CN106057469B - A kind of preparation method of mesohigh solid electrolyte Ta capacitor cathode - Google Patents
A kind of preparation method of mesohigh solid electrolyte Ta capacitor cathode Download PDFInfo
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- CN106057469B CN106057469B CN201610719935.4A CN201610719935A CN106057469B CN 106057469 B CN106057469 B CN 106057469B CN 201610719935 A CN201610719935 A CN 201610719935A CN 106057469 B CN106057469 B CN 106057469B
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- 239000003990 capacitor Substances 0.000 title claims abstract description 72
- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 65
- 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 43
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 29
- 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 15
- 239000000654 additive Substances 0.000 claims abstract description 13
- 230000000996 additive effect Effects 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- 238000002803 maceration Methods 0.000 claims description 16
- 238000007598 dipping method Methods 0.000 claims description 8
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 8
- 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 7
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 238000003487 electrochemical reaction Methods 0.000 claims description 2
- 238000001816 cooling 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
- 238000000034 method Methods 0.000 abstract description 9
- 238000005457 optimization Methods 0.000 abstract description 5
- 238000002955 isolation Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000005684 electric field Effects 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000001514 detection 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
- 238000002386 leaching Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- 239000010439 graphite Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000203 mixture Substances 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
- 238000005245 sintering 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
- 239000003795 chemical substances by application 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
- 238000005516 engineering 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
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000002708 enhancing effect Effects 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
- 239000004615 ingredient Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 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
- 239000007787 solid 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
The invention discloses a kind of preparation methods preparing mesohigh solid electrolyte Ta capacitor cathode.The present invention creatively applies additive of the common ammonium hydrogen phosphate being easy to get as manganese nitrate solution, it is used as catalyst in manganese nitrate carries out thermal decomposition process, accurate optimization determination and the optimization of preparation process by the applicant to additive amount, based on a kind of preparation method of mesohigh solid electrolyte Ta capacitor cathode provided by the invention, the cathode manganese dioxide layer being prepared is continuously fine and close, and it can be in close contact with oxide isolation film, the electric-field intensity distribution generated under high voltage load is uniform, distortion is not will produce, not only leakage current is small for the middle-and high-voltage capacitor for the rated voltage 40V or more being prepared especially with the method for the present invention, and the stability of electrical property was obtained and was significantly improved.Tantalum capacitor cathode preparation method stable preparation process provided by the invention is simple, raw material is cheap easy and properties that are can effectively improving gained tantalum capacitor, is easy to industrialization production.
Description
Technical field
The present invention relates to electronic technology fields, more particularly, to a kind of mesohigh solid electrolyte Ta capacitor cathode
Preparation method.
Background technology
Solid electrolyte Ta capacitor manufactures process, typically first by Ta powder used in capacitor by compression moulding,
Vacuum high temperature stove is sintered, and at tantalum base, tantalum base forms on surface through electrochemical reaction and has the anode of tantalum pentoxide dielectric layer
Tantalum core, then immerses manganese nitrate solution again, is thermally decomposed under vapour pressure, multiple by dipping-thermal decomposition cycle in this way, shape
At manganese dioxide layer, as capacitor cathode, the process of coating manganese dioxide layer is commonly called as envelope.In solid electrolyte Ta capacitor
In the manufacturing, generated thermal stress, medium oxidizing to tantalum pentoxide when anode tantalum core needs to thermally decompose through multiple high temp
Film can be influenced to different extents, it usually needs is mended and is formed by centre, repaired to dielectric oxide film, to reduce electric leakage
Stream.
In order to improve the wettability and manganese dioxide layer compactness of oxidation film surface, and reach enhancing and Ta2O5Medium oxygen
The close contact for changing film improves capacitor stability to reduce leakage current, and the work of some surfaces is usually added in manganese nitrate solution
Property agent or reductant-oxidant etc., still, to a certain extent to mesohigh tantalum capacitor reduce leakage current effect it is not largely effective.
