CN114373636A - Solid tantalum electrolytic capacitor and preparation method thereof - Google Patents

Solid tantalum electrolytic capacitor and preparation method thereof Download PDF

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CN114373636A
CN114373636A CN202111434296.4A CN202111434296A CN114373636A CN 114373636 A CN114373636 A CN 114373636A CN 202111434296 A CN202111434296 A CN 202111434296A CN 114373636 A CN114373636 A CN 114373636A
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water
acid
electrolytic capacitor
pedot
tantalum
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熊礼龙
武晶晶
杜显锋
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Xian Jiaotong University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
    • H01G9/0425—Electrodes or formation of dielectric layers thereon characterised by the material specially adapted for cathode
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
    • H01G2009/05—Electrodes or formation of dielectric layers thereon characterised by their structure consisting of tantalum, niobium, or sintered material; Combinations of such electrodes with solid semiconductive electrolytes, e.g. manganese dioxide

Abstract

The invention discloses a solid tantalum electrolytic capacitor and a preparation method thereof, wherein a water-soluble conductive polymer (S-PEDOT) with good water solubility and higher conductivity is adopted, and compared with the reported PEDOT: PSS, the water-soluble conductive polymer (S-PEDOT) has better water solubility, smaller molecular particle size and higher conductivity, so that the electrical property of the solid tantalum electrolytic capacitor can be obviously improved. According to the preparation method, the tantalum block is immersed into the water-soluble conducting polymer S-PEDOT, the tantalum block is taken out and dried after being immersed for each time, and then the tantalum block is immersed repeatedly for multiple times until the surface of the tantalum block is completely coated by the water-soluble conducting polymer S-PEDOT.

Description

Solid tantalum electrolytic capacitor and preparation method thereof
Technical Field
The invention belongs to the technical field of electronic materials and electronic components, and particularly relates to a solid tantalum electrolytic capacitor and a preparation method thereof.
Background
The solid tantalum capacitor has the advantages of small external influence on capacity change, small volume, wide use temperature range and the like, and can meet the development requirements of automation and miniaturization of the current electronic technology, so the solid tantalum capacitor is developed rapidly, the application field is continuously expanded, and the solid tantalum capacitor is expanded from the common consumer electronics field to almost all fields using electronic components including aerospace, communication, electronics, camera shooting and medical equipment.
Generally, the polymer cathode used in the conventional solid tantalum capacitor is manganese dioxide cathode, and the manganese dioxide cathode is replaced by poly-3, 4-ethylenedioxythiophene/polystyrene sulfonate (PEDOT: PSS) by Freeman et al in 2013 to prepare the tantalum electrolytic capacitor, and the preparation method is dip coating. Although the water solubility of the conductive polymer cathode used earlier is greatly improved compared with that of a conductive polymer cathode used earlier, the PEDOT/PSS has large molecular particle size, is not easy to enter a micro-nano structure of the tantalum electrolytic capacitor, is still dispersed in an aqueous solution, has poor water solubility, and has low conductivity (< 1S/cm), so that the use requirement of the solid tantalum electrolytic capacitor cannot be well met. Solid tantalum electrolytic capacitors with solid cathodes of PEDOT: PSS were prepared in 2016 by Xiiaopin Ma, Xiuyu Wang et al and treated with Ethylene Glycol (EG), wherein the conductivity of the PEDOT: PSS films without EG treatment was only 0.9S/cm, and the conductivity of the films even after EG treatment was only 130S/cm. Therefore, the conductivity of the conductive polymer cathode used in the current solid tantalum electrolytic capacitor is low, and the application requirement cannot be met.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a solid tantalum electrolytic capacitor and a preparation method thereof, so as to solve the technical problem that the performance of the electrolytic capacitor is influenced due to poor molecular water solubility, overlarge molecular particle size and low electrical conductivity of a raw material conductive polymer in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses a preparation method of a solid tantalum electrolytic capacitor, which comprises the following steps:
1) preparing a tantalum block with an anode leading-out end and a dielectric layer;
2) soaking the tantalum block into a water-soluble conductive polymer S-PEDOT, taking out and drying;
3) repeating the operation of the step 2) until the surface of the tantalum block is completely coated by the water-soluble conducting polymer S-PEDOT to prepare a tantalum block cathode;
4) dripping conductive carbon paste on the surface of the tantalum block cathode, solidifying at room temperature, dripping silver paste, and placing a silver wire as a cathode leading-out terminal to obtain a solid tantalum capacitor;
wherein the structural formula of the water-soluble conducting polymer S-PEDOT is as follows:
Figure BDA0003381063660000021
wherein n is 50-100.
