CN115831620A - Preparation method of solid electrolyte tantalum capacitor and tantalum capacitor - Google Patents
Preparation method of solid electrolyte tantalum capacitor and tantalum capacitor Download PDFInfo
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- CN115831620A CN115831620A CN202211535682.7A CN202211535682A CN115831620A CN 115831620 A CN115831620 A CN 115831620A CN 202211535682 A CN202211535682 A CN 202211535682A CN 115831620 A CN115831620 A CN 115831620A
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Abstract
The invention discloses a preparation method of a solid electrolyte tantalum capacitor and the tantalum capacitor, wherein the prepared adhesive solution is mixed with tantalum powder according to the mass ratio, and a tantalum block is formed by pressing after a solvent is volatilized; sintering after pre-sintering to form a tantalum core; enabling the sintered tantalum core to form an anode tantalum core with a dielectric layer with uniform thickness; and (3) carrying out cathode treatment on the anode tantalum core group, coating a graphite layer on the structure body of the anode tantalum core group coated by the cathode, coating a silver paste layer led out by the cathode on the outer layer, and packaging to obtain the solid electrolyte tantalum capacitor. The problems of uneven mixing and more residual quantity of the adhesive in the powder mixing process of the existing tantalum capacitor can be solved, and the quality and the qualification rate of the tantalum capacitor are improved.
Description
Technical Field
The invention belongs to the technical field of tantalum capacitors, and particularly relates to a preparation method of a solid electrolyte tantalum capacitor and the tantalum capacitor.
Background
With the continuous development of electronic technology, the demand for electronic components is also increasing, and tantalum capacitors are used as representative types of capacitors with high capacity and high voltage, and the manufacturing process and raw materials thereof are continuously changing.
The powder mixing process is used as the first step in the tantalum capacitor manufacturing process to determine the results of the subsequent tantalum capacitor processes.
When the tantalum powder and the adhesive are mixed unevenly, the pressing density of the tantalum core is uneven, so that the electric field intensity of the inner part of the device in the electrifying process is overlarge, the dielectric layer is punctured, and the product fails. When the residual elements of the adhesive are excessive, the elements are not tantalum, tantalum pentoxide cannot be formed, the energized dielectric layer generates flaws, the leakage current parameter of the energized product is too large, and the reliability is reduced.
Disclosure of Invention
The invention aims to provide a preparation method of a solid electrolyte tantalum capacitor and the tantalum capacitor, which can solve the problems of uneven mixing and more residual quantity of adhesives in the powder mixing process of the existing tantalum capacitor and improve the quality and the qualification rate of the tantalum capacitor.
The technical scheme provided by the invention is as follows:
a method of making a solid electrolyte tantalum capacitor comprising:
and 6, coating a graphite layer on the structure body of the anode tantalum core group coated by the cathode, coating a silver paste layer led out by the cathode on the outer layer, and packaging to obtain the solid electrolyte tantalum capacitor.
The adhesive comprises one or more of polyethylene glycol, sodium styrene sulfonate, polyformaldehyde, dioctyl phthalate and butylated hydroxytoluene which are mixed in any proportion.
The solvent comprises water, ethanol or acetone.
The energized forming liquid is an acidic electrolyte, and comprises one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid and boric acid which are mixed with deionized water at any ratio, and the conductivity is 0.1-100 mS/cm at 20 ℃.
The conductivity of the energized forming liquid at 20 ℃ is 0.5-20 mS/cm.
The cathode layer is made of manganese dioxide or conductive polymer.
The packaging mode comprises metal shell packaging, ceramic shell packaging, mould pressing plastic packaging or electrostatic coating.
The metal shell comprises copper, silver, gold or tantalum; the mold pressing plastic package comprises epoxy resin.
A solid electrolyte tantalum capacitor is prepared by the method.
According to the technical scheme provided by the invention, the preparation method of the solid electrolyte tantalum capacitor and the tantalum capacitor provided by the embodiment of the invention,
the problems of uneven mixing and more residual quantity of the adhesive in the powder mixing process of the existing tantalum capacitor can be solved, and the quality and the qualification rate of the tantalum capacitor are improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced,
it is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1 is a schematic flow chart of a method for manufacturing a solid electrolytic tantalum capacitor according to a first embodiment of the present invention;
fig. 2 is a schematic structural view of a solid electrolyte tantalum capacitor according to a second embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are 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 embodiments.
