CN112928352A - Step charging technology of lithium-sulfur battery - Google Patents
Step charging technology of lithium-sulfur battery Download PDFInfo
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- 238000007600 charging Methods 0.000 title claims abstract description 106
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000005516 engineering process Methods 0.000 title claims abstract description 22
- 238000010278 pulse charging Methods 0.000 claims abstract description 45
- 238000010277 constant-current charging Methods 0.000 claims abstract description 32
- 230000010287 polarization Effects 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims description 22
- 230000008569 process Effects 0.000 claims description 9
- 230000003068 static effect Effects 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052717 sulfur Inorganic materials 0.000 abstract description 11
- 239000011593 sulfur Substances 0.000 abstract description 11
- 230000000052 comparative effect Effects 0.000 description 12
- 229910001216 Li2S Inorganic materials 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- GLNWILHOFOBOFD-UHFFFAOYSA-N lithium sulfide Chemical compound [Li+].[Li+].[S-2] GLNWILHOFOBOFD-UHFFFAOYSA-N 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VDFVNEFVBPFDSB-UHFFFAOYSA-N 1,3-dioxane Chemical compound C1COCOC1 VDFVNEFVBPFDSB-UHFFFAOYSA-N 0.000 description 1
- 229910013553 LiNO Inorganic materials 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- -1 lithium salt lithium trifluoromethanesulfonate imide Chemical class 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/44—Methods for charging or discharging
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- 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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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Secondary Cells (AREA)
Abstract
The invention discloses a step charging technology of a lithium-sulfur battery, and belongs to the technical field of battery charging. The charging technology comprises two schemes: step constant current charging with gradually increased charging current; and step pulse charging with gradually increased charging current. The charging technology excavates charging potential and improves the utilization rate of active sulfur by reducing charging polarization, particularly polarization at the initial charging stage. Compared with constant-current charging, the charging technologies can improve the charging speed of the battery, shorten the charging time and improve the cycle performance of the battery on the premise of the same charging electric quantity.
Description
Technical Field
The invention belongs to the technical field of battery charging, and particularly relates to a step charging technology of a lithium-sulfur battery.
Background
The theoretical energy density of the lithium-sulfur battery is 2600Wh/Kg, which is 3-5 times of that of the traditional lithium ion battery, and the lithium-sulfur battery is an electrochemical energy storage system with a great application prospect. Over the past decade, lithium sulfur batteriesThe method has been developed greatly, and particularly, the specific capacity and the cycling stability of the button cell level are greatly improved, but still more technical challenges exist. The reason for the higher internal resistance of the lithium-sulfur battery is mainly the low conductivity of sulfur itself, the continuous dissolution of polysulfide formed by sulfur and lithium in the electrolyte, and the insoluble Li2The electronic and ionic conductivities of S are poor. In order to solve these problems, the current research reports mainly refer to the design of the sulfur cathode material, and in fact, the development of a suitable charging technology can also reduce the internal resistance of the lithium-sulfur battery to a certain extent and improve the battery performance.
The most common charging mode of the existing lithium-sulfur battery is constant current charging, in the charging process, the cathode of the lithium-sulfur battery is the deposition reaction of metal lithium ions, the anode potential does not change obviously, and the anode is insoluble Li2S and Li2S2The cathode potential shows a change trend of increasing rapidly, then decreasing and then increasing. If a large current is used for constant current charging, the cathode is insoluble Li in the initial charging period2The electronic and ionic conductivity of S is poor, the polarization of the battery is rapidly increased, and the cathode potential is rapidly increased, so that insoluble Li is caused2S and Li2S2The conversion cannot be fully carried out, and the utilization rate of sulfur is reduced. Therefore, in order to reduce the polarization of the lithium-sulfur battery in the charging process, improve the utilization rate of active substance sulfur and slow down the accumulation of insoluble solid lithium sulfide in the circulating process, according to the characteristics of the charging polarization of the lithium-sulfur battery: the polarization of the battery shows a trend of changing from large to small in the charging process. The invention provides a step charging technology for a lithium-sulfur battery.
Disclosure of Invention
The invention aims to provide a step charging technology of a lithium-sulfur battery, which improves the utilization rate of active substance sulfur, slows down the accumulation of insoluble solid lithium sulfide, exploits the charging capacity of the battery, improves the charging speed of the battery and improves the cycle performance of the battery by reducing the polarization in the charging process.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a step charging technology of a lithium-sulfur battery comprises two charging schemes: the first is stepped constant current charging with gradually increased charging current; the second kind is a step pulse charging in which the charging current is gradually increased.
