CN109916972A - A kind of reaction kettle and the test method using its evaluation anode foils and Working electrolyte matching - Google Patents

A kind of reaction kettle and the test method using its evaluation anode foils and Working electrolyte matching Download PDF

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Publication number
CN109916972A
CN109916972A CN201711319841.9A CN201711319841A CN109916972A CN 109916972 A CN109916972 A CN 109916972A CN 201711319841 A CN201711319841 A CN 201711319841A CN 109916972 A CN109916972 A CN 109916972A
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China
Prior art keywords
reaction kettle
test
paillon
working electrolyte
temperature
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喻珅
李刚
韦於正
吕军华
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Dongguan Dongyang Guangke Research and Development Co Ltd
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Dongguan Dongyang Guangke Research and Development Co Ltd
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Priority to CN201711319841.9A priority Critical patent/CN109916972A/en
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Abstract

The test method of anode foils and Working electrolyte matching is evaluated the invention discloses a kind of reaction kettle and using it.The reaction kettle includes the reaction kettle autoclave body with cavity and the reaction kettle lid being connected at the top of reaction kettle autoclave body, explosion-proof valve aperture and two electrode terminals are provided on the reaction kettle lid, one is positive terminal in described two electrode terminals, the other is negative terminal, two test paillons connect with positive terminal and negative terminal respectively and are deep into the Working electrolyte in the cavity;Explosion-proof valve is equipped in the explosion-proof valve aperture.Cooperated using the reaction kettle and I-T characteristic tester, precision high temperature testing machine and image display, it is easily achieved high-temperature current leakage test macro, using the test macro can it is succinct, efficiently, rapidly evaluation anode foils (such as aluminium electrolutic capacitor Anodic foil) and Working electrolyte matching, to effectively improve the development efficiency of aluminium electrolutic capacitor.

Description

A kind of reaction kettle and the test using its evaluation anode foils and Working electrolyte matching Method
Technical field
The test method of anode foils and Working electrolyte matching is evaluated the present invention relates to a kind of reaction kettle and using it, especially It is related to a kind of reaction kettle and efficiently and fast evaluate the anode foils and Working electrolyte for being used for aluminium electrolutic capacitor using it The test method of matching.
Background technique
Capacitor life-span experiment purpose be examination product under prescribed conditions in the stipulated time complete predetermined function Ability, that is, the adaptability that examination product is used and stored plus certain voltage under the conditions of certain temperature.
For aluminium electrolutic capacitor, Waste Acid From Hua Cheng Foil quality is poorer, and oxidation film is more easy to appear degradation phenomena at high temperature, causes High-temperature current leakage is larger;In addition, Waste Acid From Hua Cheng Foil and Working electrolyte matching are poor, it will also accelerate the deterioration of foil oxidation film, while interior Portion's temperature rise, which further increases, will also make Working electrolyte degradation phenomena occur, such as oxidation, cracking, pyrolysis side reaction occurs.This A little adverse reactions will will lead to that aluminium electrolytic capacitor product internal loss is big, fever is serious, air pressure is big, so that product be accelerated to lose Effect.Therefore the matching of the Waste Acid From Hua Cheng Foil and itself and each Working electrolyte of investigating different chemical conversion system difference specific volumes has very heavy Big meaning.
Durability test is a kind of form of life test, and test is time-consuming larger, and process is many and diverse, needs that electricity is first made Container, then the series of processes such as seasoned, finally carry out prolonged life-span accelerated test at high temperature.Not according to different product With the requirement of producer, usual test period is 2000H, 3000H, 5000H etc. even longer.
The method of industry inner evaluation aluminum electrolysis capacitor anode foil and Working electrolyte matching is generally frequently with adding at present Fast life experiment, i.e., under the conditions ofs such as 105 DEG C or 135 DEG C of high temperature equal, and to capacitor be subject to certain voltage and alternating current into Row life test, this mode can shorten test period to a certain extent, but it is even more to still need to time-consuming one or two months, so Being badly in need of a kind of method further can shorten the time on the basis of existing accelerated test.
The variation that can not observe capacitor internal leakage current in life experiment in real time at present, can not also grasp anode in real time The mating situation of foil and Working electrolyte.
Summary of the invention
For the above-mentioned problems in the prior art, anode is evaluated it is an object of that present invention to provide reaction kettle and using it The test method of foil and Working electrolyte matching more particularly to a kind of reaction kettle and efficiently and fast being evaluated using it is used for The anode foils of aluminium electrolutic capacitor and the test method of Working electrolyte matching.Reaction kettle structure of the invention is simple, uses Itself and I-T characteristic tester and precision high temperature testing machine cooperate, it is easy to accomplish high-temperature current leakage test macro, using the test system System can it is succinct, efficiently, rapidly evaluation anode foils (such as aluminium electrolutic capacitor Anodic foil) and Working electrolyte matching, To effectively improve the development efficiency of aluminium electrolutic capacitor.
