CN106057469A - Preparation method of middle and high voltage solid electrolyte tantalum capacitor cathode - Google Patents
Preparation method of middle and high voltage solid electrolyte tantalum capacitor cathode Download PDFInfo
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- CN106057469A CN106057469A CN201610719935.4A CN201610719935A CN106057469A CN 106057469 A CN106057469 A CN 106057469A CN 201610719935 A CN201610719935 A CN 201610719935A CN 106057469 A CN106057469 A CN 106057469A
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- manganese nitrate
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- 239000003990 capacitor Substances 0.000 title claims abstract description 72
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 31
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 29
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims abstract description 41
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 17
- 238000005470 impregnation Methods 0.000 claims description 15
- 238000007598 dipping method Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 7
- 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 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000002386 leaching Methods 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims 1
- 238000000197 pyrolysis Methods 0.000 claims 1
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 abstract description 20
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 3
- 230000005684 electric field Effects 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 229910002651 NO3 Inorganic materials 0.000 abstract 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 230000008901 benefit Effects 0.000 description 7
- 238000001514 detection method Methods 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 238000002048 anodisation reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- 238000002955 isolation Methods 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000035899 viability Effects 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
-
- 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
- H01G9/15—Solid electrolytic capacitors
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
The invention discloses a preparation method of a middle and high voltage solid electrolyte tantalum capacitor cathode. Common accessible ammonium hydrogen phosphate is creatively used as an additive of a manganous nitrate solution and works as a catalyst in the thermal decomposition process of manganous nitrate, the applicants precisely optimize and determine the additive amount and optimize the preparation process, a cathode manganese dioxide layer prepared by the preparation method of the middle and high voltage solid electrolyte tantalum capacitor cathode is continuous and compact and can be in tight contact with an oxidation medium film, the intensity distribution of an electric field generated under a high voltage load is uniform, distortion is avoided, and especially, a middle and high voltage capacitor with a rated voltage higher than 40V prepared by the method is small in leakage current and is highly improved in electric stability. According to the invention, the preparation process is table and simple, the raw material is low in cost, each property of the tantalum capacitor is effectively improved, and industrial production is easy.
Description
Technical field
The present invention relates to electronic technology field, more particularly, to a kind of mesohigh solid electrolyte Ta capacitor negative electrode
Preparation method.
Background technology
Solid electrolyte Ta capacitor manufactures process, it is common that first by Ta powder used in capacitor by compressing,
High temperature furnace sintering in vacuum, becomes tantalum base, and tantalum base, through electrochemical reaction, forms the anode with tantalum pentoxide dielectric layer on surface
Tantalum core, immerses manganese nitrate solution the most again, thermally decomposes under vapour pressure, through dipping-thermal decomposition so circulation repeatedly, and shape
Becoming manganese dioxide layer, as capacitor cathode, the process of coating manganese dioxide layer is commonly called as tunicle.At solid electrolyte Ta capacitor
In the manufacturing, anode tantalum core needs produced thermal stress when multiple high temp thermally decomposes, medium oxidizing to tantalum pentoxide
Film can be influenced to different extents, it usually needs is mended by centre and is formed, repairs dielectric oxide film, to reduce electric leakage
Stream.
In order to improve wettability and the manganese dioxide layer compactness on oxide-film surface, and reach to strengthen and Ta2O5Medium oxygen
Change the close contact of film, to reduce leakage current, improve capacitor stability, in manganese nitrate solution, generally add some surfaces live
Property agent or reductant-oxidant etc., but, to a certain extent to mesohigh tantalum capacitor reduce leakage current effect the most largely effective.
Summary of the invention
The technical problem to be solved in the present invention, is for the system of tantalum capacitor negative electrode in middle-and high-voltage capacitor prior art
Standby technical deficiency, it is provided that one is the finest and close and can contact close tantalum capacitor negative electrode with oxide isolation film, can effectively reduce
Tantalum capacitor leakage current, improves its stability.
The purpose of the present invention is achieved by the following technical programs:
Use and in manganese nitrate impregnation liquid, add ammonium hydrogen phosphate as thermal decomposition catalyst.
