CN112908704B - Electrolyte of high-temperature-resistant capacitor and capacitor - Google Patents
Electrolyte of high-temperature-resistant capacitor and capacitor Download PDFInfo
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- CN112908704B CN112908704B CN202110153583.1A CN202110153583A CN112908704B CN 112908704 B CN112908704 B CN 112908704B CN 202110153583 A CN202110153583 A CN 202110153583A CN 112908704 B CN112908704 B CN 112908704B
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- 239000003990 capacitor Substances 0.000 title claims abstract description 91
- 239000003792 electrolyte Substances 0.000 title claims abstract description 36
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 57
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000004327 boric acid Substances 0.000 claims abstract description 41
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 29
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 13
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 13
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 62
- 239000002041 carbon nanotube Substances 0.000 claims description 39
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 39
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 20
- 238000009210 therapy by ultrasound Methods 0.000 claims description 14
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 13
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 12
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 claims description 12
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000000967 suction filtration Methods 0.000 claims description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-YPZZEJLDSA-N carbon-10 atom Chemical group [10C] OKTJSMMVPCPJKN-YPZZEJLDSA-N 0.000 claims description 2
- 238000005470 impregnation Methods 0.000 claims 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- 238000005538 encapsulation Methods 0.000 claims 1
- 238000007598 dipping method Methods 0.000 description 21
- 238000004806 packaging method and process Methods 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 230000032683 aging Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000007743 anodising Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 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 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
- 230000008016 vaporization 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
- H01G9/022—Electrolytes; Absorbents
- H01G9/035—Liquid electrolytes, e.g. impregnating materials
-
- 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
- H01G9/145—Liquid electrolytic capacitors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention relates to the field of capacitors, and provides an electrolyte of a high-temperature-resistant capacitor and a preparation method thereof, which are used for improving the performance of a tantalum capacitor at high temperature. The electrolyte of the high-temperature resistant capacitor comprises 50-80 parts by mass of silica sol, 0.4-0.6 part by mass of copper sulfate, 0.4-0.6 part by mass of 10% chloroplatinic acid, 20-40 parts by mass of concentrated sulfuric acid and 1-2 parts by mass of boric acid. The performance of the capacitor at high temperature is obviously improved, and the capacity loss of the capacitor at high temperature is reduced.
Description
Technical Field
The invention relates to the field of capacitors, in particular to electrolyte of a high-temperature-resistant capacitor.
Background
The tantalum electrolytic capacitor is used as an important branch of the electrolytic capacitor, is widely applied to the aspects of communication, military communication, submarine cables, advanced electronic devices, civil electric appliances and the like, and the working environment of the non-solid electrolyte tantalum capacitor in China is mainly suitable for working in a low-temperature environment.
The performance of the tantalum capacitor is seriously reduced at high temperature.
Disclosure of Invention
The invention solves the technical problem of providing the electrolyte of the high-temperature resistant capacitor for improving the performance of the tantalum capacitor at high temperature.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the electrolyte of the high-temperature resistant capacitor comprises 50-80 parts by mass of silica sol, 0.4-0.6 part by mass of copper sulfate, 0.4-0.6 part by mass of 10% chloroplatinic acid, 20-40 parts by mass of concentrated sulfuric acid and 1-2 parts by mass of boric acid.
The boric acid is added into the electrolyte, so that the high-temperature resistance of the electrolyte is improved.
The performance of the capacitor at high temperature is obviously improved, and the capacity loss of the capacitor at high temperature is reduced.
Preferably, the silica sol comprises 59-80 parts by mass of silica sol, 0.5-0.6 part by mass of copper sulfate, 0.5-0.6 part by mass of 10% chloroplatinic acid, 31-40 parts by mass of concentrated sulfuric acid and 1.5-2 parts by mass of boric acid.
Preferably, the silica sol comprises 59 parts by mass of silica sol, 0.5 part by mass of copper sulfate, 0.5 part by mass of 10% chloroplatinic acid, 31 parts by mass of concentrated sulfuric acid and 1.5 parts by mass of boric acid.
Preferably, the silica sol is a modified silica sol.
