CN103325574A - Method for manufacturing cathode of total-tantalum electrolytic capacitor - Google Patents
Method for manufacturing cathode of total-tantalum electrolytic capacitor Download PDFInfo
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- CN103325574A CN103325574A CN2013102794843A CN201310279484A CN103325574A CN 103325574 A CN103325574 A CN 103325574A CN 2013102794843 A CN2013102794843 A CN 2013102794843A CN 201310279484 A CN201310279484 A CN 201310279484A CN 103325574 A CN103325574 A CN 103325574A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/13—Energy storage using capacitors
Abstract
The embodiment of the invention discloses a method for manufacturing a cathode of a total-tantalum electrolytic capacitor. The method comprises the following steps of: blasting sand to polish the inner surface of a tantalum housing of the total-tantalum electrolytic capacitor; adding graphene oxide into a dispersing solvent for dispersing to obtain graphene oxide dispersion liquid; adding the graphene oxide dispersion liquid into the tantalum housing, so that the graphene oxide in the graphene oxide dispersion liquid is dispersed on the inner surface; carrying out reduction treatment onto the graphene oxide which is dispersed on the inner surface; and forming a ruthenium oxide layer on the inner surface by an electrochemical method. According to the method disclosed by the embodiment of the invention, the graphene oxide and the ruthenium oxide are compound, so that not only can the area of the cathode of the total-tantalum capacitor be greatly increased, but also the effective area of the tantalum capacitor can be increased; and a pseudocapacitor is introduced onto the tantalum housing, so that the capacity of the capacitor is improved.
Description
Technical field
The present invention relates to technical field of electronic materials, especially relate to a kind of method of making full tantalum electrolytic capacitor negative electrode.
Background technology
Liquid tantalum electrolytic capacitor has the advantages such as large, the anti-mesohigh of capacity, leakage current be less, is particluarly suitable for using in the large capacity circuit under the mesohigh condition.But liquid tantalum electrolytic capacitor adopts acidic liquid electrolyte, in case leak of liquid occurs, may make the circuit board short circuit, and then cause equipment generation catastrophe failure.
Therefore the complete hermetically sealed liquid tantalum electrolytic capacitor of tantalum arises at the historic moment, and its sealing is fabulous, can leakage, and because what adopt is the tantalum shell, make it have very high environmental stability, and can bear larger ripple current, be applicable to require the equipment of high reliability to use.And full tantalum liquid tantalum electrolytic capacitor structure and common silver-colored shell liquid tantalum electrolytic capacitor structure are basic identical, as anode, generate unformed Ta in the anode surface oxidation by the tantalum core of high temperature sintering
2O
5Deielectric-coating is as dielectric layer, and metal shell and acidic electrolysis bath are as negative electrode, and different is that the common liq tantalum electrolytic capacitor is to draw as negative electrode with silver-colored shell, and full tantalum liquid tantalum electrolytic capacitor is to draw as negative electrode with the tantalum shell.The tantalum shell faces a problem that is difficult for electroplating platinum black as negative electrode, so that its cathode area is less, is not easy to the lifting of condenser capacity.
Summary of the invention
One of purpose of the present invention provides the method for the full tantalum electrolytic capacitor negative electrode that a kind of manufacturing property is stable, specific area is large, specific capacity is high, the full tantalum electrolytic capacitor of suitable high reliability is assembled.
Technical scheme disclosed by the invention comprises:
A kind of method of making full tantalum electrolytic capacitor negative electrode is provided, has it is characterized in that, having comprised: steps A: the polish inner surface of tantalum shell of full tantalum electrolytic capacitor of sandblast makes described rough inner surface; Step B: graphene oxide added in the dispersion solvent disperse, obtain the graphene oxide dispersion liquid; Step C: described graphene oxide dispersion liquid is added in the described tantalum shell, and rotate described tantalum shell with desired speed, the graphene oxide in the described graphene oxide dispersion liquid is scattered on the described inner surface; Step D: reduce processing to being scattered in graphene oxide on the described inner surface; Step F: form ruthenium oxide layer at described inner surface with electrochemical method.
Further, in described sandblast polishing, sand-blasting abrasive is 400 order steel sands, and sandblast pressure is 0.6 to 0.8 MPa, and the sandblast time is 0.5 to 3 minute.
