CN105070509A - Method for preparing middle-and-high-frequency non-solid electrolytic tantalum capacitor - Google Patents
Method for preparing middle-and-high-frequency non-solid electrolytic tantalum capacitor Download PDFInfo
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Abstract
The invention provides a method for preparing a middle-and-high-frequency non-solid electrolytic tantalum capacitor. The method comprises the following steps of (1) preparing tantalum powder; (2) pressing the tantalum powder to an anode tantalum block, and placing into a high-temperature furnace and calcining; (3) forming a dielectric film in a formed electrolyte; (4) performing thermal treatment on the anode tantalum block; (5) forming a dielectric film on the anode tantalum block; (6) boiling the anode tantalum block and drying; (7) preparing a working electrolyte; (8) finishing capacitor assembling; and (9) aging. The middle-and-high-frequency non-solid electrolytic tantalum capacitor mainly depends on anode tantalum core diameter limit designing and forming technique, high-penetrability and high-conductivity working electrolyte technique and stepped aging technique; the resonance point of an ESR value of the middle-and-high-frequency non-solid electrolytic tantalum capacitor is 600KHz-1.5MHz, thereby greatly expanding the application scope of the capacitor of this kind.
Description
Technical field
The present invention relates to non-solid tantalum electrolytic capacitor preparing technical field, be specifically related to a kind of preparation method of medium-high frequency non-solid tantalum electrolytic capacitor.
Background technology
Capacitor, as common electronic component, is widely used in communication, space flight and military project, submarine cable and the many-side such as advanced electronics, civil electric appliance, plays the effects such as energy storage, filtering, decoupling, bypass, phase inversion in electronic circuit.Non-solid tantalum electrolytic capacitor adopts packed by metal casing (as silver-colored shell, tantalum shell), it is little that this kind of capacitor has leakage current, the advantages such as the CV product large (storing charge ability is strong) of unit volume, be widely used in the energy storage of circuit, the aspects such as front-end filtering, but the frequency of utilization of traditional non-solid tantalum electrolytic capacitor generally within 300KHz (low-frequency range), very little in the practicality of high frequency section, therefore at the capacitor such as solid tantalum electric capacity or MLCC that high frequency section circuit designers often select medium-high frequency characteristic strong, but much little compared with non-solid tantalum electrolytic capacitor of the CV product of these capacitor unit volumes, complete machine miniaturization can not be changed from matter, the demand of lightness and high frequency.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of preparation method of medium-high frequency non-solid tantalum electrolytic capacitor.
The present invention is achieved by the following technical programs.
The preparation method of a kind of medium-high frequency non-solid tantalum electrolytic capacitor provided by the invention, comprises the following steps:
(1) select specific volume be the tantalum powder of 5000-15000 μ FV/g as anode tantalum core design powder, anode tantalum core diameter is
(2) tantalum powder is pressed into anode tantalum block, and puts into high temperature furnace and calcine;
(3) control the quantity forming groove Anodic tantalum block, in formation electrolyte, form Ta
2o
5deielectric-coating;
(4) anode tantalum block be positioned in vacuum furnace and heat-treat, the vacuum degree in stove remains on 2x10
-3within Torr, heat-treat condition is 320 ~ 360 DEG C and keeps 30 ± 10 minutes;
(5) anode tantalum block is put into again formation electrolyte and form Ta
2o
5deielectric-coating;
(6) anode tantalum block is put into deionized water to boil and wash, then put into baking oven and dry;
(7) 38% H
2sO
4add SiO2, CuSO45H2O in the aqueous solution, Ludox and surfactant and conducting polymer composite are mixed with Working electrolyte;
(8) anode tantalum block, Working electrolyte are put in plating ruthenium tantalum shell, and completed capacitor assembling;
(9) capacitor assembled is placed in constant temperature oven and carries out ageing.
Pressed density in described step (2) is 5.0g/cm
3~ 7.5g/cm
3, sintering temperature is 1200 DEG C ~ 1650 DEG C, and sintering time is 20 ~ 40 minutes.
Ionic infiltration, electron type infiltration or ionic and electron type is adopted to infiltrate product to be formed in conjunction with pattern of invasion before described step (3).
The starting voltage that described step (3) applies is 0.1 ~ 0.2 times of rated voltage, and boost current density is 0.35mA/CV; When voltage reaches 70V, current density is down to 0.22mA/CV.
In described step (6), the temperature of deionized water is 80 ± 10 DEG C, and boiling the time of washing is 100 ± 20 minutes, and the temperature of baking oven is 120 ± 10 DEG C, and drying time is 1 ~ 2 hour.
