CN110501382A - A kind of lithium ion battery heat production-measuring device and method associated with production gas - Google Patents
A kind of lithium ion battery heat production-measuring device and method associated with production gas Download PDFInfo
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- CN110501382A CN110501382A CN201910791191.0A CN201910791191A CN110501382A CN 110501382 A CN110501382 A CN 110501382A CN 201910791191 A CN201910791191 A CN 201910791191A CN 110501382 A CN110501382 A CN 110501382A
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- G—PHYSICS
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- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K17/00—Measuring quantity of heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The present invention provides a kind of lithium ion battery heat production-measuring device and methods associated with production gas, and the measuring device includes heat production measuring device, gas collector and gas analyzing apparatus；The method includes carrying out charge and discharge electric treatment to lithium ion battery；Then it disassembled, separated and is cleaned under atmosphere of inert gases；The measurement of quantity of heat production is carried out to any one after above-mentioned processing in gained anode, cathode, diaphragm and aluminum plastic film again; or by it is therein any one or more with the measurement that carries out quantity of heat production after electrolyte combination again; the measurement of the quantity of heat production carries out under a shielding gas, and method therefor is differential scanning calorimetry；Generated tail gas in quantity of heat production measurement process is collected, carries out the analysis of gas componant and content after cooling with gas chromatography-mass spectrography.Measurement method provided by the invention realizes while quantity of heat production, aerogenic composition and the gas content between lithium ion battery electrode material and each component is fast and accurately measured and being analyzed.
Description
Technical field
The present invention relates to technical field of lithium ion, in particular to survey associated with a kind of lithium ion battery heat production-production gas
Measure device and method.
Background technique
The increasingly increase of the people of requirement with to(for) the energy density and power density of lithium ion battery, lithium ion battery
Safety also increasingly attract people's attention.Under the abuse conditions such as lithium ion battery especially overcharges in charge and discharge, over-discharge
Heat production situation be understanding and analysis lithium ion battery safety performance a big important indicator.To each group of inside lithium ion cell
The heat production situation analysis divided can then explore various pieces for the contribution of total heat production, to be directed to the biggish part of heat production accounting
It optimizes.
In addition to this, lithium ion battery during heat production also can along with the generation of gas, the generation of gas for
The performance of battery has tremendous influence, and the generation of gas is the chemical reaction between each component of the internal resistance of cell and generates,
Therefore facilitate the reaction and heat production situation between each component of people's electrolytic cell for the analysis of gas.
Currently, people are separate detections for the measurement of heat production and gas, gas is had ignored while measuring heat production
The analysis of body, and the analysis of gas is not also taken into account heat production, both inter-related be divided is come.
In conclusion the heat production of battery with produce gas be it is closely bound up, interactional, it is necessory to which the two is combined
Measurement and analysis.
Summary of the invention
The present invention provides a kind of lithium ion battery heat production-measuring device and method associated with production gas, its purpose is to
It realizes and heat production is carried out to lithium ion battery each component and is detected and analysis while producing gas.
In order to achieve the above object, the invention provides the following technical scheme:
A kind of lithium ion battery heat production-measuring device associated with production gas, the measuring device includes heat production measuring device, gas
Body collection device and gas analyzing apparatus；One end of the heat production measuring device and gas collector is connected by pipeline, institute
The other end for stating gas collector is connect with gas analyzing apparatus by pipeline；The temperature test model of the heat production measuring device
Enclose is 25~400 DEG C；The volume of the gas collector is 1L；The maximum allowable operating temperature (M.A.O.T.) of the gas analyzing apparatus is 400
DEG C, lowest detection is limited to 1ppm, data acquiring frequency 300Hz.
