末と、前記第１の弁作用金属粉末と同じ粉末ＣＶを有する弁作用金属の酸化物を還元して得られる粉末からなる第２の弁作用金属粉末を前記第１の弁作用金属粉末重量に対して２０ｗｔ％（重量％）以上４０ｗｔ％（重量％）以下添加、混合したことを特徴とする。 In order to solve the above problems, the anode body for a solid electrolytic capacitor of the present invention is formed by pressure-molding a valve metal powder, planting an anode lead wire to form a molded body, and sintering at high temperature and in vacuum. In the solid electrolytic capacitor anode body, the valve metal powder is the same as the first valve metal powder made of powder obtained by reducing a fluoride of the valve metal and the first valve metal powder. The second valve action metal powder made of a powder obtained by reducing the oxide of the valve action metal having the powder CV is 20 wt% (wt%) or more and 40 wt% (weight) with respect to the weight of the first valve action metal powder. %) The following is added and mixed.
また、本発明の固体電解コンデンサは、前記固体電解コンデンサ用陽極体に、誘電体層、固体電解質層および陰極層を形成し、端子を接続して外装を施したことを特徴とする。 The solid electrolytic capacitor of the present invention is characterized in that a dielectric layer, a solid electrolyte layer, and a cathode layer are formed on the solid electrolytic capacitor anode body, and terminals are connected to provide an exterior.
本発明によれば、固体電解コンデンサ用陽極体の強度を低下させることなくコンデンサ容量の大容量化ができる。さらに固体電解コンデンサの基板実装時における熱的ストレスおよび機械的ストレスによる電気的特性の劣化を抑制することができる。 According to the present invention, the capacity of the capacitor can be increased without reducing the strength of the anode for a solid electrolytic capacitor. Further, it is possible to suppress deterioration of electrical characteristics due to thermal stress and mechanical stress when the solid electrolytic capacitor is mounted on the substrate.
次に、本発明の実施の形態について、タンタルを弁作用金属として用いた場合を、図面を参照して説明する。 Next, a case where tantalum is used as a valve action metal will be described with reference to the drawings for embodiments of the present invention.
図１は、本発明の最良の実施の形態に係る固体電解コンデンサ用陽極体を形成するための製造方法を説明するためのフローチャートである。先ず、フッ化タンタル酸カリウムの金属ナトリウムによる還元で製造されたフッ化物還元タンタル粉末を用意する（Ｓ１１）。また、これとは別に、五酸化タンタルの気体状マグネシウムによる還元で製造された酸化物還元タンタル粉末を用意する（Ｓ１２）。そして、前記酸化物還元タンタル粉末を秤量し、前記フッ化物還元タンタル粉末と混合した混合タンタル粉末を製作した（Ｓ１３）。その後、前記混合タンタル粉末に適当量のバインダを加え調合し乾燥させる（Ｓ１４）。十分に乾燥させた後に成形機にてタンタルワイヤと共に成形を行なう（Ｓ１５）。そして各成形体を真空焼結した（Ｓ１６）。 FIG. 1 is a flowchart for explaining a manufacturing method for forming an anode body for a solid electrolytic capacitor according to the preferred embodiment of the present invention. First, a fluoride-reduced tantalum powder produced by reduction of potassium fluorotantalate with metallic sodium is prepared (S11). Separately, oxide-reduced tantalum powder produced by reduction of tantalum pentoxide with gaseous magnesium is prepared (S12). Then, the oxide-reduced tantalum powder was weighed to produce a mixed tantalum powder mixed with the fluoride-reduced tantalum powder (S13). Thereafter, an appropriate amount of binder is added to the mixed tantalum powder, and the mixture is prepared and dried (S14). After sufficiently drying, molding is performed with a tantalum wire in a molding machine (S15). And each molded object was vacuum-sintered (S16).
