CN108680865B - Method for detecting circulation performance of electrolyte for lithium ion secondary battery - Google Patents
Method for detecting circulation performance of electrolyte for lithium ion secondary battery Download PDFInfo
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Abstract
The invention discloses a method for detecting the circulation performance of electrolyte for a lithium ion secondary battery, which comprises the following steps: the first step is as follows: respectively immersing a plurality of battery pole piece samples made of the same material into different electrolytes; the second step is that: inspecting the initial weight of the soaked battery pole piece samples, and then heating; the third step: for each battery pole piece sample, detecting the corresponding weight of each battery pole piece sample at intervals of preset time in real time; the fourth step: calculating the volatilization rates of different corresponding electrolytes of the multiple battery pole piece samples under different heating times; the fifth step: and judging the cycle performance of the battery finished product finally prepared by different electrolytes according to the volatilization rates of the different electrolytes corresponding to the multiple battery pole piece samples under different heating times. The invention can rapidly and reliably detect the cycle performance of different lithium ion batteries prepared by different electrolytes, and obviously improves the battery detection efficiency.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a method for detecting the circulation performance of an electrolyte for a lithium ion secondary battery.
Background
At present, lithium ion batteries have the advantages of high specific energy, many recycling times, long storage time and the like, are widely applied to portable electronic equipment such as mobile phones, digital video cameras and portable computers, and are also widely applied to large and medium-sized electric equipment such as electric automobiles, electric bicycles, electric tools and the like, so that the performance requirements on the lithium ion batteries are higher and higher.
For lithium ion batteries, the cycle life is an important index for measuring the performance of the lithium ion battery and the raw materials in the lithium ion battery, and is also an index which is relatively concerned by battery manufacturers. Therefore, the cycle performance of the battery is evaluated in a short time, and the method has important significance. At present, for different lithium ion batteries prepared from different electrolytes, a method for detecting the cycle performance of the lithium ion battery generally needs to detect the cycle performance of the battery after a finished lithium ion battery product is prepared, the cycle is long, multiple charging and discharging are needed, and more energy and time are consumed, so that the time for putting the battery into mass production is prolonged.
Therefore, there is an urgent need to develop a method that can rapidly and reliably detect the cycle performance of different lithium ion batteries prepared from different electrolytes, significantly save the detection time, improve the battery detection efficiency, and further promote the mass production and application of the lithium ion batteries.
Disclosure of Invention
In view of the above, the present invention provides a method for detecting the cycle performance of an electrolyte for a lithium ion secondary battery, which can quickly and reliably detect the cycle performance of different lithium ion batteries prepared from different electrolytes, significantly save the detection time, improve the battery detection efficiency, further promote the mass production and application of the lithium ion batteries, facilitate the improvement of the market application prospect of battery manufacturers, and have great production practice significance.
Therefore, the invention provides a method for detecting the circulation performance of an electrolyte for a lithium ion secondary battery, which comprises the following steps:
the first step is as follows: respectively immersing a plurality of battery pole piece samples made of the same material into different electrolytes, and standing for a preset time length to enable the plurality of battery pole piece samples to be completely immersed;
the second step is that: detecting the initial weight of the soaked battery pole piece samples in real time, and then heating the battery pole piece samples;
the third step: in the heating process, for each battery pole piece sample, detecting the corresponding weight of the battery pole piece sample at intervals of preset time in real time until the weight of the battery pole piece sample does not change any more, and recording the weight of the corresponding battery pole piece sample when the weight does not change any more;
the fourth step: calculating the volatilization rates of different corresponding electrolytes of the multiple battery pole piece samples under different heating times;
the fifth step: and judging the cycle performance of the battery finished product finally prepared by the electrolyte respectively immersed in the plurality of battery pole piece samples according to the corresponding different electrolytic liquid volatilization rates of the plurality of battery pole piece samples under different heating times and a judgment rule that the volatilization rate of the electrolyte is in inverse proportion to the cycle performance of the battery finished product prepared by the electrolyte immersed in the battery pole piece samples.
In the first step, the size of the plurality of battery pole piece samples is the same.
Wherein, in the first step, the preset time length of the standing is 30 minutes.
Wherein, in the second step, the plurality of battery pole piece samples are heated through an incubator or a heating balance.
Wherein, in the third step, the preset period of time is 10 seconds.
Wherein the fifth step specifically comprises: according to the electrolyte volatilization rates of the multiple battery pole piece samples under different heating times, firstly, the heating time is taken as an X axis, the volatilization rates of different electrolytes corresponding to the different battery pole piece samples are taken as a Y axis, curves of the volatilization rates of the different electrolytes changing along with the heating time are obtained, and then, according to a judgment rule that the volatilization rates of the electrolytes are in inverse proportion to the cycle performance of a battery finished product prepared from the electrolytes, the cycle performance of the battery finished product finally prepared from the different electrolytes in which the multiple battery pole piece samples are respectively immersed is judged.