Invention content
The technical problem to be solved in the present invention is the system for middle-and high-voltage capacitor tantalum capacitor cathode in the prior art
Standby technical deficiency provides a kind of continuous fine and close and can contact close tantalum capacitor cathode 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：
It is used as thermal decomposition catalyst using ammonium hydrogen phosphate is added in manganese nitrate maceration extract.
Preferably, in the manganese nitrate maceration extract ammonium hydrogen phosphate additive amount be manganese nitrate solution quality 1.0~
2.0%.
It is further preferred that the additive amount of ammonium hydrogen phosphate is the 1.2 of manganese nitrate solution quality in the manganese nitrate maceration extract
~1.5%.
Show by the numerous studies of the applicant：Suitable phosphoric acid hydrogen is added in the violent solution of nitric acid by as catalysis
The manganese dioxide layer of agent, preparation is continuously fine and close, and can be in close contact with oxide isolation film, the electric-field strength generated under high voltage load
Degree is evenly distributed, and not will produce distortion, can effectively reduce leakage current and while can improve benefit formation effect, meanwhile, by with
For preparing the solid electrolyte Ta capacitor that specification is 63V47 μ F, additive amount shadow of the experiment of single factor to ammonium hydrogen phosphate is carried out
Sound is studied, and the results are shown in Table 1, it is known that：When ammonium hydrogen phosphate additive amount is excessive, since P ingredients can be remained when thermal decomposition
In manganese dioxide layer, condenser resistance rate is caused to increase, loss increases and its impedance operator is affected；Opposite additive amount
When very few, to reducing the effect unobvious of condenser leakage current.Therefore, the additive amount of further accurate optimization ammonium hydrogen phosphate is
1.0~2.0wt%.
The influence of the additive amount of 1 ammonium hydrogen phosphate of table
| Additive amount/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 |
| % is lost | 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 mesohigh mesohigh solid electrolyte Ta capacitor cathode provided by the invention, specifically includes following
Step：
S2. the preparation of manganese nitrate maceration extract：Ammonium hydrogen phosphate is added in manganese nitrate solution, is uniformly mixed and obtains manganese nitrate leaching
Stain liquid；
S3. it impregnates：Anode tantalum core obtained by step S1 is immersed in manganese nitrate maceration extract obtained by step S2 and is impregnated, is dripped
It is dry, it is spare；
S4. it thermally decomposes：The anode tantalum core of step S3 processing gained is put into envelope stove and is thermally decomposed, thermal decomposition is completed
Postcooling；
S5. it mends and is formed：By the anode tantalum core by thermal decomposition obtained by step S4 immerse in one ethanol solution of deionized water into
Row, which is mended, to be formed, and is mended and is taken out drying after the completion of being formed；
S6. the tantalum capacitor cathode is obtained by being recycled 12~18 times described in step S3 to S5.
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：
Creatively the common ammonium hydrogen phosphate being easy to get of application is entrained in manganese nitrate dipping solution to the present invention as additive
In, it is used as catalyst in the thermal decomposition process for carrying out cathode envelope, the accurate optimization of additive amount is determined by the applicant
And the optimization of preparation process, based on a kind of preparation side of mesohigh solid electrolyte Ta capacitor cathode provided by the invention
Method, the continuous densification of the cathode manganese dioxide layer being prepared, thickness are uniform, and are in close contact with oxide isolation film, negative in high pressure
The electric-field intensity distribution generated under lotus is uniform, not will produce distortion, is suitable for manufacture mesohigh tantalum capacitor, uses present invention side
Not only leakage current is small for the middle-and high-voltage capacitor for the rated voltage 40V or 40V or more that method is prepared, but also the stability of electrical property
It obtained and significantly improved.Tantalum capacitor cathode preparation method stable preparation process provided by the invention is simple, the cheap easy and energy of raw material
The properties of gained tantalum capacitor are effectively improved, is suitable for the manufacture of mesohigh solid tantalum capacitor, can meet well
Requirement to capacitor low-leakage current high stability.