Preferably, the preparation method of the modified silica sol comprises the following steps:
taking 50-60 parts by mass of silica sol, 0.01-0.02 part by mass of carbon nano tube and 10-50 parts by mass of absolute ethyl alcohol;
dispersing the carbon nano tube into absolute ethyl alcohol to obtain dispersion liquid;
and mixing the dispersion liquid and the silica sol, uniformly stirring, and performing ultrasonic treatment for 30min to obtain the modified silica sol.
Preferably, the carbon nanotubes are modified carbon nanotubes, and the preparation method of the modified carbon nanotubes comprises the following steps:
taking 0.01-0.02 mass part of carbon nano tube, 0.1-0.5 mass part of N, N-dicyclohexylcarbodiimide, 1-3 mass parts of ethylenediamine, 0.1-0.3 mass part of boric acid, 0.2-0.3 mass part of 20% ammonia water, 1-5 mass parts of propylene glycol monomethyl ether and 1-3 mass parts of methylbenzene;
adding a carbon nano tube into ethylenediamine, adding N, N-dicyclohexylcarbodiimide, uniformly mixing, performing ultrasonic treatment for 10min, heating to 120 ℃ in an oil bath, keeping the temperature for 24h, after the reaction is finished, clarifying with absolute ethyl alcohol for three times, performing suction filtration, respectively cleaning the obtained filter residue with deionized water and absolute ethyl alcohol for 3 times, and performing vacuum drying on the filter residue for 24h at 40 ℃ to obtain a pre-modified carbon nano tube;
adding the pre-modified carbon nano tube into propylene glycol monomethyl ether, adding boric acid, carrying out ultrasonic treatment for 10min, adding 20% ammonia water and toluene, heating in a water bath to 90-100 ℃, refluxing for 6h, carrying out suction filtration, cleaning filter residues with tetrahydrofuran for 4-6 times, and then carrying out vacuum drying for 12h at 40 ℃ to obtain the modified carbon nano tube.
Preferably, 0.015 to 0.02 mass portion of carbon nano tube, 0.25 to 0.5 mass portion of N, N-dicyclohexylcarbodiimide, 2 to 3 mass portions of ethylenediamine, 0.2 to 0.3 mass portion of boric acid, 0.25 to 0.3 mass portion of 20% ammonia water, 4 to 5 mass portions of propylene glycol monomethyl ether and 1.5 to 3 mass portions of toluene are taken.
Preferably, 0.015 part by mass of carbon nano tube, 0.25 part by mass of N, N-dicyclohexylcarbodiimide, 2 parts by mass of ethylenediamine, 0.2 part by mass of boric acid, 0.25 part by mass of 20% ammonia water, 4 parts by mass of propylene glycol monomethyl ether and 1.5 parts by mass of toluene are taken.
The electrolyte is injected into the shell of the capacitor, and the capacitor is a tantalum capacitor.
Preferably, the electrode of the tantalum capacitor is subjected to dipping treatment before being assembled into the capacitor shell, and dipping liquid adopted by the dipping treatment comprises 98-100 parts by mass of 40% sulfuric acid and 0.5-2 parts by mass of boric acid.
Compared with the prior art, the invention has the beneficial effects that: the performance of the capacitor at high temperature is obviously improved, and the capacity loss of the capacitor at high temperature is reduced.
The boric acid loaded on the carbon nano tube can reduce the internal resistance of the electrolyte, and can be used together with the boric acid in the electrolyte to further prevent the electrolyte from vaporizing at high temperature. The modified carbon nano tube particles are not volatilized, and the stability of the electrolyte at high pressure and high temperature can be effectively improved by combining the modified carbon nano tube particles with silica sol; therefore, the invention is safe, greatly improves the reliability of the capacitor, and particularly improves the performance of the capacitor at high temperature.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to be limiting thereof.
Example 1
An electrolyte of a high-temperature resistant capacitor comprises 59g of silica sol, 0.5g of copper sulfate, 0.5g of 10% chloroplatinic acid, 31g of concentrated sulfuric acid and 1.5g of boric acid.
The silica sol is modified silica sol.
The preparation method of the modified silica sol comprises the following steps:
taking 59g of silica sol, 0.01-0.02 g of carbon nano tube and 15g of absolute ethyl alcohol;
dispersing the carbon nano tube into absolute ethyl alcohol to obtain dispersion liquid;
and mixing the dispersion liquid and the silica sol, uniformly stirring, and performing ultrasonic treatment for 30min to obtain the modified silica sol.
