CN104143447A - Solid electrolytic capacitor - Google Patents
Solid electrolytic capacitor Download PDFInfo
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- CN104143447A CN104143447A CN201310376487.9A CN201310376487A CN104143447A CN 104143447 A CN104143447 A CN 104143447A CN 201310376487 A CN201310376487 A CN 201310376487A CN 104143447 A CN104143447 A CN 104143447A
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- electrolytic capacitor
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Abstract
The invention provides a piece-typed solid electrolytic capacitor which contains compound crystal shown in the formula I of the piece-typed solid electrolytic capacitor, the compound crystal comprises an X-ray powder diffraction pattern generated when is roughly located at positions of 12.6, 12.7, 16.6, 18.8, 21.5 and 23.8.
Description
Technical field
The present invention relates to a kind of chip-type solid electrolytic 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.
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.
But electric capacity of the present invention comprises multiple solid electrolytic capacitor element, each element is by making to form cathode portion on the anode substrate surface except the anode part of its one end with this sequence stack with insulation oxide rete, semiconductor layer and conductive layer, the metal that anode substrate comprises valve acting or the sintered body of conductive oxide or comprise the sintered body being connected with plain conductor.
Wherein semiconductor layer is organic semiconductor layer, and it contains the organic compound crystal shown in following formula I:
I，
It has the X-ray powder diffraction figure of 2 θ at approximately 12.6,12.7,16.6,18.8,21.5 and 23.8 places.
Wherein anode part comprises the end of anode substrate; Wherein anode part comprises the plain conductor being connected with sintered body; Wherein plain conductor be selected from tantalum, niobium, aluminium, titanium, mainly comprise this metalloid alloy and these metals and the alloy of partial oxidation and/or nitrogenize; Wherein make the interface insulation between anode part and the part except anode part with insulating resin; Wherein insulation oxide rete mainly comprises and is selected from Ta
2o
5, Al
2o
3, Zr
2o
3and Nb
2o
5at least one.
Brief description of the drawings
Fig. 1 is the perspective view that represents an example of chip-type solid electrolytic capacitor of the present invention, wherein continuously lies on a terminal part of lead frame every ground parallel each three solid electrolytic capacitor element with positive wire (anode part).
Fig. 2 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 and make
Preparation Method is only used for illustrating the present invention, instead of limitation of the present invention, under design prerequisite of the present invention, preparation method's of the present invention simple modifications is all belonged 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) at 2 °
To the 2 θ angles of diffraction of 35 °, measure.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:
Fig. 1 is the perspective view of an example of chip-type solid electrolytic capacitor of the present invention.In this example, adopt three solid electrolytic capacitor element (2), each element passes through insulation oxide rete, semiconductor layer and conductive layer are manufactured to form cathode portion (3) on the surface in anode substrate (4) with this sequence stack, the metal that anode substrate comprises valve acting or conductive oxide are also connected with anode part wire, this chip-type solid electrolytic capacitor has this structure: part cathode portion is parallel to be lain on the terminal part (1a) in the terminal part of pair of opposing of lead frame (1) every ground continuously, anode part wire (4a) is lain on another terminal part (1b), by each part electrical connection or mechanical connection, outside staying by resin molded entirety but by the external cabling part of lead frame (1), lead frame outside the predetermined cutting of part (not shown) and bending resin mold.
In the manufacture of chip-type solid electrolytic capacitor of the present invention, prepare the solid electrolytic capacitor element of multiple manufactures like this; Continuously lie on a terminal part of lead frame of the terminal part with pair of opposing of separately manufacturing every ground parallel the part cathode portion of each solid electrolytic capacitor element; The anode part of anode substrate is lain on another terminal part; By the electrical connection of each part or mechanical connection, for example the former adopts conduction lotion to solidify and the latter adopts spot welding; Outside staying by resin molded entirety but by the part that forms lead frame external terminal; Then the lead frame outside the predetermined cutting of part (not shown) and bending resin mold.Particularly, for example as shown in fig. 1, continuously lie on the terminal part of pair of opposing of lead frame and molded every ground parallel three solid electrolytic capacitor element, to manufacture a kind of polygonal and the chip-type solid electrolytic capacitor of parallelepiped normally.While manufacturing this solid electrolytic capacitor, can the position that be configured for holding the lead frame after cutting on part side and/or bottom surface will be placed in jagged part, can will be with jagged part to be for example placed on end face to distinguish anode and negative electrode, or can end face and/or bottom surface be reduced with being convenient to take out the chip-type solid electrolytic capacitor of manufacturing when resin molded from metal die with certain angle.The semiconductor layer forming on insulating barrier of the present invention is organic semiconductor layer, wherein contains the organic compound crystal shown in formula I.