The temperature of the formation electrolyte in described step (5) is 80 ± 10 DEG C, and applying voltage is 1.5 ~ 2.0 times of product rated voltage, and conduction time is 3 ~ 5 hours.
The concrete steps of described step (9) are as follows:
Boost to rated voltage under A, room temperature, and speed controls at 3V/20min ~ 5V/30min, then constant voltage 6h;
B, be slowly warming up to 85 DEG C;
C, under 125 DEG C of conditions, voltage is 0.6 ~ 0.65 times of rated voltage, constant voltage 1h ~ 2h;
D, under 85 DEG C of conditions, voltage is 1.1 ~ 1.2 times of rated voltage, ageing 48h ~ 96h.
Beneficial effect of the present invention is: the quality of Working electrolyte directly affects quality and the characteristic performance of the unit for electrical property parameters of product, the Working electrolyte of preparation better can realize the medium-high frequency effect of novel medium-high frequency product, medium-high frequency non-solid tantalum electrolytic capacitor mainly relies on anode tantalum core diameter limit Design, formation technology, high osmosis and high conductivity Working electrolyte technology and the seasoned technology of ladder, the ESR value of medium-high frequency non-solid tantalum electrolytic capacitor with the resonance point of frequency in 600KHz ~ 1.5MHz scope, greatly improve the scope of application of this series products.
Embodiment
Further describe technical scheme of the present invention below, but described in claimed scope is not limited to.
Embodiment one:
For XX type 75V1200 μ F product, its preparation method comprises the following steps:
(1) select specific volume be the tantalum powder of 15000 μ FV/g as anode tantalum core design powder, according to its limit anode tantalum core diameter of design that considers of the data accumulation of this eka-tantalum powder and this specification overall dimension be
; According to various tantalum powder in specific pressed density, the sintering shrinkage under specific sintering temperature and specification product concrete size design anode tantalum core limit diameter, after determining diameter, according to specification requirement design anode tantalum core size; Adopt the tantalum powder of Fabrication of High Specific Capacitance sheet-like particle, the sintering neck that will many sectional areas be had tiny as granular tantalum powder in the matrix after sintering, be conducive to reducing leakage current and equivalent series resistance, guarantee the extraction of capacity, reduce point discharge hidden danger, puncture voltage is higher, has the feature of sintering resistance and proof voltage.
(2) adopt existing process technology that tantalum powder is pressed into anode tantalum block, and put into high temperature furnace and calcine.Pressed density is 6.0g/cm
3, sintering temperature is 1570 DEG C, constant temperature time 25 minutes; Make the anode block after sintering should have rational porosity and distribution thereof, consider specific volume and the leakage current coefficient of the rear tantalum anode of sintering.Adopt hot blending processes of powders, under 75 DEG C ~ 90 DEG C environment, make tantalum powder mix with adhesive (as odium stearate); The pressed density increasing anode tantalum block can improve green strength.
(3) ionic infiltration, electron type infiltration or ionic and electron type is adopted to infiltrate product to be formed in conjunction with pattern of invasion.Because tantalum powder belongs to high specific capacitance tantalum powder, after sintering, tantalum core inner space is little, infiltration difficulty is large, therefore the pattern of invasion adopting ionic or electron type to combine is aimed at formation product and is infiltrated, improving the product effect of impregnation of product in forming process, being conducive to reducing product because infiltrating the product failure problem not exclusively caused.
Control the quantity forming groove Anodic tantalum block, anode tantalum block is formed Ta2O5 deielectric-coating according to existing process in formation electrolyte; The starting voltage applied is less than 0.2 times of rated voltage, and boost current density is 0.35mA/CV; When voltage reaches 70V, current density is down to 0.22mA/CV; Ta2O5 deielectric-coating state directly determines the quality of the technical parameters such as capacitor is withstand voltage, capacitance, leakage current and ESR.Suitable raising coating-forming voltage, increases Ta
2o
5media coating thickness, improves medium oxidizing rete reliability.Control to form groove Anodic tantalum block overall quantity.
During formation, if the quantity tantalum number of blocks forming groove Anodic tantalum block is too much, there will be during boosting and form uneven phenomenon, be unfavorable for the heat dissipating oxidation reaction process generation in time simultaneously, very easily cause the inner heat-induced crystallization of tantalum block.Form the mixture system that electrolyte selects the inorganic acid of low concentration (phosphoric acid that mainly flash over voltage is high) and ethylene glycol, and be equipped with the special organic additive that volumetric concentration is 5%, guarantee that forming liquid has higher flash over voltage, can effectively suppress oxide-film crystallization simultaneously.
