CN111341564A - Tantalum core coating method, tantalum core, tantalum capacitor comprising tantalum core, and application - Google Patents
Tantalum core coating method, tantalum core, tantalum capacitor comprising tantalum core, and application Download PDFInfo
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- CN111341564A CN111341564A CN202010168294.4A CN202010168294A CN111341564A CN 111341564 A CN111341564 A CN 111341564A CN 202010168294 A CN202010168294 A CN 202010168294A CN 111341564 A CN111341564 A CN 111341564A
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- tantalum
- tantalum core
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical group [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 184
- 238000000576 coating method Methods 0.000 title claims abstract description 109
- 239000003990 capacitor Substances 0.000 title claims abstract description 45
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 43
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000011248 coating agent Substances 0.000 claims description 75
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 70
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 55
- 238000001035 drying Methods 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 32
- 238000007598 dipping method Methods 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 28
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 27
- 239000001301 oxygen Substances 0.000 claims description 27
- 229910052760 oxygen Inorganic materials 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000002775 capsule Substances 0.000 claims description 20
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000007654 immersion Methods 0.000 claims description 3
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 abstract description 7
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000000354 decomposition reaction Methods 0.000 description 9
- 238000002791 soaking Methods 0.000 description 8
- 238000005476 soldering Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000007723 die pressing method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/025—Solid electrolytes
- H01G9/032—Inorganic semiconducting electrolytes, e.g. MnO2
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
- H01G13/04—Drying; Impregnating
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention provides a tantalum core coating method, a tantalum core, a tantalum capacitor comprising the tantalum core and application of the tantalum core, and relates to the technical field of capacitor preparation. The coating method can form a manganese dioxide layer on the outer layer of the tantalum core, so that the tantalum pentoxide dielectric layer of the tantalum core is protected, and the reliability of the tantalum capacitor is improved.
Description
Technical Field
The invention relates to the technical field of capacitor preparation, in particular to a tantalum core coating method, a tantalum core, a tantalum capacitor comprising the tantalum core and application of the tantalum capacitor.
Background
With the continuous development of electronic technology, the trend of miniaturization of tantalum capacitors as solid electrolytes is increasingly obvious, and especially in recent years, power technology and processor technology have been changed significantly, so that chip tantalum capacitors are more and more applied to various fields such as military industry. Therefore, the reliability requirements for tantalum capacitors are also increasing.
It is well known that the capsule process is one of the key factors affecting the performance of tantalum capacitors. For the chip tantalum capacitor, the stress resistance of the chip tantalum capacitor is directly influenced by the density of the outer layer envelope, and whether the tantalum pentoxide dielectric layer can be effectively protected from being damaged or not is further determined. Because the main failure mode of the chip tantalum capacitor is breakdown failure after electrification caused by damage of the tantalum pentoxide dielectric layer, the integrity of the tantalum pentoxide dielectric layer determines the reliability of the chip tantalum capacitor. Therefore, researches and developments of a method capable of effectively improving the die pressing resistance, reflow soldering resistance and temperature impact resistance of the tantalum capacitor are urgently needed.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the present invention is to provide a tantalum core coating method, which can form a manganese dioxide layer on the outer layer of a tantalum core, further protect the tantalum pentoxide dielectric layer of the tantalum core, and improve the reliability of a tantalum capacitor.
The second object of the present invention is to provide a tantalum core produced mainly by the above tantalum core coating method.
A third object of the present invention is to provide a tantalum capacitor including the above tantalum core.
The fourth object of the present invention is to provide the tantalum core coating method, the tantalum core and the tantalum capacitor in the production of circuit board products.
The invention provides a tantalum core coating method, which comprises the following steps:
the tantalum core is entirely immersed in a manganese nitrate solution, and the tantalum core immersed in the manganese nitrate solution is then thermally decomposed to thermally decompose manganese nitrate into manganese dioxide, thereby completing the coating.
Further, the concentration of the manganese nitrate solution is 1.1-1.7 g/m3；
Preferably, the concentration of the manganese nitrate solution is 1.5g/m3And dipping the manganese nitrate solution in a concentration gradient increasing mode.
Further, the dipping time of the tantalum core in the manganese nitrate solution is 2-8 min, preferably 5 min;
preferably, the dipping temperature of the tantalum core dipped into the manganese nitrate solution is 35-50 ℃, and preferably 40 ℃.
