CN104124072A - Preparation method of low-pressure high-energy-density tantalum super-capacitor dielectric film - Google Patents
Preparation method of low-pressure high-energy-density tantalum super-capacitor dielectric film Download PDFInfo
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- CN104124072A CN104124072A CN201410335901.6A CN201410335901A CN104124072A CN 104124072 A CN104124072 A CN 104124072A CN 201410335901 A CN201410335901 A CN 201410335901A CN 104124072 A CN104124072 A CN 104124072A
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Abstract
A preparation method of a low-pressure high-energy-density tantalum super-capacitor dielectric film comprises the steps of anode design adjustment, staged forming, heat treatment and supplementary forming. The liquidity of high-specific-volume tantalum powder particles is ensured, and an obtained anode tantalum core after forming and sintering has good porosity and wettability. By adoption of the staged forming, a dielectric film layer can continuously and stably grow, and the service life of a low-pressure high-energy-density tantalum super-capacitor is prolonged. In addition, the dielectric film on the surface of an anode tantalum block of the capacitor prepared by means of the preparation method is high in strength, good in compactness and smooth in surface.
Description
Technical field
The present invention relates to technical field of electrolytic, relate in particular to the preparation method of the super tantalum capacitor deielectric-coating of a kind of low-pressure high-energy metric density.
Background technology
Electrolytic capacitor, as common electronic component, is widely used in the many-sides such as communication, space flight and military project, submarine cable and advanced electronics, civil electric appliance, plays the effects such as energy storage, filtering, decoupling, bypass, phase inversion in electronic circuit.Traditional non-solid tantalum electrolytic capacitor adopts silver-colored shell encapsulation, the advantages such as leakage current is little although this class capacitor has, the CV product of unit volume is large, but there is the defects such as intensity is low, density is poor, surface flatness is bad in the dielectric oxide film on this class capacitor anode tantalum piece surface, therefore capacitor product equivalent series resistance is high, leakage current is large, impedance is high, electric capacitance change is large.
Summary of the invention
For solving the problems of the technologies described above, the invention provides the preparation method of the super tantalum capacitor deielectric-coating of a kind of low-pressure high-energy metric density, there is the defects such as intensity is low, density is poor, surface flatness is bad in the preparation method of the super tantalum capacitor deielectric-coating of this low-pressure high-energy metric density has solved capacitor anode tantalum piece surface dielectric oxide film by adjusting the steps such as anode design, formation stage by stage, heat treatment, supplementary formation.
The present invention is achieved by the following technical programs.
A preparation method for the super tantalum capacitor deielectric-coating of low-pressure high-energy metric density, comprises the following steps:
Step is 1.: adjust anode design: reduce the pressed density of anode substrate, adopt high temperature blending processes of powders simultaneously;
Step is 2.: form stage by stage dielectric layer, by anode substrate at HNO
3in solution, soak;
Step is 3.: 0～0.5 times while forming voltage, adopting current density is that 35mA/g boosts; 0.5～1 times forms when voltage, reduces current density, and the addition of ethylene glycol be controlled at mass percent 65%～80% within, slow down formation speed, after reaching capacitor and finally forming voltage, constant voltage keeps 2h～2.5h;
Step is 4.: heat treatment, and heating destroys the oxide-film that has open defect near anode substrate surface in forming process, and removes the burr of matrix surface;
Step is 5.: supplement and form, anode substrate is after heat treatment soaked in original solution.
The described step 1. pressed density of Anodic matrix is 4.65g/m
3～4.8g/m
3.
The described step 1. ambient temperature of middle high temperature blending processes of powders is 85 DEG C～125 DEG C.
Described step 4. middle heating-up temperature is 320 DEG C～380 DEG C, and keeps 20min～60min.
Described step 2. in by anode substrate the HNO at 65～90 DEG C
3in solution, soak 0.5h～1h.
86 DEG C of described step temperature 5., the final formation magnitude of voltage that voltage is capacitor.
5. described step adopts current density is that 10～15mA/g antianode matrix carries out constant voltage maintenance 3h～5h again.
Beneficial effect of the present invention is: guarantee the mobility of Fabrication of High Specific Capacitance specification tantalum powder particles, the anode tantalum core that makes to obtain after forming and sintering have good porosity with can wettability; Form stage by stage, media coating is grown continually and steadily, improved the useful life of the super tantalum capacitor of low-pressure high-energy metric density, and the deielectric-coating intensity on the capacitor anode tantalum piece surface preparing by this preparation method is high, good compactness, smooth surface.
Embodiment
Further describe technical scheme of the present invention below, but described in claimed scope is not limited to.
Embodiment mono-:
A preparation method for the super tantalum capacitor deielectric-coating of low-pressure high-energy metric density, comprises following steps:
Steps A, adjustment anode design: the pressed density of anode substrate is down to 4.8g/m
3, adopt high temperature blending processes of powders simultaneously, the ambient temperature of high temperature blending processes of powders is 95 DEG C, guarantees the mobility of Fabrication of High Specific Capacitance specification tantalum powder particles, the anode tantalum core that makes to obtain after forming and sintering have good porosity with can wettability.