In an embodiment, the chip-type solid electrolytic capacitor of manufacturing is welded under the following conditions: make capacitor pass reflow ovens three times, setting this reflow ovens takes at 260 DEG C of temperature curves with peak value (keeping 40 seconds at 150 DEG C, after intensification, 230 DEG C or higher maintenance 30 seconds).After being welded, under 4V, measure LC 30 seconds.Units in each measurement is n=320, and those capacitors with 0.1CV or lower LC value are judged as and can be accepted.
(quality of tantalum and size (Wmm) are shown in Table 1 to prepare the sintered body that is of a size of 4.0 × W × 1.8mm as shown in table 1 with the tantalum powder that CV (product of capacitance and electrochemical voltage) is 50,000/g; Sintering temperature: 20 DEG C of Isosorbide-5-Nitraes, sintering time: 20 minutes, sintered density: 6.4g/cm
3, Ta lead-in wire: 0.24mm φ; Part Ta lead-in wire is imbedded in sintered body and stretched into 4mm with parallel longitudinal, the lead portion of being stretched out by sintering is used as to anode part).The sintered body that serves as anode is immersed in 0.1% phosphate aqueous solution except lead portion, and carry out electrochemistry formation 3 hours by apply the voltage of 18V between anode and the Ta plate electrode as negative electrode at 80 DEG C, to form by Ta
2o
5the insulation oxide rete forming.Then, this sintered body is immersed except lead-in wire in 20% lead acetate water solution and the solution of 35% ammonium persulfate aqueous solution with mixing in 1: 1, make it at 40 DEG C, leave standstill 1 hour, then extract, wash and be dried this sintered body, repeat this and operate 25 times to form the mixture (brown lead oxide: the semiconductor layer 96%) forming by brown lead oxide and lead sulfate on insulation oxide rete.On semiconductor layer, sequence stack carbon paste and silver paste, to be made into cathode portion, are manufactured solid electrolytic capacitor element thus.
On a pair of terminal part of the independent thick copper alloy lead frame with zinc-plated surface of 100 μ m of manufacturing, (there are 32 pairs of paired terminal parts, each wide 3.4mm; The terminal part that keeps flat cathode portion on it has the ladder corresponding to the 0.9mm of the ladder in Fig. 1, and the part that cathode portion is put has the length of 4.3mm; When coplanar projection, between two terminal parts, there is the gap of 1mm), by as above manufacture three solid electrolytic capacitor element parallel without compartment of terrain level connection joint (by the cathode side of solid electrolytic capacitor, 4.0 × W the face that is sintered body lies on the stepped terminal part of tool, and the anode-side of solid electrolytic capacitor is lain on another terminal part; Each is all by making silver paste solidify electrical connection or be mechanically connected to front one and be connected to rear one by spot welding; In a lead frame, on every pair of terminal part, connect three solid electrolytic capacitor element, altogether connect 96 solid electrolytic capacitor element).After this, a part for two terminal parts of lead frame and solid electrolytic capacitor element are all come molded with epoxy resin by transfer moudling, chip-type solid electrolytic capacitor taking manufacturing dimension as 7.3 × 4.3 × 2.8mm is (after molding, by each in outer pattern two terminal parts in the position cutting apart from pattern end face 3.4mm, the lead frame of excision is removed, will be connected with chip-type solid electrolytic capacitor and will stay the lead-in wire of outside
Each terminal part of frame bends and is used as external terminal along the periphery of capacitor; 32 chip-type solid electrolytic capacitors are manufactured from a lead frame).