Further, the coating method may further include the step of drying the tantalum core after the dipping and before the thermal decomposition;
preferably, the drying temperature is 80-90 ℃, and preferably 85 ℃;
preferably, the drying time is 5-7 min, preferably 6 min.
Further, the thermal decomposition is performed in a coating furnace.
Preferably, the thermal decomposition temperature is 115-260 ℃, and the thermal decomposition time is 15-21 min;
preferably, the thermal decomposition is a gradient temperature rise;
more preferably, the gradient temperature rise includes: firstly heating to 115-135 ℃ for thermal decomposition for 10-14 min, and then heating to 240-260 ℃ for thermal decomposition for 5-7 min;
preferably, the inside of the coating furnace contains water vapor mixed with oxygen;
more preferably, the volume percentage of the oxygen in the coating furnace is 8-14%, preferably 10%.
Further, the thermal decomposition comprises the steps of: putting the dipped and dried tantalum core into a coating furnace, wherein the coating furnace contains water vapor mixed with oxygen, heating to 115-135 ℃ for thermal decomposition for 10-14 min, and then heating to 240-260 ℃ for thermal decomposition for 5-7 min to thermally decompose manganese nitrate into manganese dioxide;
preferably, the thermal decomposition comprises the steps of: and putting the dipped and dried tantalum core into a coating furnace, wherein the coating furnace contains water vapor mixed with oxygen, and then heating to 125 ℃ for thermal decomposition for 12min, and then heating to 250 ℃ for thermal decomposition for 6min, so that manganese nitrate is thermally decomposed into manganese dioxide.
Further, the coating method comprises the following steps:
(a) and dipping: dipping the tantalum core into the solution with the concentration of 1.1-1.7 g/m3Dipping the manganese nitrate solution for 2-8 min at 35-50 ℃;
(b) and (3) drying: drying the dipped tantalum core for 5-7 min at the temperature of 80-90 ℃;
(c) and thermal decomposition: putting the tantalum core dried in the step (b) into a coating furnace, wherein the coating furnace contains water vapor mixed with oxygen, heating to 115-135 ℃ for thermal decomposition for 10-14 min, and then heating to 240-260 ℃ for thermal decomposition for 5-7 min, so that manganese nitrate is thermally decomposed into manganese dioxide;
preferably, the coating method further comprises (d) the step of repeatedly coating the tantalum core:
(d) and repeating the coating: repeating the steps (a) to (c) in sequence to form a dense manganese dioxide layer and complete the coating.
The tantalum core provided by the invention is mainly prepared by the tantalum core coating method.
The invention provides a tantalum capacitor, which comprises the tantalum core;
preferably, the tantalum capacitor is a chip tantalum capacitor.
The invention provides the tantalum core coating method, the tantalum core and the application of the tantalum capacitor in the preparation of circuit board products.
Compared with the prior art, the invention has the beneficial effects that:
the coating method of the tantalum core comprises the steps of firstly soaking the tantalum core into a manganese nitrate solution, and then thermally decomposing the tantalum core soaked in the manganese nitrate solution to enable the manganese nitrate to be thermally decomposed into manganese dioxide, so as to finish the coating. The coating method can form a manganese dioxide layer on the outer layer of the tantalum core, so that the tantalum pentoxide dielectric layer of the tantalum core is protected, and the reliability of the tantalum capacitor is improved.
The tantalum core provided by the invention is mainly prepared by the tantalum core coating method, and the tantalum core has better reflow soldering resistance and temperature impact resistance through detection.
The tantalum capacitor provided by the invention comprises the tantalum core, and the reliability is better compared with the existing tantalum capacitor.
The invention provides the tantalum core coating method, the tantalum core and the application of the tantalum capacitor in the preparation of circuit board products.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. 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.
According to one aspect of the invention, a tantalum core capsule method comprises the steps of:
the tantalum core is entirely immersed in a manganese nitrate solution, and the tantalum core immersed in the manganese nitrate solution is then thermally decomposed to thermally decompose manganese nitrate into manganese dioxide, thereby completing the coating.
The coating method of the tantalum core comprises the steps of firstly soaking the tantalum core into a manganese nitrate solution, and then thermally decomposing the tantalum core soaked in the manganese nitrate solution to enable the manganese nitrate to be thermally decomposed into manganese dioxide, so as to finish the coating. The coating method can effectively form a manganese dioxide layer on the outer layer of the tantalum core, so that the tantalum pentoxide dielectric layer of the tantalum core is protected, and the reliability of the tantalum capacitor is improved.
