CN109921155B - Formation method of multi-section capacitor battery - Google Patents
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- CN109921155B CN109921155B CN201910068482.7A CN201910068482A CN109921155B CN 109921155 B CN109921155 B CN 109921155B CN 201910068482 A CN201910068482 A CN 201910068482A CN 109921155 B CN109921155 B CN 109921155B
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- 239000003990 capacitor Substances 0.000 title claims abstract description 107
- 238000000034 method Methods 0.000 title claims abstract description 20
- 230000015572 biosynthetic process Effects 0.000 title abstract description 11
- 238000007600 charging Methods 0.000 claims abstract description 35
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 230000005684 electric field Effects 0.000 claims description 12
- 230000008859 change Effects 0.000 claims description 7
- 238000012360 testing method Methods 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 13
- 230000008569 process Effects 0.000 description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010280 constant potential charging Methods 0.000 description 1
- 238000010277 constant-current charging Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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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
Abstract
The invention discloses a formation method of a multi-section capacitor battery, which comprises the following steps: step one, firstly, under the condition of normal temperature and normal pressure, I is used1The voltage charged by the current constant current to the capacitor battery is V1Then with I2The voltage charged by the current constant current to the capacitor battery is V2Wherein, I1<I2，V1<V2(ii) a Step two, with I3The voltage charged by the current constant current to the capacitor battery is V3Then the power is cut off and the mixture is kept stand, wherein, I1<I3<I2，V2<V3(ii) a Step three, with I4The voltage charged by the current constant current to the capacitor battery is V4Then by V4Charging at constant voltage, and standing after power failure, wherein I2<I4，V3<V4，V4The voltage is limited for the capacitor battery. The method for forming the multi-section capacitor battery can obviously reduce the self-discharge of the capacitor battery, reduce the leakage current and prolong the service life of the battery.
Description
Technical Field
The invention relates to the field of capacitor batteries. More particularly, the present invention relates to a method for forming a multi-segment capacitor battery.
Background
The existing double-electric-layer super capacitor which is mature and applied and takes the activated carbon as the electrode material has excellent pulse charge-discharge performance and rapid charge-discharge performance, has ultrahigh power density, long cycle life and relative safety, but has lower energy density (generally less than or equal to 6 wh/kg); the lithium ion battery has high working voltage and has advantages in energy density, is the secondary battery with the most development potential at present, but has poor power performance, poor low-temperature characteristic (generally, the discharge capacity retention rate is less than 50 percent at about-20 ℃), and short cycle life (hundreds of thousands of cycle life). With the development of the fields of aerospace, national defense and military industry, electric vehicles, electronic information, instruments and meters and the like and the requirement of energy storage devices with high energy density and high power density, the research of 'internal crossing' of a super capacitor and a lithium ion battery is gradually started, namely, a lithium ion battery material is added into the positive electrode and the negative electrode of an electric double layer capacitor to form a new capacitance battery. The new capacitor battery is similar to the related preparation process of the lithium ion battery, and chemical conversion treatment is needed in the manufacturing process, however, the existing lithium ion battery chemical conversion process cannot meet the high performance requirement of the new capacitor battery, and the defects of high self-discharge, large leakage current and short service life of the capacitor battery after chemical conversion often appear.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide at least the advantages described later.
It is still another object of the present invention to provide a method for forming a multi-stage capacitor battery, which can significantly reduce the self-discharge of the capacitor battery, reduce the leakage current, and prolong the battery life.
To achieve these objects and other advantages in accordance with the purpose of the invention, a method for forming a multi-section capacitor battery is provided, comprising the steps of:
step one, firstly, under the condition of normal temperature and normal pressure, I is used1The voltage charged by the current constant current to the capacitor battery is V1Then with I2The voltage charged by the current constant current to the capacitor battery is V2Wherein, I1<I2，V1<V2；
Step two, with I3The voltage charged by the current constant current to the capacitor battery is V3Then the power is cut off and the mixture is kept stand, wherein, I1<I3<I2，V2<V3；
Step three, with I4The voltage charged by the current constant current to the capacitor battery is V4Then by V4Charging at constant voltage, and standing after power failure, wherein I2<I4，V3<V4，V4The voltage is limited for the capacitor battery.
