CN113990669B - Preparation method of high-voltage-resistance solid tantalum electrolytic capacitor - Google Patents
Preparation method of high-voltage-resistance solid tantalum electrolytic capacitor Download PDFInfo
- Publication number
- CN113990669B CN113990669B CN202111276550.2A CN202111276550A CN113990669B CN 113990669 B CN113990669 B CN 113990669B CN 202111276550 A CN202111276550 A CN 202111276550A CN 113990669 B CN113990669 B CN 113990669B
- Authority
- CN
- China
- Prior art keywords
- tantalum
- voltage
- acid
- electrolytic capacitor
- block
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 93
- 239000003990 capacitor Substances 0.000 title claims abstract description 56
- 239000007787 solid Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000002253 acid Substances 0.000 claims abstract description 16
- 238000004806 packaging method and process Methods 0.000 claims abstract description 16
- 150000003839 salts Chemical class 0.000 claims abstract description 12
- 239000003792 electrolyte Substances 0.000 claims abstract description 11
- 238000003825 pressing Methods 0.000 claims abstract description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052709 silver Inorganic materials 0.000 claims abstract description 8
- 239000004332 silver Substances 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 238000000465 moulding Methods 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 6
- 239000010439 graphite Substances 0.000 claims abstract description 6
- 230000010287 polarization Effects 0.000 claims abstract description 5
- 239000007784 solid electrolyte Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 32
- 230000002378 acidificating effect Effects 0.000 claims description 19
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- 238000009835 boiling Methods 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical class CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical class OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 7
- 239000004327 boric acid Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 235000010338 boric acid Nutrition 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical class CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 150000007513 acids Chemical class 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 239000008151 electrolyte solution Substances 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical class COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 235000011054 acetic acid Nutrition 0.000 claims description 3
- 150000003863 ammonium salts Chemical class 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 3
- 229920001940 conductive polymer Polymers 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 239000004310 lactic acid Chemical class 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 230000001502 supplementing effect Effects 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 150000001447 alkali salts Chemical class 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 238000009503 electrostatic coating Methods 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 229920001187 thermosetting polymer Polymers 0.000 claims description 2
- 238000005538 encapsulation Methods 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- 230000002159 abnormal effect Effects 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical class [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 2
- -1 carrier Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- CDMADVZSLOHIFP-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane;decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 CDMADVZSLOHIFP-UHFFFAOYSA-N 0.000 description 1
- 238000002224 dissection Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009966 trimming Methods 0.000 description 1
Images
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
- 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, 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
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
-
- 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
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/052—Sintered electrodes
-
- 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
-
- 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
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method of a high-voltage-resistance solid tantalum electrolytic capacitor, which comprises the following steps: pressing and molding tantalum powder according to a set shape and sintering the tantalum powder into a tantalum block; performing multi-stage energization on the sintered tantalum block to form an anode tantalum core which is provided with dielectric layers with different inner and outer layer thicknesses and has an outer layer thickness larger than an inner layer thickness; and carrying out negative polarization treatment on the anode tantalum block, leading out a cathode through graphite and silver paste, and then packaging to obtain the high-voltage-resistance solid electrolyte tantalum capacitor. The electrolyte containing weak acid salt is used as the energizing forming liquid to energize the tantalum block in multiple stages, a dielectric layer with higher thickness is formed on the outer surface of the tantalum block, the voltage-resistant characteristic of the manufactured capacitor is greatly improved on the premise that the volume is not increased and the capacity is not greatly reduced, compared with single-stage once energizing, the capacity of the manufactured capacitor is slightly smaller than 1% -15%, and the loss tangent, the equivalent series resistance and the electric leakage are not obviously abnormal.
Description
Technical Field
The invention relates to the field of tantalum electrolytic capacitors, in particular to a preparation method of a high-voltage-resistance solid tantalum electrolytic capacitor.
Background
The capacitor is one of electronic elements widely used in electronic equipment, and is widely applied to aspects of blocking AC, coupling, bypassing, filtering, energy conversion and the like in a circuit. Due to the volumetric efficiency, reliability and process compatibility of electrolytic capacitors (e.g., tantalum capacitors), their use in circuit design is increasing, and their reliability is also becoming more and more demanding.