In order to achieve the above object, the invention adopts the following technical scheme:
In a first aspect, the present invention provides a kind of reaction kettle, the reaction kettle includes reaction kettle autoclave body and the company with cavity The reaction kettle lid being connected at the top of the reaction kettle autoclave body is provided with explosion-proof valve aperture and two electrodes on the reaction kettle lid Binding post, one is positive terminal in described two electrode terminals, the other is negative terminal, two test paillons point It does not connect with positive terminal and negative terminal and in the Working electrolyte that is deep into cavity, is set in the explosion-proof valve aperture There is explosion-proof valve.
In reaction kettle of the invention, reaction kettle autoclave body and reaction kettle lid are tightly connected.
It is used as currently preferred technical solution below, but not as the limitation to technical solution provided by the invention, leads to Following preferred technical solution is crossed, can preferably reach and realize technical purpose and beneficial effect of the invention.
Preferably, the bottom of the reaction kettle autoclave body is additionally provided with reaction kettle pedestal, and the reaction kettle pedestal is in boss-shaped, Effect is easy for that reaction kettle is fixed after the completion of test, is then turned on.
Preferably, described two test paillons are fixed on the lower part of the reaction kettle lid.
Preferably, the test paillon is realized by fixing clip and is fixed.
Since reaction kettle of the invention is used as high-temperature current leakage reaction kettle when in use, need to be tested at high temperature, So all components require to select material resistant to high temperature.
Preferably, the material of the electrode terminal and fixing clip is stainless steel.
Preferably, the material of the reaction kettle lid, reaction kettle wall and reaction kettle pedestal is polytetrafluoroethylene (PTFE).
As the optimal technical scheme of reaction kettle of the present invention, two test paillons include three from bottom to top Point, it is respectively as follows: accredited part, middle section and extension, this three parts is accredited part in the coincident of side Width is greater than the width of middle section and extension, and the extension includes detent outstanding.
Preferably, the test paillon length direction keeps vertical, and the extension is sandwiched in and connects with electrode terminal In the fixing clip connect, the Working electrolyte just immersion test paillon is measured the upper end of part;
Preferably, described two test paillon length directions keep vertical parallel.
Preferably, the width of the accredited part is 9.95mm~10.05mm (also referred to as 10 ± 0.05mm) institute The length for stating accredited part is 49.75mm~50.25mm (also referred to as 50 ± 0.25mm).
Preferably, the width of the middle section be 2.95mm~3.05mm (also referred to as 3 ± 0.05mm), it is described in Between part length be 9mm~11mm (also referred to as 10 ± 1mm).
Preferably, the height of the reaction kettle autoclave body is 160mm, and the diameter of the reaction kettle autoclave body is 60mm.
Preferably, the diameter of the explosion-proof valve aperture (3) is 5mm, and the diameter of the electrode terminal (1) is 6mm.
Preferably, the diameter of the reaction kettle pedestal (8) is 44mm.
In reaction kettle of the invention, to prevent from screwing reaction kettle lid during paillon may be caused to damage, Ying Huan The step of slow carry out screwing hermetic reaction kettle.
Second aspect, the present invention provide a kind of test method for evaluating anode foils and Working electrolyte matching, the side Method uses test system and test leakage current numerical value, and the test macro includes that (i.e. high temperature leaks electricity reaction kettle described in first aspect Stream reaction kettle), I-T characteristic tester, precision high temperature testing machine and image display, the reaction kettle be vertically placed on precision In high[elevated, the I-T characteristic tester connection is connect with reaction kettle and image display respectively.This high-temperature current leakage is surveyed The schematic diagram of test system is referring to Fig. 1, wherein 11 be high-temperature current leakage reaction kettle, and 12 be precision high temperature testing machine, and 9 be I-T characteristic Tester, 10 be image display.
The present invention is not construed as limiting the connection type of reaction kettle and I-T characteristic tester, such as may is that will by electric wire The positive terminal and negative terminal of reaction kettle are connected on the anode and cathode of I-T characteristic tester, and are fixed.
The present invention is also not construed as limiting the connection type of image display and I-T characteristic tester, such as may is that and pass through Image display is connect by data line with I-T characteristic tester.