Preferably, in the step 2), the tantalum block is immersed in the water-soluble conductive polymer S-PEDOT for 3-60 min, and the tantalum block is dried at 80-200 ℃ for 6-48 h.
Preferably, the operation times of repeating the step 2) in the step 3) are 3-15 times.
Preferably, the water-soluble conducting polymer S-PEDOT is prepared by fully mixing and uniformly stirring water-soluble monomer materials, an oxidant and a solvent according to the dosage ratio of (0.2-2) g, (0.1-3) g, (0.5-5) mL;
the structural formula of the water-soluble monomer material is as follows:
Figure BDA0003381063660000031
further preferably, the oxidant is one or more of potassium permanganate, iron p-toluenesulfonate, sodium persulfate and ammonium persulfate; the solvent is one or more of water, sulfuric acid, citric acid, oxalic acid, boric acid, adipic acid, phosphoric acid, salicylic acid and tartaric acid; the stirring reaction time is 3-48 h.
Further preferably, the preparation method of the water-soluble monomer material comprises the following steps:
step 1: diethyl 3, 4-dihydroxythiophene-2, 5-dicarboxylate, potassium carbonate and C3H6OBr2Dissolving the mixture in a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide for reaction to obtain a mixed solution;
step 2: adding a potassium hydroxide solution into the mixed solution, and adding an acid solution for acidification treatment to obtain 2- (hydroxymethyl) -2, 3-dihydrothieno [3,4-B ] [1,4] dioxin-5, 7-dicarboxylic acid;
and step 3: mixing 2- (hydroxymethyl) -2, 3-dihydrothieno [3,4-B ] [1,4] dioxin-5, 7-dicarboxylic acid, copper oxide and a catalyst for reaction to obtain hydroxymethyl EDOT;
and 4, step 4: mixing hydroxymethyl EDOT, sodium hydride and C5H10O2And dissolving S in a tetrahydrofuran solution for reaction, and distilling tetrahydrofuran to obtain the water-soluble monomer material.
More preferably, the reaction mixture ratio is:
in step 1, diethyl 3, 4-dihydroxythiophene-2, 5-dicarboxylate, potassium carbonate and C3H6OBr2The mass ratio of (0.1-2): (0.2-1): (0.2-3); the volume ratio of the N, N-dimethylformamide to the dimethyl sulfoxide in the mixed solvent is (0.1-0.5): 2;
in the step 2, the volume ratio of the mixed solution to the potassium hydroxide solution is (0.5-6): (0.1-2), and the volume ratio of the added acid solution to the sodium hydroxide solution is 1.5: 1;
in step 3, the mass ratio of 2- (hydroxymethyl) -2, 3-dihydrothieno [3,4-B ] [1,4] dioxin-5, 7-dicarboxylic acid, copper oxide and catalyst is (0.1-2): (1-4): (0.1-0.4);
in step 4, hydroxymethyl EDOT, sodium hydride and C5H10O2The mass ratio of S to the tetrahydrofuran solution is (1-2): (0.3-1): (0.3-1): (1-5).
Still further preferably, the acidic solution is one or more of sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, and C1-C10 organic polyacid; the catalyst is one or more of pyridine, isoquinoline, quinoline and 8-hydroxyquinoline copper.
Still more preferably, the potassium hydroxide solution has a concentration of 0.01M to 10M.
