CN1045346C - 用作电解质电容器阳极材料的钽粉 - Google Patents
用作电解质电容器阳极材料的钽粉 Download PDFInfo
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000003990 capacitor Substances 0.000 title claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 11
- 239000010405 anode material Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 15
- 238000005979 thermal decomposition reaction Methods 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 10
- 229910052715 tantalum Inorganic materials 0.000 description 10
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- APLLYCDGAWQGRK-UHFFFAOYSA-H potassium;hexafluorotantalum(1-) Chemical compound [F-].[F-].[F-].[F-].[F-].[F-].[K+].[Ta+5] APLLYCDGAWQGRK-UHFFFAOYSA-H 0.000 description 4
- 239000007784 solid electrolyte Substances 0.000 description 4
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- SPAGIJMPHSUYSE-UHFFFAOYSA-N Magnesium peroxide Chemical compound [Mg+2].[O-][O-] SPAGIJMPHSUYSE-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000002048 anodisation reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000000034 method 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
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/052—Sintered electrodes
- H01G9/0525—Powder therefor
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
本发明提供了用作电解质电容器阳极材料的钽粉，包括平均粒径范围为1.0-5.0μm的钽粉，并混有平均粒径范围为10-500nm的钽粉，在前者每100份(重量)中，后者有约1-25份(重量)；一种从钽粉中制得的电解质电容器的阳极体，以及一种装有该种阳极体的电解质电容器。这种钽粉保证即使在低密度下压片并在低温下烧结，也能使钽引线与烧结体的高强度地连接，而且产生的烧结体有高强度，能经受住硝酸镁的热分解温度，使制出的阳极体有优秀的电学性质，特别除了前述性质外还有高的击穿电压(B.D.V.)，也提供了一种从钽粉中制得的阳极体，以及一种使用该阳极体的电解质电容器。
Description
本发明涉及钽粉，特别涉及用作电解质电容器阳极材料的钽粉末，还涉及使用钽粉制得的电解质电容器的阳极体，本发明也涉及有使用该种阳极体的电解质电容器。
在钽固体电容器中使用的钽粉一般通过用金属钠使氟化钽钾(K2TaF7)还原产生：
K2TaF7+5Na[FY2]Ta+2KF+5NaF
将还原制得的刮勺形(spault_like)颗粒的钽粉加以粉碎，用水洗去些副产物的盐类，再用酸洗，干燥，然后热处理。此后，部分所得的粉末进行去氧处理，如用金属镁还原氧组份得到最终产物。
向这样产生的钽粉中加入合适的粘合剂，然后压片，烧结并在烧结体的表面上通过在诸如磷酸水溶液的电解质中的阳极化处理形成五氧化二钽的阳极化薄膜。
然后，通过硝酸镁的热分解，在烧结体表面的阳极化薄膜上形成一层二氧化镁固体电解质层，在固体电解质层上进一步形成一层石墨层和银糊层，然后将产物用树脂封装得固体电解质电容器。作为引线的钽电线和烧结体间的连接强度以及烧结体的本身强度都是制备电解质电容器的重要因素。
更特定的是，当将钽电容器焊接装到基片上时，树脂会由于热应力膨胀和缩小，若钽引线和烧结体之间的连接强度很低，则树脂会剥落。这会导致漏泄电流的增加。
此外，烧结体的强度应足够高，以经受住热应力和气态硝酸的作用，气态硝酸是通过是硝酸镁的热分解使二氧化镁作为固体电解质层沉积时的副产物。
一般来说，通过增加压片时的密度和增加烧结温度可保证在钽引线和烧结体间的强连接，也保证形成有高强度的烧结体。但是，增加压片的密度和增加烧结温度也会使电学性质下降，特别CV(电容)的下降，并且还会使烧结体在硝酸镁溶液中的浸渍发生困难。
因此，本发明的一个目的是提供一种用作电解质电容器阳极材料的钽粉，它即使在低密度下压片并在低温下烧结也能保证钽引线与烧结体的高强度连接，而且产生的烧结体有高强度，能经受住硝酸镁的热分解温度，使制出的阳极体有优秀的电学性质，特别除了前述性质外。阳极体还有高的击穿电压(B.D.V.)，本发明也提供了一种从钽粉中制得的电解质电容器的阳极体，以及一种有阳极体的电解质电容器。
