CN104143443A - Capacitor - Google Patents
Capacitor Download PDFInfo
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- CN104143443A CN104143443A CN201310474929.3A CN201310474929A CN104143443A CN 104143443 A CN104143443 A CN 104143443A CN 201310474929 A CN201310474929 A CN 201310474929A CN 104143443 A CN104143443 A CN 104143443A
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- capacitor
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- sintered body
- powder
- niobium
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Abstract
The invention provides a capacitor. The capacitor comprises a compound crystal shown in the formula I and is provided with an X-ray powder diffraction diagram with 2 theta located at the positions about 5.87, 8.10, 9.72, 10.20, 11.35, 12.78, 14.39, 16.84, 17.57, 18.44, 19.22, 21.39, 22.82, 23.73, 24.78, 25.23, 26.65, 27.43, 28.82, 29.12, 30.42, 31.21, 32.95, 33.89, 36.08, 38.72 and 39.86.
Description
Technical field
The present invention relates to a kind of capacitor, there is the low and little excellent specific property of the initial disqualification rate of leakage current of equivalent series resistance.
Background technology
Along with the high frequency of electronic equipment, in the capacitor as one of electronic unit, require the large value capacitor in the impedance operator excellence of high frequency region.Recently, in order to reduce the impedance of this high frequency region, start electrolytic capacitor to using the high electroconductive polymer of conductivity and study and carry out goods.Electrolytic capacitor possesses: anode foils, the dielectric overlay film forming on the surface of anode foils and the electroconductive polymer layer forming on dielectric overlay film.The surface process of anode foils is roughened, and is formed with multiple holes.As the method that forms electroconductive polymer layer, except chemical polymerization and electrolysis polymerization, also comprise and make preformed electroconductive polymer particle be impregnated in the dispersion method of capacitor element.With regard to chemical polymerization, sometimes because the existence of oxidant damages dielectric overlay film.In addition, for chemical polymerization and electrolysis polymerization, be difficult to be formed uniformly electroconductive polymer layer.So, can form electroconductive polymer layer compared with heavy back, use a large amount of electroconductive polymers.Little molecular organic compound, it is simple that particularly little molecular organic compound crystal has preparation compared with polymer, and coating is even, rate of finished products is high, and feature easily and effectively, therefore still needs application organic micromolecule compound, particularly organic micromolecule compound crystal current electrolysis condenser.
Require to have small size and high capacitance for electronic instrument as the capacitor of portable phone and PC.In these capacitors, tantalum capacitor is preferred, because with respect to its size, capacitance is large and performance good.In addition, in recent years, require electronic device to operate under low-voltage and high-frequency, and there is low noise, and for solid electrolyte capacitators, also require lower equivalent parallel resistance (ESR).In this tantalum capacitor, the sintered body of tantalum powder is generally used as anode part.By this powder forming, then sintering, thus make described powder integration and make the electrode that is called as sintered body.This sintered body inside is formed the structure of 3 D complex by electricity and the powder particle of mechanical link each other, comprise the surface on internal void surface at this sintered body, forms dielectric film layer, floods the material of conduct to electrode, thereby prepares a kind of capacitor.As long as dielectric film layer is evenly attached to inner surface or the outer surface of described sintered body, the capacitance of the capacitor of manufacturing just depends primarily on the contact condition to electrode material and dielectric film layer on microcosmic.In order to improve the capacitance of tantalum capacitor, must improve the quality of sintered body or use the sintered body that has increased surface area by broken tantalum powder.
Summary of the invention
The general manufacture method of electrolytic capacitor comprises following steps: the step of the multiple holes that prepare to have surperficial anode foils, form on the surface of anode foils and the dielectric overlay film forming on the surface of anode foils; The first dispersion solution that anode foils is impregnated in contain the first electroconductive polymer particle and the first solvent, forms the step of the first electroconductive polymer layer on the surface of dielectric overlay film; And, the second dispersion solution that anode foils is impregnated in contain the second electroconductive polymer particle and the second solvent, form the step of the second electroconductive polymer layer that covers the first electroconductive polymer layer, wherein, compared with described the first dispersion solution, the pH of described the second dispersion solution and 7 differs farther.
The object of this invention is to provide the capacitor that a kind of unit mass capacitance is large, leakage current is little and moisture-proof is high; A kind of sintered body that can be used as the electrode material of this capacitor and can obtain the apparent ratio of high-capacitance; A kind of material as this sintered body is preferred, in shaping operation, show good fluidity, promote progressive forming and niobium powder that can steady production capacitor; Manufacture method with described capacitor, described sintered body and described niobium powder.
