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CN102820135A - Method for reducing change rate of high-temperature capacitance of niobium capacitor - Google Patents

Method for reducing change rate of high-temperature capacitance of niobium capacitor Download PDF

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Publication number
CN102820135A
CN102820135A CN2012103034388A CN201210303438A CN102820135A CN 102820135 A CN102820135 A CN 102820135A CN 2012103034388 A CN2012103034388 A CN 2012103034388A CN 201210303438 A CN201210303438 A CN 201210303438A CN 102820135 A CN102820135 A CN 102820135A
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graphite
anode block
catholyte
anode
liquid
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CN2012103034388A
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王安玖
江平
赵泽英
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China Zhenhua Group Xinyun Electronic Components Co Ltd
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China Zhenhua Group Xinyun Electronic Components Co Ltd
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Abstract

The invention provides a method for reducing a change rate of a high-temperature capacitance of a niobium capacitor and relates to a technology for preparing an auxiliary cathode layer of an electrolytic capacitor. According to the method, an anode block of a catholyte is obtained after the processing for a manganese dioxide layer of the catholyte is finished by processing an anode core block of a niobium oxide capacitor according to the traditional technology, the anode block is subjected to carbon layer preparation and a conductive leading layer is prepared, and then the subsequent processes of the capacitor are finished according to the present technology. According to the method provided by the invention, twice graphite aqueous solution dipping is adopted for preparing the carbon layer, surface activating agent dipping is performed for one time between the graphite aqueous solution dipping at two times, the anode block of the catholyte subjected to the carbon layer preparation is subjected to conductive slurry treatment, and the combination among the carbon layer, the catholyte and the conductive leading layer is more compact, so that the increasing of the capacitance of the niobium capacitor at a temperature rise moment is effectively restrained.