Preferably, the capacity of the capacitor battery is C, I1In the range of 0.016 to 0.023CmA, V1In the range of 72.5% to 77% V4。
Preferably, I2In the range of 0.056-0.064C, V2In the range of 80% to 87.5% V4。
Preferably, I3In the range of 0.034 to 0.042C, V3In the range of 90% to 95% V4。
Preferably, I4The range of (1) is 0.096-0.103C.
Preferably, the time length of the step two for stopping the electricity standing is 28-33 min.
Preferably, the constant voltage charging time in the third step is 26-40 min.
Preferably, the time length of the power-off standing in the third step is 23-27 h.
Preferably, the capacitor battery is placed in a normal pressure environment at 40-50 ℃ for standing for 22-26 hours before the first step is carried out.
Preferably, the method comprises the following steps:
step one, under the conditions of normal temperature and normal pressure, the capacitor battery is charged with a constant current of 0.02C until the voltage of the capacitor battery is 75 percent V4Meanwhile, the ultrasonic-magnetic field-electric field combined treatment is assisted, the frequency of ultrasonic waves is 40-45 KHz, the direction of the magnetic field is parallel to the axial direction of the battery, and the intensity of the magnetic field is measured according to the
Variation, H has the unit of T, T1The unit is min, the direction of the electric field is vertical to the axial direction of the battery, and the electric field intensity is equal to 0.03t according to E2+0.12 change, E units V/m, t2The unit is min, and then the constant current is charged to the voltage of 85 percent V of the capacitor battery by 0.06C current4；
Step two, charging the capacitor battery with a constant current of 0.04C until the voltage of the capacitor battery is 92.5 percent V4Meanwhile, the ultrasonic-magnetic field-electric field combined treatment is assisted, the frequency of ultrasonic waves is 28-33 KHz, the direction of the magnetic field is parallel to the axial direction of the battery, and the intensity of the magnetic field is measured according to the
Variation, H has the unit of T, T3The unit is min, the direction of the electric field is vertical to the axial direction of the battery, and the electric field intensity is equal to 0.05t according to E4+0.07 change, E units V/m, t4The unit is min, and then the power is cut off and the mixture is kept stand for 30 min;
step three, charging the capacitor battery with a constant current of 0.1C until the voltage of the capacitor battery is V4Then by V4Charging at constant voltage for 30min, and standing for 24 h.
The invention at least comprises the following beneficial effects: by designing multi-section charging current and voltage which are respectively matched with SEI film reactions generated in each stage of the formation process, the density uniformity of current in the battery during internal charging during formation can be effectively improved, a stable SEI film is generated, and then the self-discharge of the capacitor battery is remarkably reduced, the leakage current is reduced, and the service life of the battery is prolonged.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a graph of leakage current value versus time in the leakage current test of the present invention;
FIG. 2 is a final leakage current histogram in the leakage current test of the present invention;
FIG. 3 is a graph of voltage values over time in the self-discharge test of the present invention.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It should be noted that the experimental methods described in the following embodiments are conventional methods unless otherwise specified, and the reagents and materials, which are commercially available without otherwise specified, are not to be construed as limiting the present invention.
The formation process of the present invention will be described in detail below by taking a capacitor battery with a capacity of 100mAh and a limited voltage of 4V as an example.