The carbon nano tube is a modified carbon nano tube, and the preparation method of the modified carbon nano tube comprises the following steps:
taking 0.015g of carbon nano tube, 0.25g of N, N-dicyclohexylcarbodiimide, 2g of ethylenediamine, 0.2g of boric acid, 0.25g of 20% ammonia water, 4g of propylene glycol monomethyl ether and 1.5g of toluene;
adding a carbon nano tube into ethylenediamine, adding N, N-dicyclohexylcarbodiimide, uniformly mixing, performing ultrasonic treatment for 10min, heating to 120 ℃ in an oil bath, keeping the temperature for 24h, after the reaction is finished, clarifying with absolute ethyl alcohol for three times, performing suction filtration, respectively cleaning the obtained filter residue with deionized water and absolute ethyl alcohol for 3 times, and performing vacuum drying on the filter residue for 24h at 40 ℃ to obtain a pre-modified carbon nano tube;
adding the pre-modified carbon nano tube into propylene glycol monomethyl ether, adding boric acid, carrying out ultrasonic treatment for 10min, adding 20% ammonia water and toluene, heating in a water bath to 90-100 ℃, refluxing for 6h, carrying out suction filtration, cleaning filter residues with tetrahydrofuran for 4-6 times, and then carrying out vacuum drying for 12h at 40 ℃ to obtain the modified carbon nano tube.
And injecting the electrolyte into the shell of the capacitor, and packaging to obtain the high-temperature-resistant capacitor, wherein the capacitor is a tantalum capacitor. The electrode of the tantalum capacitor is subjected to dipping treatment before being assembled into a capacitor shell, and dipping liquid adopted in the dipping treatment comprises 99g of 40% sulfuric acid and 1g of boric acid.
The boric acid is added into the electrolyte, so that the high-temperature resistance of the electrolyte is improved.
The performance of the capacitor at high temperature is obviously improved, and the capacity loss of the capacitor at high temperature is reduced.
Example 2
An electrolyte of a high-temperature resistant capacitor comprises 59g of silica sol, 0.5g of copper sulfate, 0.5g of 10% chloroplatinic acid, 31g of concentrated sulfuric acid and 1.5g of boric acid.
And injecting the electrolyte into the shell of the capacitor, and packaging to obtain the high-temperature-resistant capacitor, wherein the capacitor is a tantalum capacitor. The electrode of the tantalum capacitor is subjected to dipping treatment before being assembled into a capacitor shell, and dipping liquid adopted in the dipping treatment comprises 99g of 40% sulfuric acid and 1g of boric acid.
Example 3
An electrolyte of a high-temperature resistant capacitor comprises 59g of silica sol, 0.5g of copper sulfate, 0.5g of 10% chloroplatinic acid, 31g of concentrated sulfuric acid and 1.5g of boric acid.
The silica sol is modified silica sol.
The preparation method of the modified silica sol comprises the following steps:
taking 59g of silica sol, 0.01-0.02 g of carbon nano tube and 15g of absolute ethyl alcohol;
dispersing the carbon nano tube into absolute ethyl alcohol to obtain dispersion liquid;
and mixing the dispersion liquid and the silica sol, uniformly stirring, and performing ultrasonic treatment for 30min to obtain the modified silica sol.
And injecting the electrolyte into a shell of the capacitor, and packaging to obtain the high-temperature resistant capacitor, wherein the capacitor is a tantalum capacitor. The electrode of the tantalum capacitor is subjected to dipping treatment before being assembled into a capacitor shell, and dipping liquid adopted in the dipping treatment comprises 99g of 40% sulfuric acid and 1g of boric acid.
Example 4
An electrolyte of a high-temperature resistant capacitor comprises 59g of silica sol, 0.5g of copper sulfate, 0.5g of 10% chloroplatinic acid, 31g of concentrated sulfuric acid and 1.5g of boric acid.
The silica sol is modified silica sol.