Description

A kind of process that reduces niobium capacitor high temperature rate of change of capacitance
Technical field
The present invention relates to a kind of electrolytic capacitor auxiliary cathode layer technology of preparing, relate in particular to a kind of auxiliary cathode layer preparation technology method that can reduce niobium electrolytic capacitor high temperature rate of change of capacitance.
Background technology:Along with the develop rapidly of modern electronic technology, all kinds of multimedia messages processors are to miniaturization, and high speed processingization develops with the low-power consumption direction, causes the demand sustainable growth to the electronic devices and components of miniaturization, Highgrade integration, high frequency of utilization; Semi-conductor electricity road direction high speed, low-voltage direction develop, and clock frequency improves day by day, in order to suppress High-frequency Interference and voltage fluctuation, need big capacity electrolytic capacitor to accomplish.The material that is used to make electrolytic capacitor at present mainly is tantalum, niobium, three kinds of valve metals of aluminium, and wherein the niobium resource reserve is abundant more than tantalum, and the dielectric constant of niobium oxide is maximum (being 41).Because the monoxide of niobium has not characteristics such as combustion characteristics, metallic character, ceramic powders characteristic, and, substitute tantalum as the optimal material of producing electrolytic capacitor with columbium monoxide along with the minimizing of tantalum resource.
The technological process of solid electrolyte niobium capacitor is to begin from the anode block moulding, and process is burnt till, deielectric-coating prepares, negative electrode is packaged into finished product after preparing, and is identical with the technological process of solid electrolyte Ta capacitor.Behind existing processes finished product, the capacitance of the capacitance of capacitor under high temperature (85 ℃ and 125 ℃) state during with normal temperature compared, and its rate of change is big (generally all more than 16%) very, exceeds demand of technical standard and defective; And when line applications, when the environment temperature rise changes greatly,, just cause the distortion of circuit output waveform, signal to noise ratio to reduce because electric capacitance change is big, finally cause whole set equipment to be shut down.
Summary of the invention:To the above-mentioned defective that exists in the prior art; The present invention aims to provide a kind of process that can reduce niobium capacitor high temperature rate of change of capacitance, utilizes the niobium oxide capacitor of this method manufacturing can be controlled at respectively in 10% and 12% at the rate of change of capacitance under 85 ℃ and 125 ℃.
For realizing above-mentioned purpose, a kind of process that reduces niobium capacitor high temperature rate of change of capacitance of the present invention comprises that preceding operation is that anode lead wire is pressed into niobium oxide capacitor anode pellet with the tantalum wire with columbium monoxide; And sinter porous anode body at high-temperature vacuum, and anode bodies is carried out anode form in the phosphoric acid,diluted aqueous solution, dielectric layer formed; Be deielectric-coating, and accomplish the processing of manganese dioxide cathodes layer, promptly accomplish catholyte by existing technology---manganese dioxide layer processing; Obtain the anode block of catholyte; It is characterized in that the catholyte anode block that makes is called for short anode block after carbon-coating preparation and preparation conduction are drawn layer, accomplish the encapsulation of capacitor again by existing technology, the carbon-coating preparation is meant preparing the catholyte anode block through the first step; Impregnated graphite A liquid takes out oven dry; Second step, the dipping surfactant; In the 3rd step, impregnated graphite B liquid takes out oven dry, and indication graphite A liquid is meant the mixed liquor of graphite and water, and indication graphite B liquid is meant graphite and phenmethylol mixed liquor, and the indication surfactant comprises phenmethylol;
It is that the anode block through the carbon-coating preparation is immersed in the electrocondution slurry that the preparation conduction is drawn layer, takes out after room temperature is placed a period of time, heating, drying again.
The process conditions that carbon-coating preparation and preparation conduction are drawn layer are:
The carbon-coating preparation:
The first step: the mixed liquor that will prepare catholyte anode block immersion graphite and water is in the graphite A liquid; Dip time 1S~10S; Put into drying box baking 10min~60min of 140 ℃~200 ℃ after the taking-up; Wherein the weight proportion of graphite A liquid is: in 2~10 parts of water, add 1 part of graphite, stirring gets final product;
Second step: anode block is soaked 1S~10S at surfactant, and surfactant comprises phenmethylol;
The 3rd step: will prepare the catholyte anode block and immerse graphite phenmethylol mixed liquor; Be in the graphite B liquid; Dip time 1S~10S; Put into drying box baking 10min~60min of 140 ℃~200 ℃ after the taking-up, wherein the weight proportion of graphite B liquid is: in 1~5 part of phenmethylol, add 1 part of graphite, stirring gets final product;