The invention also discloses the solid tantalum electrolytic capacitor prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method of the solid tantalum electrolytic capacitor, disclosed by the invention, the water-soluble conductive polymer (S-PEDOT) with good water solubility and higher conductivity is adopted, and compared with the reported PEDOT: PSS, the water-soluble conductive polymer (S-PEDOT) has the advantages of better water solubility, smaller molecular particle size and higher conductivity, so that the electrical property of the solid tantalum electrolytic capacitor can be obviously improved. According to the preparation method, the tantalum block is immersed into the water-soluble conducting polymer S-PEDOT, the tantalum block is taken out and dried after being immersed for each time, and then the tantalum block is immersed repeatedly for multiple times until the surface of the tantalum block is completely coated by the water-soluble conducting polymer S-PEDOT.
Furthermore, the water-soluble conducting polymer (S-PEDOT) used by the invention is obtained by adopting an innovative preparation method, and 1, 2-dibromopropanol (C) is used in the process of preparing the water-soluble monomer material S-EDOT3H6OBr2) The generation of byproducts in the step can be effectively avoided, the yield of the step is improved, and the yield of the step can reach 85%; the use amount of the organic solvent in the whole synthesis process is small, the method is economical and environment-friendly, the preparation steps are simple and easy to operate, and the final yield of the whole experimental process can reach more than 62%.
Drawings
FIG. 1 is a schematic view of a tantalum electrolytic capacitor;
FIG. 2 is a nuclear magnetic spectrum of S-EDOT monomer.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
example 1
A method for preparing a water-soluble conductive polymer comprising the steps of:
1) preparation of S-EDOT monomer
The reaction equation is as follows:
Figure BDA0003381063660000051
first, 500g of diethyl 3, 4-dihydroxythiophene-2, 5-dicarboxylate, 500g of potassium carbonate and 1000g of C3H6OBr2Dissolved in a mixed solvent of 1LN, N-Dimethylformamide (DMF) and 0.5L of dimethyl sulfoxide (DMSO) for reaction. Then, 300mL of 0.05M potassium hydroxide solution is added into the mixed solution, and 400mL of sulfuric acid is added for acidification to obtain the product 2- (hydroxymethyl) -2, 3-dihydrothieno [3,4-B][1,4]Dioxin-5, 7-dicarboxylic acid. 100g of the above-mentioned acidified product, 100g of copper oxide and 20g of copper 8-hydroxyquinoline are mixed to give the product hydroxymethyl EDOT (HMEDOT). 500g of HMEDOT, 400g of sodium hydride and 400g of C5H10O2S is mixed and dissolved in 0.5L tetrahydrofuran to sulfonate HMEDOT, and after quenching reaction with ethanol, THF is distilled under reduced pressure to obtain the product S-EDOT monomer, the nuclear magnetic spectrum of which is shown in figure 2.
2) S-PEDOT preparation:
the chemical method comprises the following steps: 500g of S-EDOT monomer and 600g of potassium permanganate are dissolved in 1L of aqueous sulfuric acid solution. Vigorously stirring at room temperature for 48h, and carrying out oxidative polymerization to obtain a polymerization solution of a conductive polymer, wherein the structure of the prepared conductive polymer is as follows, and n is 60 in the following structural formula;
Figure BDA0003381063660000061
example 2
In contrast to example 1, the acidic solution during the preparation of S-EDOT monomer was 420mL nitric acid. 22g of pyridine were used as catalyst. In the preparation process of S-PEDOT, 530g of ferric p-toluenesulfonate was used as an oxidant, and 1.5L of pure water was used as a solvent. The polymer obtained in this example had a degree of polymerization of 50.
Example 3
Unlike the other examples, the acid solution during the preparation of S-EDOT monomer was 500mL phosphoric acid. 20g of isoquinoline was used as the catalyst. In the preparation process of S-PEDOT, 480g of sodium persulfate is used as an oxidant, and 1L of sulfuric acid is used as a solvent. The polymer obtained in this example had a degree of polymerization of 80.
Example 4
Unlike the other examples, the acidic solution during the preparation of S-EDOT monomer was 530mL hydrochloric acid. The catalyst used was 30g of quinoline. In the preparation process of S-PEDOT, the oxidant is 620g of ammonium persulfate and the solvent is 1.8L of citric acid. The polymer obtained in this example had a degree of polymerization of 100.