Embodiment 2: the preparation of formula I compound crystal
(1) in 100 mL there-necked flasks, add successively Benzaldehyde,2-hydroxy (20.0 mmol), 24 mL acetone, 10 mL water, stirring at room temperature to solid all dissolves, dropwise drip the solution of NaOH (24 mmol)+20 mL water, reactant liquor becomes claret clear liquid from faint yellow clear liquid, react completely, rotary evaporation is removed acetone, in raffinate, add 70 mL hot water to red solid all to dissolve, pass into carbon dioxide 30 about min to reactant liquor no longer till variable color, there is faint yellow solid to produce, filter, washing, dry, use acetone/water recrystallization, obtain faint yellow solid, yield: 78.3%, fusing point: 137 ~ 139 ° of C.
(2) to adding successively in 100 mL there-necked flasks (
e)-4-(2-hydroxy phenyl)-3-butene-2-one (20.0 mmol), 4-fluorobenzaldehyde (20.1mmol), 50 mL absolute ethyl alcohols, 10 mL water, being stirred to solid all dissolves, dropwise drip the solution of NaOH (27 mmol)+15 mL water, reactant liquor becomes claret clear liquid from faint yellow clear liquid, after reaction finishes, rotary evaporation is removed acetone, in raffinate, add 70 mL hot water to red solid all to dissolve, pass into carbon dioxide 30 about min to reactant liquor no longer till variable color, there is faint yellow solid to produce, filter, washing, dry, with absolute ethyl alcohol/water recrystallization, obtain light yellow crystal, yield: 68%, fusing point: 126 ~ 129 ° of C.
(3) in 250 mL there-necked flasks, add successively (
1E, 4E)-1-(2-hydroxy phenyl)-5-(4-fluorophenyl)-1,4-pentadiene-3-ketone (23 mmol), KI (0.23 mmol), potash (26 mmol), 100 mL acetone, at room temperature stir, rear dropping benzyl chlorine (26 mmol), adds hot reflux, solution colour is become when faint yellow from redness, react completely, remove by filter while hot excessive KI, potash, filtrate revolving desolventized, obtain faint yellow flat crystal, yield: 83%, fusing point: 83 ~ 84 ° of C.
(4) in 100 mL single port bottles, add successively (
1E, 4E)-1-(2-benzyloxy phenyl)-5-(4-fluorophenyl)-1, 4-pentadiene-3-ketone (13 mmol), hydroxylamine hydrochloride (43 mmol), absolute ethyl alcohol 60 mL, pyridine 30 mL, at room temperature stir, solution becomes yellow clear liquid from suspension, react completely, rotary evaporation is except desolventizing, add 25 mL chloroforms, with 5% watery hydrochloric acid (volume ratio) acidifying, regulate pH value to be about 6, with 30 mL × 4 washings, dry, filter, precipitation, obtain yellow viscous fluid, add 10 mL ethyl acetate, there is solid to separate out, suction filtration, acetone/water recrystallization, obtain white solid, yield: 56%, fusing point: 130 ~ 132 ° of C.
(5) in 50 mL there-necked flasks, add sodium hydride (2.0 mmol), oxolane 7 mL, at room temperature stir, under ice-water bath condition, drip (
1E, 3Z, 4E)-1-(2-benzyloxy phenyl)-5-(4-fluorophenyl)-1, the solution of 4-pentadiene-3-ketoxime (1.45 mmol)+5 mL oxolanes, remove ice bath, at room temperature stir 2 h, reactant liquor becomes redness from yellow, drip the solution of the fluoro-5-PMC of 2-(1.5 mmol)+5 mL oxolanes, under room temperature, react, after reaction finishes, rotary evaporation is except desolventizing, add 25 mL carrene, regulate pH value to be about 6 with 5% watery hydrochloric acid (volume ratio), extraction, merge organic phase, anhydrous sodium sulfate drying, filter, precipitation, with silica gel thin-layer chromatography separate [
v(n-hexane):
v(ethyl acetate)=7:1], obtain target compound
.
1H?NMR?(500?MHz,?CDCl
3,?ppm)?δ:?7.71?(m,?1H,),?7.61~7.52?(m,?3H),?7.40~6.85?(m,?14H),?6.86?(d,
?J=5?Hz,
2H),?5.19?(s,?2H),?5.09?(s,?2H),?3.82?(s,?3H).