Further, sandblast was polished and is also comprised after the inner surface of tantalum shell of full tantalum electrolytic capacitor: with the described tantalum shell of acetone ultrasonic cleaning 0.5 to 1 hour; With the described tantalum shell of washed with de-ionized water 0.5 to 1 hour; Dry described tantalum shell.
Further, the concentration of described graphene oxide dispersion liquid is 1 ~ 5 mg/ml, and describedly rotates described tantalum shell with desired speed and comprise: rotated described tantalum shell 20 to 60 seconds with 50 to 100 rev/mins rotating speeds.
Further, describedly reduce to process and comprise being scattered in graphene oxide on the described inner surface: being higher than 5 * 10-4 handkerchief, temperature in vacuum degree is that reduction is scattered in graphene oxide 0.5 to 1 hour on the described inner surface under 200 to 220 degrees centigrade the environment.
Further, before described step F, also comprise: repeating said steps C and described step D 3 ~ 5 times.
Further, describedly form ruthenium oxide layer with electrochemical method at described inner surface and comprise: preparation electrolyte; Described electrolyte is added in the described tantalum shell; Take described tantalum shell as work electrode, platinum filament as to electrode, silver/silver chlorate as reference electrode, form ruthenium oxide layer with cyclic voltammetry at the described inner surface of described tantalum shell.
Further, described electrolyte comprises: concentration is that the ruthenium trichloride of 0.01 ~ 0.02 mol/L, potassium chloride and the concentration that concentration is 0.1 ~ 0.2 mol/L are the hydrogen chloride of 0.01 ~ 0.03 mol/L, and the temperature of described electrolyte is 40 ℃ ~ 60 ℃.
Further, in described cyclic voltammetry, cyclical voltage is-0.2 ~ 1 volt, and sweep speed is 100 ~ 800 millivolts/second, and cycle-index is 100 ~ 500 times.
Further, after forming ruthenium oxide layer, the described inner surface of described tantalum shell also comprises: be higher than 5 * 10-4 handkerchief in vacuum degree, temperature is 180 ~ 250 ℃ of lower annealing 2 ~ 3 hours.
In the method in the embodiments of the invention, compound by Graphene and ruthenium-oxide not only can increase the cathode area of whole tantalum capacitor greatly, increases the effective area of tantalum capacitor, also introduced fake capacitance at the tantalum shell, all can improve the capacity of capacitor.
Description of drawings
Fig. 1 is the schematic flow sheet of the method for the full tantalum electrolytic capacitor negative electrode of the manufacturing of one embodiment of the invention.
Fig. 2 shows the according to an embodiment of the invention figure of the parameter of the sample of the full tantalum electrolytic capacitor negative electrode of method manufacturing.
Embodiment
Describe the concrete steps of method of the full tantalum electrolytic capacitor negative electrode of manufacturing of embodiments of the invention in detail below in conjunction with accompanying drawing.
As shown in Figure 1, in the embodiments of the invention, a kind of method of making full tantalum electrolytic capacitor negative electrode comprises step 10, step 12, step 16, step 18 and step 20.The below is described in detail each step.
Step 10: sandblast polishing tantalum inner surface of outer cover.
As mentioned before, the complete hermetically sealed liquid tantalum electrolytic capacitor structure of tantalum and common silver-colored shell liquid tantalum electrolytic capacitor structure are basic identical, as anode, generate unformed Ta in the anode surface oxidation by the tantalum core of high temperature sintering
2O
5Deielectric-coating is as dielectric layer, and metal shell and acidic electrolysis bath are as negative electrode, and different is that the common liq tantalum electrolytic capacitor is to draw as negative electrode with silver-colored shell, and full tantalum liquid tantalum electrolytic capacitor is to draw as negative electrode with the tantalum shell.
Method of the present invention relates to the manufacture method of the tantalum shell of full tantalum electrolytic capacitor.
In the method for embodiments of the invention, in step 10, can obtain the tantalum shell of full tantalum electrolytic capacitor, then the inner surface of tantalum shell be carried out the roughening processing, even the inner surface of tantalum shell becomes coarse.
