CN105428095B - Improve the vacuum control unit of polythiophene solid tantalum capacitor consistency of performance - Google Patents

Improve the vacuum control unit of polythiophene solid tantalum capacitor consistency of performance Download PDF

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Publication number
CN105428095B
CN105428095B CN201510859851.6A CN201510859851A CN105428095B CN 105428095 B CN105428095 B CN 105428095B CN 201510859851 A CN201510859851 A CN 201510859851A CN 105428095 B CN105428095 B CN 105428095B
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vacuum
tantalum
core
performance
pedot
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CN105428095A (en
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王秀宇
马小品
李晨光
程强
张�浩
陈同宁
张平
张大义
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Tianjin University
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Tianjin University
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Abstract

The invention discloses a kind of vacuum control unit for improving polythiophene solid tantalum capacitor consistency of performance, it is made up of vacuum cavity system, vacuum pump system and numerical control system;First by the suspension of tantalum core on a robotic arm, by PEDOT:The PSS aqueous solution is placed in container, covers vacuum (-tight) housing, forms vacuum cavity system;Restart vavuum pump, when vacuum reaches 1~100Pa, start digital control circuit, make manipulator tantalum core is completely immersed in PEDOT:In the PSS aqueous solution;After tantalum core soaks 0.5~5min, vavuum pump is closed, then tantalum core is dried, is cooled down;Repeat the above steps 8 times, obtain the tantalum core of coated PEDOT cathode materials.Tantalum core is coated into graphite again, drying, silver paste is soaked after cooling, is dried, cooling, tantalum capacitor cathode material is made, tantalum processed obtains tantalum capacitor after encapsulation.The present invention improves the uniformity of properties of product, is adapted to the batch production of organic solid tantalum capacitor, the control device is simple in construction, easily operated, and cost is low, may extend to the production of the organic solid capacitor such as aluminium, niobium.