Compared with the prior art, the method for detecting the circulation performance of the electrolyte for the lithium ion secondary battery can quickly and reliably detect the circulation performance of different lithium ion batteries prepared from different electrolytes, obviously saves the detection time, improves the battery detection efficiency, further promotes the batch production and application of the lithium ion batteries, is beneficial to improving the market application prospect of battery manufacturers, and has great production practice significance.
Drawings
FIG. 1 is a flowchart of a method for detecting cycle performance of an electrolyte for a lithium ion secondary battery according to the present invention;
FIG. 2 is a graph showing the evaporation rate of electrolyte obtained according to the variation of heating time for two samples of battery electrode plates immersed in two different electrolytes in the example;
fig. 3 is a schematic diagram of cycle performance curves obtained after a plurality of actual charge and discharge cycles of a lithium ion battery prepared by two battery pole piece samples immersed with two different electrolytes in an example.
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, the following detailed description of the present invention is provided in conjunction with the accompanying drawings and embodiments.
Referring to fig. 1, the invention provides a method for detecting the cycle performance of an electrolyte for a lithium ion secondary battery, which detects the cycle performance of a prepared battery by means of the volatilization speed of the electrolyte in a battery pole piece soaked with the electrolyte, and specifically comprises the following steps:
the first step is as follows: for a plurality of battery pole piece samples made of the same material, respectively immersing the battery pole piece samples into different electrolytes (namely, electrolytes containing different components), and standing for a preset time length to enable the battery pole piece samples to be completely soaked;
the second step is that: detecting the initial weight of the soaked battery pole piece samples in real time, and then heating the battery pole piece samples;
the third step: in the heating process, for each battery pole piece sample, detecting the corresponding weight of the battery pole piece sample at intervals of preset time in real time until the weight of the battery pole piece sample does not change any more, and recording the weight of the corresponding battery pole piece sample when the weight does not change any more;
the fourth step: calculating the volatilization rates of different corresponding electrolytes of the battery pole piece samples under different heating times;
the fifth step: and according to the volatilization rates of different corresponding electrolytes of the multiple battery pole piece samples under different heating times and a judgment rule that the volatilization rate of the electrolytes is in inverse proportion to the cycle performance of the battery finished product prepared from the electrolytes, judging the cycle performance of the battery finished product finally prepared from the different electrolytes in which the multiple battery pole piece samples are respectively immersed.
In the first step, specifically, the size of the plurality of battery pole piece samples is the same.
In the invention, the battery pole piece refers to a lithium battery raw material which is prepared by mixing a positive active material and a negative active material with one or more of a conductive agent, a binder and a dispersing agent to prepare a slurry and coating the slurry on a current collector made of metal.
In the first step, specifically, the preset time period of the standing may be 30min (minutes).
In the second step, specifically, the plurality of battery pole piece samples can be heated by an incubator or a heating balance, and other methods.
In the third step, specifically, the preset time period may be 10 seconds, and of course, other time periods may be used according to the needs of the user.
In the fourth step, in terms of specific implementation, in order to calculate the corresponding electrolyte volatilization rate of each battery pole piece sample under different heating times, a specific calculation formula is as follows:
the electrolyte volatilization rate V ═ m of each battery pole piece sample0-mn)/(m0-mf)；
Wherein m is0The initial weight of the battery pole piece sample is obtained;
mnrecording the weight of the battery pole piece sample after n preset time intervals (n is the number of times for measuring the weight of the battery pole piece sample, and can be 1,2,3,4 … in nature); the preset time period can be 10 seconds;
mfthe weight was heated until the weight of the cell pole piece sample no longer changed.
In the fifth step, it should be noted that the cycle performance of the lithium ion battery prepared from the battery pole piece sample with the faster volatilization speed of the electrolyte is poorer.
For the present invention, the fifth step specifically is: according to the volatilization rates of different electrolytes corresponding to the multiple battery pole piece samples under different heating times, firstly, the heating time is taken as an X axis, the volatilization rates of different electrolytes corresponding to the different battery pole piece samples are taken as a Y axis, a curve of the volatilization rates of different electrolytes (namely, different electrolytes in which the different battery pole piece samples are respectively immersed) changing along with the heating time is obtained, and then, according to a judgment rule that the volatilization rates of the electrolytes and the cycle performance of a battery finished product prepared by the electrolytes are in inverse proportion, the cycle performance of the battery finished product finally prepared by the different electrolytes in which the multiple battery pole piece samples are respectively immersed is judged.
It is noted that the scope of applicability for the present invention includes, but is not limited to, square, round, polymer and flexible package batteries.
Therefore, according to the technical scheme, compared with the prior art, the invention has the advantages that a finished battery product is not required to be manufactured, the battery is not required to be charged and discharged, the cycle performance of the electrolyte can be detected only by measuring and comparing the volatilization rate of the electrolyte in the pole piece, and the energy consumption, the manufacturing time and the material cost of charging and discharging are obviously reduced.
In order to more clearly understand the technical solution of the present invention, the following description is given with reference to specific embodiments.