本发明提供了用作电解质电容器阳极材料的钽粉，包括00000平均粒径范围为1.0-5.0μm的钽粉，并混有平均粒径范围为10-500nm的钽粉，在前者每100份重量份数中，后者有约1-25份重量份数。
本发明的另一个方面是提供一种从钽粉中制得的电解质电容器的阳极体，以及一种使用该阳极体的电解质电容器。
本发明中使用的术语“一般钽粉”指如下方法制备的钽粉，即用金属钠还原氟化钽钾制得刮勺形颗粒状的钽粉粉碎。用水除去副产物的盐，然后用酸洗，干燥，进行热处理，最后用，例如金属镁，处理除去氧，所得钽粉的平均粒径范围为1.0-5.0μm，它的特定例子有：高电压/低电容的粉，CV范围为10,000-15,000μFV/g；高电压/中等电容的粉，CV范围为15,000-20,000μFV/g；中等电压/高电容的粉，CV范围为20,000-30,000μFV/g；以及低电压/高电容的粉，CV不少于30,000μFV/g。
用作本发明烧结粘合剂的粒径在毫微米级别的烧结性能很好的钽粉，可以是平均粒径不高于500nm，较好地不高于200nm，最好地在10-150nm的钽粉。这类钽粉产物可通过前述的氟化钽钾用钠金属还原或通过五氯化二钽用氢还原制得。
在本发明中，粒径在nm级别的钽粉(下面称为“纳米钽粉”)的用量范围是：对每100份(重量)一般钽粉，使用1-25份(重量)，较好的是5-15份(重量)。
这种含有纳米钽粉的粉末，其压片密度很低，如4.0-6.0/c.c.，较好地4.5-5.0g/cc，而且可在较低的温度，如1300-1550℃的范围下烧结15-30分钟，这样保证了所得烧结体的充分收缩。另外，所得的烧结体与钽引线的连接很牢，烧结体本身的强度也很高，能经受硝酸镁的热分解温度，其电学性质又足够好，能制成有高击穿电压的阳极体。
本发明将结合下列实施例作更详细的叙述。实施例1
向100份用常规方法制得的中等电压/高电容的粉(CV30000μFV/g)的一般钽粉中加入5或10份用金属钠还原氟化钽钾制成的纳米钽粉(130nm)，所得的混合物在下面所列的条件下压片和烧结，测出所得的阳极体的物理性质和电学性质。
所得的结果综述于下表1和2。
所加入的纳米钽粉的物理性质和压片、烧结和形成阳极体的条件，以及测量条件如下：
纳米钽粉：平均粒径130nm；比表面积(用BET方法测定)2.71m2/g；堆积密度0.68g/cc；氧含量0.9％阳极体-压片条件：
表1：直径3mm；片重0.15g；片的生坯初密度5.0g/cc
表2：直径3mm；片重0.15g；片的生坯初密度4.5g/cc
烧结条件：
表1：1350℃烧结30分钟
表2：1500℃烧结30分钟
形成、测量条件：
表1：CV(电容)、LC(漏泄电流)；0.01％H3PO4，在60℃下形成，在40V形成，在28V测量
B.D.V.(击穿电压)：1.0％H3PO4，在90℃下
表2：CV(电容)、LC(漏泄电流)；0.01％H3PO4，在60℃下形成，在100V形成，在70V测量
B.D.V.(击穿电压)：1.0％H2PO4，在90℃下
表 1加入纳米钽 CV LC B.D.V. S.D. 引线拉力 烧结体粉的百分数 (V) 强度 强度(％) (μFV/g) (μA/g) (g/cc) (kg) (kg)0 48,100 27 107 4.63 4.0 125 49,500 26 114 4.62 4.5 1510 50,500 24 139 4.79 5.0 19
表 2加入纳米钽 CV LC B.D.V. S.D. 引线拉力 烧结体粉的百分数 (V) 强度 强度(％) (μFV/g) (μA/g) (g/cc) (kg) (kg)0 28,300 10 152 5.520 3.5 255 8,400 10 154 5.54 4.0 2510 28,00 11 159 6.15 5.0 34实施例2
向100份用常规方法制得的中等电压/高电容的粉(CV15000μFV/g)的一般钽粉中加入5-10份实施例1中相同的纳米钽粉，所得的混合物在下面所列的条件下压片，烧结，测出所得的阳极体的物理性质和电学性质。所得的结果综述于下表3。压出的片：直径3mm；片重0.3g；片的生坯初密度5.0g/cc1500℃烧结30分钟1.0％H3PO4，在90℃形成；在140V形成；在98V测量B.D.V.：1.0％H3PO4，在90℃下
表 3加入纳米钽 CV LC B.D.V. S.D. 引线拉力 烧结体粉的百分数 (V) 强度 强度(％) (μFV/g) (μA/g) (g/cc) (kg) (kg)0 15,000 4 180 6.08 13.0 575 15,100 4 184 6.46 14.0 7210 14,700 5 190 6.63 15.5 81
从表1-3可见，加入少量纳米钽粉可使烧结密度(S.D.)增加，但不会使CV(电容)和LC(漏泄电流)的值下降，结果，使烧结体和引线间的连接、烧结片的强度和击穿电压都有了改进。
Claims (4)
1.用作电解质电容器阳极材料的钽粉，其特征在于，所述的钽粉包括平均粒径范围为1.0-5.0μm的钽粉，并混有平均粒径范围为10-500nm的钽粉，在前者每100份重量份数中，后者有1-25份重量份数。
2.根据权利要求1所述的钽粉，其特征在于，平均粒径范围为1.0-5.0μm的钽粉选自：高电压/低电容的粉，CV范围为10,000-15,000μFV/g；高电压/中等电容的粉，CV范围为15,000-20,000μFV/g；中等电压/高电容的粉，CV范围为20,000-30,000μFV/g；以及低电压/高电容的粉，CV不小于30,000μFV/g。