Example 5
Different from other examples, in the preparation process of the S-EDOT monomer, the acid solution is 2.5L mixed solution of (1: 2: 1) sulfuric acid, tartaric acid and oxalic acid. The catalyst was a mixed solution of pyridine and isoquinoline (1: 1) (30 g). In the preparation process of S-PEDOT, the oxidant is 600g of ferric p-toluenesulfonate and ammonium persulfate (1: 1), and the solvent is 1.5L of pure water. The polymer obtained in this example had a degree of polymerization of 80.
The advantages of the present invention are shown by comparing the solubility, molecular particle size and conductivity of the water-soluble conductive polymer S-PEDOT prepared in example 1 of the present invention with that of the polymer PEDOT reported in the prior art.
PSS, a polymer reported in the prior art, and S-PEDOT prepared in example 1 of the present invention, above, are shown in Table 1 for comparison of their solubility in water:
TABLE 1
Figure BDA0003381063660000071
A comparison of the particle size of PEDOT versus the S-PEDOT prepared in accordance with the invention in example 1 is shown in Table 2:
TABLE 2
Figure BDA0003381063660000072
A comparison of the conductivity of PEDOT PSS and S-PEDOT prepared in accordance with the invention in example 1 is shown in Table 3:
TABLE 3
Figure BDA0003381063660000081
As can be seen from tables 1, 2 and 3, the water-soluble conductive polymer prepared according to the present invention has better water solubility, smaller molecular particle size, and higher electrical conductivity compared to conventional PEDOT: PSS, and enables a capacitor using the water-soluble conductive polymer as a cathode to have more excellent usability.
Example 6
A method for producing a solid tantalum electrolytic capacitor using the water-soluble conductive polymer obtained in example 1 as a cathode polymer, comprising the steps of:
(1) preparing a tantalum block with an anode lead-out and a dielectric layer
(2) Manufacturing a conductive polymer cathode:
a, soaking a tantalum block in the prepared polymer solution for 3 min; drying at 80 deg.C for 6 h; repeat step a 3 times.
b, dripping a layer of conductive carbon paste on the surface of the tantalum block cathode after the step a is finished, solidifying at room temperature, dripping silver paste, and placing silver wires as a cathode leading-out end to obtain the solid tantalum electrolytic capacitor, wherein the structure is shown in figure 1.
Example 7
A method for producing a solid tantalum electrolytic capacitor using the water-soluble conductive polymer obtained in example 1 as a cathode polymer, comprising the steps of:
(1) preparing a tantalum block with an anode lead-out and a dielectric layer
(2) Manufacturing a conductive polymer cathode:
a, soaking a tantalum block in the prepared polymer solution for 60 min; drying at 200 deg.C for 48 h; repeat step a 15 times.
b, dripping a layer of conductive carbon paste on the surface of the tantalum block cathode after the step a is finished, solidifying at room temperature, dripping silver paste, and placing silver wires as a cathode leading-out end to obtain the solid tantalum electrolytic capacitor.
The comparison of the capacitive properties of the cathode material of tantalum electrolytic capacitor prepared from the conventional PEDOT: PSS polymer and the tantalum electrolytic capacitor prepared from the above-prepared water-soluble conductive polymer S-PEDOT of the present invention is shown in Table 4, and the following data are average values:
TABLE 4
Figure BDA0003381063660000091
As can be seen from Table 4, the electrical properties of the solid tantalum electrolytic capacitor prepared by the method are obviously superior to those of the prior art.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (10)

1. A preparation method of a solid tantalum electrolytic capacitor is characterized by comprising the following steps:
1) preparing a tantalum block with an anode leading-out end and a dielectric layer;
2) soaking the tantalum block into a water-soluble conductive polymer S-PEDOT, taking out and drying;
3) repeating the operation of the step 2) until the surface of the tantalum block is completely coated by the water-soluble conducting polymer S-PEDOT to prepare a tantalum block cathode;
4) dripping conductive carbon paste on the surface of the tantalum block cathode, solidifying at room temperature, dripping silver paste, and placing a silver wire as a cathode leading-out terminal to obtain a solid tantalum capacitor;
wherein the structural formula of the water-soluble conducting polymer S-PEDOT is as follows:
Figure FDA0003381063650000011
wherein n is 50-100.
