CN1549286A - Niobium monoxide electrolytic capacitor anode and manufacturing method thereof - Google Patents
Niobium monoxide electrolytic capacitor anode and manufacturing method thereof Download PDFInfo
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- CN1549286A CN1549286A CNA031242952A CN03124295A CN1549286A CN 1549286 A CN1549286 A CN 1549286A CN A031242952 A CNA031242952 A CN A031242952A CN 03124295 A CN03124295 A CN 03124295A CN 1549286 A CN1549286 A CN 1549286A
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- Prior art keywords
- electrolytic capacitor
- columbium monoxide
- capacitor anode
- anode
- columbium
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- BFRGSJVXBIWTCF-UHFFFAOYSA-N niobium monoxide Chemical compound [Nb]=O BFRGSJVXBIWTCF-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000003990 capacitor Substances 0.000 title claims abstract description 61
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000005245 sintering Methods 0.000 claims description 28
- 239000002245 particle Substances 0.000 claims description 13
- 239000010955 niobium Substances 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 11
- 229910052758 niobium Inorganic materials 0.000 claims description 10
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 239000000956 alloy Substances 0.000 claims description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 8
- 229910052715 tantalum Inorganic materials 0.000 claims description 8
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- HFLAMWCKUFHSAZ-UHFFFAOYSA-N niobium dioxide Inorganic materials O=[Nb]=O HFLAMWCKUFHSAZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 description 14
- 101100480488 Rattus norvegicus Taar8c gene Proteins 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910001362 Ta alloys Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- RHDUVDHGVHBHCL-UHFFFAOYSA-N niobium tantalum Chemical compound [Nb].[Ta] RHDUVDHGVHBHCL-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- Powder Metallurgy (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
The invention relates to an electrode of an electrolytic capacitor, in particular to an electrolytic capacitor anode prepared by niobium monoxide or doped niobium monoxide and a manufacturing method thereof. The method is characterized in that: niobium monoxide with the average grain size of 0.1 to 20 mu m or doped niobium monoxide is taken as a raw material, pressed into a blank, sintered in vacuum, and energized by an anode block, wherein the energizing liquid is 0.01 to 0.1 percent of H3PO4Energized voltage Vf: 10V-80V, energized temperature: 10 ℃ to 90 ℃, energizing current density: 10mA · g-1~120mA·g-1Constant pressure time: the time is more than or equal to 0.5h, and the niobium monoxide electrolytic capacitor anode is obtained. The electrolytic capacitor has stable anode performance and high specific volume up to 40000 mu F.V.g-1~200000μF·V·g-1(ii) a The leakage current is as small as K less than 5.0 multiplied by 10-4μA·μF-1·V-1And the requirements of large capacity and miniaturization of the electric appliance are met.
Description
Technical field:
The present invention relates to the electrode of electrolytic capacitor, especially electrolytic capacitor anode and the manufacture method thereof for preparing with columbium monoxide or doping columbium monoxide.
Background technology:
The function admirable of tantalum electrolytic capacitor, but price height, and the performance limitations of common aluminium electrolytic capacitor range of application, can not satisfy the requirement of miniaturization, high speed and the high capacity of electrical equipment such as mobile phone, computer.Because the dielectric film (Nb of niobium electrolytic capacitor
2O
5) dielectric constant be 41, the dielectric film (Ta of tantalum electrolytic capacitor
2O
5) dielectric constant be 27, so niobium electrolytic capacitor than the specific volume height of tantalum electrolytic capacitor, more helps miniaturization, the lightness of element.
Summary of the invention:
The object of the present invention is to provide a kind of electrolytic capacitor anode and manufacture method made from columbium monoxide or doping columbium monoxide thereof.Columbium monoxide electrolytic capacitor anode by manufacturing of the present invention has 40000 μ FVg
-1~200000 μ FVg
-1High specific volume, K<5.0 * 10
-4μ A μ F
-1V
-1Low-leakage current, satisfy the high capacity of electrical equipment, the requirement of miniaturization.