The model of I-T characteristic tester of the present invention for example can be, but not limited to: Shenzhen Ju Yinghui section automated system Company, TS2617-1.
The model of precision high temperature testing machine of the present invention for example can be, but not limited to: huge instrument instrument, IPO-303.
Anode paillon of the present invention for example can be the anode foils of aluminium electrolutic capacitor, leak electricity in accelerated life test The variation of stream actually reflect Waste Acid From Hua Cheng Foil quality quality and Waste Acid From Hua Cheng Foil and Working electrolyte matching (leakage current is smaller, Matching is higher).Test method according to the present invention can be from of the conditions such as anode foils and Working electrolyte and operating temperature With setting about in property, the operating condition that the Waste Acid From Hua Cheng Foil of different batches difference system is suitable for can be tentatively judged in 96H, can be had Effect shortens the time of screening anode foils, to further increase development efficiency.
In method of the invention, the reaction kettle of the first aspect is used as high-temperature current leakage test reaction in a test system Kettle.
In method of the invention, the I-T characteristic tester includes one and stablizes adjustable DC power supply.
As the optimal technical scheme of the method for the invention, the described method comprises the following steps:
(a) anode foils are struck out to the sample of same size, to guarantee the consistency of initial paillon, to obtaining initial paillon Carry out initial parameter test;
(b) the above-mentioned initial paillon surveyed is cleaned and is dried, obtain the paillon of pre-treatment, for use;
(c) take the paillon of two panels pre-treatment, i.e. two test paillons (5), two test paillons (5) respectively with reaction kettle Positive terminal is connected with negative terminal, and is deep into the Working electrolyte (7) of reaction kettle autoclave body cavity;
(d) using reaction kettle lid (2) seal reaction kettle, then access I-T characteristic tester, precision high temperature testing machine with And image display, test macro is obtained, reaction kettle is heated, the voltage of I-T characteristic tester is set, carries out high-temperature current leakage Test, records real-time leakage data, to evaluate anode foils and Working electrolyte matching.
In method of the invention, step (a) generally carries out punching press using press machine.
In method of the invention, step (a)-(d) expression is the knot individually testing two paillons of a batch and obtaining Fruit needs replacing the paillon of multiple and different batches to evaluate the matching of anode paillon and Working electrolyte, this replacement step It suddenly is the routine operation of those skilled in the art, details are not described herein again.
It, can be by the way that (including test temperature be identical, and test temperature is under the same test conditions in method of the invention The temperature of reaction kettle after heating), the paillon by changing different batches carries out high-temperature current leakage test, can evaluate this temperature Lower difference anode foils and Working electrolyte matching;Also it can change test temperature and keep other experimental conditions constant, to comment Anode foils and Working electrolyte matching under valence different temperatures;The conditions such as drying temperature can also be changed to repeat to test.
As an example, high-temperature current leakage experimental condition can be set according to such as following table one:
Table one: high-temperature current leakage experimental condition
Method of the invention can efficiently and fast evaluate the matching of anode foils and Working electrolyte, testing time Within 96h, it can be effectively shortened with further screening and the most matched Working electrolyte of anode foils by matching result The time for screening anode foils, further increase development efficiency.
In this optimal technical scheme, the type of anode foils is not construed as limiting, such as can be aluminium electrolutic capacitor Anodic Foil.Its anode foils that can be different chemical conversion systems, different specific volumes, may be simply referred to as Waste Acid From Hua Cheng Foil.
Preferably, step (a) initial parameter includes foil voltage and capacity.
Preferably, step (b) the clean step is washed using water.
Preferably, it is 85 DEG C that the temperature of step (b) drying is constant.
Preferably, it is 30min that the time of step (b) drying is constant.
Preferably, the described two test paillons of step (c) are sandwiched in positive terminal and negative terminal with reaction kettle respectively In the fixing clip that column is separately connected, and it is deep into the Working electrolyte of reaction kettle autoclave body cavity.
Preferably, described two test paillons include three parts from bottom to top, are respectively as follows: accredited part, centre Part and extension, three parts are greater than middle section and extension in the coincident of side, the width for being accredited part Width, and the extension include detent outstanding.
Preferably, the described two test paillon length directions of step (c) are kept vertically, and the extension be sandwiched in In the fixing clip of electrode terminal connection, the Working electrolyte just submerges the upper end that paillon is measured part.
Preferably, described two test paillon length directions keep vertical parallel.
Preferably, when step (d) is tested, reaction kettle is heated by baking oven.