In a preferred embodiment of the present invention, the concentration of the manganese nitrate solution is 1.1 to 1.7g/m3；
In a preferred embodiment, the manganese nitrate solution is impregnated by selecting a starting impregnation with a lower concentration, so as to effectively ensure the filling of the tantalum core.
The concentration of the manganese nitrate solution is typical but not limitedPreferred embodiments are: 1.1g/m3、 1.2g/m3、1.3g/m3、1.4g/m3、1.5g/m3、1.6g/m3And 1.7g/m3。
Preferably, the concentration of the manganese nitrate solution is 1.5g/m3And dipping the manganese nitrate solution in a concentration gradient increasing mode.
In a preferred embodiment of the invention, the immersion time of the tantalum core in the manganese nitrate solution is 2-8 min, preferably 5 min;
in a preferred embodiment, the tantalum core is immersed in the manganese nitrate solution for a short period of time, and the tantalum core cannot be completely immersed in the manganese nitrate solution, so that the production efficiency is reduced due to the long immersion time.
Typical but non-limiting preferred embodiments of the above impregnation times are: 2min, 3min, 4min, 5min, 6min, 7min and 8 min.
In a preferred embodiment of the present invention, the dipping temperature of the tantalum core into the manganese nitrate solution is 35 to 50 ℃, preferably 40 ℃.
In a preferred embodiment, the tantalum core is immersed in the manganese nitrate solution at a low temperature, and has a high surface tension, poor permeability, and decomposition may occur during long-term use at a high temperature.
Typical but non-limiting preferred embodiments of the above impregnation temperatures are: 35 deg.C, 38 deg.C, 40 deg.C, 42 deg.C, 45 deg.C, 48 deg.C and 50 deg.C.
In a preferred embodiment of the present invention, the coating method further comprises the step of drying the tantalum core after the dipping before the thermal decomposition;
in the preferred embodiment, the drying temperature is 80-90 ℃, preferably 85 ℃;
in a preferred embodiment, the drying temperature is low, water in the manganese nitrate solution cannot be sufficiently volatilized, and the high temperature may cause dry decomposition of the manganese nitrate solution.
Typical but non-limiting preferred embodiments of the above drying temperatures are: 80 deg.C, 82 deg.C, 85 deg.C, 88 deg.C and 90 deg.C.
In the preferred embodiment, the drying time is 5 to 7min, preferably 6 min.
In a preferred embodiment, the drying time is short, the water in the manganese nitrate solution cannot be sufficiently volatilized, and the drying time may be long, which may cause dry decomposition of the manganese nitrate solution and decrease in production efficiency.
Typical but non-limiting preferred embodiments of the above drying times are: 5min, 5.5min, 6min, 6.5min and 7 min.
In a preferred embodiment of the invention, the thermal decomposition is carried out in a coating furnace.
In the preferred embodiment, the thermal decomposition temperature is 115 to 260 ℃;
in a preferred embodiment, the temperature of the thermal decomposition is slowly increased from a temperature to the decomposition temperature of the manganese nitrate, which effectively ensures slow decomposition of the manganese nitrate and a more dense manganese dioxide after decomposition.
Typical but non-limiting preferred embodiments of the above thermal decomposition temperatures are: 115 ℃, 120 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 250 ℃ and 260 ℃.
In the preferred embodiment, the thermal decomposition time is 15 to 21 min;
in a preferred embodiment, the thermal decomposition does not take place completely in a short time, and the dielectric layer is damaged and the production efficiency is reduced in a long time.
Typical but non-limiting preferred embodiments of the above thermal decomposition are: 15min, 16min, 17min, 18min, 19min, 20min and 21 min.
In a preferred embodiment of the present invention, the coating furnace contains water vapor mixed with oxygen;
in the above preferred embodiment, the volume percentage of the oxygen gas in the coating furnace is 8 to 14%, preferably 10%.
In a preferred embodiment, the above-mentioned long decomposition time required for the oxygen gas to have a low volume percentage in the film furnace lowers the production efficiency, and the high oxygen content causes too fast decomposition, resulting in dry decomposition.
Typical but non-limiting preferred embodiments of the above-mentioned volume percentages of oxygen in water vapor are: 8%, 9%, 10%, 11%, 12%, 13% and 14%.