Preferably, in described manganese nitrate impregnation liquid ammonium hydrogen phosphate addition is manganese nitrate solution quality 1.0～
2.0%.
It is further preferred that in described manganese nitrate impregnation liquid addition is manganese nitrate solution quality the 1.2 of ammonium hydrogen phosphate
～1.5%.
Numerous studies through the applicant show: add appropriate phosphoric acid hydrogen in the violent solution of nitric acid by as catalysis
Agent, the manganese dioxide layer of preparation is the finest and close, and can be in close contact with oxide isolation film, the electric-field strength produced under high voltage load
Degree is evenly distributed, and will not produce distortion, can effectively reduce leakage current and can improve the effect of benefit formation simultaneously, meanwhile, by with
As a example by preparation specification is the solid electrolyte Ta capacitor of 63V47 μ F, carry out the experiment of single factor addition shadow to ammonium hydrogen phosphate
Ringing and studied, result is as shown in table 1, it is known that: when ammonium hydrogen phosphate addition is too much, during due to thermal decomposition, P composition can be remained
In manganese dioxide layer, causing condenser resistance rate to increase, loss increases and its impedance operator is affected；Contrary addition
Time very few, the effect to reducing condenser leakage current is inconspicuous.Therefore, the addition of further accurate optimization ammonium hydrogen phosphate is
1.0～2.0wt%.
The impact of the addition of table 1 ammonium hydrogen phosphate
| Addition/wt% | 0 | 0.5 | 0.8 | 1.0 | 1.3 | 1.5 | 1.7 | 2.0 | 2.5 | 3.0 | 3.5 |
| Capacitance μ F | 47.9 | 46.5 | 45.9 | 47.1 | 47.7 | 47.2 | 46.8 | 46.8 | 46.7 | 46.6 | 46.4 |
| Loss % | 2.0 | 2.1 | 2.1 | 2.2 | 2.3 | 2.3 | 2.6 | 3.0 | 4.0 | 6.2 | 7.5 |
| Leakage current μ A | 8.5 | 4.8 | 3.9 | 2.5 | 2.3 | 2.2 | 2.1 | 1.9 | 1.8 | 1.8 | 1.7 |
The preparation method of the mesohigh mesohigh solid electrolyte Ta capacitor negative electrode that the present invention provides, specifically includes following
Step:
S2. the preparation of manganese nitrate impregnation liquid: add ammonium hydrogen phosphate in manganese nitrate solution, mix homogeneously obtains manganese nitrate leaching
Stain liquid；
S3. dipping: step S1 gained anode tantalum core is immersed in step S2 gained manganese nitrate impregnation liquid and impregnates, drip
Dry, standby；
S4. thermal decomposition: the anode tantalum core of step S3 process gained being put in tunicle stove and thermally decompose, thermal decomposition completes
Rear cooling；
S5. formation is mended: immerse in deionized water one ethanol solution through the anode tantalum core of thermal decomposition by step S4 gained
Row is mended and is formed, and mends to take out after formation completes and dries；
S6. as described in step S3 to S5, circulation obtains described tantalum capacitor negative electrode for 12～18 times.
Preferably, the proportion of manganese nitrate solution described in step S2 is 1.2～1.5.
Preferably, manganese nitrate solution dipping temperature described in step S3 is 35～45 DEG C, and dip time is 5～15min.
Preferably, heat decomposition temperature described in step S4 is 260 ± 5 DEG C, and the resolving time is 6～10min.
It is further preferred that drying temperature described in step S5 is 150 ± 5 DEG C, drying time is 15～20min.
Beneficial effects of the present invention:
The present invention creatively applies the common ammonium hydrogen phosphate being easy to get as additive, is entrained in manganese nitrate dipping solution
In, as catalyst in the thermal decomposition process carrying out negative electrode tunicle, through the applicant, the accurate optimization of addition is determined
And the optimization of preparation technology, preparation side based on a kind of mesohigh solid electrolyte Ta capacitor negative electrode that the present invention provides
Method, the negative electrode manganese dioxide layer prepared fine and close, thickness continuously uniformly, and is in close contact with oxide isolation film, bears at high pressure
The electric-field intensity distribution produced under lotus is uniform, will not produce distortion, it is adaptable to manufactures mesohigh tantalum capacitor, uses side of the present invention
Rated voltage 40V or the middle-and high-voltage capacitor of more than 40V not only leakage current that method prepares are little, and the stability of electrical property
Obtained and significantly improved.The tantalum capacitor cathode preparation method stable preparation process that the present invention provides is simple, cheaper starting materials easy and energy
It is effectively improved the properties of gained tantalum capacitor, it is adaptable to the manufacture of mesohigh solid tantalum capacitor, can meet well
Requirement to capacitor low-leakage current high stability.