In the present invention, the temperature of the reaction kettle after heating is test temperature, and the present invention is to test temperature without determining number Value limits, and is changed according to the product requirements such as the specification of selected paillon, selected electrolyte and capacitor difference.Such as it can adjust Section oven temperature change test temperature (oven temperature often uses 105 DEG C in accelerated test, 135 DEG C, but according to designed aluminium electroloysis electricity Other temperature are also adjusted in the difference of containers demand).
Preferably, when step (d) is tested, to the Initial parameter sets of I-T characteristic tester with reference to positive terminal Primary data that the initial paillon of connection is obtained in step (a) is set, and reference standard is: step (d) I-T characteristic tester Voltage is the 450/600 of the initial parameter foil voltage that step (a) obtains.According to the difference of every foil voltage, by above-mentioned ratio Example adjustment setting parameter;According to the paillon of 600V described above, institute's setting parameter is 450V, if then foil voltage is 602V, institute Setting parameter will be adjusted to 602/600 × 450V=451.5V.
Preferably, when the primary data that the initial paillon connecting with positive terminal is obtained in step (a) are as follows: foil voltage 600V, foil area 5cm2When, the Initial parameter sets of I-T characteristic tester are as follows: VF voltage is set as in I-T test curve 450V, electric current are set as 2mA.
Preferably, step (d) is every the primary real-time leakage data of record for 24 hours.
Preferably, after step (d) test, by high-temperature current leakage data with the preservation of Excel format.
Preferably, after step (d) test, paillon is taken out, cleans and is saved after drying.
As the optimal technical scheme of the method for the invention, first carried out under the conditions of step (d) reaction kettle identical temperature High-temperature current leakage test, tests the paillon of four batches, the paillon of each batch individually carries out, i.e. the paillon for each batch Step (a)-(d) will be successively carried out, after the paillon for testing four batches, changes test temperature and keeps other conditions It is constant, the paillon of retest four additional batch.
As the further preferred technical solution of the method for the invention, the described method comprises the following steps:
(a) anode foils are struck out into sample, obtains initial paillon, and carry out initial parameter test;
Wherein, the initial parameter of test includes foil voltage, capacity and foil area;
(b) the above-mentioned initial paillon surveyed is eluted with water and in 85 DEG C of drying 30min, obtains the paillon of pre-treatment, to With;
(c) paillon of two panels pre-treatment, i.e. two test paillons (5) are taken, two test paillons (5) are sandwiched in respectively and react In the fixing clip (4) that the positive terminal of kettle is connected with negative terminal;
Wherein, described two tests paillon (5) include three parts from bottom to top, are respectively as follows: accredited part, centre Part and extension, three parts are greater than middle section and extension in the coincident of side, the width for being accredited part Width, and the extension include detent outstanding;
Described two test paillon (5) length directions keep vertical parallel, and the extension is sandwiched in and electrode connection In the fixing clip (4) of column connection, the Working electrolyte (7) just submerges the upper end that paillon is measured part;
(d) using reaction kettle lid (2) seal reaction kettle, then access I-T characteristic tester, precision high temperature testing machine with And image display, test macro is obtained, reaction kettle is heated using baking oven, the voltage of I-T characteristic tester is set, is carried out high Temperature electric leakage current test after test, high-temperature current leakage data is saved, are taken every recording primary real-time leakage data for 24 hours Paillon out cleans reaction kettle and injects the electrolyte of the same race that do not test after drying, repeats the above steps and tested, specifically:
When retest, first continue under the same conditions with above-mentioned test temperature test the other three batch paillon, Then it changes the step (d) oven temperature and changes test temperature, and keep other conditions constant, continue to test four additional batch Paillon, to evaluate anode foils and Working electrolyte matching.
In this optimal technical scheme, after the testing time of 96h, by comparative experimental data at each temperature, each batch The situation of change of anode foils leakage current numerical value in high-temperature current leakage test, can filter out and be adapted with selected Working electrolyte The anode foils of specification.
Compared with the prior art, the invention has the following beneficial effects:
(1) reaction kettle structure of the invention is simple, is cooperated using itself and I-T characteristic tester and precision high temperature testing machine, Be easily achieved high-temperature current leakage test macro, using the test macro can succinct, efficiently, rapidly evaluate anode foils (such as Aluminium electrolutic capacitor Anodic foil) and Working electrolyte matching.It can be under identical test environment, to different Waste Acid From Hua Cheng Foil or work Make electrolyte and carry out rationally effective comparison, to effectively improve the development efficiency of aluminium electrolutic capacitor.
(2) method of the invention passes through monitoring of the test macro to high-temperature current leakage, can effectively compare in 96H and not assimilate At the difference of foil, or different Waste Acid From Hua Cheng Foils and the matching of electrolyte etc., research and development of products efficiency is greatlyd improve.
