CN100442590C - Method for measuring gas production rate of battery formation and system therefor - Google Patents
Method for measuring gas production rate of battery formation and system therefor Download PDFInfo
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- CN100442590C CN100442590C CNB2004100281213A CN200410028121A CN100442590C CN 100442590 C CN100442590 C CN 100442590C CN B2004100281213 A CNB2004100281213 A CN B2004100281213A CN 200410028121 A CN200410028121 A CN 200410028121A CN 100442590 C CN100442590 C CN 100442590C
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The present invention relates to a battery formation gas production quantity measuring method and the system thereof. The battery formation gas production quantity measuring method comprises the following steps: (A) dry electrode core bodies of batteries to be measured with different shapes are arranged in a soft package, an electrolyte is injected in the soft package, and the soft package is sealed in a hermetic mode after the vacuum is pumped so as to obtain a sealed battery to be measured; (B) the sealed battery is submerged in a harmless liquid in a suspension mode, and the suspension weight of the sealed battery is measured; (C) the sealed battery is charged for formation sufficiently so as to obtain a formation battery to be measured; (D) the formation battery is submerged in a harmless liquid in a suspension mode, and the suspension weight of the formation battery is measured; (E) according to the change of the suspension weight before and after the formation of the battery to be measured, the corresponding volume change (the gas production volume and/or gas production weight of the soft package battery) of the battery to be measured is calculated. The method of the present invention measures the gas production quantity by utilizing the expansion of the casing after the formation of the battery, has wide accommodation, can completely collect the gas produced by the formation of the battery with high efficiency, and is hardly influenced by the outside.
Description
[technical field]
The present invention relates to the secondary ion battery and make the field, more particularly, the present invention relates to a kind of method and apparatus system thereof that the secondary ion battery changes into the gas flow of reaction generation of measuring.
[background technology]
At present, with the lithium ion battery novel battery that the secondary cell of representative belongs to high-energy-density, becoming important requisite Power Supply fittings on the communication products such as mobile phone, mobile DVD, palmtop PC day by day.The shell of the lithium ion battery on the market is generally garden cylindricality type or rectangular configuration, and housing is generally metal sheet aluminium or steel and forms.
The outside of lithium ion battery by housing to finalized the design and protected, its core is to be interacted by the electrode core body of drying and electrolyte to form; In the lithium ion battery manufacture process, the charging that battery carries out is first activated, battery charging reaction first is that changing into of battery sent out and should will generated solid electrolyte interface (solid electrolyte interface) or claim the SEI film through the wetting negative electrode active material surface of electrolyte.In this formation process of battery, follow a series of electrochemical reactions and can produce a large amount of gas.The gas flow that produces is subjected to influences such as positive and negative pole material, electrolyte content and kind thereof, chemical synthesis technology condition.
The mensuration of the gas production in the battery formation process helps the selection of battery plus-negative plate material, help understanding the quality of electrolyte, and, the gas flow that produces in the battery formation process has the influence of highly significant to capacity, cycle life and the security performance of battery, therefore, accurately no matter the gas production in the mensuration battery formation process still for the monitoring of battery production process, all has very important significance for battery design, research and development, improvement.But owing to there is following main difficulty: the gas that battery changes into generation can cause that battery case expands and electrolyte leakage, the gas generated ectocine that is subjected to is big, the gas that produces is difficult to be collected, the difficult metering of the gas of collecting etc., the detection that causes battery to change into gas production is a lithium ion battery quality Control during Production difficult point always, so that does not see so far that in this field effective detection means is open always.
Application number is arranged is 90223694.6 Chinese patent file in Xiang Guan technological improvement therewith, and it discloses a kind of floatable gas and has stored generator, and it mainly is made up of wireway, gas hood, container and reaction courage.Solid reagent is placed in the reaction courage, and the reaction courage is suspended in the gas hood, and gas hood sinks in the liquid reagent in the container, can produce hydrogen, carbon dioxide, hydrogen sulfide and acetylene gas.This instrument is except producing the gas, and the replacing annex can serve as Drexel bottle and be used for gas washing; Take the reaction courage, can be used for inventory of gas, measure gas volume.It is said that the function of this instrument is many, the utilization rate height.This instrument is filled water in container, gas hood is inserted in the water of container, by the gravity sinking of gas hood.Discharge the air in the gas hood, the gas of being stored is imported in gas hood by conduit, and gas hood rises, and realizes the purpose of air storage.Drawing on gas hood has graduation mark, and scale and the water surface relative displacement during gas hood sink-float, expression are failed the people or discharged the volume of gas, realize measuring the purpose of gas volume.But obviously this apparatus structure and corresponding method are unwell to the gas flow that measurement secondary ion battery changes into middle generation.