In the embodiments of the invention, can use the method for sandblast polishing to carry out this roughening and process, that is, the polish inner surface of tantalum shell of full tantalum electrolytic capacitor of sandblast makes this inner surface become coarse.For example, among the embodiment, can be take 400 order steel sands as sand-blasting abrasive, the inner surface to the tantalum shell under the sandblast pressure of 0.6 to 0.8 MPa carries out the sandblast grinding process, and the sandblast time can be 0.5 to 3 minute.
After the sandblast grinding process, the inner surface of tantalum shell becomes coarse, is convenient to the dispersion (described below) of graphene oxide on this inner surface in the subsequent step.
The inner surface of tantalum shell is carried out in the embodiments of the invention, can also comprising cleaning step after the sandblast polishing, namely the tantalum shell after the sandblast polishing is cleaned.
For example, among the embodiment, this cleaning step can comprise: use this tantalum shell of acetone ultrasonic cleaning 0.5 to 1 hour; With this tantalum shell of washed with de-ionized water 0.5 to 1 hour; Then dry this tantalum shell.
Here, " ultrasonic cleaning " uses ultrasonic irradiation, so that the tantalum shell is cleaned after referring to the tantalum shell that needs clean placed cleaning fluid (for example aforesaid acetone and deionized water).
Step 12: preparation graphene oxide dispersion liquid.
In the embodiments of the invention, in step 12, graphene oxide can be added in the dispersion solvent, and graphene oxide is fully disperseed in this dispersion solvent, obtain the graphene oxide dispersion liquid.
In the embodiments of the invention, the concentration of graphene oxide dispersion liquid can be 1 ~ 5 mg/ml (mg/mL).
In the embodiments of the invention, the sequencing of step 10 and step 12 is restriction not.
Step 16: graphene oxide is scattered on the inner surface of tantalum shell.
In the embodiments of the invention, obtained after the tantalum shell and graphene oxide dispersion liquid that inner surface is roughened, this graphene oxide dispersion liquid is added in this tantalum shell, and rotate this tantalum shell with desired speed, the graphene oxide in the graphene oxide dispersion liquid is scattered on the inner surface of tantalum shell.Here, because the inner surface of tantalum shell has passed through the roughening processing, therefore in the processing of step 16, the graphene oxide in the graphene oxide dispersion liquid can be scattered on this inner surface of tantalum shell.
In the embodiments of the invention, the aforesaid processing that has added the tantalum shell of graphene oxide dispersion liquid with desired speed rotation can comprise: rotated this tantalum shell 20 to 60 seconds with 50 to 100 rev/mins rotating speeds.
Through the processing of step 16, the graphene oxide in the graphene oxide dispersion liquid is scattered on the inner surface of tantalum shell.
Step 18: reduction is processed.
After graphene oxide is scattered on the inner surface of tantalum shell in the step 16, in step 18, reduce processing to being scattered in graphene oxide on this inner surface, so that the graphene oxide reduction that is scattered on the inner surface of tantalum shell becomes Graphene.
For example, among the embodiment, can use high-temperature vacuum reduction processing to make the graphene oxide reduction on the inner surface that is scattered in the tantalum shell become Graphene.For example, among the embodiment, this reduction is processed and can be comprised: be higher than 5 * 10 in vacuum degree
-4Handkerchief, temperature are that reduction is scattered in graphene oxide 0.5 to 1 hour on the inner surface of tantalum shell under 200 to 220 degrees centigrade the environment.
Process by the reduction in the step 18, the graphene oxide that is scattered in the step 16 on the inner surface of tantalum shell is reduced into Graphene.
In the embodiments of the invention, before step 20, can also repeat step 16 and step 18 3 ~ 5 times, like this can be with good being scattered on the whole inner surface of tantalum shell of Graphene.
Step 20: form ruthenium oxide layer at inner surface.
In step 18, be scattered in the interior table of the tantalum shell graphene oxide on full and be reduced into after the Graphene, in step 20, can form ruthenium oxide layer at this inner surface.For example, form ruthenium oxide layer with electrochemical method at this inner surface.
In one embodiment of the present of invention, can comprise with the concrete steps of electrochemical method in the inner surface formation ruthenium oxide layer of tantalum shell:
Preparation electrolyte;
This electrolyte is added in the tantalum shell;
Take state the tantalum shell as work electrode, platinum filament as to electrode, silver/silver chlorate as reference electrode, form ruthenium oxide layer with cyclic voltammetry at the inner surface of tantalum shell.