(3) for the present invention by carrying out high-temperature current leakage test in Working electrolyte to different batches anode foils, observation is real Leakage current changes to verify the anode foils of different chemical conversion systems, different specific volumes to electrolyte under various operating temperatures during testing Mating situation, thus effectively filter out with each scale aluminum electrolytic capacitor the anode that is matched using Working electrolyte Screening time is greatly shortened in foil compared with the existing technology, realizes the rapidly and efficiently screening to anode foils.
Detailed description of the invention
Fig. 1 is the schematic diagram of high-temperature current leakage test macro of the invention, wherein 11 be high-temperature current leakage reaction kettle, 12 It is I-T characteristic tester for precision high temperature testing machine, 9,10 be image display.
Fig. 2 a is the structural schematic diagram of reaction kettle described in the embodiment of the present invention 1, wherein 1- electrode terminal, 2- reaction kettle Lid, 3- explosion-proof valve aperture, 4- fixing clip, 5- test paillon, 6- reaction kettle wall, 7- Working electrolyte, 8- reaction kettle pedestal.
Fig. 2 b is the structural schematic diagram that paillon is tested in the embodiment of the present invention 1, wherein 51- is measured part, among 52- Part, 53- extension, unit in figure are as follows: mm.
Fig. 3 a- Fig. 3 c is the structure size figure of reaction kettle described in the embodiment of the present invention 1 respectively, and wherein Fig. 3 a is main view, Fig. 3 b is side view, and Fig. 3 c is top view, unit in figure are as follows: mm.
Fig. 4 is four kinds of anode foils leakage current change curves at 105 DEG C in the embodiment of the present invention 3.
Fig. 5 is four kinds of anode foils leakage current change curves at 135 DEG C in the embodiment of the present invention 4.
Specific embodiment
To further illustrate the technical scheme of the present invention below with reference to the accompanying drawings and specific embodiments.
Embodiment 1
The present embodiment provides a kind of reaction kettle, the reaction kettle includes having the reaction kettle autoclave body of cavity and being sealedly attached to Reaction kettle lid 2 at the top of reaction kettle autoclave body is provided with explosion-proof valve aperture 3 and two electrode connections on the reaction kettle lid 2 Column 1, one is positive terminal in described two electrode terminals, the other is negative terminal, two test paillons 5 pass through Fixing clip 4 is fixed on the lower part of reaction kettle lid 2, thus the connection with positive terminal and negative terminal respectively;
Described two test paillons 5 include three parts from bottom to top, be respectively as follows: accredited part, middle section and Extension, three parts are greater than the width of middle section and extension in the coincident of side, the width for being accredited part, And the extension includes that (referring to fig. 2 b), fully according to HEC, " aluminium foil is sliced modulo operation to structural schematic diagram to detent outstanding Regulation " obtained (in figure unit: mm);
5 length direction of test paillon keeps vertical, and the extension is sandwiched in consolidating of connecting with electrode terminal On clamp piece 4, the Working electrolyte 7 just immersion test paillon 5 is measured the upper end of part;
Explosion-proof valve is equipped in the explosion-proof valve aperture 3;
The bottom of the reaction kettle autoclave body is additionally provided with reaction kettle pedestal 8;
The material of the electrode terminal 1 and fixing clip 4 is stainless steel, reaction kettle lid 2, reaction kettle wall 6 and anti- The material for answering bottom seat 8 is polytetrafluoroethylene (PTFE).
Fig. 2 a is the structural schematic diagram of reaction kettle described in the embodiment of the present invention 1, wherein 1- electrode terminal, and 2- reacts kettle cover Son, 3- explosion-proof valve aperture, 4- fixing clip, 5- test paillon, 6- reaction kettle wall, 7- Working electrolyte, 8- reaction kettle pedestal.
Fig. 2 b is the structural schematic diagram that paillon is tested in the present embodiment 1, wherein 51- is measured part, the middle section 52-, 53- extension.
Fig. 3 a- Fig. 3 c is the structure size figure of reaction kettle described in the embodiment of the present invention 1 respectively, and wherein Fig. 3 a is main view, Fig. 3 b is side view, and Fig. 3 c is top view.
Embodiment 2
The present embodiment provides a kind of test macros for high-temperature current leakage test, and the system comprises reaction kettle, I-T are special Property tester, precision high temperature testing machine and image display, reaction kettle is first vertically placed in precision high temperature testing machine, then is led to It crosses electric wire and is connected to I-T characteristic tester anode and cathode for the anode of reaction kettle is corresponding with cathode, and fix, image is shown Showing device then is directly connected with I-T characteristic tester by data line.