The present invention also provides a kind of lithium ion battery heat production-measurement methods associated with production gas, include the following steps:
(1) charge and discharge electric treatment is carried out to lithium ion battery；
(2) to charge and discharge, treated that battery is disassembled, separated and cleaned under atmosphere of inert gases, obtain anode,
Cathode, diaphragm and aluminum plastic film；
(3) measurement of quantity of heat production is carried out to any one in anode obtained by step (2), cathode, diaphragm and aluminum plastic film, or
By it is therein any one or more with the measurement that carries out quantity of heat production after electrolyte combination again, the measurement of the quantity of heat production is being protected
It is carried out under gas, method therefor is differential scanning calorimetry；
Wherein, temperature test range is 25-400 DEG C；Heating rate is 5K/min；
(4) generated tail gas in the measurement process of quantity of heat production is collected, carries out gas with gas chromatography-mass spectrography after cooling
The analysis of body ingredient and content.
Preferably, atmosphere of inert gases described in step (2) is nitrogen or argon atmosphere.
Preferably, dismantling described in step (2) carries out in glove box, and the glove box water oxygen pressure is less than 0.1ppm.
It is highly preferred that cleaning described in step (2) is specially with dimethyl carbonate to anode, cathode, diaphragm and aluminum plastic film
It is cleaned, removes remaining electrolyte.
It is highly preferred that further including the placement 12h or more in glove box after the completion of cleaning described in step (2), to carbonic acid two
Methyl esters volatilizees completely.
Preferably, protective gas described in step (3) is argon gas or nitrogen；The protective gas flow velocity is 10mL/min.
Preferably, when carrying out the analysis of gas componant and content in step (4) with gas chromatography-mass spectrography, thermal conductivity is examined
It surveys device detection limit and is set as 0.1%, the range of linearity is set as 106, data acquiring frequency is set as 300Hz；Flame ionic detector detection
Limit is set as being less than 1.4pgC/s, and the range of linearity is set as 106, data acquiring frequency is set as 300Hz.
Above scheme of the invention have it is following the utility model has the advantages that
Measuring device provided by the invention realizes while to the heat production between lithium ion battery electrode material and each component
Amount, aerogenic composition and gas content are measured and are analyzed, and can effectively promote the deeper for lithium ion battery security
Secondary analysis and understanding.
Method provided by the invention can be gentle to the quantity of heat production between lithium ion battery electrode material and each component simultaneously
Body ingredient is fast and accurately measured with content, can adapt to the lithium-ion electric of different material systems, different structure designs
Pond has many advantages, such as to have a wide range of application, efficiently and accurately.
Detailed description of the invention
Fig. 1 shows measuring device schematic diagram provided by the invention；
Fig. 2 shows measuring method flow charts provided by the invention；
Fig. 3 is the heat production flow diagram of lithium cobaltate cathode material in the embodiment of the present invention 1；
Fig. 4 is the heat production flow diagram that lithium cobaltate cathode material is overcharged in the embodiment of the present invention 2.
Detailed description of the invention: 1, heat production measuring device；2, gas collector；3, gas analyzing apparatus；4, test cabinet；5, tail gas
Mouthful；6, air inlet.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with specific implementation
Example is described in detail.
As shown in Figure 1, lithium ion battery heat production-measuring device associated with production gas provided by the invention includes heat production measurement dress
Set 1, gas collector 2 and gas analyzing apparatus 3；The heat production measuring device is used to carry out detected materials the survey of quantity of heat production
Amount inside sets sensing chamber 4, tail gas mouth 5 is equipped with above sensing chamber, and one end of pipeline is connected on tail gas mouth, and the other end of pipeline connects
Gas collector 2 is connect, the gas collector 2 is used to collect the tail gas generated in the measurement process of quantity of heat production, and tail gas is received
On acquisition means 2 another pipeline connection gas analyzing apparatus air inlet 6, the gas analyzing apparatus be used for above-mentioned tail gas into
The analysis of row gas componant and content.