Specific implementation mode
It is further illustrated the present invention with reference to specific embodiment.Following embodiment is only illustrative examples, not structure
At inappropriate limitation of the present invention, the multitude of different ways that the present invention can be limited and be covered by invention content is implemented.Unless special
Do not mentionlet alone bright, reagent, compound and the equipment that the present invention uses is the art conventional reagent, compound and equipment.
1 63V47 μ F solid electrolyte Ta capacitors of embodiment
S1 uses tantalum powder specific volume 3500CV/g, and 1950 DEG C of sintering temperature is arranged, and is to use phosphorus by sintered anode substrate
The formation solution of acid-sweet alcohol and water composition, under 250V voltages carrying out anodization forms, and forms tantalum pentoxide film as capacitance
Capacitor anode tantalum core is made in device dielectric layer：Then tantalum capacitor cathode layer is prepared in accordance with the following steps：
S2. manganese nitrate maceration extract is prepared：15g ammonium hydrogen phosphates are weighed, are added in the manganese nitrate solution that 1000g proportions are 1.2
It is stirred, and heating makes ammonium hydrogen phosphate fully dissolve；
S3. it impregnates：Anode tantalum core obtained by S1 is immersed in manganese nitrate maceration extract and is impregnated, manganese nitrate solution dipping temperature
It is 45 DEG C, dip time 15min,
S4 is thermally decomposed：The anode tantalum core that S3 impregnates is put into envelope stove and is thermally decomposed, setting temperature is 260 DEG C,
Time is 8min, takes out and is cooled down after the completion of thermal decomposition；
S5. it mends and is formed：Anode tantalum core by step S4 by thermal decomposition immerses in deionized water-ethanol solution, forms electricity
Pressure is 120V, and benefit forms the time as 20min, mends after the completion of being formed, and it is 150 DEG C to take out in temperature, is dried in baking oven, the time
20min；
S6. it presses and is recycled 18 times described in step S3 to S5, the manganese dioxide layer of coating densification is as tantalum capacitor cathode.
Tantalum core prepared by tantalum capacitor cathode will be completed obtained by above step and carries out leaching graphite silver paste, then encapsulates copper shell
It is interior, 63V47 μ F solid electrolyte Ta capacitors are obtained, 10 capacitor produced progress electrical property detections are randomly selected, are detected
As a result such as table 2.
1 63V47 μ F solid electrolyte Ta capacitors of comparative example
It is remaining using the anode tantalum core with batch capacitor anode tantalum core as this comparative example made from step S1 in example 1
Lower step is same as Example 1, unlike：Step S2 manganese nitrate solutions do not add ammonium hydrogen phosphate when preparing, and 63V47 μ F are made
Solid electrolyte Ta capacitor randomly selects 10 capacitor produced progress electrical property detections, testing result such as table 3.
2 40V100 μ F solid electrolyte Ta capacitors of embodiment
S1 uses tantalum powder specific volume 8000CV/g, and 1750 DEG C of sintering temperature is arranged, and is to use phosphorus by sintered anode substrate
The formation solution of acid-sweet alcohol and water composition, under 160V voltages carrying out anodization forms, and forms tantalum pentoxide film as capacitance
Capacitor anode tantalum core has been made in device dielectric layer：Then tantalum capacitor cathode layer is prepared in accordance with the following steps：
S2. manganese nitrate maceration extract is prepared：20g ammonium hydrogen phosphates are weighed, are added in the manganese nitrate solution that 1000g proportions are 1.5
It is stirred, and heating makes ammonium hydrogen phosphate fully dissolve；
S3. it impregnates：Anode tantalum core obtained by S1 is immersed in manganese nitrate maceration extract and is impregnated, manganese nitrate solution dipping temperature
It is 45 DEG C, dip time 10min；
S4 is thermally decomposed：The anode tantalum core that S3 impregnates is put into envelope stove and is thermally decomposed, setting temperature is 260 DEG C,
Time is 8min, takes out and is cooled down after the completion of thermal decomposition；
S5. it mends and is formed：Anode tantalum core by step S4 by thermal decomposition immerses in deionized water-ethanol solution, forms electricity
Pressure is 80V, and benefit forms the time as 20min, mends after the completion of being formed, and takes out and is dried in temperature is 150 DEG C of baking ovens, time 20min；
S6. it presses and is recycled described in step S3 to S5 12 times (being determined according to the thickness of manganese dioxide layer), coating one fine and close two
Manganese oxide layer is as tantalum capacitor cathode.