In the above preferred embodiment, the thermal decomposition comprises the steps of: putting the dipped and dried tantalum core into a coating furnace, wherein the coating furnace contains water vapor mixed with oxygen, heating to 115-135 ℃ for thermal decomposition for 10-14 min, and then heating to 240-260 ℃ for thermal decomposition for 5-7 min to thermally decompose manganese nitrate into manganese dioxide;
preferably, the thermal decomposition comprises the steps of: and putting the dipped and dried tantalum core into a coating furnace, wherein the coating furnace contains water vapor mixed with oxygen, and then heating to 125 ℃ for thermal decomposition for 12min, and then heating to 250 ℃ for thermal decomposition for 6min, so that manganese nitrate is thermally decomposed into manganese dioxide.
In a preferred embodiment of the present invention, the coating method comprises the steps of:
(a) and dipping: dipping the tantalum core into a manganese nitrate solution with the concentration of 1.1-1.7 g/m3, and dipping for 2-8 min at 35-50 ℃;
(b) and (3) drying: drying the dipped tantalum core for 5-7 min at the temperature of 80-90 ℃;
(c) and thermal decomposition: putting the tantalum core dried in the step (b) into a coating furnace, wherein the coating furnace contains water vapor mixed with oxygen, heating to 115-135 ℃ for thermal decomposition for 10-14 min, and then heating to 240-260 ℃ for thermal decomposition for 5-7 min, so that manganese nitrate is thermally decomposed into manganese dioxide;
preferably, the coating method further comprises (d) the step of repeatedly coating the tantalum core:
(d) and repeating the coating: repeating the steps (a) to (c) in sequence to form a dense manganese dioxide layer and complete the coating.
According to one aspect of the present invention, a tantalum core is produced primarily by the above tantalum core coating method.
The tantalum core provided by the invention is mainly prepared by the tantalum core coating method, and the tantalum core has better capabilities of resisting mould pressing, reflow soldering and temperature impact through detection.
According to an aspect of the present invention, a tantalum capacitor comprising the above tantalum core;
the tantalum capacitor provided by the invention comprises the tantalum core, and the reliability is better compared with the existing tantalum capacitor.
Preferably, the tantalum capacitor is a chip tantalum capacitor.
The invention provides the tantalum core coating method, the tantalum core and the application of the tantalum capacitor in the preparation of electric appliance and instrument circuit board products.
The technical solution of the present invention will be further described with reference to examples and comparative examples.
Example 1
A tantalum core capsule method, said capsule method comprising the steps of:
(a) and dipping: soaking the tantalum core in a manganese nitrate solution for 2min at 35 ℃;
(b) and (3) drying: drying the dipped tantalum core at 80 ℃ for 5 min;
(c) and thermal decomposition: putting the tantalum core dried in the step (b) into a coating furnace, wherein the coating furnace contains water vapor mixed with oxygen, heating to 115 ℃ and placing for 10min, and then heating to 240 ℃ and placing for 5min to thermally decompose manganese nitrate into manganese dioxide;
the volume percentage of the oxygen in the water vapor is 8%;
(d) and repeating the coating: sequentially repeating the steps (a) to (c), wherein the dipping manganese nitrate solution is increased in gradient, and the coating procedure is as follows: 1.1g/m for 3 times33 times 1.2, 2 times 1.35, 2 times 1.55, 2 times 1.7, 1 times 2.1, 2 times 1.5, a dense manganese dioxide layer was formed, and the coating was completed to obtain a tantalum core.
Example 2
A tantalum core capsule method, said capsule method comprising the steps of:
(a) and dipping: soaking the tantalum core in a manganese nitrate solution for 2-8 min at 50 ℃;
(b) and (3) drying: drying the dipped tantalum core at 90 ℃ for 7 min;
(c) and thermal decomposition: putting the tantalum core dried in the step (b) into a coating furnace, wherein the coating furnace contains water vapor mixed with oxygen, heating to 135 ℃ and placing for 10-14 min, and then heating to 260 ℃ and placing for 5-7 min, so that manganese nitrate is thermally decomposed into manganese dioxide;
the volume percentage of the oxygen in the water vapor is 14%;
(d) and repeating the coating: sequentially repeating the steps (a) to (c), wherein the dipping manganese nitrate solution is increased in gradient, and the coating procedure is as follows: 1.1g/m for 3 times33 times 1.2, 2 times 1.35, 2 times 1.55, 2 times 1.7, 1 times 2.1, 2 times 1.5, a dense manganese dioxide layer was formed, and the coating was completed to obtain a tantalum core.