Detailed description of the invention
The present invention is further illustrated below in conjunction with specific embodiment.Following example are only illustrative examples, not structure
Becoming inappropriate limitation of the present invention, the multitude of different ways that the present invention can be limited by summary of the invention and cover is implemented.Unless it is special
Not mentionleting alone bright, reagent, compound and equipment that the present invention uses are the art conventional reagent, compound and equipment.
Embodiment 1 63V47 μ F solid electrolyte Ta capacitor
S1 uses tantalum powder specific volume 3500CV/g, arranges sintering temperature 1950 DEG C, is to use phosphorus by the anode substrate after sintering
The formation solution of acid-sweet alcohol and water composition, carries out anodization formation under 250V voltage, forms tantalum pentoxide film as electric capacity
Device dielectric layer, prepares capacitor anode tantalum core: then according to following steps prepare tantalum capacitor cathode layer:
S2. manganese nitrate impregnation liquid preparation: weigh 15g ammonium hydrogen phosphate, adds in the manganese nitrate solution that 1000g proportion is 1.2
It is stirred, and heating makes ammonium hydrogen phosphate fully dissolve；
S3. dipping: S1 gained anode tantalum core is immersed in manganese nitrate impregnation liquid and impregnates, manganese nitrate solution dipping temperature
Being 45 DEG C, dip time is 15min,
S4 thermally decomposes: the anode tantalum core impregnated by S3 is put in tunicle stove and thermally decomposed, and arranging temperature is 260 DEG C,
Time is 8min, takes out and cool down after having thermally decomposed；
S5. formation is mended: immerse in deionized water-ethanol solution by step S4 through the anode tantalum core of thermal decomposition, form electricity
Pressure is 120V, and the benefit formation time is 20min, and after benefit formation completes, taking out in temperature is 150 DEG C, dries, the time in baking oven
20min；
S6. circulating 18 times as described in step S3 to S5, coating fine and close manganese dioxide layer is as tantalum capacitor negative electrode.
Above step gained completes tantalum core prepared by tantalum capacitor negative electrode carry out soaking graphite silver slurry, then encapsulate copper shell
In, i.e. prepare 63V47 μ F solid electrolyte Ta capacitor, randomly draw 10 and capacitor produced carry out electrical property detection, detection
Result such as table 2.
Comparative example 1 63V47 μ F solid electrolyte Ta capacitor
The same batch capacitor anode tantalum core that in employing example 1, step S1 prepares is as the anode tantalum core of this comparative example, remaining
Lower step is same as in Example 1, except for the difference that: without ammonium hydrogen phosphate during the preparation of step S2 manganese nitrate solution, prepare 63V47 μ F
Solid electrolyte Ta capacitor, randomly draws 10 and capacitor produced carries out electrical property detection, testing result such as table 3.
Embodiment 2 40V100 μ F solid electrolyte Ta capacitor
S1 uses tantalum powder specific volume 8000CV/g, arranges sintering temperature 1750 DEG C, is to use phosphorus by the anode substrate after sintering
The formation solution of acid-sweet alcohol and water composition, carries out anodization formation under 160V voltage, forms tantalum pentoxide film as electric capacity
Device dielectric layer, has prepared capacitor anode tantalum core: then according to following steps prepare tantalum capacitor cathode layer:
S2. manganese nitrate impregnation liquid preparation: weigh 20g ammonium hydrogen phosphate, adds in the manganese nitrate solution that 1000g proportion is 1.5
It is stirred, and heating makes ammonium hydrogen phosphate fully dissolve；
S3. dipping: S1 gained anode tantalum core is immersed in manganese nitrate impregnation liquid and impregnates, manganese nitrate solution dipping temperature
Being 45 DEG C, dip time is 10min；
S4 thermally decomposes: the anode tantalum core impregnated by S3 is put in tunicle stove and thermally decomposed, and arranging temperature is 260 DEG C,
Time is 8min, takes out and cool down after having thermally decomposed；
S5. formation is mended: immerse in deionized water-ethanol solution by step S4 through the anode tantalum core of thermal decomposition, form electricity
Pressure is 80V, and the benefit formation time is 20min, after benefit formation completes, takes out and dries in temperature is 150 DEG C of baking ovens, time 20min；
S6. as described in step S3 to S5, circulate 12 times (determining according to the thickness of manganese dioxide layer), the two of a coating densification
Manganese oxide layer is as tantalum capacitor negative electrode.