The first charging scheme is a step constant current charging mode with gradually increasing current, and the specific scheme is as follows: setting a group of gradually increasing constant current charging current values Ic{Ic1,Ic2,Ic3,……,IcnA set of gradually increasing constant-current charging cut-off voltages V { V }1,V2,V3,.....,VnOr a set of gradually increasing charge cutoff SOCs1,SOC2,SOC3,.....,SOCm}; the first stage of constant current charging of the battery, the charging current is the minimum value Ic1Charging time of tc1Charging the battery to SOC1(ii) a The second stage of constant current charging of the battery, the charging current is Ic2Charging time of tc2Charging the battery to SOC2Or charged to a cut-off voltage V1,.., the battery is charged to the nth stage with a charging current of IcnCharging time of tcnCharging the battery to SOCnOr charged to a cut-off voltage Vn-1The above steps are repeated until the battery voltage reaches the cut-off voltage Vmax。
The step constant current charging with gradually increased current at least comprises two constant current charging stages, and the battery is required to be completely discharged in the last charging and discharging period. The step constant current charging technology with gradually increased current comprises a first constant current charging stage of the battery, wherein the charging current Ic1、SOC1、V1Is a minimum value, and SOC1And V1It is necessary that the battery has overcome the initial stage of charging due to solid-state Li2S and Li2S2Resulting in a larger polarized value.
The second charging scheme is a specific scheme of step pulse charging with gradually increased current, which is as follows: setting a set of gradually increasing pulse charging current values Ic{Ic1,Ic2,Ic3,……,IcnA set of gradually increasing charge cut-off voltages V { V }1,V2,V3,.....,VnEither set a set of progressively larger charge cutoff SOCs1,SOC2,SOC3,.....,SOCmThe first step of battery stepped pulse charging, pulse charging current Ic1At minimum, the pulse is cyclically charged to the battery charge SOC1Step pulse charging of the battery at a second stage with a pulse charging current of Ic2Setting negative pulse or standing time, and charging the pulse to the battery electric quantity SOC2Or voltage V1,.. step pulse charging of battery at nth stage with pulse charging current of IcnSetting negative pulse or standing time, and charging the pulse to the battery electric quantity SOCnOr voltage Vn-1Circulating the above steps until the cut-off voltage V of the batterymax。
The step pulse charging technology with gradually increased current at least comprises two pulse charging stages, and the battery needs to be completely discharged in the last charging and discharging period. The current gradually increasing step pulse charging technology comprises a first step of battery step pulse charging, wherein the first step is pulse charging current Ic1、SOC1、V1Is a minimum value, and SOC1And V1It is necessary that the battery has overcome the initial charge due to Li2S and Li2S2Resulting in a larger ohmic polarized value. In the step pulse charging technology with the gradually increased current, the pulse charging current value in each pulse charging stage is a fixed value, and in all the pulse charging stages, each pulse charging time value, each negative pulse time value and each standing time value are fixed values.
Drawings
Fig. 1 shows a stepped constant current charge with gradually increasing current.
Fig. 2 shows a step pulse charging with increasing current.
FIG. 3 is a graph of the charging curves of example 1 and a comparative example.
Fig. 4 is a graph of the charging curves of example 2 and a comparative example.
FIG. 5 is a graph showing the cycle performance of examples and comparative examples.
Detailed Description
In order to better understand the technical solution of the present invention, the following further describes the content of the present invention with reference to specific implementation examples.
The battery systems adopted in all the examples and the comparative examples of the invention are consistent, and the actual capacities of all the batteries are in the range of 1.0-1.1 mAh. The cathode is a sulfur anode taking the ordered mesoporous carbon as a sulfur carrier, the cathode is metallic lithium, the button cell further comprises an isolating membrane and electrolyte, and the button cell is obtained through the processes of cell assembly, activation and the like. During the preparation process of the cathode, firstly, the ordered mesoporous carbon and sulfur powder are mixed in a proportion of 7: 3, then placing the mixed material in a reaction kettle at 155 ℃ for 12 hours, cooling, and mixing with PVDF and conductive carbon black in a weight ratio of 8: 1:1, and the components are uniformly mixed according to the weight ratio and are prepared by taking N-methyl pyrrolidone as a solvent. The isolating membrane is a microporous PP film, the electrolyte is lithium salt lithium trifluoromethanesulfonate imide dissolved in 1, 3-dioxane/1, 2-dimethoxyethane (DOL/DME, volume ratio is 1:1), and 2 wt% of LiNO is added3And (b) an additive, wherein the solubility of lithium salt is 1 mol/L. In addition, all tests are carried out in the environment of normal temperature 25 ℃, and the voltage test range is 1.7-2.8V.