3.一种电解质电容器的阳极体，其特征在于，该阳极体通过烧结权利要求1或2所述的钽粉制成。
4.一种电解质电容器，其特征在于，电解电容器的阳极体用权利要求1或2所述的钽粉制成。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23330694A JP3434041B2 (ja) | 1994-09-28 | 1994-09-28 | タンタル粉末及びそれを用いた電解コンデンサ |
| JP233306/94 | 1994-09-28 |
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| Publication Number | Publication Date |
|---|---|
| CN1131803A CN1131803A (zh) | 1996-09-25 |
| CN1045346C true CN1045346C (zh) | 1999-09-29 |
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| CN95116756A Expired - Lifetime CN1045346C (zh) | 1994-09-28 | 1995-09-28 | 用作电解质电容器阳极材料的钽粉 |
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| Country | Link |
|---|---|
| US (1) | US5560761A (zh) |
| JP (1) | JP3434041B2 (zh) |
| CN (1) | CN1045346C (zh) |
| DE (1) | DE19536014C2 (zh) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU6396398A (en) * | 1997-02-19 | 1998-09-09 | H.C. Starck Gmbh & Co. Kg | Tantalum powder, method for producing same powder and sintered anodes obtained from it |
| AU6495398A (en) | 1997-02-19 | 1998-09-09 | H.C. Starck Gmbh & Co. Kg | Tantalum powder, method for producing same powder and sintered anodes obtained from it |
| JP2894326B2 (ja) * | 1997-06-30 | 1999-05-24 | 日本電気株式会社 | タンタル粉末及びそれを用いた固体電解コンデンサ |
| GB2359823A (en) * | 1998-08-28 | 2001-09-05 | Kemet Electronics Corp | Phosphate anodizing electrolyte and its use to prepare capacitors valve metal anodes produced from very fine metal powders |
| US6183618B1 (en) | 1999-02-02 | 2001-02-06 | Kemet Electronics Corporation | Process for treating impregnated electrolytic capacitor anodes |
| JP3871824B2 (ja) | 1999-02-03 | 2007-01-24 | キャボットスーパーメタル株式会社 | 高容量コンデンサー用タンタル粉末 |
| US6235181B1 (en) | 1999-03-10 | 2001-05-22 | Kemet Electronics Corporation | Method of operating process for anodizing valve metals |
| CN100491022C (zh) * | 2000-03-01 | 2009-05-27 | 卡伯特公司 | 氮化的电子管金属及其制造方法 |
| US6436268B1 (en) * | 2000-08-02 | 2002-08-20 | Kemet Electronics Corporation | Non-aqueous electrolytes for anodizing |
| US6267861B1 (en) | 2000-10-02 | 2001-07-31 | Kemet Electronics Corporation | Method of anodizing valve metals |
| GB0622463D0 (en) * | 2006-11-10 | 2006-12-20 | Avx Ltd | Powder modification in the manufacture of solid state capacitor anodes |
| US20100085685A1 (en) * | 2008-10-06 | 2010-04-08 | Avx Corporation | Capacitor Anode Formed From a Powder Containing Coarse Agglomerates and Fine Agglomerates |
| US8619410B2 (en) | 2010-06-23 | 2013-12-31 | Avx Corporation | Solid electrolytic capacitor for use in high voltage applications |
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| CN110234451B (zh) * | 2017-01-17 | 2021-10-15 | 凯米特电子公司 | 改进的线到阳极连接 |
| US11081288B1 (en) | 2018-08-10 | 2021-08-03 | Avx Corporation | Solid electrolytic capacitor having a reduced anomalous charging characteristic |
| US11380492B1 (en) | 2018-12-11 | 2022-07-05 | KYOCERA AVX Components Corporation | Solid electrolytic capacitor |
| US11756742B1 (en) | 2019-12-10 | 2023-09-12 | KYOCERA AVX Components Corporation | Tantalum capacitor with improved leakage current stability at high temperatures |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5211741A (en) * | 1987-11-30 | 1993-05-18 | Cabot Corporation | Flaked tantalum powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3130392C2 (de) * | 1981-07-31 | 1985-10-17 | Hermann C. Starck Berlin, 1000 Berlin | Verfahren zur Herstellung reiner agglomerierter Ventilmetallpulver für Elektrolytkondensatoren, deren Verwendung und Verfahren zur Herstellung von Sinteranoden |
| US4940490A (en) * | 1987-11-30 | 1990-07-10 | Cabot Corporation | Tantalum powder |
| US4957541A (en) * | 1988-11-01 | 1990-09-18 | Nrc, Inc. | Capacitor grade tantalum powder |
| DE4214722C2 (de) * | 1992-05-04 | 1994-08-25 | Starck H C Gmbh Co Kg | Feinteilige Metallpulver |
| US5284531A (en) * | 1992-07-31 | 1994-02-08 | Cabot Corporation | Cylindrical metal fibers made from tantalum, columbium, and alloys thereof |
-
1994
- 1994-09-28 JP JP23330694A patent/JP3434041B2/ja not_active Expired - Lifetime
-
1995
- 1995-09-06 US US08/523,962 patent/US5560761A/en not_active Expired - Lifetime
- 1995-09-27 DE DE19536014A patent/DE19536014C2/de not_active Expired - Lifetime
- 1995-09-28 CN CN95116756A patent/CN1045346C/zh not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5211741A (en) * | 1987-11-30 | 1993-05-18 | Cabot Corporation | Flaked tantalum powder |
Also Published As
| Publication number | Publication date |
|---|---|
| DE19536014C2 (de) | 1998-04-09 |
| JPH0897095A (ja) | 1996-04-12 |
| JP3434041B2 (ja) | 2003-08-04 |
| CN1131803A (zh) | 1996-09-25 |
| US5560761A (en) | 1996-10-01 |
| DE19536014A1 (de) | 1996-04-04 |
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