All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The terms that may be used herein are first described as follows:
the term "and/or" means that either or both can be achieved, for example, X and/or Y means that both cases include "X" or "Y" as well as three cases including "X and Y".
The terms "comprising," "including," "containing," "having," or other similar terms of meaning should be construed as non-exclusive inclusions. For example: including a feature (e.g., material, component, ingredient, carrier, formulation, material, dimension, part, component, mechanism, device, process, procedure, method, reaction condition, processing condition, parameter, algorithm, signal, data, product, or article of manufacture), is to be construed as including not only the particular feature explicitly listed but also other features not explicitly listed as such which are known in the art.
The term "consisting of 823070 \8230composition" means to exclude any technical characteristic elements not explicitly listed. If used in a claim, the term shall render the claim closed except for the inclusion of the technical features that are expressly listed except for the conventional impurities associated therewith. If the term occurs in only one clause of the claims, it is defined only to the elements explicitly recited in that clause, and elements recited in other clauses are not excluded from the overall claims.
The term "parts by mass" is intended to indicate a mass ratio relationship between a plurality of components, for example: if X component is X parts by mass and Y component is Y parts by mass, the mass ratio of the X component to the Y component is X: Y;1 part by mass may represent any mass, for example: 1 part by mass may be 1kg or 3.1415926 kg. The sum of the parts by mass of all the components is not necessarily 100 parts, and may be more than 100 parts, less than 100 parts, or equal to 100 parts. Unless otherwise indicated, parts, ratios, and percentages described herein are by mass.
Unless expressly stated or limited otherwise, the terms "mounted," "connected," and "secured," etc., are to be construed broadly, as for example: can be fixedly connected, can also be detachably connected or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms herein can be understood by those of ordinary skill in the art as appropriate.
When concentrations, temperatures, pressures, dimensions, or other parameters are expressed as ranges of values, the ranges are to be understood as specifically disclosing all ranges formed from any pair of upper, lower, and preferred values within the range, regardless of whether ranges are explicitly recited; for example, if a numerical range of "2 to 8" is recited, then that numerical range should be interpreted to include ranges such as "2 to 7," "2 to 6," "5 to 7," "3 to 4 and 6 to 7," "3 to 5 and 7," "2 and 5 to 7," and the like. Unless otherwise indicated, the numerical ranges recited herein include both the endpoints thereof and all integers and fractions within the numerical range.
The terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," and the like are used in an orientation or positional relationship that is indicated based on the orientation or positional relationship shown in the drawings for ease of description and simplicity of description only, and are not intended to imply or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be considered limiting herein.
Embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.
Example one
A method of making a solid electrolyte tantalum capacitor comprising:
the adhesive comprises one or more of polyethylene glycol, sodium styrene sulfonate, polyformaldehyde, dioctyl phthalate and butylated hydroxytoluene which are mixed in any proportion.
The solvent includes water, ethanol and acetone, and one skilled in the art can select a suitable solvent according to the adhesive.
and 3, presintering at 200-300 ℃ for 30min, and sintering at 1650 ℃ for 30min. Sintering to form a tantalum core;
the energized forming liquid is an acidic electrolyte, and comprises one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid and boric acid which are mixed with deionized water at any ratio, and the conductivity is 0.1-100 mS/cm at 20 ℃. Preferably, the conductivity of the energized forming liquid at 20 ℃ is 0.5-20 mS/cm.
The energizing process is a process known in the art and is not described in detail, and reference is made to the following examples for various examples.
In this example, a final rinse with deionized water is included to remove residual energized forming liquid.
the cathode layer is made of manganese dioxide or conductive polymer.
The conductive polymer is a high molecular material with a conjugated main electron system in a main chain, can reach a conductive state through doping, and has the conductivity of more than 1000S/cm.
The cathode treatment process is a well-known process in the art and will not be described in detail, and for this example, reference is made to the following examples.
And 6, coating a graphite layer on the structure body of the anode tantalum core group coated by the cathode, coating a silver paste layer led out by the cathode on the outer layer, and packaging to obtain the solid electrolyte tantalum capacitor.
The packaging mode comprises metal shell packaging, ceramic shell packaging, mold pressing plastic packaging or electrostatic coating.
The metal shell comprises copper, silver, gold or tantalum; the molding plastic package material is thermosetting resin, such as epoxy resin.
This step is also a known process in the art, and is not described in detail, for which reference is made to the following examples.