< example 1>
The capacitor battery is firstly placed in a normal pressure environment at 40 ℃ for standing for 22h, and then the following steps are carried out:
under the conditions of normal temperature and normal pressure, firstly, charging the capacitor battery with a constant current of 1.6mA until the voltage of the capacitor battery is 2.9V, and then charging the capacitor battery with a constant current of 5.6mA until the voltage of the capacitor battery is 3.2V;
step two, charging the capacitor battery with 3.4mA current in a constant current manner until the voltage of the capacitor battery is 3.6V, and then powering off and standing for 28 min;
and step three, charging the capacitor battery at a constant current of 9.6mA until the voltage of the capacitor battery is 4V, then charging the capacitor battery at a constant voltage of 4V for 26min, and finally powering off and standing for 23 h.
< example 2>
The capacitor battery is firstly placed in a normal pressure environment at 45 ℃ for standing for 24 hours, and then the following steps are carried out:
under the conditions of normal temperature and normal pressure, firstly, charging the capacitor battery to 3V by using a constant current of 2mA, and then charging the capacitor battery to 3.4V by using a constant current of 6 mA;
step two, charging the capacitor battery with a constant current of 4mA until the voltage of the capacitor battery is 3.7V, and then powering off and standing for 30 min;
and step three, charging the capacitor battery at a constant current of 10mA until the voltage of the capacitor battery is 4V, then charging the capacitor battery at a constant voltage of 4V for 30min, and finally powering off and standing the capacitor battery for 24 h.
< example 3>
The capacitor battery is firstly placed in a 50 ℃ normal pressure environment for standing for 26 hours, and then the following steps are carried out:
under the conditions of normal temperature and normal pressure, firstly, charging the capacitor battery with a constant current of 2.3mA until the voltage of the capacitor battery is 3.1V, and then charging the capacitor battery with a constant current of 6.4mA until the voltage of the capacitor battery is 3.5V;
step two, charging the capacitor battery with a constant current of 4.2mA until the voltage of the capacitor battery is 3.8V, and then powering off and standing for 33 min;
and step three, charging the capacitor battery at a constant current of 10.3mA until the voltage of the capacitor battery is 4V, then charging the capacitor battery at a constant voltage of 4V for 40min, and finally powering off and standing for 27 h.
< example 4>
The capacitor battery is firstly placed in a normal pressure environment at 45 ℃ for standing for 24 hours, and then the following steps are carried out:
under the conditions of normal temperature and normal pressure, charging the capacitor battery at constant current of 2mA till the voltage of the capacitor battery is 3V, and simultaneously assisting ultrasonic-magnetic field-electric field combined treatment, wherein the frequency of ultrasonic waves is 43KHz, the direction of a magnetic field is parallel to the axial direction of the battery, and the intensity of the magnetic field is determined according to the axial direction of the battery
Variation, H has the unit of T, T1Unit is min, electric field direction and battery axisThe line direction is vertical, and the electric field intensity is equal to 0.03t according to E2+0.12 change, E units V/m, t2The unit is min, and then the constant current charging is carried out by 6mA until the voltage of the capacitor battery is 3.4V;
step two, charging the capacitor battery with a constant current of 4mA until the voltage of the capacitor battery is 3.7V, and simultaneously assisting with ultrasonic-magnetic field-electric field combined treatment, wherein the frequency of ultrasonic waves is 28-33 KHz, the direction of the magnetic field is parallel to the axial direction of the battery, and the intensity of the magnetic field is according to the intensity of the magnetic field
Variation, H has the unit of T, T3The unit is min, the direction of the electric field is vertical to the axial direction of the battery, and the electric field intensity is equal to 0.05t according to E4+0.07 change, E units V/m, t4The unit is min, and then the power is cut off and the mixture is kept stand for 30 min;
and step three, charging the capacitor battery at a constant current of 10mA until the voltage of the capacitor battery is 4V, then charging the capacitor battery at a constant voltage of 4V for 30min, and finally powering off and standing the capacitor battery for 24 h.