The content of the embodiments of the invention and the comparative examples is as follows:
comparative example 1
And (4) constant current charging and discharging, wherein the charging current and the discharging current are both 0.5C.
Example 1
The step constant current charging with gradually increasing current is characterized in that the multi-stage constant current charging is realized, and the charging current I is shown in figure 1cGradually increased, and at least comprises 2 charging stages.
The specific procedure of example 1 is as follows:
setting a group of gradually increasing constant current charging current values Ic{Ic1,Ic2,Ic3,Ic4A set of progressively increasing charge cut-off SOCs1,SOC2,SOC3,.....,SOCmIn which the battery is in a first stage of constant-current charging, Ic10.2046mA, charged to SOC1At 15% SOC, a second stage of constant current charging of the battery, Ic20.4204mA, charged to SOC2At 40% SOC, a third stage of constant current charging of the battery, Ic30.6268mA, charged to SOC3At 70% SOC, a fourth stage of constant current charging of the battery, Ic41.0466mA, charged to SOC4Is 100% SOC.
Example 2
Referring to fig. 2, the technology is characterized in that the step pulse charging is performed, pulse charging currents in the same step are consistent, and the pulse charging currents in different steps have a trend of changing from small to large and at least comprise 2 charging steps.
The specific procedure of example 2 is as follows:
setting a set of gradually increasing pulse charging current values Ic{Ic1,Ic2,Ic3,Ic4A set of gradually increasing charge cut-off voltages V { V }1,V2,VmaxSetting each pulse charging time tc10s, each pulse standing time trIs 1 s. Wherein the battery is pulsed in a first phase, Ic10.475mA, pulse charging to SOC1At 19% SOC, a second stage of battery pulse charging, Ic20.7094mA, pulse charging to voltage V12.3V, a third stage of battery pulse charging, Ic3Is charged to a voltage V for 1.1812mA pulsemaxIt was 2.8V.
Fig. 3 to 4 are graphs showing the charging voltage and charging current as a function of capacity for examples 1 and 2 and comparative example, respectively. It can be seen from the figure that the charging technology of the present invention can effectively reduce the charging polarization during the charging process, especially in the initial stage of charging, and in the later stage of charging, although the charging current of the example is higher than that of the comparative example, the charging polarization is not significantly increased. Therefore, the charging technology of the invention can reasonably reduce polarization and improve the charging speed to a certain extent on the premise of ensuring the same charging capacity.
FIG. 5 is a graph showing cycle performance of examples 1 and 2 and a comparative example. As can be seen from the figure, all examples of the present invention can not only improve the charge rate of the battery but also maintain good cycle performance after 50 cycles, compared to the comparative example.
In order to more clearly express the charging advantages of all the examples, table 1 briefly summarizes the charging parameters and the charging speeds of the examples and the comparative examples.
TABLE 1 table of Performance parameters for examples and comparative examples
In combination with the above-described embodiments, the lithium-sulfur battery charging technique of the present invention utilizes the step constant current charging or step pulse charging with gradually increasing charging current to slow the polarization accumulation during the charging process, reduce the polarization potential, promote the conversion of different intermediate phases of sulfur and lithium, and particularly improve the solid-state Li2S and Li2S2Slow the insoluble solid Li in the cycle2And the accumulation of S improves the utilization rate of active sulfur and the cycle performance of the battery.
Finally, it should be noted that the above-described embodiments are only used for describing the technical solutions of the present invention, and are not limited thereto. The present invention may be suitably modified in the above-described embodiments, or some or all of the technical features may be equivalently replaced. Therefore, some modifications or changes to the present invention should also fall within the protection scope of the claims of the present invention.
Claims (10)
1. A step charging technique for a lithium sulfur battery, characterized by: the charging technology is a step constant current charging mode with gradually increased charging current; or, the charging technology is a step pulse charging mode in which the charging current gradually increases.