The preparation conduction is drawn layer:
(1) particle diameter is joined smaller or equal to the gold of 50 μ m or silver or copper powder to be configured to mass concentration in the phenmethylol be 10%~20% electrocondution slurry, the back that stirs is for use;
(2) anode block is immersed in the electrocondution slurry, infiltrating time is 1S~10S;
(3) anode block is at room temperature placed 5min~10min after taking out;
(4) drying oven of anode block being put into 160 ℃~230 ℃ band extractor fan dries by the fire 10min~60min.
The optimization process conditions that carbon-coating preparation and preparation conduction are drawn layer are:
The carbon-coating preparation:
The first step: the anode block immersion graphite water liquid that will prepare catholyte is in the graphite A liquid; Dip time 10S; Put into 140 ℃ drying box baking 50min after the taking-up, wherein the weight proportion of graphite A liquid is: in 7 parts of water, add 1 part of graphite, stirring gets final product;
Second step: anode block is soaked 1S~10S at surfactant, and surfactant comprises a kind of in carboxylic acid ammonia, carboxylic acid betaine, phenmethylol, ethylene propylene three polyol fatty acid ammoniums, the butyl acetate;
The 3rd step: the anode block that will prepare catholyte immerses the mixed liquor of graphite phenmethylol; Be in the graphite B liquid, dip time 10S puts into 180 ℃ drying box baking 20min after the taking-up; Wherein the weight proportion of graphite B liquid is: in 3 parts of phenmethylols, add 1 part of graphite, stirring gets final product;
The preparation conduction is drawn layer:
(1) particle diameter is joined smaller or equal to the gold of 50 μ m or silver or copper powder to be configured to mass concentration in the phenmethylol be 15% electrocondution slurry, the back that stirs is for use;
(2) anode block is immersed in the electrocondution slurry, infiltrating time is 10S;
(3) anode block is at room temperature placed 7min after taking out;
(4) drying oven of anode block being put into 230 ℃ band extractor fan dries by the fire 15min.
Through the anode block after the present invention's processing, accomplish to be contained in the metal shell or to carry out resin molding press seal dress on the lead frame forming product again by existing technology, and test its performance.
Compare with existing technology; Because the technology of flooding two schungite water liquid and between twice dipping, flooding one-time surface activating agent liquid has been adopted in the preparation of carbon-coating of the present invention; What make that carbon-coating and catholyte layer, conduction draw interlayer combines closelyr, has effectively suppressed the capacitance increase of niobium oxide capacitor when temperature raises.
Embodiment
Example below in conjunction with concrete is further described the inventive method:
Embodiment:
Chip-type solid electrolyte oxidation niobium capacitor by existing technology input 4V330 μ F, two specifications of 4V470 μ F is produced, and accomplishes to prepare carbon-coating and silver slurry layer by following processing step after manganese dioxide cathode is separated the preparation of matter layer.
(1) A, two kinds of graphite liquid of B and the preparation of silver slurry:
The configuration of graphite A liquid: in 7 parts of weight water, add 1 part of scheelite China ink, the back that stirs is for use.
The configuration of graphite B liquid: in 3 parts of weight benzyl alcohols, add 1 part of scheelite China ink, the back that stirs is for use.
Silver slurry: the silver powder 100g that takes by weighing average grain diameter and be 40 μ m joins 650ml phenmethylol (density of phenmethylol is 1.0419g/ml), and the back that stirs is for use.
(2) anode block soaks 10S in graphite A liquid, and the drying box baking 50min that puts into 140 ℃ after the taking-up takes out.
(3) being flooded 10S in phenmethylol after, takes out anode block.
(4) after anode block soaks 10S in graphite B liquid, take out the drying box baking 20min that puts into 180 ℃ and take out.
(5) anode block soaks 10S at electrocondution slurry, takes out to put 7min at room temperature.
(6) anode block is put into 230 ℃ baking oven and dry by the fire 15min.
To prepare silver by existing technology and draw the anode block of layer and encapsulate with epoxy resin, and accomplish ageing screening and test, in the capacitance of 85 ℃, 125 ℃ measurement products, test and result of calculation are seen table 1, table 2 respectively.
Figure 850964DEST_PATH_IMAGE001
Comparative example:
Accomplish all production stages of chip-type solid electrolyte oxidation niobium capacitor (the design and implementation example of two products is identical) of 4V330 μ F, two specifications of 4V470 μ F by existing technology; In the capacitance of 85 ℃, 125 ℃ measurement products, test and result of calculation are seen table 3, table 4 respectively.
The 4V330 μ F test data of the existing explained hereafter of table 3
Figure 2012103034388100002DEST_PATH_IMAGE002
Data through table 1, table 2, table 3, table 4 compare, and can find out, adopt the rate of change of capacitance of niobium capacitor when high temperature of explained hereafter of the present invention to have substantial degradation, basic technical merit near tantalum capacitor.
  