High voltage is applied to the solid sheet tantalum capacitor, and a high electric field is formed inside the solid sheet tantalum capacitor, so that the solid sheet tantalum capacitor is easy to break down locally, and the solid sheet tantalum capacitor is easy to fail, namely, the solid sheet tantalum capacitor is frequently called 'field failure'. During dissection of failed products, it was found that the breakdown sites were mostly concentrated at the core surface. In order to improve the reliability of the high-voltage solid tantalum capacitor, a currently common method is to de-rate the high-voltage solid tantalum capacitor, but this not only increases the cost, but also affects the application range of the high-voltage solid tantalum capacitor.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a preparation method of a high-voltage-resistance solid tantalum electrolytic capacitor, which can solve the problem of insufficient voltage resistance of the tantalum capacitor on the premise of small capacity loss.
The purpose of the invention is realized by the following technical scheme:
the embodiment of the invention provides a preparation method of a high-voltage-resistance solid tantalum electrolytic capacitor, which comprises the steps of pressing and molding tantalum powder according to a set shape and sintering the tantalum powder into a tantalum block;
performing multi-stage energization on the sintered tantalum block to form an anode tantalum core which is provided with dielectric layers with different inner and outer layer thicknesses and has an outer layer thickness larger than an inner layer thickness;
and carrying out negative polarization treatment on the anode tantalum block, leading out a cathode through graphite and silver paste, and then packaging to obtain the high-voltage-resistance solid electrolyte tantalum capacitor.
Compared with the prior art, the preparation method of the high-voltage-resistance solid tantalum electrolytic capacitor provided by the invention has the beneficial effects that:
the sintered tantalum block is energized in stages to form an anode tantalum core which has an outer layer thickness larger than an inner layer thickness and has dielectric layers with different inner and outer layer thicknesses, and the thickness of an oxide film on the outer surface of the tantalum core is increased on the premise of not changing the thickness of the inner dielectric layer, so that the voltage withstanding characteristic of the capacitor is improved, and the failure probability of the capacitor caused by voltage breakdown is reduced; and the secondary formation does not significantly reduce the product capacity. By adopting the capacitor, the breakdown voltage of a product can be improved on the basis of the original design.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
Fig. 1 is a flow chart of a method for manufacturing a high withstand voltage solid tantalum electrolytic capacitor according to an embodiment of the present invention.
Detailed Description
The technical scheme in the embodiment of the invention is clearly and completely described below by combining the specific content of the invention; it should be understood that the described embodiments are only some of the embodiments of the present invention, not all of the embodiments, and are not intended to limit the present invention. 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 in describing these terms are to 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. Parts, ratios and percentages described herein are by mass unless otherwise indicated.
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 of values should be understood to specifically disclose all ranges formed by any pair of upper values, lower values, or preferred values within the range, regardless of whether the 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.
The method for manufacturing the high withstand voltage solid tantalum electrolytic capacitor according to the present invention will be described in detail below. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to the person skilled in the art. Those not specifically mentioned in the examples of the present invention were carried out according to the conventional conditions in the art or conditions suggested by the manufacturer. The reagents and instruments used in the examples of the present invention are not specified by manufacturers, and are conventional products commercially available.
As shown in fig. 1, an embodiment of the present invention provides a method for manufacturing a high withstand voltage solid tantalum electrolytic capacitor, which can solve the problem of insufficient withstand voltage capability of the existing tantalum capacitor with a small capacity loss, and the method includes the following steps:
pressing and molding tantalum powder according to a set shape and sintering the tantalum powder into a tantalum block;
performing multi-stage energization on the sintered tantalum block to form an anode tantalum core with a dielectric layer with different inner and outer layer thicknesses, wherein the outer layer thickness of the anode tantalum core is larger than the inner layer thickness of the anode tantalum core;
and carrying out negative polarization treatment on the anode tantalum block, leading out a cathode through graphite and silver paste, and then packaging to prepare the high-voltage-resistance solid electrolyte tantalum capacitor.