Relevant technological improvement also sees the Chinese patent file that application number is 85200510.U, and it discloses the quick analyzer that a kind of battery industry monitoring positive mix mixes rate.This instrument is made up of cooling vortex mixer, gas burette, absorption unit of dioxide carbon.This instrument is by measuring the volume of mixed combustion gas, after recording the mixed combustion gas volume, absorb and remove carbon dioxide, measure the residual gas volume again, promptly try to achieve the percentage composition of carbon, and then the mixing quality of calculating acetylene carbon black is extrapolated acetylene carbon black and is mixed rate.Obviously, the structure of this instrument and method are unwell to the gas flow that measurement secondary ion battery changes into middle generation equally.
[summary of the invention]
At the above-mentioned shortcoming of prior art, the technical purpose that the present invention will reach is a kind of wide accommodation will be provided, can collect fully, efficiently that gas, ectocine that secondary cell changes into generation are little, the battery of the gas flow that can utilize the shell of battery after changing into to expand to measure generation changes into gas production assay method and apparatus system thereof.
For this reason, one of technical scheme of the present invention is that a kind of battery changes into the gas production assay method, this battery changes into the gas production assay method and comprises the steps: A) the dried electrode core body of difform mesuring battary is inserted in the flexible package, in flexible package, inject electrolyte, vacuumize the back hermetic sealing is carried out in flexible package, obtain sealed battery to be measured; B) described sealed battery is immersed in the harmless liquid with suspending, measures the weight suspension of this sealed battery; C) described sealed battery is charged fully change into, obtain the battery that changes into to be measured; D) the described battery that changes into is immersed in the harmless liquid with suspending, measures the weight suspension that this changes into battery; E) change aerogenesis volume and/or gas generated weight that to calculate its corresponding change in volume be described flexible-packed battery according to the weight suspension of mesuring battary before and after changing into.Method of the present invention has utilized the buoyancy in the physics to decide rate dexterously, it is attached in the measurement of battery formation gas of the present invention: method utilization of the present invention is in can hermetically sealed battery flexible package splendid attire different shape mesuring battary, to be changed, the dried electrode core body, what the original electrolyte of injection mesuring battary was simulated in the battery flexible package then is wetting, and that simulates after the flexible package hermetic sealing changes into, with originally change into all gas that identical simulation formation process produced and be not kept in the battery flexible package with leaking, utilize the volumetric expansion of the battery flexible package that takes place because gas occurs again, and the buoyancy of this volumetric expansion generation increases the minimizing of the weight suspension that equals tested battery, can obtain the bulking value that formation process produces gas by inverse, the combining environmental temperature is used gas equation again, can further calculate to such an extent that produce the gravimetric value of gas.And owing to be immersed in battery in the water fully, the big as far as possible so that influence of external environment reduces to and ignores and water container can be done, thereby method of the present invention can be collected the gas that the electric core body in the battery of various shell shapes is produced fully, efficiently in changing into, and utilize the shell of battery after changing into to expand and accurately measure the gas flow that battery is produced in changing into, and extraneous very little for the influence of test result, thereby the test specification of the inventive method is very wide, adaptability is very strong.
In order to increase measuring accuracy, at step B), D), E) in, the certainty of measurement of described weight is not less than 0.01g.