At this moment, electrolyte is put in the tantalum shell, and platinum filament and silver/silver chloride electrode are to be inserted in the tantalum shell and not to contact with shell, and namely whole tantalum shell is the electrochemical reaction groove, and electrolyte adds highly can be 80% ~ 90% of tantalum outer cover height.
In the embodiments of the invention, the electrolyte here can comprise: concentration is that the ruthenium trichloride of 0.01 ~ 0.02 mol/L, potassium chloride and the concentration that concentration is 0.1 ~ 0.2 mol/L are the hydrogen chloride of 0.01 ~ 0.03 mol/L, and the temperature of described electrolyte is 40 ℃ ~ 60 ℃.Wherein hydrogen chloride is used for regulating the pH value of electrolyte.In the embodiments of the invention, the pH value of electrolyte can be between 2.2 to 2.5.
In the embodiments of the invention, in this cyclic voltammetry, cyclical voltage can be-0.2 ~ 1 volt, and sweep speed can be 100 ~ 800 millivolts/second, and cycle-index can be 100 ~ 500 times.
Through aforesaid electrochemical treatments, can form ruthenium oxide layer at the inner surface of tantalum shell.
In the embodiments of the invention, the thickness of this ruthenium oxide layer can be determined according to actual conditions.
In the embodiments of the invention, form ruthenium oxide layer by the inner surface at the tantalum shell, can greatly improve the cathode area of full tantalum electrolytic capacitor, thereby improve the capacity of capacitor.
In the embodiments of the invention, after the inner surface of tantalum shell forms ruthenium oxide layer, also comprise annealing steps, for example, among the embodiment, this annealing steps comprises: be higher than 5 * 10-4 handkerchief in vacuum degree, temperature is 180 ~ 250 ℃ of lower annealing 2 ~ 3 hours.
In the method in the embodiments of the invention, as continuous phase, being scattered in Graphene on the tantalum shell as decentralized photo, can improve specific capacity by the two synergy take the synthetic ruthenium-oxide of electrochemistry.While is that the porous oxidation ruthenium can increasing specific surface area the formation of Graphene rough surface.Like this, compound by Graphene and ruthenium-oxide not only can increase the cathode area of whole tantalum capacitor greatly, increases the effective area of tantalum capacitor, also introduced fake capacitance at the tantalum shell, thereby improved the capacity of capacitor.
The below illustrates the detailed step of method of the present invention according to several concrete examples.
Example 1:
(1) with the tantalum inner surface of outer cover of Φ 10 * 100mm, with 400 order steel sands, sandblast 1min under 0.6Mpa pressure;
(2) the tantalum shell that sandblast is finished passes through respectively acetone, deionized water ultrasonic cleaning 1h, and 100 ℃ of lower dry for standby;
(3) add 2 ml in the tantalum shell that cleans up, concentration is 2mg/ml graphene oxide dispersion liquid;
The tantalum shell that (4) the graphene oxide dispersion liquid will be housed turns 50/rotate 30s under the min speed;
(5) be 1.1 * 10 with the tantalum shell in vacuum degree
-4Pa, temperature is 200 ℃ of constant temperature 1h, this moment, graphene oxide was reduced to Graphene;
(6) (4) ~ (5) process is repeated 3 times;
(7) with whole tantalum shell as being electrochemical reaction groove and work electrode, add 7ml electrolyte, insert respectively platinum filament and silver/silver chloride electrode, be-0.2 ~ 1V in cyclical voltage, sweep speed is 200mV/s, cycle-index is 100 lower ruthenium-oxide electrodes that prepare;
(8) after preparation is finished, use deionized water rinsing tantalum inner surface of outer cover 3 ~ 5 times;
(9) be 3.2 * 10 with the tantalum shell in vacuum degree
-4The pa temperature is 200 ℃ of lower annealing 2h.
Like this, obtain full tantalum electrolytic capacitor cathode sample 1.