The temperature test range of the heat production measuring device 1 is 25~400 DEG C；The volume of the gas collector 2 is
1L；The maximum allowable operating temperature (M.A.O.T.) of the gas analyzing apparatus 3 is 400 DEG C, and lowest detection is limited to 1ppm, and data acquiring frequency is
300Hz。
Lithium ion battery heat production-measurement method associated with production gas provided by the invention includes the following steps:
S1, charge and discharge electric treatment；
A lithium ion battery selected first, is then connected to charge-discharge test cabinet for lithium ion battery and carries out charge and discharge, will
Battery charge or discharge is to required state, including overcharges, over-discharge, circulation, the conditions such as storage；
S2, dismantling, separation and cleaning treatment；
Specifically, the battery for having reached required state is disassembled, anode, cathode, diaphragm, aluminum plastic film are separated；
Preferably, dismantling can carry out in glove box, and water oxygen pressure is kept to be less than 0.1ppm, and atmosphere is that argon gas protects atmosphere, such
Inert atmosphere can prevent lithium ion battery electrode material and component ingress of air and chemical environment changes, and test is caused to be tied
Fruit generates error.Preferably, it after anode, cathode, diaphragm, aluminum plastic film are isolated in dismantling, is carried out using dimethyl carbonate clear
It washes, is placed at least 12 hours in glove box again after the completion of cleaning, dimethyl carbonate can effectively dissolve electrolyte and easily
Volatilization, can remove electrolyte, prevent electrolyte from having an impact to subsequent calorimetric process.
S3, heat production measurement；
It, can be with specifically, once purged anode, cathode, diaphragm, aluminum plastic film to be carried out to the measurement of quantity of heat production respectively
The quantity of heat production in the case where anode, cathode, diaphragm, aluminum plastic film individualism is measured respectively, can also measure anode and electrolyte
It coexists, the various coexisting states such as cathode and coexistent electrolyte solution, positive electrode and negative electrode coexist, positive electrode and negative electrode and electrolyte three coexist
Under quantity of heat production；Preferably, 25-400 DEG C of temperature test range, heating rate 5K/min, protection gas are argon gas and its stream
Speed should be 10mL/min.
S4, gas componant and content analysis；
The gas generated in heat production measurement process is collected, in heat production measurement process since correspondingization has occurred
It learns reaction and generates gas, by the way that subsequent gas analysis will can be carried out after gas collection and cooling；Preferably, device volume
For 1L, and flow velocity needed for adjustable gas analyzing apparatus, and keep protective atmosphere.Gas will be collected into gas collector
The analysis for carrying out gas componant and content, by the analysis to gas can effectively analyze generation chemical reaction and its
Contribution for quantity of heat production；Preferably, maximum allowable operating temperature (M.A.O.T.) is 400 DEG C, and lowest detection is limited to 1ppm, data acquiring frequency
300Hz。
Embodiment 1
A battery is chosen to be disassembled: choose 493446 type soft bag lithium ionic cells, design capacity 1000mAh, lithium from
Sub- cell positive material is cobalt acid lithium, and negative electrode material is graphite, carries out perseverance after this lithium ion battery is melted into 0.1C
Constant-voltage charge is flowed to 4.2V, cut-off current 0.01C, is placed 2 hours after charging complete.
Lithium ion battery is put into glove box and is disassembled, glove box water oxygen pressure is less than 0.1ppm, and recycling is completed in dismantling
Positive electrode cleans positive electrode using dimethyl carbonate, places 12 hours after the completion of cleaning, after its completely volatilization
It takes fritter to be put into closed crucible, and electrolyte is added dropwise, the mass ratio of positive electrode and electrolyte is 5:1, carries out differential afterwards
Calorimeter test is scanned, 25-400 DEG C of temperature test range, heating rate 5K/min, protection gas is nitrogen.Test result is such as
Shown in Fig. 3.
Can be seen that positive electrode from the analysis of Fig. 3, mainly there are two the presence at heat production peak, for cobalt acid lithium,
First peak is located at 212.6 DEG C, and hot-fluid 0.2864mW/mg, second peak is located at 264.9 DEG C, hot-fluid 5.64mW/mg, produces
Heat is 535.7J/g, and the presence at the two peaks is that decomposition due to anode and solvent with positive react generation respectively, with
For EC, reaction is respectively:
LixCoO2→x LiCoO2+(1-x)/3Co3O4+(1-x)/3O2 (1)
Li0.5CoO2+0.1C3H4O3→0.5LiCoO2+0.5CoO+0.3CO2+0.2H2O (2)
It collects gas componant: collecting the tail gas after the completion of differential scanning calorimeter test, include protection gas nitrogen in tail gas
And the gas that electrode material is generated due to chemical reaction during the test, gas analysis is injected into after collecting cooling
Instrument.The analysis of gas componant and content, thermal conductivity detector (TCD) detection limit 0.1%, linear model are carried out using gas chromatography-mass spectrography
Enclose 106, data acquiring frequency 300Hz, flame ionic detector detection limit < 1.4pgC/s, the range of linearity 106, data acquiring frequency
300Hz.Test result is as shown in table 1.