The invention provides a kind of capacitor, a kind of capacitor, it comprises that an electrode, one are to electrode and dielectric material, described electrode is for comprising that volume is 10mm
3niobium sintered body, described dielectric material comprises niobium oxide, described is organic semiconductor to electrode, it comprises the organic compound of following structure:
I，
It has the X-ray powder diffraction figure of 2 θ at approximately 5.87,8.10,9.72,10.20,11.35,12.78,14.39,16.84,17.57,18.44,19.22,21.39,22.82,23.73,24.78,25.23,26.65,27.43,28.82,29.12,30.42,31.21,32.95,33.89,36.08,38.72,39.86 places.
Brief description of the drawings
Fig. 1 is the X ray diffracting spectrum of formula I compound.
Embodiment
Below by embodiment, the invention will be further described.It should be understood that described in the embodiment of the present invention that preparation method is only used for illustrating the present invention, instead of limitation of the present invention, right under design prerequisite of the present invention
Preparation method's of the present invention simple modifications all belongs to the scope of protection of present invention.All raw materials of using in embodiment and solvent are all purchased from Sigma Biochemical and Organic Compounds for Research and Diagnostic Clinical Reagents company.
In powder X-ray x ray diffraction (XRD), use Cu K α 1 as X ray tube, at room temperature use powder x-ray diffraction device RINT2200/Ultima+ (RIGAKU) or X'Pert Pro MPD (PANalytical) to measure within the scope of the 2 θ angles of diffraction of 2 ° to 35 °.For used each diffraction instrument, measuring condition is as follows.
Diffraction instrument: RINT2200/Ultima+ (RIGAKU)
Tube current: 40mA, tube voltage: 40kV, sweep speed: 4 °/minute
Diffraction instrument: X'Pert Pro MPD (PANalytical)
Tube current: 40 mA, tube voltage: 45kV, sweep speed: 40.1 °/minute
Although 2 θ values generally illustrate 0.2 ° of about scholar's error, may cause larger error due to measuring condition etc.
Use thermogravimetric/differential thermal analyzer TG/SDTA851e (TG/DTA) (Mettler Toledo) or differential scanning calorimeter DSC821e (DSC), in the dry nitrogen air-flow of 40ml/ minute and under the intensification degree speed of 10 DEG C/min, carry out heat analysis.
Embodiment 1:
Be the sodium of 10 times of fluoro potassium niobates to packing 5,000 grams in nickel crucible at 80 DEG C of abundant vacuum drying fluoro potassium niobates and mole, and make it under argon atmospher, carry out the reduction reaction of 20 hours at 1,000 DEG C.After reacting completely, reduzate is cooling, wash with water successively, with 95% sulfuric acid scrubbing, then wash with water, vacuumize is also used the oxidation aluminium pot ball mill that contains silica alumina ball to pulverize 40 hours.Crushed products is flooded and stirred in the 3:2 (by mass) of 50% nitric acid and 10% aqueous hydrogen peroxide solution mixed solution.Then, crushed products water is fully washed, until pH value reaches 7, to remove impurity, then vacuumize.The particle mean size of raw material niobium powder is 1.2 microns.
In niobium tank, place 500 grams of this raw material niobium powder and add wherein 50 grams of polybutyl methacrylates and 1 liter of toluene.In addition, add zirconia ball and use shaking mixer by contents mixed 1 hour.Removing after zirconia ball, this mixture is being placed in circular cone drier and 1 × 10
2vacuumize under the condition of Pa and 80 DEG C.
Subsequently, by this niobium powder at 250-400 DEG C 1 × 10
-2pa heating 12 hours, to decompose and to remove polybutyl methacrylate, then 4 × 10
-3under the decompression of Pa 1,150 DEG C of sintering 2 hours.Until being reduced to 30 DEG C or lower, product temperature then uses roll pelletizer fragmentation by cooling niobium powder sintering agglomerate, to obtain particle mean size as the broken powder of the niobium of 100 microns.
The broken powder of this niobium, by passing into nitrogen through the nitrogen treatment at 300 DEG C, 2 hours adding to depress, obtains the niobium powder of approximately 450 grams.Nitrogen content is 0.22%.
Pack the niobium powder (approximately 0.1 gram) so obtaining into tantalum device automatic forming machine (TAP-2R, manufactured by Seiken) hopper in, and with automatic forming together with the niobium silk of 0.3mm φ, carry out the molded article that manufacturing dimension is about 0.3cm × 0.18cm × 0.45cm.This molded article is 4 × 10
-3in the vacuum of Pa, leave standstill 30 minutes at 1,250 DEG C, to obtain sintered body.Prepare this sintered body of 100, and each uses 0.1% phosphate aqueous solution electrochemical shaping 200 minutes under 20V voltage, to form from the teeth outwards oxide dielectric film.