Example 2:
(1) with the tantalum inner surface of outer cover of Φ 20 * 120mm, with 400 order steel sands, sandblast 2min under 0.6Mpa pressure;
(2) the tantalum shell that sandblast is finished passes through respectively acetone, deionized water ultrasonic cleaning 1h, and 100 ℃ of lower dry for standby;
(3) add 9 ml in the tantalum shell that cleans up, concentration is 2mg/ml graphene oxide dispersion liquid;
The tantalum shell that (4) the graphene oxide dispersion liquid will be housed turns 50/rotate 30s under the min speed;
(5) be 9.7 * 10 with the tantalum shell in vacuum degree
-5Pa, temperature is 200 ℃ of constant temperature 1h, this moment, graphene oxide was reduced to Graphene;
(6) (4) ~ (5) process is repeated 3 times;
(7) with whole tantalum shell as being electrochemical reaction groove and work electrode, adding 32ml electrolyte, insert respectively platinum filament and silver/silver chloride electrode, is-0.2 ~ 1V in cyclical voltage, sweep speed is 250mV/s, and cycle-index is 100 lower preparation ruthenium-oxide electrodes;
(8) after preparation is finished, use deionized water rinsing tantalum inner surface of outer cover 3 ~ 5 times;
(9) be 3.5 * 10 with the tantalum shell in vacuum degree
-4The pa temperature is 200 ℃ of lower annealing 2h.
Like this, obtain full tantalum electrolytic capacitor cathode sample 2.
Example 3:
(1) with the tantalum inner surface of outer cover of Φ 10 * 100mm, with 400 order steel sands, sandblast 1min under 0.6Mpa pressure;
(2) the tantalum shell that sandblast is finished passes through respectively acetone, deionized water ultrasonic cleaning 1h, and 100 ℃ of lower dry for standby;
(3) add 2 ml in the tantalum shell that cleans up, concentration is 5mg/ml graphene oxide dispersion liquid;
The tantalum shell that (4) the graphene oxide dispersion liquid will be housed turns 50/rotate 30s under the min speed;
(5) be 8.7 * 10 with the tantalum shell in vacuum degree
-5Pa, temperature is 200 ℃ of constant temperature 1.5h, this moment, graphene oxide was reduced to Graphene;
(6) (4) ~ (5) process is repeated 3 times;
(7) with whole tantalum shell as being electrochemical reaction groove and work electrode, add 7ml electrolyte, insert respectively platinum filament and silver/silver chloride electrode, be-0.2 ~ 1V in cyclical voltage, sweep speed is 200mV/s, cycle-index is 100 lower ruthenium-oxide electrodes that prepare;
(8) after preparation is finished, use deionized water rinsing tantalum inner surface of outer cover 3 ~ 5 times;
(9) be 1.2 * 10 with the tantalum shell in vacuum degree
-4The pa temperature is 200 ℃ of lower annealing 2h.
Like this, obtain full tantalum electrolytic capacitor cathode sample 3.
Example 4:
(1) with the tantalum inner surface of outer cover of Φ 20 * 120mm, with 400 order steel sands, sandblast 2min under 0.6Mpa pressure;
(2) the tantalum shell that sandblast is finished passes through respectively acetone, deionized water ultrasonic cleaning 1h, and 100 ℃ of lower dry for standby;
(3) add 9 ml in the tantalum shell that cleans up, concentration is 5mg/ml graphene oxide dispersion liquid;
The tantalum shell that (4) the graphene oxide dispersion liquid will be housed turns 50/rotate 30s under the min speed;
(5) be 9.4 * 10 with the tantalum shell in vacuum degree
-5Pa, temperature is 200 ℃ of constant temperature 1.5h, this moment, graphene oxide was reduced to Graphene;
(6) (4) ~ (5) process is repeated 3 times;
(7) with whole tantalum shell as being electrochemical reaction groove and work electrode, adding 32ml electrolyte, insert respectively platinum filament and silver/silver chloride electrode, is-0.2 ~ 1V in cyclical voltage, sweep speed is 250mV/s, and cycle-index is 100 lower preparation ruthenium-oxide electrodes;
(8) after preparation is finished, use deionized water rinsing tantalum inner surface of outer cover 3 ~ 5 times;
(9) be 4.1 * 10 with the tantalum shell in vacuum degree
-4The pa temperature is 200 ℃ of lower annealing 2h.
Like this, obtain full tantalum electrolytic capacitor cathode sample 4.
Through test, the design parameter of four samples that the above obtains as shown in Figure 2.