In the above method, the step of energizing the sintered tantalum block by the following steps comprises:
step 21) placing the sintered tantalum block in the acidic forming liquid A, introducing a forming voltage, keeping the constant voltage for 1-6 h after the forming voltage is increased to a design voltage, and keeping the current density of 10-100 mA/g in the boosting process;
step 22) putting the tantalum block treated in the step 21 into deionized water at 100 ℃ for boiling and washing for 10-120 min;
step 23) placing the tantalum block boiled in the step 22 in an acid forming liquid B, applying a voltage 20-300V higher than a design voltage, and keeping the constant voltage for 5-600 s;
step 24) putting the tantalum block treated in the step 23 into deionized water at 100 ℃ for boiling and washing for 2 times, wherein the boiling and washing time is 10-120 min each time, and putting the tantalum block into an oven for heat treatment after boiling and washing;
and 25) performing constant pressure compensation on the tantalum block after heat treatment in the acidic forming liquid A used in the step 21 for 0.5-4 h at a designed voltage, and completing the staged energization of the tantalum block after sintering.
In the method, the acidic forming liquid A adopts an acidic electrolyte composed of an acidic compound and a solvent; preferably, the acidic compound is any one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid and boric acid; the solvent is any one of deionized water and ethylene glycol or a mixture of the deionized water and the ethylene glycol. The conductivity of the acidic forming liquid A can be adjusted to a stable value at 40 ℃, and the range of the conductivity is 0.1mS/cm to 50mS/cm.
The acidic forming liquid B adopts a weak acid salt electrolyte solution; preferably, the weak acid salt electrolyte solution is any one or more of ammonium salts or alkali salts of formic acid, acetic acid, boric acid, borate, oxalic acid, lactic acid and carbonic acid. The conductivity of the acidic forming solution B can be adjusted to a stable value at 40 ℃, optionally in the range of 0.1mS/cm to about 50mS/cm.
In step 24 of the method, the heat treatment temperature of the tantalum block in the oven is 280-450 ℃, and the treatment time is 5-60 min.
In the above method, the cathode comprises a manganese dioxide cathode and/or an electrically conductive polymer cathode.
In the method, the packaging mode adopts any one of metal shell packaging, ceramic shell packaging, mold pressing plastic packaging and electrostatic coating packaging.
Preferably, the metal used for the metal shell package includes: any one of copper, silver, gold, tantalum.
Preferably, the material for mold pressing and plastic packaging is thermosetting resin.
In conclusion, according to the preparation method provided by the embodiment of the invention, the secondary formation operation of weak acid salt is added after the tantalum core is conventionally formed, and the thickness of the oxide film on the outer surface of the tantalum core is increased on the premise of not changing the thickness of the internal dielectric layer, so that the voltage withstanding property of the capacitor is improved, and the failure probability of the capacitor caused by voltage breakdown is reduced; and the secondary formation can not greatly reduce the capacity of the finally manufactured capacitor, and the solid tantalum electrolytic capacitor manufactured by the method can improve the breakdown voltage of the product on the basis of the original design.
In order to more clearly show the technical solutions and the technical effects provided by the present invention, the following detailed description is provided with specific examples of the method for manufacturing the high withstand voltage solid tantalum electrolytic capacitor provided by the embodiments of the present invention.
As shown in fig. 1, an embodiment of the present invention provides a method for manufacturing a high withstand voltage solid tantalum electrolytic capacitor, including the following steps:
pressing and molding tantalum powder according to a certain shape and sintering into tantalum blocks;
performing multi-stage energization on the sintered tantalum block to form an anode tantalum core with a medium layer with different thicknesses, wherein the medium layer is thick at the outer layer and thin at the inner layer;
and (3) cathodically treating the anode tantalum block, leading out a cathode through graphite and silver paste, and then packaging to prepare the high-voltage-resistance solid tantalum electrolytic capacitor.