Subsequently, repeat this sintered body to be immersed in and in 60% manganese nitrate aqueous solution, then to make it in 220 DEG C of heating operation of 30 minutes, to form manganese dioxide layer as to electrode layer on oxide dielectric film.This to electrode layer on, stack gradually carbon-coating and silver stick with paste layer.After lead frame being installed thereon, this device is shaped with epoxy resin as a whole, to manufacture chip capacitor.Average electrical capacity and the average leakage current (hereinafter referred is " LC ") of the apparent ratio of capacitance of this capacitor and chip capacitor (n=100) represent in table 1.LC value is the 1 minute value at room temperature measuring of voltage by applying 6.3V.
Embodiment 2: the preparation of formula I compound crystal
In the reaction bulb of being furnished with mechanical agitation and reflux condensing tube, add 0.4mol 4-toluene bromide and 14.4g benzoyl peroxide, after being heated under stirring reflux, by bromo-0.4mol 2-2,5-pyrroledione (NBS) added reaction bulb in 20 minutes in batches, add hot reflux 2 hours, reaction yield 65% (GC).Reactant liquor adds sodium carbonate neutralization, concentrated, refluxes and dissolves with industry anhydrous ethanol (1g: 1mL), is cooled to-15 DEG C and carries out recrystallization, purity approximately 90% (GC).Repeatedly its purity > 99% after recrystallization.
Under nitrogen protection, add 0.05mol triphenylamine in the reaction bulb of being furnished with mechanical agitation and reflux condensing tube, 100mL DMF, is cooled to 5 DEG C in ice bath, stirs the lower phosphorus oxychloride 0.1mol that slowly drips, and after being added dropwise to complete, removes ice bath, after 1 hour, rises to room temperature.Add hot reflux 12 hours.Reactant liquor adds 100mL water, then divides and extract for 4 times with 400mL ethyl acetate, and organic phase merges, and is washed to neutrality, and anhydrous magnesium sulfate drying, removes after ethyl acetate, and silica gel chromatography, obtains white solid, isolated yield 62%.
Under nitrogen protection, add the bromo-benzyl bromide a-bromotoluene of 0.03mol 4-in the reaction bulb of being furnished with mechanical agitation and reflux condensing tube, 0.09mol triethyl phosphite, is heated under stirring reflux, and reacts 1 hour.After reaction stops, decompression distillation goes out excessive triethyl phosphite.After having distilled, be cooled to room temperature, by cooling reaction temperature to 5 DEG C in ice bath.Keeping reaction temperature is 5 DEG C, adds 0.03mol potassium tert-butoxide in 20 minutes in batches, reacts after 1 hour, drips the THF solution 35mL that contains 0.03mol 4-diphenylamines benzaldehyde, reacts 2 hours.Reactant liquor adds 100mL water and 100mL carrene, separatory, and water is used 100mL dichloromethane extraction again, and merging organic phase water and a small amount of watery hydrochloric acid are washed till after neutrality, and anhydrous magnesium sulfate drying, removes carrene, silicagel column look
Spectrum purifying, obtains yellow solid, isolated yield 45%.
Under nitrogen protection; in the reaction bulb of being furnished with mechanical agitation, reflux condensing tube, add 0.01mol 1-(4-triphenylamine base)-2-(4-bromophenyl) ethene; 0.012mol 2-(tributyl tinbase) oxazole; 3%mol tetra-(triphenylphosphinyl) palladium; 50mL toluene; stir, be heated to reflux, react 48 hours.Reactant liquor is dry under vacuum, adds 100mL carrene to dissolve, and divides three washings with 6M hydrochloric acid 60mL, water is used 10% ammonia neutralization under the state of cooling, use again 100mL dichloromethane extraction, merge organic phase, add 50mL water extremely neutral with 10% ammonia scrubbing.Collect organic phase, dry, cross silica gel column chromatography and purify, obtain yellow solid, isolated yield 43%.
Nuclear-magnetism: δ (ppm), 8.744-8.753 (d, 1H, J=4.5Hz), 7.889 (s, 1H), 7.830-7.845 (d, 1H, J=7.5Hz), 7.764 (s, 1H), 7.674-7.691 (d, 1H, J=8.5Hz), 7.519-7.535 (d, 1H, J=8.0Hz), 7.396-7.439 (m, 2H), 7.341 (s, 1H), 7.248-7.280 (m, 4H), 7.174-7.207 (d, 1H, J=16.5Hz), 7.112-7.127 (d, 4H, J=7.5Hz), 7.019-7.069 (m, 4H)
The organic compound of above-mentioned preparation is placed in quartz ampoule (quartz ampoule).At 100 DEG C of temperature, by this compound vacuum dehydration of preparing.This pipe is thrown off, and be placed in crystal growing furnace.Having in the dual stove of barrier film (double furnace) by Bridgman (Bridgman) method grown crystal.Finally, obtain without color strip-shaped crystal.The capacity of the capacitor of the present invention of use formula I compound crystal is 698 μ F, and LC is 20 μ A.