From the analysis of table 1 as can be seen that the ingredient for the gas that the reaction of this lithium ion battery electrode material generates is mainly
C2H4、C2H6、CH4、C3H8、H2、CO2、O2Deng, wherein nitrogen be protective gas composition, analyze result when ignored, it can be seen that
Mainly by alkane and CO2Composition, this is all to be mainly derived from electrolyte to react with positive electrode and the decomposition of positive electrode
Reaction and generate.
Lithium cobaltate cathode material produces gas analysis in 1 embodiment 1 of table
Embodiment 2
A battery is chosen to be disassembled: choose 493446 type soft bag lithium ionic cells, design capacity 1000mAh, lithium from
Sub- cell positive material is cobalt acid lithium, and negative electrode material is graphite, carries out perseverance after this lithium ion battery is melted into 0.1C
Constant-voltage charge is flowed to 4.2V, cut-off current 0.01C, is placed 2 hours after charging complete；By battery with 0.05C after the completion of placement
Electric current overcharge 16 hours, test carried out in safety box, prevent thermal runaway.
Lithium ion battery after the completion of test is put into glove box and is disassembled, glove box water oxygen pressure is less than 0.1ppm,
Recycling positive electrode is completed in dismantling, and positive electrode is cleaned using dimethyl carbonate, is placed 12 hours after the completion of cleaning, to
It takes fritter to be put into closed crucible after volatilizing completely, and electrolyte is added dropwise, and the mass ratio of positive electrode and electrolyte is 5:
1, rear to carry out differential scanning calorimeter test, 25-400 DEG C of temperature test range, heating rate 5K/min, protection gas is nitrogen
Gas.Test results are shown in figure 4.
Can be seen that positive electrode from the analysis of Fig. 4, mainly there are two the presence at heat production peak, for cobalt acid lithium,
First peak is located at 195.2 DEG C, and hot-fluid 33.61J/g, second is located at 240.3 DEG C, hot-fluid 15.07mW/mg, quantity of heat production
It overcharges rear positive electrode quantity of heat production compared with the positive electrode heat production of the 4.2V in embodiment 1 for 773.7J/g and obviously increases,
Peak temperature also have it is biggish in advance, illustrate that its activity is stronger, heat production is more violent.The presence at the two peaks is due to just respectively
The decomposition of pole and solvent react generations with anode, by taking EC as an example, react and may be respectively:
LixCoO2→x LiCoO2+(1-x)/3Co3O4+(1-x)/3O2 (1)
Li0.5CoO2+0.1C3H4O3→0.5LiCoO2+0.5CoO+0.3CO2+0.2H2O (2)
It collects gas componant: collecting the tail gas after the completion of differential scanning calorimeter test, include protection gas nitrogen in tail gas
And the gas that electrode material is generated due to chemical reaction during the test, gas analysis is injected into after collecting cooling
Instrument.The analysis of gas componant and content, thermal conductivity detector (TCD) detection limit 0.1%, linear model are carried out using gas chromatography-mass spectrography
Enclose 106, data acquiring frequency 300Hz, flame ionic detector detection limit < 1.4pgC/s, the range of linearity 106, data acquiring frequency
300Hz.Test result is as shown in table 2.
From the analysis of table 2 as can be seen that the ingredient for the gas that the reaction of this lithium ion battery electrode material generates is mainly
C2H4、C2H6、CH4、C3H8、H2、CO2、O2Deng, wherein the content of CO2 accounts for the overwhelming majority, has reached 70%, illustrate electrolyte and electricity
The reaction of pole material is more violent；Remaining is mainly made of alkane, this is all that the organic matter being mainly derived from electrolyte occurs
Redox reaction and generate.