In the method, the staged energization is mainly divided into three sections:
the first stage is as follows: placing the sintered tantalum block in the acidic forming liquid A, introducing a forming voltage, and keeping the voltage constant for 1-4 hours after the forming voltage is increased to a design voltage; placing the treated tantalum block in deionized water at 100 ℃ for boiling and washing for 10-120 min;
and a second stage: placing the treated tantalum block in an acid forming solution B, applying a constant voltage 20-300V higher than a design voltage, and keeping for 5-600 s; placing the treated tantalum block in deionized water at 100 ℃ for boiling and washing for 2 times, wherein the boiling and washing time is 10-120 min each time, and placing the tantalum block in an oven for heat treatment after boiling and washing;
and finally, performing constant voltage compensation on the treated tantalum block in the acidic forming liquid A in the first stage for 0.5-4 h by using a designed voltage, thus obtaining the anode tantalum core with the medium layer with the different thickness, which is thick at the outer layer and thin at the inner layer.
In the above step energization, the acidic forming liquid a used in the first step is an acidic electrolyte composed of an acidic mixture and a solvent, for example: the acid mixture is one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, boric acid, etc., and the solvent is one or a mixture of deionized water and ethylene glycol. The acid electrolyte has a conductivity of about 0.1 to 100mS/cm, preferably 0.5 to 20mS/cm, at 40 ℃.
The acidic forming liquid B used in the second stage is a weak acid salt electrolyte, for example, one or more of ammonium salt or alkali metal salt (e.g., sodium, potassium, etc.) of formic acid, acetic acid, boric acid, borate, oxalic acid, lactic acid, carbonic acid, etc., and the conductivity of the weak acid salt electrolyte can be adjusted to a stable value at 40 ℃, preferably in the range of 0.1mS/cm to about 50mS/cm.
And after each section of forming stage is finished, the residual electrolyte can be removed by using the boiling and washing of the deionized water, so that the influence among the forming stages is avoided.
In the method, a capacitor cathode layer is formed by subjecting an anode tantalum core to a cathodic polarization treatment. The cathode layer material can be one or two of manganese dioxide and conductive polymer.
According to the preparation method, the tantalum block is energized through the staged forming process, particularly the second-stage forming process using the weak acid salt electrolyte as the energizing forming liquid is adopted, a thicker dielectric layer is formed on the outer layer of the tantalum block, the voltage-resistant characteristic of the capacitor is ensured, the failure phenomenon caused by surface breakdown of the product is effectively reduced, the reliability of the product is improved, and the service life of the product is prolonged.
Examples
As shown in fig. 1, in this embodiment, the preparation method of the present invention is illustrated by taking an E-shell tantalum electrolytic capacitor product of 16V and 150 μ F as an example, and includes the following steps:
firstly, tantalum powder with specific volume of 32000 mu F.V/g and 3 percent (mass ratio) of binder are mixed uniformly, the powder is pressed into an anode sample after being dried, the sample size is 3.5 multiplied by 3.3, the weight is 228mg, and the tantalum block is obtained by sintering and molding at 1450 ℃;
the forming process adopts a three-stage forming process:
the first stage, placing tantalum block in phosphoric acid solution (volume concentration) of 1 ‰ at 85 deg.C, heating to 48V at current density of 50mA/g after temperature is constant, maintaining constant pressure for 2 hr, and then boiling with deionized water for 30min;
in the second stage, the treated tantalum block is placed in boric acid/sodium borate solution with the conductivity of 5mS/cm at the temperature of 40 ℃, the voltage of 90V is applied for 5min, and then the tantalum block is boiled and washed twice by deionized water, wherein the time duration of each time is 30min;
and (3) putting the treated tantalum block into a 350 ℃ oven for heat treatment for 10min, and then performing a third-stage complementary formation process in the acidic formation liquid A used in the first stage, wherein the design voltage of the first stage is used for keeping the voltage constant for 2h, so that the anode tantalum core is prepared.
Performing cathodic treatment on the formed anode tantalum core, repeatedly soaking the anode tantalum core in a 1.30g/mL manganese nitrate solution for 10 times, supplementing the anode tantalum core with half of the energizing voltage in the first stage for 20min after the treatment, soaking the anode tantalum core in a 1.70g/mL manganese nitrate solution for 6 times, and supplementing the anode tantalum core with half of the energizing voltage in the first stage for 10min;
and sequentially coating a graphite layer and a silver paste layer on the anode tantalum core forming the cathode layer, and then carrying out subsequent assembling, molding, printing, trimming and screening according to the flow of the figure 1 to obtain the finished high-voltage-resistant solid tantalum capacitor.