Description

Improve the vacuum control unit of polythiophene solid tantalum capacitor consistency of performance
Technical field
The present invention will can be gathered by vacuum control circuit on polythiophene solid tantalum capacitor, more particularly to one kind The negative electrode that thiophene conductive material quickly contacted, realized solid tantalum capacitor with tantalum wicking surface under vacuum conditions is drawn, improved together The vacuum control unit and its operating method of series-produced product electrical property consistency.
Background technology
Solid tantalum capacitor has the characteristics that Large Copacity, long-life, stability are high as liquid tantalum capacitor, but solid The shortcomings that body tantalum capacitor is due to using solid conductive material as drawing negative electrode, therefore can overcome solid tantalum capacitor leakage. Solid tantalum capacitor because of electroless liquid, therefore can chip type, miniaturization, surface mounting technology (SMT) is can adapt to, ultra-thin small Type electronic product and portable electric appts etc. are used widely.As performance of integrated circuits improves constantly, to institute Solid tantalum capacitor is needed to propose higher requirement, especially high frequency characteristics.Current solid tantalum capacitor mainly uses MnO2Make Material, but MnO are drawn for negative electrode2Electrical conductivity is relatively low (about 0.1S/cm) so that solid tantalum capacitor equivalent series resistance (ESR) It is larger, it is unfavorable for the raising of its high frequency performance.Therefore an urgent demand uses high conductivity material substitution MnO2As solid tantalum electricity The negative electrode of container draws material.
Conducting polymer poly- 3,4 ethene dioxythiophenes (PEDOT) are because its electrical conductivity is higher (1~500S/cm), synthesis side Method is simple, therefore substitutes MnO with PEDOT2Cathode material as solid tantalum capacitor is following solid tantalum capacitor development Trend.PEDOT is a kind of difficult dissolving polymer material, is not easy to reprocess, and limits its application.To solve this problem, people is studied Member introduces poly styrene sulfonate (PSS) in PEDOT building-up processes, and the aqueous dispersion PEDOT of polythiophene is made:PSS, To meet the process requirements of various applications.Tantalum core be suppressed, sintered by tantalum powder, energize after particle surface formed Ta2O5Medium Film, its microscopic appearance are a kind of multi-pore structures being made up of many particles, have larger surface area, this be also its have compared with One of the reason for Large Copacity.Use PEDOT:The PSS aqueous solution prepares the cathode material of solid tantalum capacitor, conventional method be In the case of normal pressure, tantalum core is immersed in PEDOT:In the PSS aqueous solution, so as to be coated to PEDOT in tantalum core inner and outer surface: PSS thin-film materials.But experiment is found, can not fully be drawn by tantalum capacitance made from immersion in the case of normal pressure, and it is same The polythiophene solid tantalum capacitor electrical property consistency that batch makes is poor, (~5min), this shortcoming when soak time is shorter It is just more prominent.This is primarily due at ambient pressure, the air full of absorption in tantalum core inner micropore, hinders PEDOT:PSS is water-soluble Liquid is fully infiltrated into tantalum core inner;In addition, the surface tension effects of liquid and tantalum wicking surface particle so that the gas in tantalum core micropore It is not easy to discharge, so as to cause the same batch polythiophene solid tantalum capacitor prepared under condition of normal pressure, performance difference is larger.
The problem of running into and the analysis of causes are drawn based on polythiophene solid tantalum capacitor negative electrode, so as to generate the present invention, To improve a kind of new method is conformity provided with batch polythiophene solid tantalum capacitor performance.
The content of the invention
The purpose of the present invention, it is the polythiophene solid tantalum capacitor electrical property for overcoming the same batch of prior art to make The defects of uniformity difference, there is provided a kind of vacuum automatic control device and its operating method, the device first exclude tantalum core inner hole In air, reduce gas-liquid surface tension force, promote PEDOT:The PSS aqueous solution enters in tantalum core micropore, makes PEDOT:PSS conduction materials Material can rapid Cover in tantalum wicking surface, capacitance is fully drawn, so as to improve the uniformity of polythiophene solid tantalum capacitor performance.
The present invention is achieved by following technical solution.