Example 3
A tantalum core capsule method, said capsule method comprising the steps of:
(a) and dipping: soaking the tantalum core in a manganese nitrate solution for 3min at 38 ℃;
(b) and (3) drying: drying the dipped tantalum core at 82 ℃ for 5.5 min;
(c) and thermal decomposition: putting the tantalum core dried in the step (b) into a coating furnace, wherein the coating furnace contains water vapor mixed with oxygen, heating to 120 ℃ and placing for 11min, and then heating to 245 ℃ and placing for 5min to thermally decompose manganese nitrate into manganese dioxide;
the volume percentage of the oxygen in the water vapor is 9%;
(d) and repeating the coating: sequentially repeating the steps (a) to (c), wherein the dipping manganese nitrate solution is increased in gradient, and the coating procedure is as follows: 1.1g/m for 3 times33 times 1.2, 2 times 1.35, 2 times 1.55, 2 times 1.7, 1 times 2.1, 2 times 1.5, a dense manganese dioxide layer was formed, and the coating was completed to obtain a tantalum core.
Example 4
A tantalum core capsule method, said capsule method comprising the steps of:
(a) and dipping: soaking the tantalum core in a manganese nitrate solution for 7min at 48 ℃;
(b) and (3) drying: drying the dipped tantalum core at 88 ℃ for 6.5 min;
(c) and thermal decomposition: putting the tantalum core dried in the step (b) into a coating furnace, wherein the coating furnace contains water vapor mixed with oxygen, heating to 130 ℃ and placing for 13min, and then heating to 255 ℃ and placing for 6.5min to thermally decompose manganese nitrate into manganese dioxide;
the volume percentage of the oxygen in the water vapor is 12%;
(d) and repeating the coating: sequentially repeating the steps (a) to (c), wherein the dipping manganese nitrate solution is increased in gradient, and the coating procedure is as follows: 1.1g/m for 3 times33 times 1.2, 2 times 1.35, 2 times 1.55, 2 times 1.7, 1 times 2.1, 2 times 1.5, a dense manganese dioxide layer was formed, and the coating was completed to obtain a tantalum core.
Example 5
A tantalum core capsule method, said capsule method comprising the steps of:
(a) and dipping: soaking the tantalum core in manganese nitrate solution at 40 ℃ for 5 min;
(b) and (3) drying: drying the dipped tantalum core at 85 ℃ for 6 min;
(c) and thermal decomposition: putting the tantalum core dried in the step (b) into a coating furnace, wherein the coating furnace contains water vapor mixed with oxygen, heating to 125 ℃ and placing for 12min, and then heating to 250 ℃ and placing for 6min to thermally decompose manganese nitrate into manganese dioxide;
the volume percentage of the oxygen in the water vapor is 10 percent;
(d) and repeating the coating: sequentially repeating the steps (a) to (c), wherein the dipping manganese nitrate solution is increased in gradient, and the coating procedure is as follows: 1.1g/m for 3 times33 times 1.2, 2 times 1.35, 2 times 1.55, 2 times 1.7, 1 times 2.1, 2 times 1.5, a dense manganese dioxide layer was formed, and the coating was completed to obtain a tantalum core.
General coating method
A tantalum core capsule method, said capsule method comprising the steps of:
(a) and dipping: the tantalum core was dipped into manganese nitrate solution and the coating procedure was: 1.1g/m for 3 times33 times of 1.2, 2 times of 1.35, 2 times of 1.55, 2 times of 1.7, 1 time of 2.1, 2 times of 1.5, soaking for 5min at 50 ℃;
(b) and (3) drying: drying the dipped tantalum core at 85 ℃ for 6 min;
(c) and thermal decomposition: placing the tantalum core dried in the step (b) into a coating furnace, wherein water vapor is mixed in the coating furnace, and placing the coating furnace for 6min at 250 ℃ to thermally decompose manganese nitrate into manganese dioxide;
the volume percentage of the oxygen in the capsule furnace is 10%;
(d) and repeating the coating: repeating the steps (a) to (c) for 15 times in sequence to generate a dense manganese dioxide layer, and completing the coating to obtain the tantalum core.