The anode tantalum block of high specific capacitance tantalum powder compacting, inner aperture is less, and the formation bath resistance at this place becomes large relatively, and temperature rise and local overheating are more obvious, therefore must reduce current density a little.Under the prerequisite ensureing formation efficiency, according to different voltage section hierarchical subtractive clustering boost current density, make Ta
2o
5rete flaw is reduced as far as possible in deielectric-coating forming process.
(4) anode tantalum block be positioned in vacuum furnace and heat-treat, within the vacuum degree in stove remains on 2x10-3Torr, heat-treat condition is 360 DEG C and keeps 30 minutes; By heating, the oxide-film having open defect near matrix surface in forming process can be destroyed, tantalum matrix is made to draw oxygen from tantalum pentoxide, tantalum metal-oxide interface can to oxygenate conversion, thus reduce dielectric effective thickness, remove the burr of matrix surface, obtain the dielectric layer of uniform ground, and the benefit bringing leakage current to reduce.
(5) anode tantalum block is put into again formation electrolyte and form Ta2O5 deielectric-coating; Anode tantalum block is put into the phosphoric acid solution that temperature is 85 DEG C, phosphoric acid concentration is 0.5% (volume ratio), applying voltage is 1.5 times of product rated voltage, and conduction time is 3 hours; Select high, that flash over voltage is high, oxidation rate the is fast organic additive of boiling point to be mixed with special formation electrolyte, under specified temp and voltage, adopt low up-flow density to be formed the secondary that anode block after heat treatment carries out a few hours again.This technique after can making conventional formation still unavoidable defective media rete repaired, in former media coating Surface Creation one deck compactness and uniformity better, thicker Ta
2o
5deielectric-coating, significantly promotes media coating intensity and commutating character.
(6) deionized water anode tantalum block being put into 80 DEG C boils washes 100 minutes, and then putting into temperature is that the baking oven of 120 DEG C dries 1 hour.
(7) in the H2SO4 aqueous solution of 38%, add SiO2, CuSO45H2O, Ludox and surfactant and conducting polymer composite are mixed with Working electrolyte; In non-solid tantalum electrolytic capacitor, Working electrolyte is its actual negative electrode, and the quality of Working electrolyte directly affects quality and the characteristic performance of the unit for electrical property parameters of product.
(8) anode tantalum block, Working electrolyte are put in plating ruthenium tantalum shell, and completed capacitor assembling by existing process;
(9) capacitor assembled is placed in constant temperature oven and carries out ageing, concrete steps are:
Boost to rated voltage under A, room temperature, and speed controls at 3V/20min ~ 5V/30min, then constant voltage 6h;
B, be slowly warming up to 85 DEG C;
C, under 125 DEG C of conditions, voltage is 0.6 ~ 0.65 times of rated voltage, constant voltage 1h ~ 2h;
D, under 85 DEG C of conditions, voltage is 1.1 ~ 1.2 times of rated voltage, ageing 48h ~ 96h.
The essence of ageing process is: the process semi-finished product after encapsulation being applied direct voltage, dynamically slaking further, makes capacitor recover its intrinsic electrical property by pressurization, make it possess the condition used in dynamic electron circuit.Meanwhile, non-solid electrolytic condenser, also with " self-healing " effect, again can be formed progressively increasing under suitable applied voltage, carries out polishing reparation, finally automatically recover its ability to work to the dielectric oxide film fault being subject to local failure.
The ESR value of this product is as shown in table 1 with frequency change:
Table 1
| Frequency/KHz | 0.1 | 1 | 10 | 12 | 15 | 20 | 25 | 30 | 40 | 50 | 60 | 80 | 100 |
| ESR/mΩ | 289 | 232 | 134 | 129 | 124 | 118 | 114 | 111 | 107 | 105 | 103 | 100 | 99 |
| Frequency/KHz | 120 | 150 | 200 | 250 | 300 | 400 | 500 | 600 | 800 | 1000 | 1200 | 1500 | 2000 |
| ESR/mΩ | 97 | 96 | 94 | 92 | 90 | 88 | 86 | 85 | 84.6 | 84 | 85 | 88 | 94 |
As shown above, the resonance point of this product is in left and right, 1.0MHz place.