< comparative example >
The comparative example carries out formation on the capacitor battery by using a conventional lithium battery formation process, and the specific process is as follows:
firstly, charging the battery with 2mA constant current until the voltage of the battery is 3V, powering off and standing for 30min, then charging the battery with 10mA constant current until the voltage of the battery is 4V, and finally powering off and standing for 24 h.
< leakage Current test >
The leakage current test of the capacitor batteries respectively treated in the example 2, the example 4 and the comparative example is carried out, and the specific test process is as follows:
step 1: charging the battery monomer to 3.67V, and keeping constant current and constant voltage at 3.67V for 30 min;
step 2: at normal temperature, placing the single battery on an NGI leakage current tester clamp according to the specification;
and 3, step 3: setting the voltage to be 3.675V, selecting a 100 omega grade for charging precision resistors in a leakage current tester, sampling time before testing for 30min, sampling interval in testing for 1min, and testing total time for 48 h;
and 4, step 4: the current value at 48h was taken as the final leakage current value.
The test results are shown in fig. 1 and fig. 2, fig. 1 is a graph of the change of the leakage current value with time, wherein the abscissa is the test time, the ordinate is the leakage current value, a is the leakage current curve of the comparative example, b is the leakage current curve of the example 2, c is the leakage current curve of the example 4, fig. 2 is the final leakage current of each of the examples 2, 4 and the comparative example at the time point of the test ending, and it can be seen from fig. 1 and fig. 2 that the leakage current of the examples 2 and 4 is obviously smaller than that of the comparative example from the beginning to the end, which illustrates that the formation method of the multi-stage capacitor battery provided by the present invention can significantly reduce the leakage current of the capacitor battery.
< self discharge test >
The self-discharge test of the capacitor batteries respectively treated in the example 2, the example 4 and the comparative example is carried out, and the specific test process is as follows:
step 1: at normal temperature, placing the single battery on a test fixture according to the specification;
step 2: charging the battery monomer to 3.67V at a constant current of 50mA and at a constant voltage of 3.67V, and cutting off the current of 2.5 mA;
and 3, step 3: and (4) opening the circuit of the single battery and standing, storing and standing for a certain time, and recording the voltage value of the single battery at the moment.
The test results are shown in fig. 3, fig. 3 is a graph of the voltage of the battery as a function of time, in which the abscissa is the standing time and the ordinate is the voltage value, a is the voltage curve of example 4, b is the voltage curve of example 2, and c is the voltage curve of the comparative example, and in order to further illustrate the advantageous effects of the present invention, voltage data of a portion of time points in fig. 3 are shown in table 1.
TABLE 1
| Shelf life (h) | Example 2 | Example 4 | Comparative example |
| 0 | 3.6680 | 3.6696 | 3.6684 |
| 100 | 3.6600 | 3.6608 | 3.6532 |
| 200 | 3.6588 | 3.6602 | 3.6514 |
| 400 | 3.6561 | 3.6594 | 3.6495 |
| 600 | 3.6555 | 3.6603 | 3.6483 |
| 800 | 3.6543 | 3.6593 | 3.6473 |
| 900 | 3.6540 | 3.6590 | 3.6464 |
As can be seen from fig. 3 and table 1, the voltage drop of the capacitor cell 900h (37 days) treated in example 4 is 10mV, the absolute voltage of the capacitor cell is 3.6590V, the voltage drop of the capacitor cell 900h (37 days) treated in example 2 is 14mV, the absolute voltage of the capacitor cell is 3.6540V, the voltage drop of the capacitor cell 900h (37 days) treated in the comparative example is 22mV, the absolute voltage of the capacitor cell is 3.6464V, and the voltage values of the capacitor cells in examples 2 and 4 are significantly greater than those in the comparative example, which shows that the multi-stage capacitor cell formation method provided by the present invention can significantly reduce the self-discharge of the capacitor cell.