Tantalum core prepared by tantalum capacitor cathode will be completed obtained by above step and carries out leaching graphite silver paste, then encapsulates copper shell
It is interior, 40V100 μ F solid electrolyte Ta capacitors are obtained, 10 capacitor produced carry out leakage current tests are randomly selected, are detected
As a result such as table 4.
2 40V100 μ F solid electrolyte Ta capacitors of comparative example
It is remaining using the anode tantalum core with batch capacitor anode tantalum core as this comparative example made from step S1 in example 2
Lower step is same as Example 2, unlike：Step S2 manganese nitrate solutions do not add ammonium hydrogen phosphate when preparing, and 40V100 μ are made
F solid electrolyte Ta capacitors randomly select 10 capacitor produced progress electrical property detections, testing result such as table 5.
3 63V10 μ F-E shell pieces formula solid electrolyte Ta capacitors of embodiment
S1 uses tantalum powder specific volume 8000CV/g, and 1750 DEG C of sintering temperature is arranged, and is to use phosphorus by sintered anode substrate
The formation solution of acid-sweet alcohol and water composition, under 200V voltages carrying out anodization forms, and forms tantalum pentoxide film as capacitance
Capacitor anode tantalum core has been made in device dielectric layer：Then tantalum capacitor cathode layer is prepared in accordance with the following steps：
S2. manganese nitrate maceration extract is prepared：10g ammonium hydrogen phosphates are weighed, are added in the manganese nitrate solution that 1000g proportions are 1.5
It is stirred, and heating makes ammonium hydrogen phosphate fully dissolve；
S3. it impregnates：Anode tantalum core obtained by S1 is immersed in manganese nitrate maceration extract and is impregnated, manganese nitrate solution dipping temperature
It is 35 DEG C, time 15min；
S4 is thermally decomposed：The anode tantalum core that S3 impregnates is put into envelope stove and is thermally decomposed, setting temperature is 260 DEG C,
Time is 8min, takes out and is cooled down after the completion of thermal decomposition；
S5. it mends and is formed：Anode tantalum core by step S4 by thermal decomposition immerses in deionized water-ethanol solution, forms electricity
Pressure is 80V, and benefit forms the time as 20min, mends after the completion of being formed, and takes out and is dried in temperature is 150 DEG C of baking ovens, time 20min；
S6. it presses and is recycled described in step S3 to S5 16 times (being determined according to the thickness of manganese dioxide layer), coating one fine and close two
Manganese oxide layer is as tantalum capacitor cathode.
Tantalum core prepared by tantalum capacitor cathode will be completed obtained by above step and carries out leaching graphite silver paste, then is packaged, and is made
63V10 μ F-E shell pieces formula solid electrolyte Ta capacitors are obtained, 10 capacitor produced carry out leakage current tests are randomly selected, are detected
As a result such as table 6.