The present invention is that the technical scheme that adopts that achieves the above object is:
Appropriate design electrolytic capacitor anode composition is that columbium monoxide or the doping columbium monoxide of 0.1 μ m~20 μ m is raw material with particle mean size, makes electrolytic capacitor anode.
Alloy is one or more in valve metal, the valve metal low oxide, comprises its alloy and mixture, and its doping scope is greater than 0, less than 80wt%.
Valve metal is niobium, tantalum, titanium, vanadium, aluminium, zirconium etc.
Columbium monoxide electrolytic capacitor anode preparation method, at first the columbium monoxide with columbium monoxide or doping is pressed into base, and its pressed density is 2.7gcm
-3~3.8gcm
-3
Put into vacuum sintering furnace then, vacuum pressure<0.1Pa, with sintering temperature: 1100 ℃~1500 ℃, sintering 10min~120min obtains the electrolytic capacitor anode agglomerate;
Anode block is energized, its liquid of energizing is 0.01%~0.1%H again
3PO
4, voltage V energizes
f: 10V~80V, the temperature of energizing: 10 ℃~90 ℃, energized current density: 10mAg
-1~120mAg
-1, constant voltage time: 〉=0.5h obtains the columbium monoxide electrolytic capacitor anode.
The advantage and the good effect of invention
The invention has the advantages that, be matrix material with the columbium monoxide, significantly suppressed the oxygen in the anode oxide film and spread to matrix, makes the anodic oxidation film properties more stable, thus the electrolytic capacitor anode stable performance of making, and specific volume is up to 40000 μ FVg
-1~200000 μ FVg
-1Leakage current is little, reaches K<5.0 * 10
-4μ A μ F
-1V
-1Also obtained evidence from the test result of table 1.
The table 1 embodiment anode test result of energizing
Numbering | Columbium monoxide content/% | Alloy 1 | Alloy 2 | Voltage/V energizes | Specific volume/μ FV g -1 | K value/μ A μ F -1????·V -1 |
Embodiment 1 | ????100 | ????/ | ??/ | ????50 | ????135000 | ????0.7×10 -4 |
Embodiment 2 | ????79 | ????Nb21% | ??/ | ????50 | ????89500 | ????4.1×10 -4 |
Embodiment 3 | ????79 | ????/ | ??Ta21% | ????50 | ????64500 | ????1.1×10 -4 |
Embodiment 4 | ????80 | ????Nb10% | ??Ta10% | ????50 | ????71000 | ????2.7×10 -4 |
Embodiment 5 | ????70 | ????Nb20% | ??NbO 210% | ????50 | ????95600 | ????1.4×10 -4 |
Numbering | Columbium monoxide content/% | Alloy 1 | Alloy 2 | Voltage/V energizes | Specific volume/μ FV g -1 | K value/μ A μ F -1??·V -1 |
Embodiment 6 | ????80 | ??Ta10% | ??NbO 210% | ????50 | ????98000 | ??2.0×10 -4 |
Embodiment 7 | ????80 | ??Nb19.9% | ??Ti0.1% | ????50 | ????100500 | ??2.5×10 -4 |
Embodiment 8 | ????80 | ??Nb-Ta20% | ??/ | ????50 | ????72000 | ??0.9×10 -4 |
Embodiment 9 | ????100 | ??/ | ??/ | ????30 | ????142000 | ??0.6×10 -4 |
Embodiment 10 | ????79 | ??Nb21% | ??/ | ????30 | ????92600 | ??3.1×10 -4 |
The table 1 anode performance test condition of energizing is carried out with reference to standard GB/T 3137-1995.