A kind of vacuum control unit for improving polythiophene solid tantalum capacitor consistency of performance, it is characterised in that the vacuum Control device is made up of vacuum cavity system, vacuum pump system and numerical control system;
The vacuum cavity system, by tantalum core 1, container 4 and the machinery set in the vacuum (-tight) housing 2 and vacuum (-tight) housing of pressure-resistant seal Hand 3 forms;PEDOT is provided with container 4:The PSS aqueous solution;Manipulator 3 moves freely in vacuum cavity, and it is cloudy to undertake tantalum core 1 The technological operation that pole is drawn;
The vacuum pump system, it is made up of connecting conduit 7, three-way valve 8, vavuum pump 9 and pressure gauge 10;Vacuum chamber system System is connected by connecting conduit 7, three-way valve 8 with vavuum pump 9, and pressure gauge 10 is provided with vavuum pump 9;
The numerical control system, it is made up of digital control circuit 5 and electrical connecting wire 6;Digital control circuit 5 passes through electricity Connecting wire 6 is connected with the manipulator 3 in vacuum cavity system, with the technological operation of control machinery hand 3;
The operating method of the control device is as follows:
(1) tantalum core 1 is suspended on manipulator 3, by PEDOT:The PSS aqueous solution is placed in container 4, covers vacuum (-tight) housing 2, structure Into vacuum cavity system;
(2) vavuum pump 9 is started, to the vacuum cavity system vacuum of step (1);
(3) when the vacuum of vacuum cavity system in step (2) reaches 1~100Pa, digital control circuit 5 is started, will Manipulator 3 is slowly put down, and tantalum core 1 is completely immersed in the PEDOT of container 4:In the PSS aqueous solution;
(4) after the tantalum core 1 of step (3) soaks 0.5~5min, vavuum pump 9 is closed, vacuum environment is removed, removes tantalum core 1, tantalum core 1 is dried, is cooled to room temperature;
(5) repeat the above steps (1)~(4) 8 times, obtains the tantalum core of coated PEDOT cathode materials;
(6) the tantalum core 1 in step (5) is coated into graphite, drying, is cooled to room temperature;
(7) step (6) tantalum core 1 is soaked into silver paste, drying, is cooled to room temperature, completed tantalum capacitor cathode material and prepare;
(8) encapsulate, prepare tantalum capacitor, and test the performance of tantalum capacitor.
The main control chip of digital control circuit 5 is STC12C5616 series monolithics.
1 point of the tantalum core is welded in above stalloy.
The PEDOT of the step (1):PSS aqueous solution solid solubility is 1.2%, electrical conductivity 100S/cm.
Step (3) the tantalum core 1 is in PEDOT:Soak time is 0.5~5min in the PSS aqueous solution.
Step (4) drying temperature is 120 DEG C, time 10min.
Step (6) drying temperature is 150 DEG C, time 30min.
Step (7) drying temperature is 150 DEG C, time 30min.
Vacuum automatic control device provided by the invention, make tantalum core every time in PEDOT:Soak time is short in the PSS aqueous solution, And can make polythiophene solid tantalum capacitor that there is preferable electrical property, the uniformity of properties of product is improved, is adapted to organic solid The batch production of tantalum capacitor.Vacuum automatic control system of the present invention is simple in construction, easily operated, and cost is low, may extend to aluminium, The production of the organic solid electric capacity such as niobium.
Brief description of the drawings
Fig. 1 is the vacuum control unit schematic diagram for improving polythiophene solid tantalum capacitor consistency of performance;
Fig. 2 is the comparison diagram of 10V/330 μ F polythiophenes tantalum capacitors consistency of performance under normal pressure and vacuum condition.
Reference of the present invention is as follows:
1 --- tantalum core 2 --- vacuum (-tight) housing
3 --- manipulator 4 --- containers
5 --- word control circuit 6 --- electric connection lines
7 --- connecting conduit 8 --- three-way valves
9 --- vavuum pump 10 --- pressure gauges
Embodiment
The vacuum control unit of a kind of raising polythiophene solid tantalum capacitor consistency of performance of the present invention, by vacuum cavity System, vacuum pump system and numerical control system composition;Prepared using customary preparation methods.
Referring to Fig. 1, the vacuum cavity system, by set in the vacuum (-tight) housing 2 and vacuum (-tight) housing of pressure-resistant seal tantalum core 1, hold Device 4 and manipulator 3 form;Container 4 is built with PEDOT:The PSS aqueous solution;Manipulator 3 moves freely in vacuum cavity, undertakes The technological operation that the negative electrode of tantalum core 1 is drawn.1 point of the tantalum core is welded in above stalloy, is connected on manipulator 3;It is described PEDOT:The solid solubility of the PSS aqueous solution is 1.2%, electrical conductivity 100S/cm.