The interference that produces for the density and the buoyancy of gas production, harmless liquid for fear of factors vary and temperature fluctuation, in steps A) in, after inserting in the flexible package, described electrode core body also passes through vacuum drying, inject electrolyte behind the vacuum drying again in flexible package, wherein the vacuum drying temperature is 50～100 ℃, preferred 50～70 ℃, vacuum degree is≤-0.05Mpa, preferably≤-0.08Mpa, drying time is 4～48h, preferred 8～24h.Described electrolyte is the electrolyte that mesuring battary adopted, described flexible package by hermetic sealing after, described sealed battery to be measured also was placed in 10 ℃～55 ℃ constant temperature 4～48 hours, 20 ℃～45 ℃ of preferred thermostat temperatures, preferred constant temperature time is 20～30 hours.The material of described flexible package is preferably aluminum-plastic composite membrane, can also is plastic film or multilayer composite plastic film certainly.At step B) in, the uniform pure water of isothermal that described harmless liquid obtains for constant temperature at normal temperatures.At step D) and described step B) in, described harmless liquid is the uniform pure water of isothermal that constant temperature obtains under identical normal temperature.The thermostat temperature of described harmless liquid is equal to the thermostat temperature of mesuring battary.At step C) in, after fully charging changed into, the described battery that changes into to be measured also was placed in 10 ℃～55 ℃ constant temperature 4～48 hours, preferred 20～30 hours of constant temperature and then enter step D).
For making measurement result reflect fully that truly battery changes into gas production, must make that electrode is fully wetting, battery changes into and reacts completely fully, therefore, at step C) in, it is to fill speed with trickle charge or tiny stream described sealed battery is charged to change into that described charging changes into, till this battery all told is filled or suitably overcharges, be equivalent to the negative electrode active material surface and generate till the stable SEI film.At step C) in, the charge rate that described charging changes into is 0.01C～0.5C, preferred charge rate is 0.1C; The described voltage that changes into battery to be measured is 0.9～1.2 times of nominal voltage, and the preferred cell voltage that changes into to be measured is 1.0～1.1 times of nominal voltage.
Correspondingly, two of technical scheme of the present invention is mensuration systems that a kind of battery changes into gas production, this mensuration system comprises liquid container, weigh scale, the battery hanger that is used for the splendid attire harmless liquid, the battery hanger comprise bearing with its peg that is connected angularly, on this peg, be connected with the not imbibition filament that is used to hang mesuring battary; Bearing places on the pallet of weighing of described weigh scale; Sheng liquid height in the liquid container and volume are greater than the height and the volume of flexible package sealed battery to be measured, and liquid container places beyond the described pallet of weighing and is in described not imbibition filament below.Apparatus system of the present invention is used the buoyancy determinator simply and effectively, increase slightly and change, promptly form the efficient accurate battery of a cover and change into gas production mensuration system, during concrete mensuration, suspending as long as mesuring battary lain in not imbibition filament ends is immersed in the harmless liquid, and the weight suspension value that reads battery for twice can record the gas production of battery apace.
In order to increase the measure of precision of mensuration system, eliminate temperature, change in displacement for interference and the influence measured, be loaded with pure water in the liquid container of the present invention, the bottom of described liquid container places on the identical work top with the bottom of described weigh scale; Described mensuration system also comprises chronometric thermometre.Described weigh scale is that certainty of measurement is not less than the 0.01g electronic scale.
In order to increase the testing efficiency of mensuration system, so that can once carry out the mensuration of the average gas production of a plurality of batteries, battery hanger of the present invention is the double support structure, and described peg is connected between the double support, is connected with one or more not imbibition filament on the peg.
Method of testing of the present invention and apparatus system can be tested the various battery system that constitutes as the lower part and comprise: various organic nonaqueous electrolytic solutions, its solvent can be AN (acetonitrile), BC (butylene carbonic ester), DEC (diethyl carbonate), DOL (1,3 dioxolanes), DMC (dimethyl carbonate), DME (1,2 dimethoxy ethane), DPA (dipropylacetic acid ester), EA (ethylhexoate), EB (ethyl butyric acid ester), EC (vinyl carbonate), EF (ethyl ester), EMC (ethyl-methyl carbonic ester), EP (propionic acid ethyl ester), GBL (gamma-butyrolacton), MB (methylbutyrate), MF (toluic acid ester), MP (methylpropionate), MPC (carbonic acid first propyl ester), NMP (N-methyl pyrrolidone), PC (propylene carbonate), THF (oxolane), the composite electrolyte that VC (vinylene carbonate) or their binary and binary are above; Different electrolyte such as LiPF
6, LiBF
4, LiClO
4, LiAsF
6, LiCF
3SO
3Deng; The positive and negative pole material and the pole plate of different specific areas, kind and shape.
In a word, technological improvement of the present invention have be easy to implement, advantage effective, with low cost.
Below, with accompanying drawing technical solution of the present invention is described further in conjunction with specific embodiments.