The flow chart of the embodiment is shown in fig. 1, and the novel adhesive, especially the polyethylene glycol solution is used as the adhesive, so that the uniformity of the density of the pressed tantalum block and the purity of the tantalum block can be enhanced, the reliability and the service life of the capacitor are ensured, and the failure phenomenon caused by breakdown of a dielectric layer of a product is effectively reduced.
Example two
Referring to fig. 2, a solid electrolyte tantalum capacitor was fabricated using the method described in example one. Specifically, the tantalum core comprises a tantalum core body 1, a dielectric layer 2 is coated outside the tantalum core body, a cathode 3 is coated outside the tantalum core body, a graphite layer is coated on the cathode 3, a silver paste layer led out by the cathode is coated on the outer layer of the tantalum core body, finally, the tantalum core body is specially packaged by an epoxy resin shell 4, and an anode lead 5 and a cathode lead 6 are led out.
EXAMPLE III
In this example, taking an E-shell solid electrolyte tantalum capacitor of 50V10 μ F as an example, the preparation process includes:
and 3, pre-sintering the tantalum block obtained in the step 2 at 200-300 ℃ for 30min, and then sintering at 1650 ℃ for 30min for molding to form the tantalum core.
energization first, an energization voltage is calculated by the formula:
U f ＝C wet testing ×U Wet examination ÷C Forehead (forehead) ，
Wherein U is Wet examination ＝M×B s ÷C Forehead (forehead) 。
In the formula
M is the mass of tantalum powder;
C wet examination The wet test capacity;
C forehead (forehead) Is rated capacity;
U wet examination A wet test voltage;
B s is the specific volume.
The energizing forming liquid can be selected from phosphoric acid aqueous solution, and the ratio of water: phosphoric acid =1, 0.01,
and (3) placing the anode sample in energized solution at 60-90 ℃, increasing the current density of 20-60 mA/g to energized voltage after the temperature is constant, maintaining the constant voltage for 2-4 h, and then boiling and washing the anode sample with deionized water for 10-60 min to remove residual energized forming liquid.
repeatedly soaking the anode tantalum core group in 1.0-1.4 g/ml manganese nitrate solution for decomposing for 2-5 times, supplementing according to half of the energizing voltage of the first stage for 20min after finishing, soaking again in 1.5-1.8 g/ml manganese nitrate solution for decomposing for 6-10 times, and finally supplementing according to half of the energizing voltage of the first stage for 10min again; finishing cathode treatment;
and 6, coating a graphite layer on the structure body of the anode tantalum core group coated by the cathode, coating a silver paste layer led out by the cathode on the outer layer, and packaging to obtain the solid electrolyte tantalum capacitor. Referring to the flow chart of fig. 1, the subsequent treatment is carried out to obtain the finished product of the solid electrolyte tantalum capacitor using polyethylene glycol as the binder in the powder mixing process.
Table 1 experimental data for leakage current testing of example three versus the conventional method of the prior art in table units: μ A
| Leakage current | 1 | 2 | 3 | 4 | 5 | Mean value of |
| General of | 1.4 | 1.5 | 1.5 | 1.6 | 1.5 | 1.50 |
| EXAMPLE III | 0.9 | 1.1 | 1.2 | 1.0 | 1.1 | 1.06 |
Example four
In this example, taking an F-shell solid electrolyte tantalum capacitor of 16V and 330 μ F as an example, the preparation process includes:
energization first, an energization voltage is calculated by the formula:
U f ＝C wet examination ×U Wet examination ÷C Forehead (forehead) ，
Wherein U is Wet examination ＝M×B s ÷C Forehead (forehead) 。
In the formula
M is the mass of tantalum powder;
C wet examination The wet test capacity;
C forehead (forehead) Is rated capacity;
U wet examination A wet test voltage;
B s is the specific volume.