In conclusion, the electrolyte containing the weak acid salt is used as the energizing forming liquid to energize the tantalum block in multiple stages, the dielectric layer with higher thickness is formed on the outer surface of the tantalum block, the voltage-resistant characteristic of the manufactured capacitor is greatly improved, compared with a capacitor energized in one stage, the capacitor manufactured in the invention has the capacity slightly smaller than 1% -15%, and the loss tangent, the equivalent series resistance and the electric leakage are not obviously abnormal.
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 should be subject to the protection scope of the claims. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Claims (9)
1. A preparation method of a high-voltage-resistance solid tantalum electrolytic capacitor is characterized by comprising the following steps:
pressing and molding tantalum powder according to a set shape and sintering the tantalum powder into tantalum blocks;
performing multi-stage energization on the sintered tantalum block to form an anode tantalum core which is provided with dielectric layers with different inner and outer layer thicknesses and has an outer layer thickness larger than an inner layer thickness;
carrying out negative polarization treatment on the anode tantalum core, leading out a cathode through graphite and silver paste, and then packaging to prepare the high-voltage-resistance solid electrolyte tantalum capacitor;
staged energization of sintered tantalum blocks by:
step 21) placing the sintered tantalum block in the acidic forming liquid A, introducing a forming voltage, keeping the constant voltage for 1-6 h after the forming voltage is increased to a design voltage, and keeping the current density of 10-100 mA/g in the boosting process;
step 22) putting the tantalum block treated in the step 21 into deionized water at 100 ℃ for boiling and washing for 10-120 min;
step 23) placing the tantalum block boiled in the step 22 in an acidic forming solution B, applying a voltage 20-300V higher than a design voltage, and keeping the constant voltage for 5-600 s;
step 24) putting the tantalum block treated in the step 23 into deionized water at 100 ℃ for boiling and washing for 2 times, wherein the boiling and washing time is 10-120 min each time, and putting the tantalum block into an oven for heat treatment after boiling and washing;
step 25) supplementing the tantalum block after heat treatment in the acidic forming liquid A used in the step 21 for 0.5-4 h at a designed voltage, namely completing the phased energization of the tantalum block after sintering;
and the acidic forming solution B adopts weak acid salt electrolyte solution.
2. The method for producing a high withstand voltage solid tantalum electrolytic capacitor according to claim 1, wherein said acidic forming liquid a uses an acid salt electrolyte composed of an acidic compound and a solvent, and the acid salt electrolyte has a conductivity adjusted to a stable value at 40 ℃, and the conductivity ranges from 0.1mS/cm to 50mS/cm.
3. The method for manufacturing a high withstand voltage solid tantalum electrolytic capacitor according to claim 2, wherein the acidic compound is any one or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid and boric acid;
the solvent is any one of deionized water and ethylene glycol or a mixture of the deionized water and the ethylene glycol.
4. The method for manufacturing a high withstand voltage solid tantalum electrolytic capacitor according to claim 2, wherein the weak acid salt electrolyte solution is any one or more of ammonium salts or alkali salts of formic acid, acetic acid, boric acid, oxalic acid, lactic acid, carbonic acid.
5. The method for manufacturing a high withstand voltage solid tantalum electrolytic capacitor according to any one of claims 1 to 4, wherein in the step 24, the heat treatment temperature of the tantalum block in the oven is 280 to 450 ℃ and the treatment time is 5 to 60min.
6. The method for producing a high withstand voltage solid tantalum electrolytic capacitor according to any one of claims 1 to 4, wherein said cathode comprises a manganese dioxide cathode and/or a conductive polymer cathode.
7. The method for preparing a high voltage solid tantalum electrolytic capacitor according to any one of claims 1 to 4, wherein the packaging mode is any one of metal shell packaging, ceramic shell packaging, mold pressing plastic packaging and electrostatic coating packaging.