[description of drawings]
Fig. 1 changes into the structural representation that gas production is measured system embodiment for battery of the present invention.
[embodiment]
As Fig. 1, be depicted as the mensuration system that a kind of battery changes into gas production, this mensuration system comprises liquid container 1, weigh scale 2, the battery hanger 3 that is used for the splendid attire harmless liquid, battery hanger 3 comprise the cantilevered bearing 31 in right angle with its peg that is connected 32 with meeting at right angles, on this peg 32, be connected with the not imbibition filament 33 that is used to hang sealed battery 4 to be measured; Bearing 31 places on the pallet 21 of weighing of weigh scale 2; Sheng liquid height in the liquid container 1 and volume are greater than the height and the volume of sealed battery 4 to be measured, and liquid container 1 places beyond the pallet 21 of weighing and is in not imbibition filament 33 belows.
Be loaded with pure water 5 in the liquid container 1 of the present invention, the bottom of the bottom of liquid container 1 and weigh scale 2 places on 6 of the identical workbench; The mensuration system also comprises the chronometric thermometre (not shown).Weigh scale 2 is an electronic scale.
Apparatus system of the present invention is used buoyancy simply and effectively and is measured system, increase slightly and change, promptly form the efficient accurate battery of a cover and change into gas production mensuration system, during concrete mensuration, suspending as long as sealed battery 4 to be measured lain in not imbibition filament ends 33 is immersed in the harmless liquid, and the weight suspension value that reads battery for twice can record the gas production of battery apace.
Take with as shown in fig. 1 and following concrete apparatus system following concrete lithium-ion battery system carried out gas production measure:
It is 25 ℃ of normal temperature that apparatus of the present invention system embodiment adopts pure water temperature, adopts the balance of high precision, and precision is 〉=0.01g to carry out following concrete test operation:
1, the lithium ion battery cell to be checked of the different systems (A, B, C, D system) of cylinder and rectangle is inserted in the different aluminum-plastic composite membrane bags.Wherein, the negative pole of different tested battery system A, B, C, D is different with anodal specific area, packed density and kind, proportioning, composition or the addition of the electrolyte of different tested battery system A, B, C, D is also different, and each battery system details is not given unnecessary details;
2, in the aluminum-plastic composite membrane bag of the battery (C, D system) of cylindrical cell (A, B system) and rectangle, inject the electrolyte of mesuring battary system behind the vacuum drying, then vacuum-pumping and sealing.
3, seal the back battery 4 still aging under 25 ℃ of dry environments.Time is 24h.
4, get the pure water 5 of the about 200g of beaker 1 splendid attire, under the normal temperature isoperibol, leave standstill, treat with the environment equality of temperature after be positioned on the workbench 6.
5, two bearings 31 with battery hanger 3 all place on the pallet 21 of weighing of weigh scale 2, make the peg 32 of level and go up the not imbibition filament 33 that connects and place the beaker top, hang on sealed battery 4 on the peg 32 and sealed battery 4 complete submergences are suspended in the pure water 5 with not imbibition filament 33, read the numerical value of weigh scale 2, be sealed battery 4 and change into preceding weight M
Before
6, take off sealed battery 4 from peg 32 and not imbibition filament 33, two bearings 31 of battery hanger 3 all place on the pallet 21 of weighing of weigh scale 2 constant, change into discharging and recharging cashier's office in a shop with the 0.1C electric current sealed battery 4 to be charged, charging stops until 4.2V.
7, will change into back battery 4 usefulness same filament 33 and hang on the peg 32, be suspended in sealed battery 4 complete submergences in the pure water 5 after, read the numerical value of weigh scale 2, be sealed battery 4 and change into weight suspension M afterwards
After
8, V=(M by formula
Before-M
After)/ρ
LiquidCalculate the gas flow V that sealed battery 4 produces, wherein ρ
LiquidFor measuring with the density of liquid under 25 ℃.
Use said method different battery system A, B, C, D are measured, tested battery system A, B, C, D gas production test result are as shown in table 1.
Table 1
| Battery system | A | B | C | D |
| Gas production (g/ ρ Liquid) | 1.772 | 2.067 | 2.316 | 2.796 |
Adopt gas production assay method of the present invention and apparatus system embodiment, also leading factor and other many Correlative Influence Factors of aerogenesis have been done further deep research and analysis, experiment confirm: gas production assay method of the present invention and apparatus system have become further investigation lithium ion battery performance, exploitation lithium electricity new product, have effectively controlled the sharp weapon of lithium electricity production technology process.