(6) preparation of formula I compound crystal form
Under 40 DEG C of conditions that also stir, in the solution to formula I compound (2.5g) in ethanol (80ml), dropwise add acetone soln.Further this mixture is stirred 10 minutes at 40 DEG C, to obtain settled solution, and left standstill 6 hours.Filter the formula I compound of collecting precipitation.The crystal of collecting is dissolved in methyl alcohol (40ml), and vapourisation under reduced pressure methyl alcohol.Add aqueous acetone (1 0ml, acetone 9ml+ water 1ml), to obtain settled solution, and left standstill 2 days.Filter the crystal of collecting precipitation, and at 60 DEG C by crystal vacuumize 2 hours, thereby obtain the formula I compound of white block crystal form.
The indices of the electrolytic capacitor of the present invention of use formula I compound crystal is shown in Table 1.
Table 1
Claims (7)
1. a chip-type solid electrolytic capacitor, comprise multiple solid electrolytic capacitor element, each element is by making with this sequence stack insulation oxide rete, semiconductor layer and conductive layer to form cathode portion on the anode substrate surface except the anode part of its one end, the metal that anode substrate comprises valve acting or the sintered body of conductive oxide or comprise the sintered body being connected with plain conductor, wherein semiconductor layer is organic semiconductor layer, and it contains the organic compound crystal shown in following formula I:
I，
It has the X-ray powder diffraction figure of 2 θ at approximately 12.6,12.7,16.6,18.8,21.5 and 23.8 places.
2. chip-type solid electrolytic capacitor as described in claim 1, wherein anode part comprises the end of anode substrate.
3. chip-type solid electrolytic capacitor as described in claim 1, wherein anode part comprises the plain conductor being connected with sintered body.
4. chip-type solid electrolytic capacitor as described in claim 3, wherein plain conductor be selected from tantalum, niobium, aluminium, titanium, mainly comprise this metalloid alloy and these metals and the alloy of partial oxidation and/or nitrogenize.
5. chip-type solid electrolytic capacitor as described in claim 1, wherein makes the interface insulation between anode part and the part except anode part with insulating resin.
6. chip-type solid electrolytic capacitor as described in claim 1, wherein insulation oxide rete mainly comprises and is selected from Ta
2o
5, Al
2o
3, Zr
2o
3and Nb
2o
5at least one.
7. 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 12.6,12.7,16.6,18.8,21.5 and 23.8 places.
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| CN201310376487.9A CN104143447A (en) | 2013-08-27 | 2013-08-27 | Solid electrolytic capacitor |
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| CN201310376487.9A CN104143447A (en) | 2013-08-27 | 2013-08-27 | Solid electrolytic capacitor |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104003932A (en) * | 2014-05-05 | 2014-08-27 | 成都尔珏科技有限公司 | Compound applicable to prepare medicines for treating asthma |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1225495A (en) * | 1998-01-28 | 1999-08-11 | 松下电器产业株式会社 | Electrolytic capacitor and method for making same |
| CN101973934A (en) * | 2010-09-06 | 2011-02-16 | 贵州大学 | 1,5-disubstituted aryl-1,4-pentadiene-3-ketoxime ether compound and preparation method thereof and insecticidal activity application |
| WO2012112676A2 (en) * | 2011-02-15 | 2012-08-23 | Kemet Electronics Corporation | Materials and methods for improving corner and edge coverage of solid electrolytic capacitors |
-
2013
- 2013-08-27 CN CN201310376487.9A patent/CN104143447A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1225495A (en) * | 1998-01-28 | 1999-08-11 | 松下电器产业株式会社 | Electrolytic capacitor and method for making same |
| CN101973934A (en) * | 2010-09-06 | 2011-02-16 | 贵州大学 | 1,5-disubstituted aryl-1,4-pentadiene-3-ketoxime ether compound and preparation method thereof and insecticidal activity application |
| WO2012112676A2 (en) * | 2011-02-15 | 2012-08-23 | Kemet Electronics Corporation | Materials and methods for improving corner and edge coverage of solid electrolytic capacitors |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104003932A (en) * | 2014-05-05 | 2014-08-27 | 成都尔珏科技有限公司 | Compound applicable to prepare medicines for treating asthma |
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