Embodiment two:
For XX type 125V100 μ F product, its preparation method comprises the following steps:
(1) select specific volume be the tantalum powder of 5000 μ FV/g as anode tantalum core design powder, according to the data accumulation of this eka-tantalum powder and this specification overall dimension to consider its limit anode tantalum core diameter of design be φ 8.6;
(2) adopt existing process technology that tantalum powder is pressed into anode tantalum block, and put into high temperature furnace and calcine.Pressed density is 8.0g/cm
3, sintering temperature is 1700 DEG C, constant temperature time 30 minutes;
(3) ionic infiltration, electron type infiltration or ionic and electron type is adopted to infiltrate product to be formed in conjunction with pattern of invasion;
Control the quantity forming groove Anodic tantalum block, anode tantalum block is formed Ta2O5 deielectric-coating according to existing process in formation electrolyte; The starting voltage applied is less than 0.15 times of rated voltage, and boost current density is 0.5mA/CV; When voltage reaches 70V, current density is down to 0.22mA/CV; When voltage reaches 120V, current density is down to 0.15mA/CV, and when voltage reaches 160V, current density is down to 0.1mA/CV; Control starting voltage, when mesolow section is formed, adopt slightly large current density boosting, ensure that coating mass can take into account production efficiency again simultaneously; When high pressure section is formed, apply less boost current density, make anode substrate temperature rise slowly and evenly, effectively can prevent crystallization.
(4) anode tantalum block be positioned in vacuum furnace and heat-treat, the vacuum degree in stove remains on 2x10-3Torr, and heat-treat condition is 380 DEG C and keeps 30 minutes;
(5) anode tantalum block is put into again formation electrolyte and form Ta2O5 deielectric-coating; Anode tantalum block is put into the phosphoric acid solution that temperature is 85 DEG C, phosphoric acid concentration is 0.5% (volume ratio), applying voltage is 1.5 times of product rated voltage, and conduction time is 3 hours;
(6) deionized water anode tantalum block being put into 80 DEG C boils washes 100 minutes, and then putting into temperature is that the baking oven of 120 DEG C dries 1 hour.
(7) in the H2SO4 aqueous solution of 38%, SiO2, Ludox and surfactant is added and conducting polymer composite is mixed with Working electrolyte;
(8) anode tantalum block, Working electrolyte are put in plating ruthenium tantalum shell, and completed capacitor assembling by existing process;
(9) capacitor assembled is placed in constant temperature oven and carries out ageing, concrete steps are:
Boost to rated voltage under A, room temperature, and speed controls at 3V/20min ~ 5V/30min, then constant voltage 6h;
B, be slowly warming up to 85 DEG C;
C, under 125 DEG C of conditions, voltage is 0.6 ~ 0.65 times of rated voltage, constant voltage 1h ~ 2h;
D, under 85 DEG C of conditions, voltage is 1.1 ~ 1.2 times of rated voltage, ageing 48h ~ 96h.The ESR value of this product is as shown in table 2 with frequency change:
Table 2
| Frequency/KHz | 0.1 | 1 | 10 | 12 | 15 | 20 | 25 | 30 | 40 | 50 | 60 | 80 | 100 |
| ESR/mΩ | 467 | 416 | 343 | 330 | 313 | 291 | 274 | 261 | 242 | 228 | 218 | 203 | 193 |
| Frequency/KHz | 120 | 150 | 200 | 250 | 300 | 400 | 500 | 600 | 800 | 1000 | 1200 | 1500 | 2000 |
| ESR/mΩ | 184 | 174 | 161 | 150 | 142 | 130 | 121 | 116 | 109 | 105 | 103 | 102 | 104 |
As shown above, the resonance point of this product is in left and right, 1.5MHz place.
Claims (7)
1. a preparation method for medium-high frequency non-solid tantalum electrolytic capacitor, is characterized in that comprising the following steps:
(1) select specific volume be the tantalum powder of 5000-15000 μ FV/g as anode tantalum core design powder, anode tantalum core diameter is
(2) tantalum powder is pressed into anode tantalum block, and puts into high temperature furnace and calcine;
(3) control the quantity forming groove Anodic tantalum block, in formation electrolyte, form Ta
2o
5deielectric-coating;
(4) anode tantalum block be positioned in vacuum furnace and heat-treat, the vacuum degree in stove remains on 2x10
-3within Torr, heat-treat condition is 320 ~ 360 DEG C and keeps 30 ± 10 minutes;
(5) anode tantalum block is put into again formation electrolyte and form Ta
2o
5deielectric-coating;
(6) anode tantalum block is put into deionized water to boil and wash, then put into baking oven and dry;
(7) 38% H
2sO
4add SiO2, CuSO45H2O in the aqueous solution, Ludox and surfactant and conducting polymer composite are mixed with Working electrolyte;
(8) anode tantalum block, Working electrolyte are put in plating ruthenium tantalum shell, and completed capacitor assembling;
(9) capacitor assembled is placed in constant temperature oven and carries out ageing.