フッ化物還元タンタル粉末よりも２〜４倍大きな平均粒径を持つ酸化物還元タンタル粉末を添加することにより粉末粒子間の接触面積を大きくし、陽極体成形時における粉末同士の接合力を高めることができ、これにより陽極体の成形体強度を高めることができる。 By adding oxide-reduced tantalum powder having an average particle size 2-4 times larger than fluoride-reduced tantalum powder, the contact area between the powder particles is increased, and the bonding force between the powders during anode body molding is increased. As a result, the strength of the molded body of the anode body can be increased.
まず、第１の弁作用金属粉末として、平均粒径が０．８５μｍである１００，０００μＦＶ／ｇのフッ化物還元タンタル粉末を使用した。また、これとは別に、第２の弁作用金属粉末として、平均粒径が２．００μｍである１００，０００μＦＶ／ｇの酸化物還元タンタル粉末を用意した。そして、酸化物還元タンタル粉末を表１に示した添加量になるよう秤量し、前記フッ化物還元タンタル粉末と混合した。その後、混合した粉末に適当量のバインダを加え調合し乾燥させ、十分に乾燥させたあと成形機にて陽極リード線となるタンタルワイヤと共に成形し、１２５０℃にて３０分間真空焼結を行い、陽極体を得た。 First, 100,000 μFV / g fluoride-reduced tantalum powder having an average particle diameter of 0.85 μm was used as the first valve action metal powder. Separately, as the second valve action metal powder, an oxide-reduced tantalum powder with an average particle size of 100,000 μFV / g having an average particle diameter of 2.00 μm was prepared. The oxide-reduced tantalum powder was weighed so as to have the addition amount shown in Table 1, and mixed with the fluoride-reduced tantalum powder. Thereafter, an appropriate amount of binder is added to the mixed powder, dried, sufficiently dried, and then molded together with a tantalum wire serving as an anode lead wire in a molding machine, vacuum-sintered at 1250 ° C. for 30 minutes, An anode body was obtained.
前記陽極体を０．６ｗｔ％のリン酸水溶液中に浸漬し、８．２Ｖで２４０分間陽極酸化することにより、酸化皮膜を形成した。 The anode body was immersed in a 0.6 wt% phosphoric acid aqueous solution and anodized at 8.2 V for 240 minutes to form an oxide film.
次いで、硝酸マンガンに浸漬した後、熱分解して、二酸化マンガン層を形成し、カーボンおよび銀ペーストによる陰極層を形成して、従来公知の方法に従い、端子を接続し、外装を施して、定格４Ｖ−１００μＦの固体電解コンデンサを完成させた。 Next, after being immersed in manganese nitrate, pyrolyzed to form a manganese dioxide layer, a cathode layer made of carbon and silver paste is formed, terminals are connected according to a conventionally known method, an exterior is applied, and rated A solid electrolytic capacitor of 4V-100 μF was completed.
図２は、実施例における固体電解コンデンサ用陽極体の模式断面図である。図２に示すとおり、酸化物還元タンタル粉末４の平均粒径がフッ化物還元タンタル粉末３に比べ大きいことから、粉末結合に要する接触面積が大きくなることで、陽極体１の強度が高くなったと考えられる。
FIG. 2 is a schematic cross-sectional view of an anode body for a solid electrolytic capacitor in an example. As shown in FIG. 2, since the average particle size of the oxide-reduced
本発明の効果を確認するため、酸化物還元タンタル粉末の添加量を変えた固体電解コンデンサを作成し、その時のｔａｎδ不良率を比較した。また製作した固体電解コンデンサを２６０℃１０秒保持のリフローの５回繰り返し試験を供して、試験後の漏れ電流の変化量を評価した。評価結果を表１に示す。尚、評価試料は酸化物還元タンタル粉末の添加量を５，１０，２０，３０，４０，５０ｗｔ％の６水準とし、各水準の試料数を１００個とした。表１に示すリフロー５回繰り返し試験後の漏れ電流の変化量および静電容量初期値は、各１００個の試料の平均値である。 In order to confirm the effect of the present invention, solid electrolytic capacitors with different amounts of oxide-reduced tantalum powder were prepared, and the tan δ defect rates at that time were compared. In addition, the manufactured solid electrolytic capacitor was subjected to repetitive five reflow tests at 260 ° C. for 10 seconds to evaluate the amount of change in leakage current after the test. The evaluation results are shown in Table 1. In addition, the evaluation sample made the addition amount of oxide reduction tantalum powder into 6 levels, 5, 10, 20, 30, 40, and 50 wt%, and set the number of samples of each level to 100. The amount of change in leakage current and the initial capacitance value after the five reflow repetitive tests shown in Table 1 are average values of 100 samples each.