< Battery Life test >
The capacitor batteries treated in example 2, example 4 and comparative example were used for battery life test, and the specific test procedure was as follows
Step 1: placing the monomer on a tester clamp according to the specification at normal temperature, charging the monomer to 3.67V with 50mA current, and keeping the voltage at 3.67V for 30 min;
step 2: discharging the monomer to 2.5V with 50mA current, and taking the discharge capacity of the step as C0；
And 3, step 3: repeating the step 1 to the step 2 for 1000 times, and sequentially recording the discharge capacity as C1、C2、……、C1000。
And 4, step 4: after the 1000 th charge-discharge was completed, C was calculated1000/C0I.e. discharge capacity retention (compared to first-pass discharge).
The discharge capacity retention rates of the capacitor batteries respectively treated in the examples 2, 4 and the comparative examples are respectively 95%, 97% and 81%, namely after multiple charge and discharge cycles, the capacitor batteries treated in the examples 2 and 4 still maintain higher discharge capacities, which shows that the service life of the capacitor batteries can be remarkably prolonged by the multi-stage capacitor battery formation method provided by the invention.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (2)
1. The method for forming the multi-section capacitor battery is characterized by comprising the following steps of:
step one, under the conditions of normal temperature and normal pressure, the capacitor battery is charged with a constant current of 0.02C until the voltage of the capacitor battery is 75 percent V4Meanwhile, the ultrasonic-magnetic field-electric field combined treatment is assisted, the frequency of ultrasonic waves is 40-45 KHz, the direction of the magnetic field is parallel to the axial direction of the battery, and the intensity of the magnetic field is measured according to the
Variation, H has the unit of T, T1The unit is min, the direction of the electric field is vertical to the axial direction of the battery, and the electric field intensity is equal to 0.03t according to E2+0.12 change, E units V/m, t2The unit is min, and then the constant current is charged to the voltage of 85 percent V of the capacitor battery by 0.06C current4；
Step two, charging the capacitor battery with a constant current of 0.04C until the voltage of the capacitor battery is 92.5 percent V4Meanwhile, the ultrasonic-magnetic field-electric field combined treatment is assisted, the frequency of ultrasonic waves is 28-33 KHz, the direction of the magnetic field is parallel to the axial direction of the battery, and the intensity of the magnetic field is measured according to the
Variation, H has the unit of T, T3The unit is min, the direction of the electric field is vertical to the axial direction of the battery, and the electric field intensity is equal to 0.05t according to E4+0.07 change, E units V/m, t4The unit is min, and then the power is cut off and the mixture is kept stand for 30 min;
step three, charging the capacitor battery with a constant current of 0.1C until the voltage of the capacitor battery is V4Then by V4Charging at constant voltage for 30min, and finally powering off and standing for 24 h;
wherein C is the capacity of the capacitor battery, V4Is the limit voltage of the capacitor battery.
2. The method for forming a multi-segment capacitor battery as claimed in claim 1, wherein the capacitor battery is left to stand at 40-50 ℃ for 22-26 hours under normal pressure before the first step.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2358622Y (en) * | 1999-02-04 | 2000-01-12 | 北京有色金属研究总院 | Constant current constant-voltage charging device for secondary battery |
| CN102324570A (en) * | 2011-09-07 | 2012-01-18 | 惠州Tcl金能电池有限公司 | Lithium ion battery, its formation method and preparation method |
| CN103390770A (en) * | 2013-07-25 | 2013-11-13 | 天津力神电池股份有限公司 | Lithium ion battery formation sectional charging method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2358622Y (en) * | 1999-02-04 | 2000-01-12 | 北京有色金属研究总院 | Constant current constant-voltage charging device for secondary battery |
| CN102324570A (en) * | 2011-09-07 | 2012-01-18 | 惠州Tcl金能电池有限公司 | Lithium ion battery, its formation method and preparation method |
| CN103390770A (en) * | 2013-07-25 | 2013-11-13 | 天津力神电池股份有限公司 | Lithium ion battery formation sectional charging method |
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