The preparation method of the modified silica sol comprises the following steps:
taking 59g of silica sol, 0.01-0.02 g of carbon nano tube and 15g of absolute ethyl alcohol;
dispersing the carbon nano tube into absolute ethyl alcohol to obtain dispersion liquid;
and mixing the dispersion liquid and the silica sol, uniformly stirring, and performing ultrasonic treatment for 30min to obtain the modified silica sol.
The carbon nano tube is a modified carbon nano tube, and the preparation method of the modified carbon nano tube comprises the following steps:
taking 0.015g of carbon nano tube, 0.25g of N, N-dicyclohexylcarbodiimide and 2g of ethylenediamine;
adding carbon nano tubes into ethylenediamine, adding N, N-dicyclohexylcarbodiimide, uniformly mixing, performing ultrasonic treatment for 10min, heating to 120 ℃ in an oil bath, keeping the temperature for 24h, after the reaction is finished, clarifying with absolute ethyl alcohol for three times, performing suction filtration, respectively cleaning the obtained filter residue with deionized water and absolute ethyl alcohol for 3 times, and performing vacuum drying on the filter residue for 24h at 40 ℃ to obtain the modified carbon nano tubes.
And injecting the electrolyte into the shell of the capacitor, and packaging to obtain the high-temperature-resistant capacitor, wherein the capacitor is a tantalum capacitor. The electrode of the tantalum capacitor is subjected to dipping treatment before being assembled into a capacitor shell, and dipping liquid adopted in the dipping treatment comprises 99g of 40% sulfuric acid and 1g of boric acid.
Example 5
An electrolyte of a high-temperature resistant capacitor comprises 59g of silica sol, 0.5g of copper sulfate, 0.5g of 10% chloroplatinic acid, 31g of concentrated sulfuric acid and 1.5g of boric acid.
The silica sol is modified silica sol.
The preparation method of the modified silica sol comprises the following steps:
taking 59g of silica sol, 0.01-0.02 g of carbon nano tube and 15g of absolute ethyl alcohol;
dispersing the carbon nano tube into absolute ethyl alcohol to obtain dispersion liquid;
and mixing the dispersion liquid and the silica sol, uniformly stirring, and performing ultrasonic treatment for 30min to obtain the modified silica sol.
The carbon nano tube is a modified carbon nano tube, and the preparation method of the modified carbon nano tube comprises the following steps:
taking 0.015g of carbon nano tube, 0.2g of boric acid, 0.25g of 20% ammonia water, 4g of propylene glycol monomethyl ether and 1.5g of toluene;
adding the carbon nano tube into propylene glycol monomethyl ether, adding boric acid, carrying out ultrasonic treatment for 10min, adding 20% ammonia water and toluene, heating in a water bath to 90-100 ℃, refluxing for 6h, carrying out suction filtration, cleaning filter residues with tetrahydrofuran for 4-6 times, and carrying out vacuum drying for 12h at 40 ℃ to obtain the modified carbon nano tube.
And injecting the electrolyte into the shell of the capacitor, and packaging to obtain the high-temperature-resistant capacitor, wherein the capacitor is a tantalum capacitor. The electrode of the tantalum capacitor is subjected to dipping treatment before being assembled into a capacitor shell, and dipping liquid adopted in the dipping treatment comprises 99g of 40% sulfuric acid and 1g of boric acid.
Comparative example 1
An electrolyte of a high-temperature resistant capacitor comprises 59g of silica sol, 0.5g of copper sulfate, 0.5g of 10% chloroplatinic acid, 31g of concentrated sulfuric acid, 1.6g of boric acid and 0.015g of carbon nano tubes.
And injecting the electrolyte into the shell of the capacitor, and packaging to obtain the high-temperature-resistant capacitor, wherein the capacitor is a tantalum capacitor. The electrode of the tantalum capacitor is subjected to dipping treatment before being assembled into a capacitor shell, and dipping liquid adopted in the dipping treatment comprises 99g of 40% sulfuric acid and 1g of boric acid.
The preparation method of the silica sol in the above embodiment is:
taking 1.5g of silicon simple substance, 12g of deionized water and 0.015g of sodium hydroxide;
fully stirring deionized water and a silicon simple substance, adding sodium hydroxide, heating in a water bath to 80 ℃, and reacting for 1h;
cooling the obtained product to room temperature, standing for 10h, then performing suction filtration at 0.0001-0.001 Pa, and performing centrifugal separation on the suction-filtered product to obtain liquid, namely the silica sol.