The energizing forming liquid can be selected from phosphoric acid aqueous solution, and the ratio of water: phosphoric acid =1, 0.01,
and (3) placing the anode sample in energized solution at 60-90 ℃, increasing the current density of 20-60 mA/g to energized voltage after the temperature is constant, maintaining the constant voltage for 2-4 h, and then boiling and washing the anode sample with deionized water for 10-60 min to remove residual energized forming liquid.
repeatedly soaking the anode tantalum core group in a low specific gravity manganese nitrate solution for decomposing for 2-5 times, supplementing according to a half of the energizing voltage of the first stage for 20min after finishing, soaking in the low specific gravity manganese nitrate solution for decomposing for 6-10 times, and supplementing according to a half of the energizing voltage of the first stage for 10min; finishing cathode treatment;
and 6, coating a graphite layer on the structure body of the anode tantalum core group coated by the cathode, coating a silver paste layer led out by the cathode on the outer layer, and packaging to obtain the solid electrolyte tantalum capacitor. Referring to the flow chart of fig. 1, the subsequent treatment is carried out to obtain the finished product of the solid electrolyte tantalum capacitor using polyethylene glycol as the binder in the powder mixing process.
Table 2 example four experimental data for conventional leakage current testing of the conventional method of the prior art are compared in table units: μ A
| Leakage current | 1 | 2 | 3 | 4 | 5 | Mean value of |
| General of | 5.8 | 6.1 | 5.7 | 6.2 | 5.6 | 5.88 |
| Example four | 3.2 | 3.5 | 3.4 | 3.6 | 3.5 | 3.44 |
According to the invention, the polyethylene glycol solution is added in the powder mixing process, so that the internal uniformity of the tantalum block is improved, the content of impurity elements in the tantalum block is reduced and the reliability of the product is greatly improved on the premise of ensuring the flowability of the tantalum powder.
The above description is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A method for manufacturing a solid electrolyte tantalum capacitor, comprising:
step 1, mixing a solvent and an adhesive according to a mass ratio of 5-10 to 1, and fully stirring to fully dissolve the adhesive in the solvent to prepare an adhesive solution;
step 2, mixing the prepared adhesive solution and tantalum powder according to a mass ratio of 1-5: mixing at a ratio of 100, and pressing to form a tantalum block after the solvent is volatilized;
step 3, presintering at 200-300 ℃ for 30min, and sintering to form a tantalum core;
step 4, placing the sintered tantalum core into energizing forming liquid, and energizing to form an anode tantalum core with a dielectric layer with uniform thickness;
step 5, performing cathode treatment on the anode tantalum core group to form a structural body of the anode tantalum core group consisting of a cathode layer, a dielectric layer and an anode tantalum core;
and 6, coating a graphite layer on the structure body of the anode tantalum core group coated by the cathode, coating a silver paste layer led out by the cathode on the outer layer, and packaging to obtain the solid electrolyte tantalum capacitor.
2. The method of manufacturing a solid electrolyte tantalum capacitor according to claim 1, further comprising boiling with deionized water to remove residual energized forming liquid after step 4.
3. The method for manufacturing a solid electrolyte tantalum capacitor as claimed in claim 1 or 2, wherein said adhesive comprises one or more of polyethylene glycol, sodium styrene sulfonate, polyoxymethylene, dioctyl phthalate and butylated hydroxytoluene mixed in any ratio.
4. The method of producing a solid electrolytic tantalum capacitor as claimed in claim 1 or 2, wherein said solvent comprises water, ethanol or acetone.
5. The method of claim 1 or 2, wherein the energized forming liquid is an acidic electrolyte solution comprising one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, and boric acid mixed with deionized water at any ratio, and has a conductivity of 0.1-100 mS/cm at 20 ℃.
6. The method for producing a solid electrolytic tantalum capacitor as claimed in claim 5, wherein said energization forming liquid has a conductivity of 0.5 to 20mS/cm at 20 ℃.
7. The method of producing a solid electrolytic tantalum capacitor as claimed in claim 1 or 2, wherein said cathode layer is made of manganese dioxide or a conductive polymer.
8. The method for manufacturing a solid electrolytic tantalum capacitor as claimed in claim 1 or 2, wherein the packaging manner comprises metal housing packaging, ceramic housing packaging, mold pressing plastic packaging or electrostatic coating.
9. The method of producing a solid electrolyte tantalum capacitor as claimed in claim 8, wherein said metal case comprises copper, silver, gold or tantalum; the mold pressing plastic package comprises epoxy resin.
10. A solid electrolyte tantalum capacitor, characterized in that it is produced by the method of any one of claims 1 to 9.
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| CN202211535682.7A CN115831620A (en) | 2022-11-30 | 2022-11-30 | Preparation method of solid electrolyte tantalum capacitor and tantalum capacitor |
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| CN202211535682.7A CN115831620A (en) | 2022-11-30 | 2022-11-30 | Preparation method of solid electrolyte tantalum capacitor and tantalum capacitor |
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