Embodiment 3
The present embodiment provides a kind of test methods for evaluating anode foils and Working electrolyte matching, and the method is using real It applies test macro described in example 2 and carries out high-temperature current leakage test, specifically, comprising the following steps:
Four kinds of Waste Acid From Hua Cheng Foils are distinguished punching press sample by 4.1, and initial parameter test is carried out to it (as reached voltage and capacity Deng), test result is recorded in papery table;
4.2 clean the above-mentioned initial paillon surveyed with pure water, dry (85 DEG C, 30min) under the same conditions, and be put into It is stand-by in drier;
It is anti-that 4.3 paillons that the identical lot number of two panels is taken out from the foil sample of above-mentioned pre-treatment are sandwiched in high-temperature current leakage respectively The positive and negative polarities of kettle are answered, and pours into appropriate electrolyte and carries out high-temperature current leakage test, wherein initial parameter setting will be according to anode To be arranged, (the arrival voltage that such as foil voltage i.e. step 4.1 obtains is 600V to folded paillon initial parameter, then I-T test curve Middle VF voltage should be set as 450V, foil area 5cm2When electric current be set as 2mA, according to the difference of every foil voltage, in proportion Adjustment setting parameter), and every the primary leakage current numerical value in real time of record in table two for 24 hours;
After 4.4 to the 96H testing time, take out paillon clean dry after save;
4.5 change another batch paillon carries out high-temperature current leakage test under the same conditions, and records data.
The data saved after the test are carried out software processing by 4.6, make leakage current change curve shown in Fig. 3.
In the present embodiment, test specimen information is shown in Table two:
Table two: test specimen information
The condition that high pressure Waste Acid From Hua Cheng Foil by investigating different chemical conversion systems, different specific volumes is H411C in 105 DEG C and electrolyte The case where lower leakage current, so that filtering out suitable for temperature is 105 DEG C and the Waste Acid From Hua Cheng Foil of H411C Working electrolyte.
In the present embodiment, experimental condition is shown in Table three:
Table three: experimental condition
In the present embodiment, 105 DEG C of 450V DC load high-temperature current leakage records the results are shown in Table four:
Four: 105 DEG C of 450V DC load high-temperature current leakage record sheets of table
In the present embodiment, four kinds of anode foils leakage current change curves are shown in Fig. 4 at 105 DEG C, by observing Fig. 4 and in real time electric leakage Flow data, under the conditions of 105 DEG C, minimum is integrally presented in the high-temperature current leakage numerical value of D sample, is then secondly C < A < B, this shows D sample is more suitable for that operating temperature is 105 DEG C and Working electrolyte is H411C.
Embodiment 4
The present embodiment 4 only changes test temperature (becoming 135 DEG C from 105 DEG C), other experimental conditions compared to embodiment 3 It is constant.
In the present embodiment, experimental condition is shown in Table five:
Table five: experimental condition
In the present embodiment, 135 DEG C of 450V DC load high-temperature current leakage records the results are shown in Table six:
Six: 135 DEG C of 450V DC load high-temperature current leakage record sheets of table
In the present embodiment, four kinds of anode foils leakage current change curves are shown in Fig. 5, six data of comparative analysis table and Fig. 5 at 135 DEG C It is found that minimum is integrally presented in the high-temperature current leakage numerical value of B sample under the conditions of 135 DEG C, it is secondly D < C < A;This shows to compare In other three samples, B sample is more suitable for that operating temperature is 135 DEG C and Working electrolyte is H411C.
The Applicant declares that the present invention is explained by the above embodiments method detailed of the invention, but the present invention not office Be limited to above-mentioned method detailed, that is, do not mean that the invention must rely on the above detailed methods to implement.Technical field Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention Addition, selection of concrete mode etc., all of which fall within the scope of protection and disclosure of the present invention.

Claims (10)

1. a kind of reaction kettle, which is characterized in that the reaction kettle includes having the reaction kettle autoclave body of cavity and being connected to reaction kettle Reaction kettle lid (2) at the top of autoclave body, which is characterized in that be provided with explosion-proof valve aperture (3) and two on the reaction kettle lid (2) A electrode terminal (1), one is positive terminal in described two electrode terminals, the other is negative terminal, two The Working electrolyte (7) that test paillon (5) connect with positive terminal and negative terminal respectively and is deep into the cavity In;
Explosion-proof valve is equipped in the explosion-proof valve aperture (3).