Above step gained completes tantalum core prepared by tantalum capacitor negative electrode carry out soaking graphite silver slurry, then encapsulate copper shell
In, i.e. prepare 40V100 μ F solid electrolyte Ta capacitor, randomly draw 10 capacitor produced leakage current tests that carry out, detection
Result such as table 4.
Comparative example 2 40V100 μ F solid electrolyte Ta capacitor
The same batch capacitor anode tantalum core that in employing example 2, step S1 prepares is as the anode tantalum core of this comparative example, remaining
Lower step is same as in Example 2, except for the difference that: without ammonium hydrogen phosphate during the preparation of step S2 manganese nitrate solution, prepare 40V100 μ
F solid electrolyte Ta capacitor, randomly draws 10 and capacitor produced carries out electrical property detection, testing result such as table 5.
Embodiment 3 63V10 μ F-E shell pieces formula solid electrolyte Ta capacitor
S1 uses tantalum powder specific volume 8000CV/g, arranges sintering temperature 1750 DEG C, is to use phosphorus by the anode substrate after sintering
The formation solution of acid-sweet alcohol and water composition, carries out anodization formation under 200V voltage, forms tantalum pentoxide film as electric capacity
Device dielectric layer, has prepared capacitor anode tantalum core: then according to following steps prepare tantalum capacitor cathode layer:
S2. manganese nitrate impregnation liquid preparation: weigh 10g ammonium hydrogen phosphate, adds in the manganese nitrate solution that 1000g proportion is 1.5
It is stirred, and heating makes ammonium hydrogen phosphate fully dissolve；
S3. dipping: S1 gained anode tantalum core is immersed in manganese nitrate impregnation liquid and impregnates, manganese nitrate solution dipping temperature
Being 35 DEG C, the time is 15min；
S4 thermally decomposes: the anode tantalum core impregnated by S3 is put in tunicle stove and thermally decomposed, and arranging temperature is 260 DEG C,
Time is 8min, takes out and cool down after having thermally decomposed；
S5. formation is mended: immerse in deionized water-ethanol solution by step S4 through the anode tantalum core of thermal decomposition, form electricity
Pressure is 80V, and the benefit formation time is 20min, after benefit formation completes, takes out and dries in temperature is 150 DEG C of baking ovens, time 20min；
S6. as described in step S3 to S5, circulate 16 times (determining according to the thickness of manganese dioxide layer), the two of a coating densification
Manganese oxide layer is as tantalum capacitor negative electrode.
Above step gained completes tantalum core prepared by tantalum capacitor negative electrode carry out soaking graphite silver slurry, then be packaged, system
Obtain 63V10 μ F-E shell pieces formula solid electrolyte Ta capacitor, randomly draw 10 capacitor produced leakage current tests that carry out, detection
Result such as table 6.
