CN115911572A - Functional electrolyte suitable for aluminized composite film current collector and lithium ion battery - Google Patents
Functional electrolyte suitable for aluminized composite film current collector and lithium ion battery Download PDFInfo
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- CN115911572A CN115911572A CN202211633863.3A CN202211633863A CN115911572A CN 115911572 A CN115911572 A CN 115911572A CN 202211633863 A CN202211633863 A CN 202211633863A CN 115911572 A CN115911572 A CN 115911572A
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Abstract
The invention relates to the technical field of battery electrolytes, in particular to a functional electrolyte and a lithium ion battery suitable for an aluminized composite membrane current collector, which comprise a basic electrolyte and/or a lithium salt and/or an additive, wherein the basic electrolyte is prepared by the following method: firstly, uniformly mixing ethylene carbonate and methyl ethyl carbonate in a glove box, adding vinylene carbonate and fluoroethylene carbonate into the mixture, and uniformly mixing to obtain the ethylene carbonate/methyl ethyl carbonate composite material. And manufacturing the positive pole piece and the negative pole piece, and then sequentially carrying out rolling, die cutting, drying, winding, assembling, injecting functional electrolyte, sealing, forming and secondary sealing to obtain the lithium ion battery. According to the invention, through the adjustment of the electrolyte formula, the content of HF acid in a battery system is at an extremely low level, the problem of corrosion and falling of the aluminum-plated composite film is effectively inhibited, and the comprehensive performance of the lithium ion battery using the aluminum-plated composite film is improved. The aluminum-plated composite film has no delamination phenomenon with the PET base film; the alternating current impedance of the battery is reduced, and the cycle performance of the battery is improved.
Description
Technical Field
The invention relates to the technical field of battery electrolytes, in particular to a functional electrolyte suitable for an aluminized composite film current collector and a lithium ion battery.
Background
The aluminized composite film prepared by taking polyethylene terephthalate (PET) and polypropylene (PP) films as representatives has a huge market in the field of packaging. The aluminized composite film prepared by the evaporation process has good metal characteristics, can effectively improve the needling safety performance of the battery by replacing the traditional aluminum foil, and compared with the traditional aluminum foil, the composite film prepared based on physical vapor deposition has poorer bonding force between a polymer substrate and a metal coating, so that the metal coating is easy to fall off from the surface of the substrate, and the long-term stability of the composite film in the battery is seriously influenced. The composite current collector is corroded by HF in electrolyte to cause delamination and cracking of Al and PET, and the impedance of the battery is increased.
In the prior art, lithium hexafluorophosphate (LiPF) is mainly used as the current commercial electrolyte of the lithium ion battery 6 ) The electrolytic liquid system mainly comprises the organic carbonate solvent and has better electrochemical stability. However, the electrolyte lithium salt LiPF 6 The application field is limited due to easy decomposition by heat and poor hydrolytic stability, and the formulas (1) to (4) are that trace amount of water (H) exists in the electrolyte 2 O) reaction equation induced:
LiPF 6 →LiF+PF 5 (1)
PF 5 +H 2 O→POF 3 +2HF(2)
POF 3 +H 2 O→POF 2 (OH)+HF(3)
POF 2 (OH)+H 2 O→POF(OH) 2 +HF(4)
wherein POF formed by the reaction of the formula (1) and the formula (2) 3 May further react with water to form other undesirable products, such as POF shown in equations (3) and (4) 2 (OH) and POF (OH) 2 And further generates hydrofluoric acid (HF).
Therefore, in the prior art, since the content of HF generated by the lithium salt is high and moisture introduced during the production process cannot be removed, when the aluminum-plated composite film is applied to a battery as a positive current collector, al and PET are easily delaminated and cracked under the corrosion of HF in the electrolyte, so that the impedance of the battery is increased. In addition, these products resulting from the water and HF side reactions deposit on the negative electrode material, resulting in an increase in the cell impedance. Meanwhile, hydrogen Fluoride (HF) generated by the reaction is easily dissolved in the positive electrode material and destroys the active material, so that the capacity of the battery is rapidly attenuated.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a functional electrolyte suitable for an aluminized composite film current collector and a lithium ion battery.