As can be seen from Fig. 2, full tantalum electrolytic capacitor cathode performance made according to the method for the present invention is stable, and specific area is large, specific capacity is high, is fit to the full tantalum electrolytic capacitor assembling of high reliability.
Abovely describe the present invention by specific embodiment, but the present invention is not limited to these specific embodiments.It will be understood by those skilled in the art that and can also make various modifications to the present invention, be equal to replacement, change etc., these conversion all should be within protection scope of the present invention as long as do not deviate from spirit of the present invention.In addition, the different embodiment of above many places described " embodiment " expression can certainly be with its all or part of combination in one embodiment.
Claims (10)
1. a method of making full tantalum electrolytic capacitor negative electrode is characterized in that, comprising:
Steps A: the polish inner surface of tantalum shell of full tantalum electrolytic capacitor of sandblast makes described rough inner surface;
Step B: graphene oxide added in the ultra-pure water disperse, obtain the graphene oxide dispersion liquid;
Step C: described graphene oxide dispersion liquid is added in the described tantalum shell, and rotate described tantalum shell with desired speed, the graphene oxide in the described graphene oxide dispersion liquid is scattered on the described inner surface, and oven dry;
Step D: reduce processing to being scattered in graphene oxide on the described inner surface;
Step F: form ruthenium oxide layer at described inner surface with electrochemical method.
2. the method for claim 1 is characterized in that: in described sandblast polishing, sand-blasting abrasive is 400 order steel sands, and sandblast pressure is 0.6 to 0.8 MPa, and the sandblast time is 0.5 to 3 minute.
3. the method for claim 1 is characterized in that: sandblast is polished and is also comprised after the inner surface of tantalum shell of full tantalum electrolytic capacitor:
With the described tantalum shell of acetone ultrasonic cleaning 0.5 to 1 hour;
With the described tantalum shell of washed with de-ionized water 0.5 to 1 hour;
Dry described tantalum shell.
4. the method for claim 1, it is characterized in that: the concentration of described graphene oxide dispersion liquid is 1 ~ 5 mg/ml, and describedly rotates described tantalum shell with desired speed and comprise: rotated described tantalum shell 20 to 60 seconds with 50 to 100 rev/mins rotating speeds.
5. the method for claim 1 is characterized in that: describedly reduce to process and comprise being scattered in graphene oxide on the described inner surface: be higher than 5 * 10 in vacuum degree
-4Handkerchief, temperature are that reduction is scattered in graphene oxide 0.5 to 1 hour on the described inner surface under 200 to 220 degrees centigrade the environment.
6. the method for claim 1 is characterized in that, also comprises before described step F: repeating said steps C and described step D 3 ~ 5 times.
7. the method for claim 1 is characterized in that: describedly form ruthenium oxide layer with electrochemical method at described inner surface and comprise:
Preparation electrolyte;
Described electrolyte is added in the described tantalum shell;
Take described tantalum shell as work electrode, platinum filament as to electrode, silver/silver chlorate as reference electrode, form ruthenium oxide layer with cyclic voltammetry at the described inner surface of described tantalum shell.
8. method as claimed in claim 7, it is characterized in that, described electrolyte comprises: concentration is that the ruthenium trichloride of 0.01 ~ 0.02 mol/L, potassium chloride and the concentration that concentration is 0.1 ~ 0.2 mol/L are the hydrogen chloride of 0.01 ~ 0.03 mol/L, and the temperature of described electrolyte is 40 ℃ ~ 60 ℃.
9. method as claimed in claim 7, it is characterized in that: in described cyclic voltammetry, cyclical voltage is-0.2 ~ 1 volt, and sweep speed is 100 ~ 800 millivolts/second, and cycle-index is 100 ~ 500 times.
10. method as claimed in claim 7 is characterized in that: also comprise after the described inner surface of described tantalum shell forms ruthenium oxide layer: be higher than 5 * 10 in vacuum degree
-4Handkerchief, temperature are 180 ~ 250 ℃ of lower annealing 2 ~ 3 hours.
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| WO2020052096A1 (en) * | 2018-09-11 | 2020-03-19 | 南京理工大学 | Three-dimentional ordered porous ruthenium dioxide film electrode and preparation method thereof |
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