Method of testing:
Capacity (C):
2V direct current biasing+0.5V exchanges (100Hz)
38%H
2SO
4Solution (20 ℃)
Specific volume=CV
fM
-1(μ FVg
-1)
Wherein: C-test capacity/μ F
V
f-voltage/V energizes
M-anode weight/g
DC leakage current (I
L):
70%V
f(voltage of promptly energizing 70%)
0.01%H
3PO
4Solution (20 ℃)
180 second charging interval
Wherein: I
L-DC leakage current/μ A
C-test capacity/μ F
V
f-voltage/V energizes
Embodiment:
Embodiment 1
Make the columbium monoxide electrolytic capacitor anode, at first take by weighing the columbium monoxide of 200g granularity 1.0 μ m, be pressed into base by every 200mg, its pressed density is 3.4gcm
-3Put into vacuum furnace then, vacuum pressure<0.02Pa, sintering temperature is 1300 ℃, sintering 20min obtains the electrolytic capacitor anode agglomerate; Anode block is energized, its liquid of energizing is 0.1%H again
3PO
4, voltage V energizes
fBe 50V, the temperature of energizing is 90 ℃, and energized current density is 60mAg
-1, constant voltage time is 2h, obtains the columbium monoxide electrolytic capacitor anode, its test result is listed in table 1.
Embodiment 2
Make the doping columbium monoxide and make electrolytic capacitor anode, at first take by weighing the doping columbium monoxide powder 200g that columbium monoxide 79wt%, niobium 21wt% are mixed into particle mean size 1.3 μ m, be pressed into base by every 200mg, its pressed density is 3.4gcm
-3Put into vacuum furnace then, vacuum pressure<0.02Pa, sintering temperature is 1300 ℃, sintering 20min obtains the electrolytic capacitor anode agglomerate; Anode block is energized, its liquid of energizing is 0.1%H again
3PO
4, voltage V energizes
fBe 50V, the temperature of energizing is 90 ℃, and energized current density is 60mAg
-1, constant voltage time is 2h, obtains the columbium monoxide electrolytic capacitor anode, its test result is listed in table 1.
Embodiment 3
Make doping columbium monoxide electrolytic capacitor anode, at first take by weighing the doping columbium monoxide powder 200g that columbium monoxide 79wt%, tantalum 21wt% are mixed into particle mean size 1.8 μ m, be pressed into base by every 200mg, its pressed density is 3.4gcm
-3Put into vacuum furnace then, vacuum pressure<0.02Pa, sintering temperature is 1300 ℃, sintering 20min obtains the electrolytic capacitor anode agglomerate; Anode block is energized, its liquid of energizing is 0.1%H again
3PO
4, voltage V energizes
fBe 50V, the temperature of energizing is 90 ℃, and energized current density is 60mAg
-1, constant voltage time is 2h, obtains the columbium monoxide electrolytic capacitor anode, its test result is listed in table 1.
Embodiment 4
Make doping columbium monoxide electrolytic capacitor anode, at first take by weighing the doping columbium monoxide powder 200g that columbium monoxide 80wt%, niobium 10wt%, tantalum 10wt% are mixed into particle mean size 1.5 μ m; Be pressed into base by every 200mg, its pressed density is 3.4gcm
-3Put into vacuum furnace then, vacuum pressure<0.02Pa, sintering temperature is 1300 ℃, sintering 20min obtains the electrolytic capacitor anode agglomerate; Anode block is energized, its liquid of energizing is 0.1%H again
3PO
4, voltage V energizes
fBe 50V, the temperature of energizing is 90 ℃, and energized current density is 60mAg
-1, constant voltage time is 2h, obtains the columbium monoxide electrolytic capacitor anode, its test result is listed in table 1.
Embodiment 5
Make doping columbium monoxide electrolytic capacitor anode, at first take by weighing the doping columbium monoxide powder 200g that columbium monoxide 70wt%, niobium 20wt%, columbium dioxide 10wt% are mixed into particle mean size 1.3 μ m; Be pressed into base by every 200mg, its pressed density is 3.4gcm
-3Put into vacuum furnace then, vacuum pressure<0.02Pa, sintering temperature is 1300 ℃, sintering 20min obtains the electrolytic capacitor anode agglomerate; Anode block is energized, its liquid of energizing is 0.1%H again
3PO
4, voltage V energizes
fBe 50V, the temperature of energizing is 90 ℃, and energized current density is 60mAg
-1, constant voltage time is 2h, obtains the columbium monoxide electrolytic capacitor anode, its test result is listed in table 1.
Embodiment 6
Make doping columbium monoxide electrolytic capacitor anode, at first take by weighing the doping columbium monoxide powder 200g that columbium monoxide 80wt%, tantalum 10wt%, columbium dioxide 10wt% are mixed into particle mean size 1.5 μ m; Be pressed into base by every 200mg, its pressed density is 3.4gcm
-3Put into vacuum furnace then, vacuum pressure<0.02Pa, sintering temperature is 1300 ℃, sintering 20min obtains the electrolytic capacitor anode agglomerate; Anode block is energized, its liquid of energizing is 0.1%H again
3PO
4, voltage V energizes
fBe 50V, the temperature of energizing is 90 ℃, and energized current density is 60mAg
-1, constant voltage time is 2h, obtains the columbium monoxide electrolytic capacitor anode, its test result is listed in table 1.
Embodiment 7
Make doping columbium monoxide electrolytic capacitor anode, at first take by weighing the doping columbium monoxide powder 200g that columbium monoxide 80wt%, niobium 19.9wt%, titanium 0.1wt% are mixed into particle mean size 1.5 μ m; Be pressed into base by every 200mg, its pressed density is 3.4gcm
-3Put into vacuum furnace then, vacuum pressure<0.02Pa, sintering temperature is 1300 ℃, sintering 20min obtains the electrolytic capacitor anode agglomerate; Anode block is energized, its liquid of energizing is 0.1%H again
3PO
4, voltage V energizes
fBe 50V, the temperature of energizing is 90 ℃, and energized current density is 60mAg
-1, constant voltage time is 2h, obtains the columbium monoxide electrolytic capacitor anode, its test result is listed in table 1.
Embodiment 8
Make doping columbium monoxide electrolytic capacitor anode, at first take by weighing the doping columbium monoxide powder 200g that columbium monoxide 80wt%, niobium-tantalum alloy (1: 1) 20wt% are mixed into particle mean size 1.7 μ m; Be pressed into base by every 200mg, its pressed density is 3.4gcm
-3Put into vacuum furnace then, vacuum pressure<0.02Pa, sintering temperature is 1300 ℃, sintering 20min obtains the electrolytic capacitor anode agglomerate; Anode block is energized, its liquid of energizing is 0.1%H again
3PO
4, voltage V energizes
fBe 50V, the temperature of energizing is 90 ℃, and energized current density is 60mAg
-1, constant voltage time is 2h, obtains the columbium monoxide electrolytic capacitor anode, its test result is listed in table 1.
Embodiment 9
Make the columbium monoxide electrolytic capacitor anode, at first take by weighing the columbium monoxide powder of 200g particle mean size 1.0 μ m, be pressed into base by every 200mg, its pressed density is 3.4gcm
-3Put into vacuum furnace then, vacuum pressure<0.02Pa, sintering temperature is 1300 ℃, sintering 20min obtains the electrolytic capacitor anode agglomerate; Anode block is energized, its liquid of energizing is 0.1%H again
3PO
4, voltage V energizes
fBe 30V, the temperature of energizing is 90 ℃, and energized current density is 60mAg
-1, constant voltage time is 2h, obtains the columbium monoxide electrolytic capacitor anode, its test result is listed in table 1.
Embodiment 10
Make doping columbium monoxide electrolytic capacitor anode, at first take by weighing the doping columbium monoxide powder 200g that columbium monoxide 79wt%, niobium 21wt% are mixed into particle mean size 1.3 μ m, be pressed into base by every 200mg, its pressed density is 3.4gcm
-3Put into vacuum furnace then, vacuum pressure<0.02Pa, sintering temperature is 1300 ℃, sintering 20min obtains the electrolytic capacitor anode agglomerate; Anode block is energized, its liquid of energizing is 0.1%H again
3PO
4, voltage V energizes
fBe 30V, the temperature of energizing is 90 ℃, and energized current density is 60mAg
-1, constant voltage time is 2h, obtains the columbium monoxide electrolytic capacitor anode, its test result is listed in table 1.