Claims (3)

1. a process that reduces niobium capacitor high temperature rate of change of capacitance comprises that preceding operation is that anode lead wire is pressed into niobium oxide capacitor anode pellet with the tantalum wire with columbium monoxide, and sinters porous anode body at high-temperature vacuum; And anode bodies is carried out anode form in the phosphoric acid,diluted aqueous solution, form dielectric layer, i.e. deielectric-coating; And accomplish the manganese dioxide cathodes layer by existing technology and process; Promptly accomplish catholyte---manganese dioxide layer processing, obtain the anode block of catholyte, it is characterized in that the catholyte anode block that makes is called for short anode block after carbon-coating preparation and preparation conduction are drawn layer; Accomplish the encapsulation of capacitor again by existing technology; The carbon-coating preparation is meant that impregnated graphite A liquid takes out oven dry with preparing the catholyte anode block through the first step; Second step, the dipping surfactant; In the 3rd step, impregnated graphite B liquid takes out oven dry, and indication graphite A liquid is meant the mixed liquor of graphite and water, and indication graphite B liquid is meant graphite and phenmethylol mixed liquor, and the indication surfactant comprises phenmethylol;
It is that the anode block through the carbon-coating preparation is immersed in the electrocondution slurry that the preparation conduction is drawn layer, takes out after room temperature is placed a period of time, heating, drying again.
2. a kind of process that reduces niobium capacitor high temperature rate of change of capacitance according to claim 1 is characterized in that carbon-coating preparation and preparation conduction draw the process conditions of layer and be:
The carbon-coating preparation:
The first step: the mixed liquor that will prepare catholyte anode block immersion graphite and water is in the graphite A liquid; Dip time 1S~10S; Put into drying box baking 10min~60min of 140 ℃~200 ℃ after the taking-up; Wherein the weight proportion of graphite A liquid is: in 2~10 parts of water, add 1 part of graphite, stirring gets final product;
Second step: anode block is soaked 1S~10S at surfactant, and surfactant comprises phenmethylol;
The 3rd step: will prepare the catholyte anode block and immerse graphite phenmethylol mixed liquor; Be in the graphite B liquid; Dip time 1S~10S; Put into drying box baking 10min~60min of 140 ℃~200 ℃ after the taking-up, wherein the weight proportion of graphite B liquid is: in 1~5 part of phenmethylol, add 1 part of graphite, stirring gets final product;
The preparation conduction is drawn layer:
(1) particle diameter is joined smaller or equal to the gold of 50 μ m or silver or copper powder to be configured to mass concentration in the phenmethylol be 10%~20% electrocondution slurry, the back that stirs is for use;
(2) anode block is immersed in the electrocondution slurry, infiltrating time is 1S~10S;
(3) anode block is at room temperature placed 5min~10min after taking out;
(4) drying oven of anode block being put into 160 ℃~230 ℃ band extractor fan dries by the fire 10min~60min.
3. a kind of process that reduces niobium capacitor high temperature rate of change of capacitance according to claim 1 and 2 is characterized in that carbon-coating preparation and preparation conduction draw the process conditions of layer and be: the carbon-coating preparation:
The first step: will prepare the anode block immersion graphite of catholyte and the mixed liquor of water is in the graphite A liquid; Dip time 10S; Put into 140 ℃ drying box baking 50min after the taking-up, wherein the weight proportion of graphite A liquid is: in 7 parts of water, add 1 part of graphite, stirring gets final product;
Second step: anode block is soaked 1S~10S at surfactant, and surfactant comprises a kind of in carboxylic acid ammonia, carboxylic acid betaine, phenmethylol, ethylene propylene three polyol fatty acid ammoniums, the butyl acetate;
The 3rd step: the anode block that will prepare catholyte immerses the mixed liquor of graphite phenmethylol; Be during graphite B dissolves, dip time 10S puts into 180 ℃ drying box baking 20min after the taking-up; Wherein the weight proportion of graphite B liquid is: in 3 parts of phenmethylols, add 1 part of graphite, stirring gets final product;
The preparation conduction is drawn layer:
(1) particle diameter is joined smaller or equal to the gold of 50 μ m or silver or copper powder to be configured to mass concentration in the phenmethylol be 15% electrocondution slurry, the back that stirs is for use;
(2) anode block is immersed in the electrocondution slurry, infiltrating time is 10S;
(3) anode block is at room temperature placed 7min after taking out;
(4) drying oven of anode block being put into 230 ℃ band extractor fan dries by the fire 15min.
CN2012103034388A 2012-08-24 2012-08-24 Method for reducing change rate of high-temperature capacitance of niobium capacitor Pending CN102820135A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103065798A (en) * 2013-01-15 2013-04-24 中国振华(集团)新云电子元器件有限责任公司 Slice-typed niobium oxide capacitor graphite and silver paste layer preparation method
CN115188593A (en) * 2022-08-15 2022-10-14 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) Tantalum capacitor manganese dioxide cathode layer interface processing method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101286419A (en) * 2007-04-09 2008-10-15 松下电器产业株式会社 Solid electrolytic capacitor and manufacturing method thereof
CN102054588A (en) * 2009-10-23 2011-05-11 Avx公司 External coating for a solid electrolytic capacitor
CN102364583A (en) * 2011-09-30 2012-02-29 宁波广博纳米新材料股份有限公司 Silver paste for back face of lead-free crystal silicon solar cell and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101286419A (en) * 2007-04-09 2008-10-15 松下电器产业株式会社 Solid electrolytic capacitor and manufacturing method thereof
CN102054588A (en) * 2009-10-23 2011-05-11 Avx公司 External coating for a solid electrolytic capacitor
CN102364583A (en) * 2011-09-30 2012-02-29 宁波广博纳米新材料股份有限公司 Silver paste for back face of lead-free crystal silicon solar cell and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103065798A (en) * 2013-01-15 2013-04-24 中国振华(集团)新云电子元器件有限责任公司 Slice-typed niobium oxide capacitor graphite and silver paste layer preparation method
CN115188593A (en) * 2022-08-15 2022-10-14 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) Tantalum capacitor manganese dioxide cathode layer interface processing method
CN115188593B (en) * 2022-08-15 2023-06-02 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) Interface treatment method for manganese dioxide cathode layer of tantalum capacitor

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Application publication date: 20121212