The vacuum pump system, it is made up of connecting conduit 7, three-way valve 8, vavuum pump 9 and pressure gauge 10;Vacuum chamber system System is connected by connecting conduit 7, three-way valve 8 with vavuum pump 9, and pressure gauge 10 is provided with vavuum pump 9;Vavuum pump 9 is true Cavity body system provides required vacuum environment, if removing the vacuum state of vacuum cavity system, can open three-way valve 8, Realize that vacuum cavity communicates with ambient atmosphere.
The numerical control system, it is made up of digital control circuit 5 and electrical connecting wire 6;Digital control circuit 5 passes through electricity Connecting wire 6 is connected with the manipulator 3 in vacuum cavity system, with the technological operation of control machinery hand 3, by hanging tantalum core Slowly it is put into PEDOT:In the PSS aqueous solution.The main control chip of digital control circuit 5 is STC12C5616 series monolithics.
The operating method of the control device is as follows:
(1) tantalum core 1 is suspended on manipulator 3, by PEDOT:The PSS aqueous solution is placed in container 4, covers vacuum (-tight) housing 2, structure Into vacuum cavity system;
(2) vavuum pump 9 is started, to the vacuum cavity system vacuum of step 1;
(3) when the vacuum in step (1) reaches 1~100Pa, digital control circuit 5 is started, manipulator 3 is slow Put down, tantalum core 1 is completely immersed in the PEDOT of container 4:In the PSS aqueous solution;
(4) after the tantalum core 1 of step (3) soaks 0.5~5min, vavuum pump 9 is closed, vacuum environment is removed, removes tantalum core (1) tantalum core 1 time 10min, is cooled to room temperature in 120 DEG C of drying;
(5) repeat the above steps (1)~(4) 8 times, obtains the tantalum core of coated PEDOT cathode materials;
(6) the tantalum core 1 in step (5) is coated into graphite, in 150 DEG C of drying, time 30min, is cooled to room temperature;
(7) step (6) tantalum core 1 is soaked into silver paste, in 150 DEG C of drying, time 30min, is cooled to room temperature, completes tantalum electric capacity It is prepared by device cathode material;
(8) encapsulate, prepare tantalum capacitor, and test the performance of tantalum capacitor.
The specific embodiment of the invention is as follows.
Embodiment 1 (comparative example)
Embodiment 1 is carried out at ambient pressure, as follows for performance comparison, embodiment:
By tantalum core in PEDOT:Taken out after soaking 1min in the PSS aqueous solution, then bakee 10min at 120 DEG C, then cool down To room temperature.After said process is repeated 8 times, graphite is coated in tantalum wicking surface, 30min is bakeed at 150 DEG C, is soaked after being cooled to room temperature Silver paste, and 30min is bakeed at 150 DEG C, it is cooled to the performance of test tantalum capacitor after room temperature.
Embodiment 2
Embodiment 2 is carried out in the vacuum automatic control system of the present invention, and according to vacuum automatic control system in the present invention The operating procedure of system is implemented, and the wherein vacuum in operating procedure (3) is 2Pa, and the soak time in operating procedure (4) is 1min, other operating procedures are constant.
The bound value and interval value of the technological parameter (vacuum, temperature, time) of the present invention can also realize this Invention, is not illustrated one by one herein.
Embodiment 1, embodiment 2 use the tantalum core of 10V/330 μ F specifications, respectively take the tantalum that 10 specifications are 10V/330 μ F Core compares experiment, Fig. 2 10V/330 μ F polythiophenes tantalum capacitors consistency of performance comparison diagram under normal pressure and vacuum condition, examination It is as shown in Figure 2 to test result.
As shown in Figure 2, in terms of capacitance extraction, the capacitor extraction of product is than product in embodiment 1 in embodiment 2 Extraction it is big, basically reach the design specification of capacitor, and capacitance fluctuates smaller near average value, shows in vacuum Under the conditions of the polythiophene tantalum capacitor for preparing, good capacitance consistency.Equally, the condenser loss of product is small in embodiment 2, loss Fluctuation is also smaller, embodies the preferable uniformity of properties of product.
In a word, vacuum automatic control system provided by the invention, tantalum core is every time in PEDOT:When being soaked in the PSS aqueous solution Between it is short, and can make polythiophene solid tantalum capacitor that there is preferable electrical property, and properties of product uniformity is also preferable, is adapted to organic The batch production of solid tantalum capacitor.The vacuum automatic control system of the present invention is simple in construction, and easily operated, cost is low, can push away Extensively to the production of the organic solid electric capacity such as aluminium, niobium.