Claims (4)
1. columbium monoxide electrolytic capacitor anode is characterized in that: with particle mean size is that columbium monoxide or the doping columbium monoxide of 0.1 μ m~20 μ m is the raw material manufacturing; Its alloy is one or more in valve metal, the valve metal low oxide, comprises its alloy and mixture, and its doping scope is greater than 0, less than 80wt%; Its valve metal is niobium, tantalum, titanium, vanadium, aluminium, zirconium.
2. according to claim 1 columbium monoxide electrolytic capacitor anode, it is characterized in that: doping columbium monoxide electrolytic capacitor anode is mixed by columbium monoxide 70wt%, niobium 20wt%, columbium dioxide 10wt%, particle mean size 1.3 μ m.
3. columbium monoxide electrolytic capacitor anode preparation method is characterized in that: at first columbium monoxide or the columbium monoxide that mixes by composition proportion are pressed into base, its pressed density is 2.7gcm
-3~3.8gcm
-3
Put into vacuum sintering furnace then, vacuum pressure<0.1Pa, with sintering temperature: 1100 ℃~1500 ℃, sintering 10min~120min obtains the electrolytic capacitor anode agglomerate;
Anode is energized, its liquid of energizing is 0.01%~0.1%H again
3PO
4, voltage V energizes
f: 10V~80V, the temperature of energizing: 10 ℃~90 ℃, energized current density: 10mAg
-1~120mAg
-1, constant voltage time: 〉=0.5h obtains the columbium monoxide electrolytic capacitor anode.
4. according to claim 3 columbium monoxide electrolytic capacitor anode preparation method, it is characterized in that: at first take by weighing the columbium monoxide powder of 200g particle mean size 1.0 μ m, be pressed into base by every 200mg, its pressed density is 3.4gcm
-3Put into vacuum furnace then, vacuum pressure<0.02Pa, sintering temperature is 1300 ℃, sintering 20min obtains the electrolytic capacitor anode agglomerate; Anode block is energized, its liquid of energizing is 0.1%H again
3PO
4, voltage V energizes
fBe 30V, the temperature of energizing is 90 ℃, and energized current density is 60mAg
-1, constant voltage time is 2h, obtains the columbium monoxide electrolytic capacitor anode.
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CNA031242952A CN1549286A (en) | 2003-05-08 | 2003-05-08 | Niobium monoxide electrolytic capacitor anode and manufacturing method thereof |
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CNA031242952A CN1549286A (en) | 2003-05-08 | 2003-05-08 | Niobium monoxide electrolytic capacitor anode and manufacturing method thereof |
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US7649730B2 (en) | 2007-03-20 | 2010-01-19 | Avx Corporation | Wet electrolytic capacitor containing a plurality of thin powder-formed anodes |
US7760487B2 (en) | 2007-10-22 | 2010-07-20 | Avx Corporation | Doped ceramic powder for use in forming capacitor anodes |
US7760488B2 (en) | 2008-01-22 | 2010-07-20 | Avx Corporation | Sintered anode pellet treated with a surfactant for use in an electrolytic capacitor |
US7768773B2 (en) | 2008-01-22 | 2010-08-03 | Avx Corporation | Sintered anode pellet etched with an organic acid for use in an electrolytic capacitor |
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2003
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US7649730B2 (en) | 2007-03-20 | 2010-01-19 | Avx Corporation | Wet electrolytic capacitor containing a plurality of thin powder-formed anodes |
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US7760488B2 (en) | 2008-01-22 | 2010-07-20 | Avx Corporation | Sintered anode pellet treated with a surfactant for use in an electrolytic capacitor |
US7768773B2 (en) | 2008-01-22 | 2010-08-03 | Avx Corporation | Sintered anode pellet etched with an organic acid for use in an electrolytic capacitor |
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US8203827B2 (en) | 2009-02-20 | 2012-06-19 | Avx Corporation | Anode for a solid electrolytic capacitor containing a non-metallic surface treatment |
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CN104025221A (en) * | 2011-10-26 | 2014-09-03 | H.C.施塔克股份有限公司 | Distortion-free screen-printed anodes on ta/nb sheet |
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