Comparative example 3 63V10 μ F-E shell pieces formula solid electrolyte Ta capacitor
The same batch capacitor anode tantalum core that in employing example 3, step S1 prepares is as the anode tantalum core of this comparative example, remaining
Lower step is same as in Example 2, except for the difference that: without ammonium hydrogen phosphate during the preparation of step S3 manganese nitrate solution, prepare 63V10 μ
F-E shell pieces formula solid electrolyte Ta capacitor, randomly draws 10 and capacitor produced carries out electrical property detection, testing result such as table
7。
Table 2
| Sequence number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | Average |
| Capacitance μ F | 47.9 | 48.5 | 46.9 | 47.3 | 47.1 | 46.9 | 47.9 | 46.6 | 47.5 | 48.2 | 47.5 |
| Loss % | 2.3 | 2.5 | 2.1 | 2.4 | 2.2 | 2.2 | 2.4 | 2.3 | 2.6 | 2.5 | 2.34 |
| Leakage current μ A | 2.0 | 2.2 | 1.9 | 2.4 | 2.3 | 2.5 | 2.0 | 2.6 | 1.8 | 2.3 | 2.2 |
Table 3
| Sequence number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | Average |
| Capacitance μ F | 47.1 | 47.5 | 47.2 | 48.1 | 46.9 | 47.2 | 47.1 | 47.6 | 46.8 | 47.1 | 47.3 |
| Loss % | 2.5 | 2.4 | 2.3 | 2.8 | 2.0 | 2.6 | 2.5 | 2.1 | 2.3 | 2.1 | 2.36 |
| Leakage current μ A | 5.8 | 7.5 | 6.8 | 5.5 | 5.8 | 8.5 | 6.5 | 6.6 | 5.8 | 7.0 | 6.58 |
Table 4
| Sequence number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | Average |
| Capacitance μ F | 100.6 | 99.8 | 98.7 | 100.8 | 100.4 | 97.9 | 98.3 | 99.6 | 99.7 | 103.2 | 99.9 |
| Loss % | 3.1 | 2.8 | 3.2 | 3.1 | 3.4 | 3.0 | 3.3 | 2.9 | 3.5 | 3.2 | 3.15 |
| Leakage current μ A | 2.8 | 4 | 3.6 | 4.2 | 3.2 | 3.5 | 3.7 | 2.5 | 2.4 | 3.0 | 3.29 |
Table 5
| Sequence number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | Average |
| Capacitance μ F | 102.4 | 101.6 | 99.9 | 101.3 | 98.9 | 99.2 | 100.3 | 99.1 | 105.2 | 98.9 | 100.7 |
| Loss % | 3.2 | 3.1 | 2.9 | 2.8 | 3.5 | 2.9 | 3.5 | 3.1 | 3.2 | 3.0 | 3.12 |
| Leakage current μ A | 8.5 | 6.5 | 7.6 | 6.0 | 5.5 | 8.5 | 6.5 | 6.8 | 9.5 | 7.8 | 7.32 |
Table 6
| Sequence number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | Average |
| Capacitance μ F | 9.5 | 9.4 | 9.6 | 9.6 | 9.4 | 9.5 | 9.5 | 9.4 | 9.4 | 9.5 | 9.5 |
| Loss % | 1.3 | 1.5 | 1.7 | 1.6 | 1.6 | 1.5 | 1.6 | 1.4 | 1.3 | 1.6 | 1.51 |
| Leakage current μ A | 0.5 | 0.2 | 0.6 | 0.5 | 0.3 | 0.8 | 0.4 | 0.3 | 0.5 | 0.6 | 0.47 |
Table 7
| Sequence number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | Average |
| Capacitance μ F | 9.7 | 9.5 | 9.5 | 9.8 | 9.7 | 9.8 | 9.9 | 9.5 | 9.3 | 9.8 | 9.65 |
| Loss % | 1.6 | 1.7 | 1.3 | 1.5 | 1.6 | 1.6 | 1.5 | 1.7 | 1.6 | 1.4 | 1.55 |
| Leakage current μ A | 2.4 | 2.1 | 1.8 | 2.8 | 3.2 | 4.0 | 3.2 | 2.5 | 3.8 | 3.6 | 2.94 |
From table 2, table 3, table 4, table 5, table 6, table 7 it can be seen that use the electric leakage of tantalum capacitor prepared by present invention process
Lumen shows little, and concordance is good, and uses chip 63V10 μ F-E shell tantalum capacitor prepared by present invention process to be 2000h's
Viability is tested, and result of the test is qualified, shows gained tantalum capacitor electric performance stablity.