Claims (8)

  1. A kind of 1. vacuum control unit for improving polythiophene solid tantalum capacitor consistency of performance, it is characterised in that the vacuum control Device processed is made up of vacuum cavity system, vacuum pump system and numerical control system;
    The vacuum cavity system, by tantalum core (1), container (4) and the machine set in the vacuum (-tight) housing (2) and vacuum (-tight) housing of pressure-resistant seal Tool hand (3) forms;PEDOT is provided with container (4):The PSS aqueous solution;Manipulator (3) moves freely in vacuum cavity, undertakes The technological operation that tantalum core (1) negative electrode is drawn;
    The vacuum pump system, it is made up of connecting conduit (7), three-way valve (8), vavuum pump (9) and pressure gauge (10);Vacuum chamber System system is connected by connecting conduit (7), three-way valve (8) with vavuum pump (9), and vavuum pump is provided with pressure gauge on (9) (10);
    The numerical control system, it is made up of digital control circuit (5) and electrical connecting wire (6);Digital control circuit (5) passes through Electrical connecting wire (6) is connected with the manipulator (3) in vacuum cavity system, with the technological operation of control machinery hand (3);
    The operating method of the control device is as follows:
    (1) tantalum core (1) is suspended on manipulator (3), by PEDOT:The PSS aqueous solution is placed in container (4), covers vacuum (-tight) housing (2) vacuum cavity system, is formed;
    (2) vavuum pump (9) is started, to the vacuum cavity system vacuum of step (1);
    (3) when the vacuum of vacuum cavity system in step (2) reaches 1~100Pa, digital control circuit (5) is started, by machine Tool hand (3) is slowly put down, and tantalum core (1) is completely immersed in the PEDOT of container (4):In the PSS aqueous solution;
    (4) after the tantalum core (1) of step (3) soaks 0.5~5min, vavuum pump (9) is closed, vacuum environment is removed, removes tantalum core (1), tantalum core (1) is dried, is cooled to room temperature;
    (5) repeat the above steps (1)~(4) 8 times, obtains the tantalum core of coated PEDOT cathode materials;
    (6) the tantalum core (1) in step (5) is coated into graphite, drying, is cooled to room temperature;
    (7) step (6) tantalum core (1) is soaked into silver paste, drying, is cooled to room temperature, completed tantalum capacitor cathode material and prepare;
    (8) encapsulate, prepare tantalum capacitor, and test the performance of tantalum capacitor.
  2. 2. the vacuum control unit according to claim 1 for improving polythiophene solid tantalum capacitor consistency of performance, it is special Sign is that digital control circuit (5) main control chip is STC12C5616 series monolithics.
  3. 3. the vacuum control unit according to claim 1 for improving polythiophene solid tantalum capacitor consistency of performance, it is special Sign is that tantalum core (1) point is welded in above stalloy.
  4. 4. the vacuum control unit according to claim 1 for improving polythiophene solid tantalum capacitor consistency of performance, it is special Sign is, the PEDOT of the step (1):PSS aqueous solution solid solubility is 1.2%, electrical conductivity 100S/cm.
  5. 5. the vacuum control unit according to claim 1 for improving polythiophene solid tantalum capacitor consistency of performance, it is special Sign is that step (3) the tantalum core (1) is in PEDOT:Soak time is 0.5~5min in the PSS aqueous solution.
  6. 6. the vacuum control unit according to claim 1 for improving polythiophene solid tantalum capacitor consistency of performance, it is special Sign is that step (4) drying temperature is 120 DEG C, time 10min.
  7. 7. the vacuum control unit according to claim 1 for improving polythiophene solid tantalum capacitor consistency of performance, it is special Sign is that step (6) drying temperature is 150 DEG C, time 30min.
  8. 8. the vacuum control unit according to claim 1 for improving polythiophene solid tantalum capacitor consistency of performance, it is special Sign is that step (7) drying temperature is 150 DEG C, time 30min.
CN201510859851.6A 2015-11-30 2015-11-30 Improve the vacuum control unit of polythiophene solid tantalum capacitor consistency of performance Expired - Fee Related CN105428095B (en)

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CN105788890B (en) * 2016-05-10 2019-05-31 湖南艾华集团股份有限公司 A kind of impregnation method of capacitor element

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5551979A (en) * 1993-07-02 1996-09-03 Electro Scientific Industries, Inc. Apparatus for applying termination paste to electronic components
CN101404214A (en) * 2008-11-18 2009-04-08 北京七一八友益电子有限责任公司 Polymer solid sheet type tantalum electrolyte capacitor and its manufacturing method
CN102270535A (en) * 2011-05-13 2011-12-07 株洲宏达电子有限公司 Method for manufacturing polymer ethylenedioxythiophene (PEDT) cathode plate type tantalum electrolytic capacitor by two-step method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5551979A (en) * 1993-07-02 1996-09-03 Electro Scientific Industries, Inc. Apparatus for applying termination paste to electronic components
CN101404214A (en) * 2008-11-18 2009-04-08 北京七一八友益电子有限责任公司 Polymer solid sheet type tantalum electrolyte capacitor and its manufacturing method
CN102270535A (en) * 2011-05-13 2011-12-07 株洲宏达电子有限公司 Method for manufacturing polymer ethylenedioxythiophene (PEDT) cathode plate type tantalum electrolytic capacitor by two-step method

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