2. The method for preparing a solid tantalum electrolytic capacitor as claimed in claim 1, wherein in the step 2), the tantalum block is immersed in the water-soluble conductive polymer S-PEDOT for 3-60 min, and the tantalum block is dried at 80-200 ℃ for 6-48 h.
3. The method for producing a solid tantalum electrolytic capacitor as claimed in claim 1, wherein the number of times of repeating the operation of step 2) in step 3) is 3 to 15.
4. The method for preparing a solid tantalum electrolytic capacitor as claimed in claim 1, wherein the water-soluble conductive polymer S-PEDOT is prepared by mixing and stirring a water-soluble monomer material, an oxidant and a solvent in a ratio of (0.2-2) g, (0.1-3) g, (0.5-5) mL;
the structural formula of the water-soluble monomer material is as follows:
Figure FDA0003381063650000021
5. the method for producing a solid tantalum electrolytic capacitor according to claim 4, wherein said oxidizing agent is one or more of potassium permanganate, iron p-toluenesulfonate, sodium persulfate, and ammonium persulfate; the solvent is one or more of water, sulfuric acid, citric acid, oxalic acid, boric acid, adipic acid, phosphoric acid, salicylic acid and tartaric acid; the stirring reaction time is 3-48 h.
6. The method for producing a solid tantalum electrolytic capacitor as claimed in claim 4 or 5, wherein said method for producing a water-soluble monomer material comprises the steps of:
step 1: diethyl 3, 4-dihydroxythiophene-2, 5-dicarboxylate, potassium carbonate and C3H6OBr2Dissolving the mixture in a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide for reaction to obtain a mixed solution;
step 2: adding a potassium hydroxide solution into the mixed solution, and adding an acid solution for acidification treatment to obtain 2- (hydroxymethyl) -2, 3-dihydrothieno [3,4-B ] [1,4] dioxin-5, 7-dicarboxylic acid;
and step 3: mixing 2- (hydroxymethyl) -2, 3-dihydrothieno [3,4-B ] [1,4] dioxin-5, 7-dicarboxylic acid, copper oxide and a catalyst for reaction to obtain hydroxymethyl EDOT;
and 4, step 4: mixing hydroxymethyl EDOT, sodium hydride and C5H10O2And dissolving S in a tetrahydrofuran solution for reaction, and distilling tetrahydrofuran to obtain the water-soluble monomer material.
7. The method for manufacturing a solid tantalum electrolytic capacitor according to claim 6, wherein the reaction mixture ratio is as follows:
in step 1, diethyl 3, 4-dihydroxythiophene-2, 5-dicarboxylate, potassium carbonate and C3H6OBr2The mass ratio of (0.1-2): (0.2-1): (0.2-3); the volume ratio of the N, N-dimethylformamide to the dimethyl sulfoxide in the mixed solvent is (0.1-0.5): 2;
in the step 2, the volume ratio of the mixed solution to the potassium hydroxide solution is (0.5-6): (0.1-2), and the volume ratio of the added acid solution to the sodium hydroxide solution is 1.5: 1;
in step 3, the mass ratio of 2- (hydroxymethyl) -2, 3-dihydrothieno [3,4-B ] [1,4] dioxin-5, 7-dicarboxylic acid, copper oxide and catalyst is (0.1-2): (1-4): (0.1-0.4);
in step 4, hydroxymethyl EDOT, sodium hydride and C5H10O2The mass ratio of S to the tetrahydrofuran solution is (1-2): (0.3-1): (0.3-1): (1-5).
8. The method for producing a solid tantalum electrolytic capacitor as claimed in claim 6 wherein said acidic solution is one or more of sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid and C1-C10 organic polybasic acids; the catalyst is one or more of pyridine, isoquinoline, quinoline and 8-hydroxyquinoline copper.
9. The method for producing a solid tantalum electrolytic capacitor as claimed in claim 6, wherein said potassium hydroxide solution has a concentration of 0.01M to 10M.
10. A solid tantalum electrolytic capacitor produced by the production method according to any one of claims 1 to 9.
CN202111434296.4A 2021-11-29 2021-11-29 Solid tantalum electrolytic capacitor and preparation method thereof Pending CN114373636A (en)

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