Firstly, a battery pole piece sample made of the same material is taken, so that the size of the pole piece sample is 3cm by 3 cm. Then, the two samples are respectively immersed into two different electrolytes, and the two samples are respectively marked as a battery pole piece sample A and a pole piece sample B, and the sample is kept stand for 30 min. The immersion amount of the electrolyte is recommended to be controlled to be 5 mg-500 mg, so that volatilization is convenient to observe and measurement is easy;
the battery pole piece sample a may include, by mass, 95% of lithium iron phosphate LFP, 2% of polyvinylidene fluoride PVD, and 3% of carbon nanotube CNT; the battery pole piece sample B may include 96% lithium iron phosphate LFP, 2% polyvinylidene fluoride PVD, and 2% carbon nanotube CNT by mass percent.
The electrolyte corresponding to the battery pole piece sample a may contain, by mass, 40% of ethylene carbonate EC, 38.5% of ethyl methyl carbonate EMC, 5% of propylene carbonate PC, and 13.5% of lithium hexafluorophosphate LiPF62% of vinylene carbonate VC and 1% of propylene sulfite PS.
The electrolyte corresponding to the battery pole piece sample B may include, by mass, 41.75% of ethylene carbonate EC, 41.75% of ethyl methyl carbonate EMC, and 13.5% of lithium hexafluorophosphate LiPF62% of vinylene carbonate VC and 1% of propylene sulfite PS.
Next, the temperature of the heating balance was set to 80 ℃. Placing the soaked pole piece in a measuring container, placing the measuring container on a preheated heating balance, and recording the initial weight m of the pole piece after the pole piece is completely soaked in the electrolyteA0And mB0；
The weight of cell pole piece samples a and B was then recorded every 10 seconds. The weight of the battery pole piece sample A is mA1、mA2、mA3…mAn. Weight of battery plate sample B is mB1、mB2、mB3…mBn。
Then, calculating the electrolyte volatilization rates V of the battery pole piece samples A and B at different timeA1、VA2、VA3…VAnAnd VB1、VB2、VB3…VBn。
Then, by setting the heating time to the X-axis, the volatilization rate was set to the Y-axis. Drawing a curve of the electrolyte volatilization rate V of the battery pole piece samples A and B along with the change of the heating time t according to the measurement data;
as shown in the curve of fig. 2, the electrolyte volatilization rate of the battery pole piece sample B is high, and as seen from the comparison graph (fig. 3) of the circulation effect of the battery manufactured next, the circulation performance of the battery pole piece sample B is relatively poor, and the actual test result is consistent with the judgment result of the present invention.
Similarly, it should be noted that the detection method of the present invention can also be applied to a polymer lithium ion battery, and the specific detection process is similar to that of the above lithium ion battery, and is not described herein again.
In summary, compared with the prior art, the method for detecting the circulation performance of the electrolyte for the lithium ion secondary battery provided by the invention can quickly and reliably detect the circulation performance of different lithium ion batteries prepared from different electrolytes, obviously save the detection time, improve the battery detection efficiency, further promote the mass production and application of the lithium ion batteries, is beneficial to improving the market application prospect of battery manufacturers, and has great production practice significance.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A method for detecting the circulation performance of an electrolyte for a lithium ion secondary battery is characterized by comprising the following steps:
the first step is as follows: respectively immersing a plurality of battery pole piece samples made of the same material into different electrolytes, and standing for a preset time length to enable the plurality of battery pole piece samples to be completely immersed;
the second step is that: detecting the initial weight of the soaked battery pole piece samples in real time, and then heating the battery pole piece samples;
the third step: in the heating process, for each battery pole piece sample, detecting the corresponding weight of the battery pole piece sample at intervals of preset time in real time until the weight of the battery pole piece sample does not change any more, and recording the weight of the corresponding battery pole piece sample when the weight does not change any more;
the fourth step: calculating the corresponding electrolyte volatilization rates of the multiple battery pole piece samples under different heating times;
the fifth step: according to the volatilization rates of different corresponding electrolytes of the multiple battery pole piece samples under different heating times and according to a judgment rule that the volatilization rate of the electrolytes is in inverse proportion to the cycle performance of the battery finished product prepared from the electrolytes, the cycle performance of the battery finished product finally prepared from the different electrolytes in which the multiple battery pole piece samples are respectively immersed is judged;
the fifth step is specifically as follows: according to the volatilization rates of different electrolytes corresponding to the multiple battery pole piece samples in different heating times, firstly, taking the heating time as an X axis and the volatilization rates of different electrolytes corresponding to the different battery pole piece samples as a Y axis, obtaining curves of the volatilization rates of the different electrolytes changing along with the heating time, and then, according to a judgment rule that the volatilization rates of the electrolytes are in inverse proportion to the cycle performance of a battery finished product prepared from the electrolytes, judging the cycle performance of the battery finished product finally prepared from the different electrolytes in which the multiple battery pole piece samples are respectively immersed.
2. The detection method according to claim 1, wherein in the first step, the plurality of battery pole piece samples are the same size.
3. The detection method according to claim 1, wherein in the first step, the preset length of time for the standing is 30 minutes.
4. The method of claim 1, wherein in the second step, the plurality of samples of battery pole pieces are heated by an incubator or a heating balance.
5. The detection method according to claim 1, wherein in the third step, the predetermined period of time is 10 seconds.
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