2. the preparation method of medium-high frequency non-solid tantalum electrolytic capacitor as claimed in claim 1, is characterized in that: the pressed density in described step (2) is 5.0g/cm
3~ 7.5g/cm
3, sintering temperature is 1200 DEG C ~ 1650 DEG C, and sintering time is 20 ~ 40 minutes.
3. the preparation method of medium-high frequency non-solid tantalum electrolytic capacitor as claimed in claim 1, is characterized in that: adopt ionic infiltration, electron type infiltration or ionic and electron type to infiltrate product to be formed in conjunction with pattern of invasion before described step (3).
4. the preparation method of medium-high frequency non-solid tantalum electrolytic capacitor as claimed in claim 1, is characterized in that: the starting voltage that described step (3) applies is 0.1 ~ 0.2 times of rated voltage, and boost current density is 0.35mA/CV; When voltage reaches 70V, current density is down to 0.22mA/CV.
5. the preparation method of medium-high frequency non-solid tantalum electrolytic capacitor as claimed in claim 1, it is characterized in that: in described step (6), the temperature of deionized water is 80 ± 10 DEG C, boiling the time of washing is 100 ± 20 minutes, and the temperature of baking oven is 120 ± 10 DEG C, and drying time is 1 ~ 2 hour.
6. the preparation method of medium-high frequency non-solid tantalum electrolytic capacitor as claimed in claim 1, it is characterized in that: the temperature of the formation electrolyte in described step (5) is 80 ± 10 DEG C, applying voltage is 1.5 ~ 2.0 times of product rated voltage, and conduction time is 3 ~ 5 hours.
7. the preparation method of medium-high frequency non-solid tantalum electrolytic capacitor as claimed in claim 1, is characterized in that: the concrete steps of described step (9) are as follows:
Boost to rated voltage under A, room temperature, and speed controls at 3V/20min ~ 5V/30min, then constant voltage 6h;
B, be slowly warming up to 85 DEG C;
C, under 125 DEG C of conditions, voltage is 0.6 ~ 0.65 times of rated voltage, constant voltage 1h ~ 2h;
D, under 85 DEG C of conditions, voltage is 1.1 ~ 1.2 times of rated voltage, ageing 48h ~ 96h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108091491A (en) * | 2017-12-12 | 2018-05-29 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | The method for reducing the method for non-solid electrolyte tantalum capacity fall off flow valuve and preparing non-solid electrolyte tantalum capacitance |
| CN110797216A (en) * | 2019-11-15 | 2020-02-14 | 中国振华（集团）新云电子元器件有限责任公司 | Preparation method of high-voltage ultra-small-capacity non-solid electrolyte tantalum electrolytic capacitor |
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| CN1889212A (en) * | 2005-06-30 | 2007-01-03 | 天津大学 | Electrolyte for liquid Ta electrolytic condenser and producing method thereof |
| CN103310981A (en) * | 2013-07-03 | 2013-09-18 | 中国振华（集团）新云电子元器件有限责任公司 | Producing method for full-tantalum-gas sealed capacitor |
| CN103887085A (en) * | 2014-03-28 | 2014-06-25 | 贵州中航聚电科技有限公司 | High-voltage electrolyte for hybrid super tantalum capacitor and preparation method thereof |
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2015
- 2015-07-15 CN CN201510415379.7A patent/CN105070509A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1889212A (en) * | 2005-06-30 | 2007-01-03 | 天津大学 | Electrolyte for liquid Ta electrolytic condenser and producing method thereof |
| CN103310981A (en) * | 2013-07-03 | 2013-09-18 | 中国振华（集团）新云电子元器件有限责任公司 | Producing method for full-tantalum-gas sealed capacitor |
| CN103887085A (en) * | 2014-03-28 | 2014-06-25 | 贵州中航聚电科技有限公司 | High-voltage electrolyte for hybrid super tantalum capacitor and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108091491A (en) * | 2017-12-12 | 2018-05-29 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | The method for reducing the method for non-solid electrolyte tantalum capacity fall off flow valuve and preparing non-solid electrolyte tantalum capacitance |
| CN110797216A (en) * | 2019-11-15 | 2020-02-14 | 中国振华（集团）新云电子元器件有限责任公司 | Preparation method of high-voltage ultra-small-capacity non-solid electrolyte tantalum electrolytic capacitor |
| CN110797216B (en) * | 2019-11-15 | 2022-01-21 | 中国振华（集团）新云电子元器件有限责任公司 | Preparation method of high-voltage ultra-small-capacity non-solid electrolyte tantalum electrolytic capacitor |
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