2. The step charging technique for a lithium sulfur battery according to claim 1, characterized in that: the specific scheme of the charging technology which is a step constant current charging mode with gradually increased charging current comprises the following steps (A1) - (A2):
(A1) setting a group of gradually increasing constant current charging current values Ic{Ic1,Ic2,Ic3,……,Icn}, a set of charge time values tc1,tc2,tc3,.....,tcnA set of gradually increasing constant-current charging cut-off voltages V { V }1,V2,V3,.....,VnEither set a set of progressively larger charge cutoff SOCs1,SOC2,SOC3,.....,SOCm}, setting a cut-off voltage Vmax；
(A2) The first stage of constant current charging of the battery, the charging current is Ic1Charging time of tc1Charging the battery to SOC1(ii) a The second stage of constant current charging of the battery, the charging current is Ic2Charging time of tc2Charging the battery to SOC2Or charged to a cut-off voltage V1(ii) a Sequentially until the battery is charged to the nth stage, the charging current is IcnCharging time of tcnCharging the battery to SOCnOr charged to a cut-off voltage Vn-1The above steps are repeated until the battery voltage reaches the cut-off voltage Vmax。
3. The step charging technique for a lithium sulfur battery according to claim 1, characterized in that: the specific scheme of the charging technology which is a step pulse charging mode with gradually increased charging current comprises the following steps (B1) - (B2):
(B1) setting a set of gradually increasing pulse charging current values Ic{Ic1,Ic2,Ic3,……,IcnA charging time value tcA value of discharge current IdA value of discharge time tdOr a value of rest time trA set of gradually increasing charge cut-off voltages V { V }1,V2,V3,.....,VnEither set a set of progressively larger charge cutoff SOCs1,SOC2,SOC3,....., SOCm}, setting a cut-off voltage Vmax；
(B2) The first stage of battery step pulse charging with pulse charging current of Ic1Time value t of pulse chargingcNegative pulse current is IdDischarge time of negative pulse tdOr a standing time trThe above steps are repeated until the battery electric quantity SOC1(ii) a The second stage of battery step pulse charging, the pulse charging current is Ic2Time value t of pulse chargingcNegative pulse current is IdDischarge time of negative pulse tdOr a standing time trThe above steps are repeated until the battery electric quantity SOC2Or voltage V1(ii) a Sequentially carrying out the steps until the nth stage of the battery step pulse charging, wherein the pulse charging current is IcnTime value t of pulse chargingcNegative pulse current is IdDischarge time of negative pulse tdOr a standing time trUntil the battery power SOCnOr voltage Vn-1(ii) a The operation is circulated until the cut-off voltage V of the batterymax。
4. The step charging technique for a lithium sulfur battery according to claim 2, characterized in that: in the step A2, the stepped constant-current charging current values are increased in sequence, wherein Ic1The value is minimal.
5. The step charging technique for a lithium sulfur battery according to claim 2 or 3, characterized in that: SOC in the step (A2) or the step (B2)1It must be satisfied that the lithium-sulfur battery has overcome the problem of insoluble Li in the initial stage of charging2S or Li2S2Resulting in a large ohmic polarization and provided that the cell needs to be fully discharged during the last discharge cycle.
6. According to claim2 or 3, wherein: the charge cut-off voltage V in the step (A2) or the step (B2), wherein V1It must be satisfied that the lithium-sulfur battery has overcome the problem of insoluble Li in the initial stage of charging2S or Li2S2Resulting in a large ohmic polarization and provided that the cell needs to be fully discharged during the last discharge cycle.
7. The step charging technique for a lithium sulfur battery according to claim 2, characterized in that: the constant current charging current value I in the step (A1)c{Ic1,Ic2,Ic3,……,IcnThe rate is in the range of 0.05C-10C.
8. The step charging technique for a lithium sulfur battery according to claim 2 or 3, characterized in that: in the step (A2) or the step (B2), the step constant current charging current and the step pulse charging current of the corresponding battery are gradually increased, wherein Ic1The value is minimal.
9. The step charging technique for a lithium sulfur battery according to claim 3, wherein: the pulse charging current value I in the step (B1)c{Ic1,Ic2,Ic3,……,IcnThe value is in the range of 0.05C-10C; charging time value tcIn the range of 0.1s to 30 s; a discharge current value IdIn the range of 0C-0.2C; discharge time value tdIn the range of 0.01s to 5 s; a static charging time trIn the range of 0.01 to 30 seconds.
10. The step charging technique for a lithium sulfur battery according to claim 2 or 3, characterized in that: and (3) after the battery is placed in an environment with the temperature of-80-60 ℃, carrying out the charging process of the step (A2) or the step (B2) on the battery.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113972411A (en) * | 2021-09-28 | 2022-01-25 | 天津力神电池股份有限公司 | Method for determining lithium battery quick-charging strategy |
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Application publication date: 20210608 |