8. The method for manufacturing a high withstand voltage solid tantalum electrolytic capacitor according to claim 7, wherein the metal used for the metal case encapsulation comprises: any one of copper, silver, gold, and tantalum.
9. The method for manufacturing a high withstand voltage solid tantalum electrolytic capacitor according to claim 7, wherein the material for mold pressing and plastic sealing is thermosetting resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111276550.2A CN113990669B (en) | 2021-10-29 | 2021-10-29 | Preparation method of high-voltage-resistance solid tantalum electrolytic capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111276550.2A CN113990669B (en) | 2021-10-29 | 2021-10-29 | Preparation method of high-voltage-resistance solid tantalum electrolytic capacitor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113990669A CN113990669A (en) | 2022-01-28 |
| CN113990669B true CN113990669B (en) | 2023-02-21 |
Family
ID=79744815
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111276550.2A Active CN113990669B (en) | 2021-10-29 | 2021-10-29 | Preparation method of high-voltage-resistance solid tantalum electrolytic capacitor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113990669B (en) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4804235B2 (en) * | 2005-08-29 | 2011-11-02 | 三洋電機株式会社 | Solid electrolytic capacitor element, manufacturing method thereof and solid electrolytic capacitor |
| JP2013074163A (en) * | 2011-09-28 | 2013-04-22 | Sanyo Electric Co Ltd | Capacitor |
| WO2013073332A1 (en) * | 2011-11-18 | 2013-05-23 | 三洋電機株式会社 | Solid electrolytic capacitor and method for manufacturing same |
| CN111696786B (en) * | 2020-05-19 | 2022-03-08 | 北京七一八友益电子有限责任公司 | Preparation method of high-voltage chip type solid electrolyte tantalum capacitor |
-
2021
- 2021-10-29 CN CN202111276550.2A patent/CN113990669B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN113990669A (en) | 2022-01-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1773640B (en) | Solid electrolytic capacitor and producing method thereof | |
| KR101076312B1 (en) | Solid electrolyte capacitor | |
| CN1862729B (en) | High-specific volume cathode foil solid electrolytic capacitor and preparing method thereof | |
| KR100880482B1 (en) | Solid electrolytic capacitor and method of producing the same | |
| EP1592029B1 (en) | Production method for the capacitor | |
| EP1876612B1 (en) | Solid electrolytic capacitor element, method for manufacturing same, and solid electrolytic capacitor | |
| EP1898433B1 (en) | Solid electrolytic capacitor and production method thereof | |
| US9048024B2 (en) | Solid electrolytic capacitor and method for producing the same | |
| CN113990669B (en) | Preparation method of high-voltage-resistance solid tantalum electrolytic capacitor | |
| EP2866238B1 (en) | Capacitor production method | |
| CN114360911B (en) | Preparation method of chip solid electrolyte tantalum capacitor | |
| WO2002103727A1 (en) | Formed substrate used for solid electrolytic capacitor, production method thereof and solid electrolytic capacitor using the substrate | |
| EP1665301B1 (en) | Production method of a capacitor | |
| CN104538179B (en) | A kind of axially molding tantalum capacitor and its manufacture method | |
| EP1676285B1 (en) | Production method of a capacitor | |
| EP1901319B1 (en) | Method for manufacturing solid electrolytic capacitor device | |
| EP1654745B1 (en) | Chip solid electrolyte capcitor and production method of the same | |
| CN110797216B (en) | Preparation method of high-voltage ultra-small-capacity non-solid electrolyte tantalum electrolytic capacitor | |
| CN114188162B (en) | Solid electrolyte tantalum capacitor and preparation method thereof | |
| CN113611538A (en) | Powder cell solid polymer capacitor and manufacturing method thereof | |
| JP4396970B2 (en) | Tantalum sintered body and capacitor using the sintered body | |
| EP2866237A1 (en) | Capacitor element | |
| CN115831620A (en) | Preparation method of solid electrolyte tantalum capacitor and tantalum capacitor | |
| CN201323135Y (en) | Solid electrolytic capacitor for chip niobium oxides | |
| EP1909298B1 (en) | Method for producing solid electrolytic capacitor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |