CN1889213B - Titanium monoxide electrolytic capacitor anode and producing method thereof - Google Patents
Titanium monoxide electrolytic capacitor anode and producing method thereof Download PDFInfo
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- CN1889213B CN1889213B CN200510031766A CN200510031766A CN1889213B CN 1889213 B CN1889213 B CN 1889213B CN 200510031766 A CN200510031766 A CN 200510031766A CN 200510031766 A CN200510031766 A CN 200510031766A CN 1889213 B CN1889213 B CN 1889213B
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- electrolytic capacitor
- titanium monoxide
- anode
- energizing
- valve metal
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Abstract
The invention relates to the pole of the electrolyzing capacitor, especially the positive pole of the electrolyzing capacitor made of titanium oxide or adulterated titanium oxide, and its producing method. Its character is as follow. Oxygen index range of titanium oxide is more than 0.8 and less than 1.2. The adulterant includes valve metal, one or several kinds of low price oxide of valve metal or their alloy and mixture. The adulterant range is between 0 and 50 wt%. The invention decreases the producing cost, ionization energy and the content of low price titanium oxide in the TiO2 oxide film and increases oxidation rate. The positive pole of the electrolyzing capacitor made of it has high stabilization and high specific votume up to 40000 muF .V .g-1-240000 muF .V .g-1. The creepage current is weak and K is 0.1 muA . muF-1 . V-10.005 muA . muF-1 .V-1.
Description
Technical field:
The present invention relates to the electrode of electrolytic capacitor, especially electrolytic capacitor anode and the manufacture method made from titanium monoxide and doping titanium monoxide thereof.
Background technology:
Along with electronics industry, the demand of electrolytic capacitor is increased considerably.The electrolytic capacitor anode material by aluminium-tantalum-niobium-low price niobium oxide etc. in continuous update.Relatively, though the aluminium electrolytic capacitor price is lower, performance can not satisfy the requirement of increasingly stringent from the cost performance aspect; The function admirable of tantalum electrolytic capacitor, but price height have limited its extensive use at civil area; Niobium and low price niobium oxide electrolytic capacitor are in advanced development, also do not have extensive industrialization.
Mainly there is following problem in titanium as electrolytic capacitor anode: (1) titanium anode is the Ti of+4 valencys by the simple substance titanium ionization of 0 valency
4+, its ionization energy is very big, makes oxidation efficiency very low, even oxidation can not be carried out.(2) Ti and TiO
2Between, there is multiple titanium suboxide, as TiO, Ti
2O
3, Tiu
3O
5Deng, make that the anode oxidation membrane of Ti not exclusively is unformed TiO
2, but the mixed membranous layer of multiple titanium suboxide causes TiO
2The decreased performance of oxide-film.
Summary of the invention:
The objective of the invention is to adopt titanium monoxide or doping titanium monoxide is that raw material is made electrolytic capacitor anode, to reduce ionization energy, improves oxidation efficiency, reduces TiO
2Oxidation film layer is the content of titanium oxide at a middle or low price, improves TiO
2The performance of oxide-film.
Titanium monoxide electrolytic capacitor anode of the present invention is characterized in that:
Titanium monoxide oxygen index scope is greater than 0.8, less than 1.2;
The alloy of doping titanium monoxide comprises one or more in valve metal, the valve metal low oxide, or their alloy and mixture; Its doping scope is greater than 0, less than 50wt%;
Valve metal comprises niobium, tantalum, titanium, vanadium, aluminium, zirconium.
The manufacture method of titanium monoxide electrolytic capacitor anode of the present invention mainly comprises batching, compacting, sintering, oxidation technology process, it is characterized in that:
1. the particle mean size of titanium monoxide and various alloys is 0.1 μ m～70 μ m;
2. the pressed density of pressed-powder anode base: 2.0gcm
-3～4.0gcm
-3
3. sintering temperature: 850～1500 ℃, sintering time: 15min～120min, vacuum pressure＜0.1Pa;
4. the liquid of energizing that anode is energized: based on ammonium pentaborate or boric acid+ammonium pentaborate, the voltage Vf:10V～80V that energizes, the temperature of energizing: 10 ℃～90 ℃, energized current density: 15mAg
-1～90mAg
-1, constant voltage time: 〉=1h.