Claims (10)
1, a kind of battery changes into the gas production assay method, and this assay method comprises the steps:
A) the dried electrode core body of difform mesuring battary is inserted in the flexible package, in flexible package, inject electrolyte, vacuumize the back hermetic sealing is carried out in flexible package, obtain sealed battery to be measured;
B) described sealed battery is immersed in the harmless liquid with suspending, measures the weight suspension of this sealed battery;
C) described sealed battery is charged fully change into, obtain the battery that changes into to be measured;
D) the described battery that changes into is immersed in the harmless liquid with suspending, measures the weight suspension that this changes into battery;
E) change aerogenesis volume and/or gas generated weight that to calculate its corresponding change in volume be described flexible-packed battery according to the weight suspension of mesuring battary before and after changing into.
2, battery as claimed in claim 1 changes into the gas production assay method, it is characterized in that: in described steps A) in, after inserting in the flexible package, described electrode core body also passes through vacuum drying, in flexible package, inject electrolyte behind the vacuum drying again; Described sealed battery to be measured also was placed in 10 ℃～55 ℃ constant temperature 4～48 hours; The material of described flexible package is an aluminum-plastic composite membrane.
3, battery as claimed in claim 2 changes into the gas production assay method, it is characterized in that: in described steps A) in, the vacuum drying temperature is 50～100 ℃, vacuum degree≤-0.05Mpa, drying time is 4～48h; At described step B) in, the uniform pure water of isothermal that described harmless liquid obtains for constant temperature at normal temperatures.
4, battery as claimed in claim 1 changes into the gas production assay method, it is characterized in that: at described step B), D), E) in, the certainty of measurement of described weight is not less than 0.01g.
5, battery as claimed in claim 1 changes into the gas production assay method, it is characterized in that: at described step C) in, it is to fill speed with trickle charge or tiny stream described sealed battery is charged to change into that described charging changes into, till this battery all told is filled or suitably overcharges.
6, battery as claimed in claim 1 changes into the gas production assay method, it is characterized in that: at described step D) and described step B) in, described harmless liquid is the uniform pure water of isothermal that constant temperature obtains under identical normal temperature; The thermostat temperature of described harmless liquid is equal to the thermostat temperature of mesuring battary.
7, battery as claimed in claim 1 changes into the gas production assay method, it is characterized in that: at described step C) in, after fully charging changed into, the described battery that changes into to be measured also was placed in 10 ℃～55 ℃ constant temperature 4～48 hours, and then entered described step D).
8, a kind of mensuration system that changes into the gas production assay method as the described battery of one of claim 1～7 that adopts, it is characterized in that: described mensuration system comprises liquid container, weigh scale, the battery hanger that is used for the splendid attire harmless liquid, described battery hanger comprise bearing with its peg that is connected angularly, on this peg, be connected with the not imbibition filament that is used to hang mesuring battary; Described bearing places on the pallet of weighing of described weigh scale; Sheng liquid height in the described liquid container and volume are greater than the height and the volume of flexible package sealed battery to be measured, and described liquid container places beyond the described pallet of weighing and is in described not imbibition filament below.
9, battery as claimed in claim 8 changes into the mensuration system of gas production, it is characterized in that: be loaded with pure water in the described liquid container, the bottom of described liquid container places on the identical work top with the bottom of described weigh scale; Described mensuration system also comprises chronometric thermometre.
10, battery as claimed in claim 8 changes into the mensuration system of gas production, it is characterized in that: described weigh scale is the electronic scale that certainty of measurement is not less than 0.01g; Described battery hanger is the double support structure, and described peg is connected between the double support, is connected with one or more not imbibition filament on the described peg.
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|---|---|---|---|
| CNB2004100281213A CN100442590C (en) | 2004-07-19 | 2004-07-19 | Method for measuring gas production rate of battery formation and system therefor |
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| CNB2004100281213A CN100442590C (en) | 2004-07-19 | 2004-07-19 | Method for measuring gas production rate of battery formation and system therefor |
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| CN100442590C true CN100442590C (en) | 2008-12-10 |
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