Examples of the experiments
Adopting 8500CV/g specific volume of tantalum powder and 1700 ℃ of sintering temperature, anodizing the sintered anode substrate by using a forming solution consisting of phosphoric acid and water at 100V voltage to form tantalum pentoxide as a capacitor medium, then preparing a tantalum anode core into a capacitor according to the preparation method in comparative example 1 of grade 1-6, testing electrical properties, and testing the electrical properties of the product through packaging, normal-temperature aging, aging at 85 ℃, aging at 125 ℃ and high-temperature aging at 220 ℃; then, a lifetime test of applying a voltage of 16V at a high temperature of 220 ℃ was carried out for 240 hours.
As can be seen from the above table, in example 1, the modified silica sol is added to the solution, and the carbon nanotubes are loaded with boric acid, so that the carbon nanotubes have excellent high temperature resistance and less capacity loss after a high temperature life test.
In example 2, the modified silica sol was not used, and in example 3, the carbon nanotubes for modifying the silica sol were not loaded with boric acid, and the capacity was greatly decreased after the high-temperature life test, and the performance at high temperature was weaker than that in example 1.
The carbon nanotubes in examples 4 to 5 were modified by a method different from that in example 1, and the effect was weaker than that in example 1, indicating that the high temperature resistance of the capacitor could be improved to some extent by loading the carbon nanotubes with boric acid in a certain manner.
The electrolyte in the comparative example 1 directly increases the content of boric acid, and directly disperses the carbon nanotubes in the electrolyte, and the high temperature resistance of the capacitor is not improved.
The above detailed description is specific to possible embodiments of the present invention, and the above embodiments are not intended to limit the scope of the present invention, and all equivalent implementations or modifications that do not depart from the scope of the present invention should be included in the present claims.
Claims (7)
1. The electrolyte of the high-temperature resistant capacitor is characterized by comprising 50-80 parts by mass of silica sol, 0.4-0.6 part by mass of copper sulfate, 0.4-0.6 part by mass of 10% chloroplatinic acid, 20-40 parts by mass of concentrated sulfuric acid and 1-2 parts by mass of boric acid;
the silica sol is modified silica sol;
the preparation method of the modified silica sol comprises the following steps:
taking 50-60 parts by mass of silica sol, 0.01-0.02 part by mass of carbon nano tube and 10-50 parts by mass of absolute ethyl alcohol;
dispersing the carbon nano tube into absolute ethyl alcohol to obtain dispersion liquid;
mixing the dispersion liquid and the silica sol, uniformly stirring, and performing ultrasonic treatment for 30min to obtain modified silica sol;
the carbon nano tube is a modified carbon nano tube, and the preparation method of the modified carbon nano tube comprises the following steps:
taking 0.01-0.02 mass part of carbon nano tube, 0.1-0.5 mass part of N, N-dicyclohexylcarbodiimide, 1-3 mass parts of ethylenediamine, 0.1-0.3 mass part of boric acid, 0.2-0.3 mass part of 20% ammonia water, 1-5 mass parts of propylene glycol monomethyl ether and 1-3 mass parts of methylbenzene;
adding a carbon nano tube into ethylenediamine, adding N, N-dicyclohexylcarbodiimide, uniformly mixing, performing ultrasonic treatment for 10min, heating to 120 ℃ in an oil bath, keeping the temperature for 24h, after the reaction is finished, clarifying with absolute ethyl alcohol for three times, performing suction filtration, respectively cleaning the obtained filter residue with deionized water and absolute ethyl alcohol for 3 times, and performing vacuum drying on the filter residue for 24h at 40 ℃ to obtain a pre-modified carbon nano tube;
adding the pre-modified carbon nano tube into propylene glycol monomethyl ether, adding boric acid, carrying out ultrasonic treatment for 10min, adding 20% ammonia water and toluene, heating in a water bath to 90-100 ℃, refluxing for 6h, carrying out suction filtration, cleaning filter residues with tetrahydrofuran for 4-6 times, and then carrying out vacuum drying for 12h at 40 ℃ to obtain the modified carbon nano tube.