The invention has the advantages that, be that raw material is made electrolytic capacitor anode, its low cost of manufacture with titanium monoxide or doping titanium monoxide; Reduce ionization energy, improved oxygenation efficiency, reduced TiO
2Oxidation film layer is the content of titanium oxide at a middle or low price, the electrolytic capacitor anode stable performance of manufacturing, and the specific volume height reaches 40000 μ FVg
-1～240000 μ FVg
-1, leakage current is little, K is 0.1 μ A μ F
-1V
-10.005 μ A μ F
-1V
-1
Embodiment:
Performance test condition (with reference to standard GB/T 3137-1995)
Method of testing:
Capacity (C), loss (D):
2V direct current biasing+0.5V exchanges (100Hz)
38%H
2SO
4Solution (20 ℃)
Specific volume=CVfm
-1(μ FVg
-1)
Wherein: C-test capacity/μ F
Vf-voltage/the V that energizes
M-anode weight/g
DC leakage current (IL):
70%Vf (voltage of promptly energizing 70%)
The former solution of energizing (20 ℃)
180 second charging interval
K＝IL·C
-1·Vf
-1(μA·μF
-1·V
-1)
Wherein: IL-DC leakage current/μ A
C-test capacity/μ F
Vf-voltage/the V that energizes
Embodiment 1
Make the anode block method, the titanium monoxide powder (TiO1.00) that takes by weighing 100g particle mean size 5.4 μ m is used to make electrolytic capacitor anode, every 125mg, compacting tool set internal diameter: Φ 3.5mm, pressed density: 3.0gcm
-3, sintering temperature: 1150 ℃, sintering time: 30min, vacuum pressure＜0.02Pa.(2) the anode method of energizing, the liquid of energizing: 5% boric acid+1% ammonium pentaborate, the voltage Vf:50V that energizes, the temperature of energizing: 10 ℃, energized current density: 30mAg
-1, constant voltage time: 2h.The anode test result of energizing is listed in table 1.
Embodiment 2
The titanium monoxide powder (TiO0.85) that takes by weighing 100g particle mean size 6.5 μ m is used to make electrolytic capacitor anode, the anode method of energizing: the liquid of energizing: 1% ammonium pentaborate, and the voltage Vf:30V that energizes, the temperature of energizing: 10 ℃, energized current density: 30mAg
-1, constant voltage time: 2h.Compacting, sintering are with embodiment 1, and the anode test result of energizing is listed in table 1.
Embodiment 3
The titanium monoxide powder (TiO1.00) that takes by weighing 100g particle mean size 5.2 μ m is used to make electrolytic capacitor anode.Every 125mg.Anode method: the liquid of energizing: the 0.05%Ba (OH) that energizes
2, the voltage Vf:50V that energizes, the temperature of energizing: 10 ℃, energized current density: 30mAg
-1, constant voltage time: 2h, compacting, sintering condition are with embodiment 1, and the anode test result of energizing is listed in table 1.
Embodiment 4
The titanium monoxide powder (TiO1.00) that takes by weighing 100g particle mean size 5.4 μ m is used to make electrolytic capacitor anode, every 125mg, and sintering temperature: 1000 ℃, sintering time: 30min, vacuum pressure＜0.02Pa.Compacting, the condition of energizing are with embodiment 1, and the anode test result of energizing is listed in table 1.
Embodiment 5
The titanium monoxide powder (TiO1.00) that takes by weighing 100g particle mean size 6.0 μ m is used to make electrolytic capacitor anode, every 125mg, and sintering temperature: 1150 ℃, sintering time: 45min, vacuum pressure＜0.02Pa.Compacting, the condition of energizing are with embodiment 1, and the anode test result of energizing is listed in table 1.
Embodiment 6
The titanium monoxide powder (TiO1.15) that takes by weighing 100g particle mean size 5.6 μ m is used to make electrolytic capacitor anode, every 125mg, pressed density: 2.5gcm
-3, sintering temperature: 1150 ℃, sintering time: 45min, vacuum pressure＜0.02Pa, the liquid of energizing: 1% ammonium pentaborate, the voltage Vf:30V that energizes, the temperature of energizing: 10 ℃, energized current density: 30mAg
-1, constant voltage time: 2h.The anode test result of energizing is listed in table 1.
Embodiment 7
The titanium monoxide powder (TiO1.00) that takes by weighing 100g particle mean size 8.0 μ m is used to make electrolytic capacitor anode, every 125mg, anode method of energizing, the liquid of energizing: 5% boric acid+1% ammonium pentaborate, the voltage Vf:50V that energizes, the temperature of energizing: 10 ℃, energized current density: 15mAg
-1, constant voltage time: 2h.Compacting, sintering condition are with embodiment 1.The anode test result of energizing is listed in table 1.
Embodiment 8
The titanium monoxide powder (TiO1.00) that takes by weighing 100g particle mean size 7.8 μ m is used to make electrolytic capacitor anode, every 125mg, anode method of energizing, the liquid of energizing: 5% boric acid+1% ammonium pentaborate, the voltage Vf:50V that energizes, the temperature of energizing: 10 ℃, energized current density: 75mAg
-1, constant voltage time: 2h.Compacting, sintering condition are with embodiment 1.The anode test result of energizing is listed in table 1.