3 63V10 μ F-E shell pieces formula solid electrolyte Ta capacitors of comparative example
It is remaining using the anode tantalum core with batch capacitor anode tantalum core as this comparative example made from step S1 in example 3
Lower step is same as Example 2, unlike：Step S3 manganese nitrate solutions do not add ammonium hydrogen phosphate when preparing, and 63V10 μ are made
F-E shell pieces formula solid electrolyte Ta capacitors randomly select 10 capacitor produced progress electrical property detections, testing result such as table
7。
Table 2
| Serial number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | Mean value |
| 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 |
| % is lost | 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
| Serial number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | Mean value |
| 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 |
| % is lost | 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
| Serial number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | Mean value |
| 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 |
| % is lost | 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
| Serial number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | Mean value |
| 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 |
| % is lost | 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
| Serial number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | Mean value |
| 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 |
| % is lost | 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
| Serial number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | Mean value |
| 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 |
| % is lost | 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 as can be seen that using the electric leakage of tantalum capacitor prepared by present invention process
Lumen shows small, and consistency is good, and has been 2000h's using chip 63V10 μ F-E shell tantalum capacitors prepared by present invention process
Viability is tested, and test result is qualified, shows gained tantalum capacitor electric performance stablity.
Claims (6)
1. a kind of preparation method of mesohigh solid electrolyte Ta capacitor cathode, which is characterized in that add in manganese nitrate solution
Enter ammonium hydrogen phosphate as manganese nitrate maceration extract；Catalyst of the ammonium hydrogen phosphate as pyrolysis；Using anode tantalum base into
Tantalum pentoxide dielectric layer is formed after row electrochemical reaction, to obtain anode tantalum core, then anode tantalum core is soaked by manganese nitrate
It is put into envelope stove and is thermally decomposed after stain liquid dipping, carry out benefit formation after cooling, it is final to obtain tantalum capacitor cathode；
The additive amount of ammonium hydrogen phosphate is the 1.0~2.0% of manganese nitrate solution quality in the manganese nitrate maceration extract；
The proportion of the manganese nitrate maceration extract is 1.2~1.5.
2. the preparation method of mesohigh solid electrolyte Ta capacitor cathode according to claim 1, which is characterized in that including
Following steps：
S1. the preparation of anode tantalum core：It takes the anode tantalum base prepared to be electrochemically reacted, forms tantalum pentoxide dielectric layer,
It is spare to obtain anode tantalum core；
S2. the preparation of manganese nitrate maceration extract：Ammonium hydrogen phosphate is added in manganese nitrate solution, is uniformly mixed and obtains manganese nitrate dipping
Liquid；
S3. it impregnates：Anode tantalum core obtained by step S1 is immersed in manganese nitrate maceration extract obtained by step S2 and is impregnated, is drained, it is standby
With；
S4. it thermally decomposes：The anode tantalum core of step S3 processing gained is put into envelope stove and is thermally decomposed, it is cold after the completion of thermal decomposition
But；
S5. it mends and is formed：Anode tantalum core by thermal decomposition obtained by step S4 is immersed in deionized water-ethanol solution and carries out benefit shape
At mending formation, taking-up is dried after the completion；
S6. the tantalum capacitor cathode is obtained by being recycled 12~18 times described in step S3 to S5.
3. the preparation method of mesohigh solid electrolyte Ta capacitor cathode according to claim 2, which is characterized in that step
The proportion of manganese nitrate solution described in S2 is 1.2~1.5.
4. the preparation method of mesohigh solid electrolyte Ta capacitor cathode according to claim 2, which is characterized in that step
Manganese nitrate dipping temperature described in S3 is 35~45 DEG C, and dip time is 10~15min.
5. the preparation method of mesohigh solid electrolyte Ta capacitor cathode according to claim 2, which is characterized in that step
Heat decomposition temperature described in S4 is 260 ± 5 DEG C, and the time is 6~10min.
6. the preparation method of mesohigh solid electrolyte Ta capacitor cathode according to claim 2, which is characterized in that step
It is 150 ± 5 DEG C to be mended described in S5 and form post-baking temperature, and drying time is 15~20min.
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