Claims (8)
1. the preparation method of a mesohigh solid electrolyte mesohigh solid electrolyte Ta capacitor negative electrode, it is characterised in that
Ammonium hydrogen phosphate is added as manganese nitrate impregnation liquid in manganese nitrate solution；Described ammonium hydrogen phosphate is as the catalysis for pyrolysis
Agent.
The preparation method of mesohigh solid electrolyte Ta capacitor negative electrode the most according to claim 1, it is characterised in that described
In manganese nitrate impregnation liquid, the addition of ammonium hydrogen phosphate is the 1.0～2.0% of manganese nitrate solution quality.
The preparation method of mesohigh solid electrolyte Ta capacitor negative electrode the most according to claim 1, it is characterised in that described
The proportion of manganese nitrate leaching solution is 1.2～1.5.
The preparation method of mesohigh solid electrolyte Ta capacitor negative electrode the most according to claim 1 or claim 2, it is characterised in that
Comprise the following steps:
S1. the preparation of anode tantalum core: take the anode tantalum base prepared and be electrochemically reacted, forms tantalum pentoxide dielectric layer,
Obtain anode tantalum core standby；
S2. the preparation of manganese nitrate impregnation liquid: add ammonium hydrogen phosphate in manganese nitrate solution, mix homogeneously obtains manganese nitrate dipping
Liquid；
S3. dipping: step S1 gained anode tantalum core is immersed in step S2 gained manganese nitrate impregnation liquid and impregnates, drain, standby
With；
S4. thermal decomposition: the anode tantalum core of step S3 process gained is put in tunicle stove and thermally decomposes, after having thermally decomposed
Cooling；
S5. formation is mended: mended in anode tantalum core immersion deionized water one ethanol solution of thermal decomposition by step S4 gained
Formed, mend to take out after formation completes and dry；
S6. as described in step S3 to S5, circulation obtains described tantalum capacitor negative electrode for 12～18 times.
The preparation method of mesohigh solid electrolyte Ta capacitor negative electrode the most according to claim 4, it is characterised in that step
The proportion of manganese nitrate solution described in S2 is 1.2～1.5.
The preparation method of mesohigh solid electrolyte Ta capacitor negative electrode the most according to claim 4, it is characterised in that step
Manganese nitrate dipping temperature described in S3 is 35～45 DEG C, and dip time is 10～15min.
The preparation method of mesohigh solid electrolyte Ta capacitor negative electrode the most according to claim 4, it is characterised in that step
Heat decomposition temperature described in S4 is 260 ± 5 DEG C, and the time is 6～10min.
The preparation method of mesohigh solid electrolyte Ta capacitor negative electrode the most according to claim 4, it is characterised in that step
Mending described in S5 and forming post-baking temperature is 150 ± 5 DEG C, and temperature-time is 15～20 min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109285703A (en) * | 2018-10-26 | 2019-01-29 | 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 improving the method for tantalum capacitor voltage endurance capability and making tantalum capacitor |
| CN113722952A (en) * | 2021-08-20 | 2021-11-30 | 常州工学院 | Electric field distribution optimization method and device for hydrogen production by water electrolysis of solid polymer electrolyte |
| CN114974901A (en) * | 2022-06-07 | 2022-08-30 | 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) | Coating method for improving capacitance extraction rate of tantalum capacitor |
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| JPS59117210A (en) * | 1982-12-24 | 1984-07-06 | 日立コンデンサ株式会社 | Method of producing solid electrolytic condenser |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109285703A (en) * | 2018-10-26 | 2019-01-29 | 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 improving the method for tantalum capacitor voltage endurance capability and making tantalum capacitor |
| CN113722952A (en) * | 2021-08-20 | 2021-11-30 | 常州工学院 | Electric field distribution optimization method and device for hydrogen production by water electrolysis of solid polymer electrolyte |
| CN113722952B (en) * | 2021-08-20 | 2023-12-19 | 常州工学院 | Electric field distribution optimization method and device for hydrogen production by solid polymer electrolyte water electrolysis |
| CN114974901A (en) * | 2022-06-07 | 2022-08-30 | 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) | Coating method for improving capacitance extraction rate of tantalum capacitor |
| CN114974901B (en) * | 2022-06-07 | 2023-05-23 | 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) | Coating method for improving capacitance extraction rate of tantalum capacitor |
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