2. reaction kettle according to claim 1, which is characterized in that reaction kettle autoclave body and reaction kettle lid (2) are tightly connected;
Preferably, the bottom of the reaction kettle autoclave body is additionally provided with reaction kettle pedestal (8);
Preferably, described two tests paillon (5) are fixed on the lower part of reaction kettle lid (2);
Preferably, the test paillon (5) is realized by fixing clip (4) and is fixed.
3. reaction kettle according to claim 1 or 2, which is characterized in that the electrode terminal (1) and fixing clip (4) Material be stainless steel;
Preferably, the material of the reaction kettle lid (2), reaction kettle wall (6) and reaction kettle pedestal (8) is polytetrafluoroethylene (PTFE).
4. reaction kettle according to claim 1-3, which is characterized in that described two test paillons (5) include Three parts from bottom to top, are respectively as follows: accredited part, middle section and extension, three parts side coincident, The width of accredited part is greater than the width of middle section and extension, and the extension includes detent outstanding;
Preferably, test paillon (5) length direction keeps vertical, and the extension is sandwiched in and connect with electrode terminal Fixing clip (4) on, the Working electrolyte (7) just immersion test paillon (5) be measured part upper end;
Preferably, described two test paillon (5) length directions keep vertical parallel;
Preferably, the width of the accredited part is 9.95mm~10.05mm, and the length of the accredited part is 49.75mm~50.25mm;
Preferably, the width of the middle section is 2.95mm~3.05mm, and the length of the middle section is 9mm~11mm;
Preferably, the height of the reaction kettle autoclave body is 160mm, and the diameter of the reaction kettle autoclave body is 60mm;
Preferably, the diameter of the explosion-proof valve aperture (3) is 5mm, and the diameter of the electrode terminal (1) is 6mm;
Preferably, the diameter of the reaction kettle pedestal (8) is 44mm.
5. a kind of test method for evaluating anode foils and Working electrolyte matching, which is characterized in that the survey that the method uses Test system tests leakage current numerical value, and the test macro includes the described in any item reaction kettles of claim 1-4, the survey of I-T characteristic Examination instrument, precision high temperature testing machine and image display, the reaction kettle are vertically placed in precision high temperature testing machine, the I-T Characteristic tester connection is connect with reaction kettle and image display respectively.
6. according to the method described in claim 5, it is characterized in that, the described method comprises the following steps:
(a) anode foils are struck out to the sample of same size, to guarantee the consistency of initial paillon, are carried out to initial paillon is obtained Initial parameter test;
(b) the above-mentioned initial paillon surveyed is cleaned and is dried, obtain the paillon of pre-treatment, for use;
(c) take the paillon of two panels pre-treatment, i.e. two test paillons (5), two test paillons (5) respectively with the anode of reaction kettle Binding post is connected with negative terminal, and is deep into the Working electrolyte (7) of reaction kettle autoclave body cavity;
(d) reaction kettle is sealed using reaction kettle lid (2), then accesses I-T characteristic tester, precision high temperature testing machine and figure As display, test macro is obtained, reaction kettle is heated, the voltage of I-T characteristic tester is set, carries out high-temperature current leakage survey Examination, records real-time leakage data, to evaluate anode foils and Working electrolyte matching.
7. according to the method described in claim 6, it is characterized in that, step (a) initial parameter includes foil voltage and appearance Amount;
Preferably, step (b) the clean step is washed using water;
Preferably, it is 85 DEG C that the temperature of step (b) drying is constant;
Preferably, it is 30min that the time of step (b) drying is constant;
Preferably, described two tests paillon (5) of step (c) are sandwiched in positive terminal and negative terminal with reaction kettle respectively In the fixing clip (4) being separately connected, and it is deep into the Working electrolyte of reaction kettle autoclave body cavity;
Preferably, described two tests paillon (5) include three parts from bottom to top, are respectively as follows: accredited part, middle part Point and extension, three parts be greater than middle section and extension in the coincident of side, the width for being accredited part Width, and the extension includes detent outstanding;
Preferably, described two test paillon (5) length directions of step (c) are kept vertically, and the extension be sandwiched in In the fixing clip (4) of electrode terminal connection, the Working electrolyte (7) just submerges the upper end that paillon is measured part;
Preferably, described two test paillon (5) length directions keep vertical parallel.