表１を参照して、酸化物還元タンタル粉末の添加量が０ｗｔ％から５０ｗｔ％まで漸次増大にするに従って、リフロー５回繰り返し試験後の漏れ電流の変化量は小さくなっていく。しかし、添加量が０ｗｔ％つまり従来の固体電解コンデンサと１０ｗｔ％の固体電解コンデンサの場合は、リフロー５回繰り返し試験後の漏れ電流の変化量がほぼ同等で、他の添加量の固体電解コンデンサに比べ大きいことから、リフローによる熱的および機械的ストレスによる漏れ電流の劣化を効果的に抑制するには、酸化物還元タンタル粉末の添加量を２０ｗｔ％以上にしなければならず、且つ、その添加量が大きいほど効果が大であるといえる。しかし、酸化物還元タンタル粉末の添加量が５０ｗｔ％の場合は、無添加（従来の固体電解コンデンサ）のときに比べ、ｔａｎδの不良率が増大する結果となった。これは、酸化物還元タンタル粉末の１次粒子間が密な結合状態であることから、１次粒子の空孔径が小となるため、電解質である二酸化マンガンの形成が不十分であるため、ｔａｎδが増加したと考えられる。 Referring to Table 1, as the addition amount of the oxide-reduced tantalum powder is gradually increased from 0 wt% to 50 wt%, the amount of change in leakage current after the 5 reflow repeated tests becomes smaller. However, in the case of the addition amount of 0 wt%, that is, the conventional solid electrolytic capacitor and the solid electrolytic capacitor of 10 wt%, the amount of change in the leakage current after the reflow 5 times repeated test is almost the same. In order to effectively suppress the deterioration of leakage current due to thermal and mechanical stress due to reflow, the added amount of oxide-reduced tantalum powder must be 20 wt% or more, and the added amount. The larger the value, the greater the effect. However, when the addition amount of the oxide-reduced tantalum powder was 50 wt%, the defective rate of tan δ increased as compared with the case of no addition (conventional solid electrolytic capacitor). This is because the primary particles of the oxide-reduced tantalum powder are in a tightly bonded state, and the pore size of the primary particles is small, so that the formation of manganese dioxide as an electrolyte is insufficient, and tan δ Is considered to have increased.
また、１２０Ｈｚでの静電容量初期値については、添加量５０ｗｔ％においては二酸化マンガンの形成不良に起因する静電容量初期値の減少が発生するため、酸化物還元タンタル粉末の添加量は４０ｗｔ％以下であることが望ましい。 In addition, with respect to the initial capacitance value at 120 Hz, since the initial capacitance value decreases due to poor formation of manganese dioxide at an addition amount of 50 wt%, the addition amount of the oxide-reduced tantalum powder is 40 wt%. The following is desirable.
以上のことから、酸化物還元タンタル粉末の添加量は、２０〜４０ｗｔ％の範囲であることが望ましい。 From the above, it is desirable that the amount of oxide-reduced tantalum powder added is in the range of 20 to 40 wt%.
以上、本発明を実施するための最良の形態および実施例を説明したが、本発明は、以上の形態に限られるものではなく、本発明の要旨を逸脱しない範囲の設計変更があっても、本発明に含まれる。すなわち、当業者であれば、なし得るであろう各種変形、修正を含むことはもちろんである。 As mentioned above, although the best form and an example for carrying out the present invention were explained, the present invention is not limited to the above form, and even if there is a design change within a range not departing from the gist of the present invention, It is included in the present invention. That is, it goes without saying that various modifications and corrections that can be made by those skilled in the art are included.
１ 陽極体
２ 陽極リード線
３ フッ化物還元タンタル粉末
４ 酸化物還元タンタル粉末
1
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