Embodiment 9
The doping titanium monoxide powder (TiO1.00 is 70wt%, NbO30wt%) that takes by weighing 100g particle mean size 3.8 μ m is used to make electrolytic capacitor anode, every 125mg, and compacting, sintering, the condition of energizing are with embodiment 1.The anode test result of energizing is listed in table 1.
Embodiment 10
The doping titanium monoxide powder (TiO1.00 is 50wt%, NbO50wt%) that takes by weighing 100g particle mean size 2.4 μ m is used to make electrolytic capacitor anode, every 125mg, and compacting, sintering, the condition of energizing are with embodiment 1.The anode test result of energizing is listed in table 1.
The table 1 embodiment anode test result of energizing
| Numbering | TiOX | Alloy | Voltage/V energizes | Specific volume/μ FVg -1 | K value/μ A μ F -1·V -1 |
| Embodiment 1 | 1.00 | 0 | 50 | 139200 | 0.0920 |
| Embodiment 2 | 0.85 | 0 | 30 | 44000 | 0.1313 |
| Embodiment 3 | 1.00 | 0 | 50 | 225000 | 0.1110 |
| Embodiment 4 | 1.00 | 0 | 50 | 114000 | 0.0168 |
| Embodiment 5 | 1.00 | 0 | 50 | 74400 | 0.0142 |
| Numbering | TiOX | Alloy | Voltage/V energizes | Specific volume/μ FVg -1 | K value/μ A μ F -1·V -1 |
| Embodiment 6 | 1.15 | 0 | 30 | 48000 | 0.0433 |
| Embodiment 7 | 1.00 | 0 | 50 | 113600 | 0.0100 |
| Embodiment 8 | 1.00 | 0 | 50 | 133000 | 0.0578 |
| Embodiment 9 | 1.00 | 30％ | 50 | 69600 | 0.0113 |
| Embodiment 10 | 1.00 | 50％ | 50 | 58800 | 0.0060 |
Claims (3)
1. titanium monoxide electrolytic capacitor anode is characterized in that:
Titanium monoxide oxygen index scope is greater than 0.8, less than 1.2;
The alloy of doping titanium monoxide comprises one or more in valve metal, the valve metal low oxide; Its doping scope is greater than 0, less than 50wt%.
2. must ask 1 described titanium monoxide electrolytic capacitor anode according to power, it is characterized in that: described valve metal is niobium, tantalum, titanium, vanadium, aluminium or zirconium.
3. the manufacture method of titanium monoxide electrolytic capacitor anode mainly comprises batching, compacting, sintering, oxidation technology process, it is characterized in that:
1. the particle mean size of titanium monoxide and various alloys is 0.1 μ m～70 μ m; Described alloy comprises one or more in valve metal, the valve metal low oxide;
2. the pressed density of pressed-powder anode base: 2.0gcm
-3～4.0gcm
-3
3. sintering temperature: 850～1500 ℃; Sintering time: 15min～120min, vacuum pressure＜0.1Pa;
4. the liquid of energizing that anode is energized: based on ammonium pentaborate, or based on boric acid and ammonium pentaborate, the voltage Vf:10V～80V that energizes, the temperature of energizing: 10 ℃～90 ℃, energized current density: 15mAg
-1～90mAg
-1, constant voltage time: 〉=1h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200510031766A CN1889213B (en) | 2005-06-27 | 2005-06-27 | Titanium monoxide electrolytic capacitor anode and producing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200510031766A CN1889213B (en) | 2005-06-27 | 2005-06-27 | Titanium monoxide electrolytic capacitor anode and producing method thereof |
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|---|---|
| CN1889213A CN1889213A (en) | 2007-01-03 |
| CN1889213B true CN1889213B (en) | 2010-05-26 |
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|---|---|---|---|
| CN200510031766A Expired - Fee Related CN1889213B (en) | 2005-06-27 | 2005-06-27 | Titanium monoxide electrolytic capacitor anode and producing method thereof |
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| CN101359534B (en) * | 2008-08-18 | 2011-08-03 | 东莞市迈科科技有限公司 | Electrochemical capacitor containing titanium dioxide and method for preparing same |
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|---|---|---|---|---|
| CN1497629A (en) * | 2002-10-03 | 2004-05-19 | ������������ʽ���� | Electrolytic condenser and its manufacturing metod |
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|---|---|---|---|---|
| CN1497629A (en) * | 2002-10-03 | 2004-05-19 | ������������ʽ���� | Electrolytic condenser and its manufacturing metod |
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