8. method according to claim 6 or 7, which is characterized in that when step (d) is tested, added by baking oven to reaction kettle Heat;
Preferably, the voltage of step (d) I-T characteristic tester is the 450/ of the initial parameter foil voltage that step (a) obtains 600;
Preferably, when the primary data that the initial paillon connecting with positive terminal is obtained in step (a) are as follows: foil voltage 600V, foil area 5cm2When, the Initial parameter sets of I-T characteristic tester are as follows: VF voltage is set as in I-T test curve 450V, electric current are set as 2mA;
Preferably, step (d) is every the primary real-time leakage data of record for 24 hours;
Preferably, after step (d) test, by high-temperature current leakage data with the preservation of Excel format;
Preferably, after step (d) test, paillon is taken out, cleans and is saved after drying.
9. according to the described in any item methods of claim 6-8, which is characterized in that in the identical temperature condition of step (d) reaction kettle Lower progress high-temperature current leakage test, tests the paillon of four batches, and the paillon of each batch is individually tested, and is testing four batches After secondary paillon, changes test temperature and keep other conditions constant, the paillon of retest four additional batch.
10. the method according to claim 6, which is characterized in that the described method comprises the following steps:
(a) anode foils are struck out into sample, obtains initial paillon, and carry out initial parameter test;
Wherein, the initial parameter of test includes foil voltage, capacity and foil area;
(b) the above-mentioned initial paillon surveyed is eluted with water and in 85 DEG C of drying 30min, obtains the paillon of pre-treatment, for use;
(c) paillon of two panels pre-treatment, i.e. two test paillons (5) are taken, two test paillons (5) are sandwiched in and reaction kettle respectively In the fixing clip (4) that positive terminal is connected with negative terminal;
Wherein, described two tests paillon (5) include three parts from bottom to top, are respectively as follows: accredited part, middle section And extension, three parts are greater than the width of middle section and extension in the coincident of side, the width for being accredited part Degree, and the extension includes detent outstanding;
Described two test paillon (5) length directions keep vertical parallel, and the extension is sandwiched in and connects with electrode terminal In the fixing clip (4) connect, the Working electrolyte (7) just submerges the upper end that paillon is measured part;
(d) reaction kettle is sealed using reaction kettle lid (2), then accesses I-T characteristic tester, precision high temperature testing machine and figure As display, test macro is obtained, reaction kettle is heated using baking oven, the voltage of I-T characteristic tester is set, high temperature leakage is carried out After test, high-temperature current leakage data are saved, take out foil every recording primary real-time leakage data for 24 hours for testing current Piece cleans reaction kettle and injects the electrolyte of the same race that do not test after drying, repeats the above steps and tested, specifically:
When retest, first in the paillon for continuing test the other three batch under the same conditions with above-mentioned test temperature, then It changes the step (d) oven temperature and changes test temperature, and keep other conditions constant, continue the foil for testing four additional batch Piece, to evaluate anode foils and Working electrolyte matching.
CN201711319841.9A 2017-12-12 2017-12-12 A kind of reaction kettle and the test method using its evaluation anode foils and Working electrolyte matching Pending CN109916972A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06215988A (en) * 1992-09-25 1994-08-05 Hidaka Electron Kk Evaluating method for anode foil of aluminum electrolytic capacitor
CN101443865A (en) * 2006-05-15 2009-05-27 松下电器产业株式会社 Aluminum electrolytic capacitor
CN102592846A (en) * 2011-01-17 2012-07-18 周旺龙 Embedded type wiring terminal sealing cover for large aluminium electrolytic capacitors
CN103534774A (en) * 2011-05-16 2014-01-22 松下电器产业株式会社 Electrode foil and method for manufacturing same, and capacitor
CN103700507A (en) * 2013-12-25 2014-04-02 佛山市高明区利明电子有限公司 100V electrolytic capacitor and producing process thereof
CN206003632U (en) * 2016-07-27 2017-03-08 佛山市蓝钻电子有限公司 A kind of new type explosion proof aluminium electrolutic capacitor

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06215988A (en) * 1992-09-25 1994-08-05 Hidaka Electron Kk Evaluating method for anode foil of aluminum electrolytic capacitor
CN101443865A (en) * 2006-05-15 2009-05-27 松下电器产业株式会社 Aluminum electrolytic capacitor
CN102592846A (en) * 2011-01-17 2012-07-18 周旺龙 Embedded type wiring terminal sealing cover for large aluminium electrolytic capacitors
CN103534774A (en) * 2011-05-16 2014-01-22 松下电器产业株式会社 Electrode foil and method for manufacturing same, and capacitor
CN103700507A (en) * 2013-12-25 2014-04-02 佛山市高明区利明电子有限公司 100V electrolytic capacitor and producing process thereof
CN206003632U (en) * 2016-07-27 2017-03-08 佛山市蓝钻电子有限公司 A kind of new type explosion proof aluminium electrolutic capacitor

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