Lithium cobaltate cathode material is overcharged in 2 embodiment 2 of table produces gas analysis
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (8)
1. a kind of lithium ion battery heat production-measuring device associated with production gas, which is characterized in that the measuring device includes that heat production is surveyed
Measure device, gas collector and gas analyzing apparatus；One end of the heat production measuring device and gas collector passes through pipe
Road connection, the other end of the gas collector are connect with gas analyzing apparatus by pipeline；The heat production measuring device
Temperature test range is 25~400 DEG C；The volume of the gas collector is 1L；The highest of the gas analyzing apparatus operates
Temperature is 400 DEG C, and lowest detection is limited to 1ppm, data acquiring frequency 300Hz.
2. a kind of lithium ion battery heat production-measurement method associated with production gas, which comprises the steps of:
(1) charge and discharge electric treatment is carried out to lithium ion battery；
(2) to charge and discharge, treated that battery is disassembled, separated and cleaned under atmosphere of inert gases, obtain anode, cathode,
Diaphragm and aluminum plastic film；
(3) to the measurement of any one progress quantity of heat production in anode, cathode obtained by step (2), diaphragm and aluminum plastic film, or by its
In any one or more and the measurement for carrying out quantity of heat production after electrolyte combination again, the measurement of the quantity of heat production is in protective gas
Lower progress, method therefor are differential scanning calorimetry；
Wherein, temperature test range is 25-400 DEG C；Heating rate is 5K/min；
(4) collect generated tail gas in the measurement process of quantity of heat production, it is cooling after with gas chromatography-mass spectrography carry out gas at
Divide the analysis with content.
3. measurement method according to claim 2, which is characterized in that atmosphere of inert gases described in step (2) be nitrogen or
Argon atmosphere.
4. measurement method according to claim 2, which is characterized in that dismantling described in step (2) carries out in glove box, institute
It states glove box water oxygen pressure and is less than 0.1ppm.
5. measurement method according to claim 4, which is characterized in that cleaning described in step (2) is specially to use carbonic acid diformazan
Ester cleans anode, cathode, diaphragm and aluminum plastic film, removes remaining electrolyte.
6. measurement method according to claim 5, which is characterized in that further include in hand after the completion of cleaning described in step (2)
12h or more is placed in casing, is volatilized completely to dimethyl carbonate.
7. measurement method according to claim 2, which is characterized in that protective gas described in step (3) is argon gas or nitrogen；
The protective gas flow velocity is 10mL/min.
8. measurement method according to claim 2, which is characterized in that carry out gas with gas chromatography-mass spectrography in step (4)
When the analysis of body ingredient and content, thermal conductivity detector (TCD) detection limit is set as 0.1%, and the range of linearity is set as 106, data acquiring frequency sets
For 300Hz；Flame ionic detector detection limit is set as being less than 1.4pgC/s, and the range of linearity is set as 106, data acquiring frequency is set as
300Hz。
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| CN112858496A (en) * | 2020-12-28 | 2021-05-28 | 国联汽车动力电池研究院有限责任公司 | Device and method for detecting thermal runaway gas production of lithium ion battery |
| CN113340967A (en) * | 2021-05-19 | 2021-09-03 | 上海大学 | Device and method for analyzing gas production components of battery through electrochemistry-gas chromatography-mass spectrometry |
| CN113484780A (en) * | 2021-06-02 | 2021-10-08 | 苏州领湃新能源科技有限公司 | Method for testing short-circuit resistance in soft package battery |
| CN113671392A (en) * | 2021-06-30 | 2021-11-19 | 国联汽车动力电池研究院有限责任公司 | Method for measuring over-charging safety boundary of battery |
| CN113671392B (en) * | 2021-06-30 | 2024-07-02 | 国联汽车动力电池研究院有限责任公司 | Method for measuring overcharge safety boundary of battery |
| DE102023105675A1 (en) | 2022-12-29 | 2024-07-04 | GM Global Technology Operations LLC | Systems and methods for performing differential scanning calorimetry (DCS) measurements on battery cells |
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