Experimental example 1
In order to show that the tantalum core prepared by the method has better reliability compared with the existing tantalum core, the tantalum core with the specification of 35V10 mu F-D is prepared by the coating of the embodiment 1-5, then the tantalum core prepared by the embodiment 1-5 is respectively prepared into the tantalum capacitor containing 1144 tantalum cores, and meanwhile, the tantalum core prepared by the common coating method is also prepared into the corresponding tantalum capacitor as a comparison. Then, 200 products are respectively extracted to continuously perform 5 times of reflow soldering and 10 times of temperature impact, and the qualification condition of the leakage current is tested, and the test results are shown in the following table:
as can be seen from the table above, the tantalum capacitor prepared by the coating tantalum core has stronger reflow resistance and temperature impact resistance, and the qualification rate is improved by 25.5 percent compared with the tantalum capacitor processed by the conventional method. The tantalum capacitor has the advantages that the capacity of resisting reflow soldering and temperature impact is obviously superior to that of the prior art through multiple tests, small-batch trial production is already carried out in the prior art, and the effect is obvious.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A tantalum core coating method, characterized in that said coating method comprises the steps of:
the tantalum core is entirely immersed in a manganese nitrate solution, and the tantalum core immersed in the manganese nitrate solution is then thermally decomposed to thermally decompose manganese nitrate into manganese dioxide, thereby completing the coating.
2. The method for coating tantalum core according to claim 1, wherein said manganese nitrate solution has a concentration of 1.1 to 1.7g/m3；
Preferably, the concentration of the manganese nitrate solution is 1.5g/m3And dipping the manganese nitrate solution in a concentration gradient increasing mode.
3. The method for coating tantalum core according to claim 1, wherein said tantalum core is immersed in manganese nitrate solution for 2-8 min, preferably 5 min;
preferably, the dipping temperature of the tantalum core dipped into the manganese nitrate solution is 35-50 ℃, and preferably 40 ℃.
4. The tantalum core coating method of claim 1, further comprising the step of drying the tantalum core after immersion before thermal decomposition;
preferably, the drying temperature is 80-90 ℃, and preferably 85 ℃;
preferably, the drying time is 5-7 min, preferably 6 min.
5. The tantalum core capsule method of claim 1, wherein said thermal decomposition is performed in a capsule furnace;
preferably, the thermal decomposition temperature is 115-260 ℃, and the thermal decomposition time is 15-21 min;
preferably, the thermal decomposition is a gradient temperature rise;
more preferably, the gradient temperature rise includes: firstly heating to 115-135 ℃ for thermal decomposition for 10-14 min, and then heating to 240-260 ℃ for thermal decomposition for 5-7 min;
preferably, the inside of the coating furnace contains water vapor mixed with oxygen;
more preferably, the volume percentage of the oxygen in the coating furnace is 8-14%, preferably 10%.
6. The tantalum core capsule method of claim 5, wherein said thermal decomposition comprises the steps of: putting the dipped and dried tantalum core into a coating furnace, wherein the coating furnace contains water vapor mixed with oxygen, heating to 115-135 ℃ for thermal decomposition for 10-14 min, and then heating to 240-260 ℃ for thermal decomposition for 5-7 min to thermally decompose manganese nitrate into manganese dioxide;
preferably, the thermal decomposition comprises the steps of: and putting the dipped and dried tantalum core into a coating furnace, wherein the coating furnace contains water vapor mixed with oxygen, and then heating to 125 ℃ for thermal decomposition for 12min, and then heating to 250 ℃ for thermal decomposition for 6min, so that manganese nitrate is thermally decomposed into manganese dioxide.
7. The tantalum core capsule method of claim 1, wherein said capsule method comprises the steps of:
(a) and dipping: dipping the tantalum core into the solution with the concentration of 1.1-1.7 g/m3Dipping the manganese nitrate solution for 2-8 min at 35-50 ℃;
(b) and (3) drying: drying the dipped tantalum core for 5-7 min at the temperature of 80-90 ℃;
(c) and thermal decomposition: putting the tantalum core dried in the step (b) into a coating furnace, wherein the coating furnace contains water vapor mixed with oxygen, heating to 115-135 ℃ for thermal decomposition for 10-14 min, and then heating to 240-260 ℃ for thermal decomposition for 5-7 min, so that manganese nitrate is thermally decomposed into manganese dioxide;
preferably, the coating method further comprises (d) the step of repeatedly coating the tantalum core:
(d) and repeating the coating: repeating the steps (a) to (c) for 15-20 times in sequence to generate a dense manganese dioxide layer and complete the coating.
8. A tantalum core produced by the tantalum core coating method according to any one of claims 1 to 7.
9. A tantalum capacitor, wherein said tantalum capacitor comprises the tantalum core of claim 8;
preferably, the tantalum capacitor is a chip tantalum capacitor.
10. Use of the tantalum core coating method according to any one of claims 1 to 7, the tantalum core according to claim 8, or the tantalum capacitor according to claim 9 for the production of circuit board products.
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