Step B, deielectric-coating form stage by stage, and concrete steps are as follows:
A.0 when～0.5 times of formation voltage, the HNO by anode substrate at 80 DEG C
3in solution, soak 0.5h, the air in hole is discharged substantially, then adopting current density is that 35mA/g boosts, to obtain uniform dielectric layer.
B.0.5 when～1 times of formation voltage, suitably reduce current density, the addition of ethylene glycol is controlled at 75% left and right of mass percent, effectively slow down formation speed, media coating is grown continually and steadily, reach capacitor and finally form after the about 24V of voltage constant voltage again and keep 2.2h, guarantee that residual current is down to minimum.
Step C, heat treatment: the temperature of anode substrate is heated to 360 DEG C, keep 35min, can destroy the oxide-film that has open defect near matrix surface in forming process, make tantalum matrix from tantalum pentoxide, draw oxygen, tantalum metal---oxide interface can be to oxygenate conversion, thereby reduces dielectric effective thickness, removes the burr of matrix surface, obtain evenly smooth dielectric layer, and the benefit of bringing leakage current to reduce.
Step D, supplement and form: selecting boiling point organic additive high, that flash over voltage is high, oxidation rate is fast to be mixed with special formation electrolyte, is under 86 DEG C, the voltage condition that is 24V, at former HNO in temperature
3in solution, adopting current density is 12mA/g carries out 5h again supplementary formation to anode block after heat treatment.Note paying close attention to the situation of change of electric current on power meter, prevent that electric field phenomenon from occurring.
After the capacitor of choosing 10V4700 μ F specification adopts respectively prior art and is prepared according to the method for embodiment mono-, therefrom extract 5 capacitors and carry out Contrast of Electrical Parameter, comparing result is in table one.
The electrical quantity of the 10V4700 μ F that table one is prepared at 85 DEG C, through 192h performance test latter two technology of preparing
Embodiment bis-:
A preparation method for the super tantalum capacitor deielectric-coating of low-pressure high-energy metric density, comprises following steps:
Steps A, adjustment anode design: the pressed density of anode substrate is down to 4.65g/m
3, adopt high temperature blending processes of powders simultaneously, the ambient temperature of high temperature blending processes of powders is 110 DEG C, guarantees the mobility of Fabrication of High Specific Capacitance specification tantalum powder particles, the anode tantalum core that makes to obtain after forming and sintering have good porosity with can wettability.
Step B, deielectric-coating form stage by stage, and concrete steps are as follows:
A.0 when～0.5 times of formation voltage, the HNO by anode substrate at 75 DEG C
3in solution, soak 0.7h, the air in hole is discharged substantially, then adopting current density is that 35mA/g boosts, to obtain uniform dielectric layer.
B.0.5 when～1 times of formation voltage, suitably reduce current density, the addition of controlling ethylene glycol is controlled at 70% of mass percent, effectively slow down formation speed, media coating is grown continually and steadily, reach capacitor electrode container and finally form after the about 22V of voltage constant voltage again and keep 2.5h, guarantee that residual current is down to minimum.
Step C, heat treatment: the temperature of anode substrate is heated to 380 DEG C, keep 45min, can destroy the oxide-film that has open defect near matrix surface in forming process, make tantalum matrix from tantalum pentoxide, draw oxygen, tantalum metal---oxide interface can be to oxygenate conversion, thereby reduces dielectric effective thickness, removes the burr of matrix surface, obtain evenly smooth dielectric layer, and the benefit of bringing leakage current to reduce.
Step D, supplement and form: selecting boiling point organic additive high, that flash over voltage is high, oxidation rate is fast to be mixed with special formation electrolyte, is under 86 DEG C, the voltage condition that is 22V, at former HNO in temperature
3in solution, adopting current density is 10mA/g carries out 4.5h again supplementary formation to anode block after heat treatment.Note paying close attention to the situation of change of electric current on power meter, prevent that electric field phenomenon from occurring.
After the capacitor of choosing 10V10000 μ F specification adopts respectively prior art and embodiment 2 to be prepared, therefrom extract 5 capacitors and carry out Contrast of Electrical Parameter, comparing result is in table two.
The electrical quantity of the 10V10000 μ F that table two is prepared at 85 DEG C, through 192h performance test latter two technology of preparing
Embodiment tri-:
A preparation method for the super tantalum capacitor deielectric-coating of low-pressure high-energy metric density, comprises following steps:
Steps A, adjustment anode design: the pressed density of anode substrate is down to 4.7g/m
3, adopt high temperature blending processes of powders simultaneously, the ambient temperature of high temperature blending processes of powders is 115 DEG C, guarantees the mobility of Fabrication of High Specific Capacitance specification tantalum powder particles, the anode tantalum core that makes to obtain after forming and sintering have good porosity with can wettability.
Step B, deielectric-coating form stage by stage, and concrete steps are as follows:
A.0 when～0.5 times of formation voltage, the HNO by anode substrate at 86 DEG C
3in solution, soak 1h, the air in hole is discharged substantially, then adopting current density is that 35mA/g boosts, to obtain uniform dielectric layer.