2. The electrolyte of a high-temperature-resistant capacitor according to claim 1, comprising 59 to 80 parts by mass of silica sol, 0.5 to 0.6 part by mass of copper sulfate, 0.5 to 0.6 part by mass of 10% chloroplatinic acid, 31 to 40 parts by mass of concentrated sulfuric acid, and 1.5 to 2 parts by mass of boric acid.
3. The electrolyte for a high-temperature-resistant capacitor according to claim 1, comprising 59 parts by mass of silica sol, 0.5 part by mass of copper sulfate, 0.5 part by mass of 10% chloroplatinic acid, 31 parts by mass of concentrated sulfuric acid, and 1.5 parts by mass of boric acid.
4. The electrolyte for a high-temperature-resistant capacitor according to claim 1, wherein 0.015 to 0.02 parts by mass of carbon nanotubes, 0.25 to 0.5 parts by mass of N, N-dicyclohexylcarbodiimide, 2 to 3 parts by mass of ethylenediamine, 0.2 to 0.3 parts by mass of boric acid, 0.25 to 0.3 parts by mass of 20% aqueous ammonia, 4 to 5 parts by mass of propylene glycol monomethyl ether, and 1.5 to 3 parts by mass of toluene are taken.
5. The electrolyte for a high-temperature-resistant capacitor according to claim 1, wherein 0.015 part by mass of carbon nanotubes, 0.25 part by mass of N, N-dicyclohexylcarbodiimide, 2 parts by mass of ethylenediamine, 0.2 part by mass of boric acid, 0.25 part by mass of 20% ammonia water, 4 parts by mass of propylene glycol methyl ether, and 1.5 parts by mass of toluene are taken.
6. A high-temperature-resistant capacitor is characterized in that the electrolyte according to any one of claims 1 to 5 is injected into a shell of the capacitor, and the high-temperature-resistant capacitor is obtained after encapsulation, wherein the capacitor is a tantalum capacitor.
7. The high-temperature capacitor according to claim 6, wherein the electrodes of the tantalum capacitor are subjected to an impregnation treatment before being assembled into the capacitor case, and the impregnation solution used for the impregnation treatment comprises 98 to 100 parts by mass of 40% sulfuric acid and 0.5 to 2 parts by mass of boric acid.
Priority Applications (1)
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| CN101439854A (en) * | 2008-12-18 | 2009-05-27 | 同济大学 | Preparation of boric acid or borate modified nano-carbon tube |
| CN101587780A (en) * | 2008-12-15 | 2009-11-25 | 株洲日望电子科技有限公司 | Method for manufacturing liquid tantalum electrolytic capacitors, and electrolyte preparation thereof |
| CN105355432A (en) * | 2015-11-03 | 2016-02-24 | 铜陵市科峰电子有限责任公司 | High-temperature-resistant capacitor electrolyte |
| CN109326447A (en) * | 2018-11-07 | 2019-02-12 | 广州金立电子有限公司 | A kind of electrolytic capacitor |
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| CN101698485B (en) * | 2009-07-03 | 2011-10-05 | 长春维鸿东光电子器材有限公司 | Method for manufacturing non-solid electrolyte high-frequency tantalum capacitor electrolyte by using silica sol |
| JP6256970B2 (en) * | 2013-06-17 | 2018-01-10 | テイカ株式会社 | Electrolytic capacitor and manufacturing method thereof |
| CN107331872B (en) * | 2017-07-02 | 2019-07-02 | 湖南科技大学 | A kind of preparation method and applications of the MnO 2/silver composite nano materials based on graphene/carbon nano-tube |
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| CN101587780A (en) * | 2008-12-15 | 2009-11-25 | 株洲日望电子科技有限公司 | Method for manufacturing liquid tantalum electrolytic capacitors, and electrolyte preparation thereof |
| CN101439854A (en) * | 2008-12-18 | 2009-05-27 | 同济大学 | Preparation of boric acid or borate modified nano-carbon tube |
| CN105355432A (en) * | 2015-11-03 | 2016-02-24 | 铜陵市科峰电子有限责任公司 | High-temperature-resistant capacitor electrolyte |
| CN109326447A (en) * | 2018-11-07 | 2019-02-12 | 广州金立电子有限公司 | A kind of electrolytic capacitor |
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