Claims (3)
1. a capacitor, it comprises that an electrode, one are to electrode and dielectric material, described electrode is for comprising that volume is 10mm
3niobium sintered body, described dielectric material comprises niobium oxide, described is organic semiconductor to electrode, it comprises the organic compound of following structure:
I，
It has the X-ray powder diffraction figure of 2 θ at approximately 5.87,8.10,9.72,10.20,11.35,12.78,14.39,16.84,17.57,18.44,19.22,21.39,22.82,23.73,24.78,25.23,26.65,27.43,28.82,29.12,30.42,31.21,32.95,33.89,36.08,38.72,39.86 places.
2. capacitor as described in claim 1, is characterized in that, described electrode is contained to organic sulfonic acid root anion as dopant.
3. a compound crystal, it has suc as formula the structure shown in I:
I，
And there is the X-ray powder diffraction figure of 2 θ at approximately 5.87,8.10,9.72,10.20,11.35,12.78,14.39,16.84,17.57,18.44,19.22,21.39,22.82,23.73,24.78,25.23,26.65,27.43,28.82,29.12,30.42,31.21,32.95,33.89,36.08,38.72,39.86 places.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310474929.3A CN104143443A (en) | 2013-10-12 | 2013-10-12 | Capacitor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310474929.3A CN104143443A (en) | 2013-10-12 | 2013-10-12 | Capacitor |
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3257203A (en) * | 1958-08-20 | 1966-06-21 | Azoplate Corp | Electrophotographic reproduction material |
| JPS5640834A (en) * | 1979-09-12 | 1981-04-17 | Hitachi Ltd | Composite type electrophotographic plate and electrophotographic method |
| JPS63155053A (en) * | 1986-12-18 | 1988-06-28 | Alps Electric Co Ltd | Organic photoconductive material for electrophotography |
| JPH0254272A (en) * | 1988-08-19 | 1990-02-23 | Canon Inc | Electrophotographic sensitive body |
| CN2291695Y (en) * | 1996-04-04 | 1998-09-16 | 张志林 | Long-life organic thin-film electroluminescent screen |
| CN1837168A (en) * | 2006-04-25 | 2006-09-27 | 扬州大学 | Process for synthesizing1,3,5-triphenyl benzene |
| CN101044125A (en) * | 2004-08-25 | 2007-09-26 | 塔尔基公司 | Heterocyclic compounds and methods of use |
| CN101103470A (en) * | 2004-12-23 | 2008-01-09 | 不伦瑞克工业大学 | Material for doped and undoped hole and electron transport layer |
| CN101116148A (en) * | 2004-12-30 | 2008-01-30 | E.I.内穆尔杜邦公司 | Electrically conductive polymers |
| CN101114700A (en) * | 2007-08-30 | 2008-01-30 | 电子科技大学 | Organic electroluminescent device capable of emitting white light and method for fabricating the same |
-
2013
- 2013-10-12 CN CN201310474929.3A patent/CN104143443A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3257203A (en) * | 1958-08-20 | 1966-06-21 | Azoplate Corp | Electrophotographic reproduction material |
| JPS5640834A (en) * | 1979-09-12 | 1981-04-17 | Hitachi Ltd | Composite type electrophotographic plate and electrophotographic method |
| JPS63155053A (en) * | 1986-12-18 | 1988-06-28 | Alps Electric Co Ltd | Organic photoconductive material for electrophotography |
| JPH0254272A (en) * | 1988-08-19 | 1990-02-23 | Canon Inc | Electrophotographic sensitive body |
| CN2291695Y (en) * | 1996-04-04 | 1998-09-16 | 张志林 | Long-life organic thin-film electroluminescent screen |
| CN101044125A (en) * | 2004-08-25 | 2007-09-26 | 塔尔基公司 | Heterocyclic compounds and methods of use |
| CN101103470A (en) * | 2004-12-23 | 2008-01-09 | 不伦瑞克工业大学 | Material for doped and undoped hole and electron transport layer |
| CN101116148A (en) * | 2004-12-30 | 2008-01-30 | E.I.内穆尔杜邦公司 | Electrically conductive polymers |
| CN1837168A (en) * | 2006-04-25 | 2006-09-27 | 扬州大学 | Process for synthesizing1,3,5-triphenyl benzene |
| CN101114700A (en) * | 2007-08-30 | 2008-01-30 | 电子科技大学 | Organic electroluminescent device capable of emitting white light and method for fabricating the same |
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Application publication date: 20141112 |