B.0.5 when～1 times of formation voltage, suitably reduce current density, the addition of ethylene glycol is controlled at 80% left and right, effectively slow down formation speed, media coating is grown continually and steadily, reach capacitor and finally form after the about 30V of voltage constant voltage again and keep 2.4h, guarantee that residual current is down to minimum.
Step C, heat treatment: the temperature of anode substrate is heated to 345 DEG C, keep 55min, can destroy the oxide-film that has open defect near matrix surface in forming process, make tantalum matrix from tantalum pentoxide, draw oxygen, tantalum metal---oxide interface can be to oxygenate conversion, thereby reduces dielectric effective thickness, removes the burr of matrix surface, obtain evenly smooth dielectric layer, and the benefit of bringing leakage current to reduce.
Step D, supplement and form: selecting boiling point organic additive high, that flash over voltage is high, oxidation rate is fast to be mixed with special formation electrolyte, is under 86 DEG C, the voltage condition that is 30V, at HNO in temperature
3in solution, adopting current density is 14mA/g, anode block is after heat treatment carried out again to the supplementary formation of 3.5h.Note paying close attention to the situation of change of electric current on power meter, prevent that electric field phenomenon from occurring.
After the capacitor of choosing 16V3300 μ F specification adopts respectively prior art and embodiment 3 to be prepared, therefrom extract 5 capacitors and carry out Contrast of Electrical Parameter, comparing result is in table three.
The electrical quantity of the 16V3300 μ F that table three is prepared at 85 DEG C, through 192h performance test latter two technology of preparing
Can find out from the experimental data of table one, table two and table three, can normally work under 85 DEG C, the condition of 192h through the product after the present invention preparation, and the unit for electrical property parameters such as equivalent series resistance ESR, leakage current is all controlled in allowed limits, and the indexs such as the consistency of its unit for electrical property parameters are better than prior art, can meet instructions for use completely.
Claims (7)
1. a preparation method for the super tantalum capacitor deielectric-coating of low-pressure high-energy metric density, is characterized in that, comprises the following steps:
Step is 1.: adjust anode design: reduce the pressed density of anode substrate, adopt high temperature blending processes of powders simultaneously;
Step is 2.: form stage by stage dielectric layer, by anode substrate at HNO
3in solution, soak;
Step is 3.: 0～0.5 times while forming voltage, adopting current density is that 35mA/g boosts; 0.5～1 times forms when voltage,, reduce current density, and the addition of ethylene glycol be controlled at mass percent 65%～80% within, slow down formation speed, after reaching capacitor and finally forming voltage, constant voltage keeps 2h～2.5h;
Step is 4.: heat treatment, and heating destroys the oxide-film that has open defect near anode substrate surface in forming process, and removes the burr of matrix surface;
Step is 5.: supplement and form, by anode substrate after heat treatment at HNO
3in solution, soak.
2. the preparation method of the super tantalum capacitor deielectric-coating of low-pressure high-energy metric density as claimed in claim 1, is characterized in that: the described step 1. pressed density of Anodic matrix is 4.65g/m
3～4.8g/m
3.
3. the preparation method of the super tantalum capacitor deielectric-coating of low-pressure high-energy metric density as claimed in claim 1, is characterized in that: the described step 1. ambient temperature of middle high temperature blending processes of powders is 85 DEG C～125 DEG C.
4. the preparation method of the super tantalum capacitor deielectric-coating of low-pressure high-energy metric density as claimed in claim 1, is characterized in that: described step 4. middle heating-up temperature is 320 DEG C～380 DEG C, and keeps 20min～60min.
5. the preparation method of the super tantalum capacitor deielectric-coating of low-pressure high-energy metric density as claimed in claim 1, is characterized in that: described step 2. in by anode substrate the HNO at 65～90 DEG C
3in solution, soak 0.5h～1h.
6. the preparation method of the super tantalum capacitor deielectric-coating of low-pressure high-energy metric density as claimed in claim 1, is characterized in that: described step solution temperature is 5. 86 DEG C, the final formation magnitude of voltage that voltage is capacitor.
7. the preparation method of the super tantalum capacitor deielectric-coating of low-pressure high-energy metric density as claimed in claim 1, is characterized in that: 5. described step adopts current density is that 10～15mA/g antianode matrix carries out constant voltage maintenance 3h～5h again.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108091491A (en) * | 2017-12-12 | 2018-05-29 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | The method for reducing the method for non-solid electrolyte tantalum capacity fall off flow valuve and preparing non-solid electrolyte tantalum capacitance |
| CN114300271A (en) * | 2021-12-29 | 2022-04-08 | 贵州师范学院 | Preparation method for prolonging service life of super capacitor |
-
2014
- 2014-07-15 CN CN201410335901.6A patent/CN104124072A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108091491A (en) * | 2017-12-12 | 2018-05-29 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | The method for reducing the method for non-solid electrolyte tantalum capacity fall off flow valuve and preparing non-solid electrolyte tantalum capacitance |
| CN114300271A (en) * | 2021-12-29 | 2022-04-08 | 贵州师范学院 | Preparation method for prolonging service life of super capacitor |
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