The technical scheme for realizing the purpose of the invention is as follows: a functional electrolyte suitable for an aluminized composite film current collector comprises a base electrolyte and/or a lithium salt and/or an additive,
the basic electrolyte is prepared by the following method: firstly, mixing ethylene carbonate and ethyl methyl carbonate in a ratio of 3:7, uniformly mixing in a glove box, adding 2wt% of vinylene carbonate and 1wt% of fluoroethylene carbonate, and uniformly mixing to obtain the ethylene carbonate/fluoroethylene carbonate composite material;
the lithium salt is one or two of LiFSI and LiPF 6;
the additive is one of IPDI, PTSI and HDI.
According to the technical scheme, the moisture content in the glove box is less than 0.01ppm, and the oxygen content is less than 0.01ppm.
In the technical scheme, the lithium salt accounts for the mass ratio of the ethylene carbonate to the methyl ethyl carbonate being 3:7..
The proportion of the lithium salt in the technical scheme is 7wt% or 14 wt%.
In the technical scheme, the content of the vinylene carbonate is 2wt%, and the content of the fluoroethylene carbonate is 1wt%.
The additive in the technical scheme is 0.2wt%.
A lithium-ion battery containing a functional electrolyte suitable for use with an aluminized composite film current collector.
The technical scheme comprises the following preparation methods:
preparing a positive electrode, dissolving PVDF powder in NMP, uniformly stirring to prepare a PVDF glue solution for later use, mixing and uniformly stirring dry materials of lithium iron phosphate and conductive carbon black, adding the PVDF glue solution into the mixed dry materials, uniformly stirring, adjusting the slurry to a proper coating viscosity and a proper solid content, and coating the slurry on a current collector of a thick aluminum-plated composite film to obtain a positive electrode piece;
preparing a negative electrode, dissolving CMC powder in deionized water to prepare a glue solution for later use, mixing and stirring artificial graphite and a conductive agent uniformly, adding a proper amount of CMC glue solution and SBR, stirring uniformly, adjusting the slurry to a proper coating viscosity and solid content, and coating the slurry on a thick copper foil current collector to obtain a negative electrode plate;
and sequentially carrying out rolling, die cutting, drying, winding, assembling and injecting the functional electrolyte suitable for the aluminized composite film current collector, sealing, forming and secondary sealing on the positive pole piece and the negative pole piece to obtain the lithium ion battery.
The conductive agent in the technical scheme is Super P Li.
The lithium ion battery in the technical scheme is a 4060D0-2.0Ah square soft package lithium ion battery.
After the technical scheme is adopted, the invention has the following positive effects:
(1) According to the invention, through the adjustment of the electrolyte formula, the content of HF acid in a battery system is at an extremely low level, the problem of corrosion and falling of the aluminum-plated composite film is effectively inhibited, and the comprehensive performance of the lithium ion battery using the aluminum-plated composite film is improved. The aluminum-plated composite film has no delamination phenomenon with the PET base film; the alternating current impedance of the battery is reduced, and the cycle performance of the battery is improved.
(2) According to the invention, by using the LiTSI and the LiTFSI as the lithium salt of the electrolyte which does not react with water, the hydrofluoric acid generated by the electrolyte in a battery system is greatly reduced; the isocyanate group — N = = C = = N atom in O may be bonded to free H in the electrolyte + The polymer is formed to suppress the generation of HF, and water and hydrofluoric acid generated in the process are absorbed by the use of a specific additive having the functional group.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments.
The English abbreviations in the text are as follows:
EC: carbonic acid ethylene ester
EMC: carbonic acid methyl ethyl ester
VC: vinylene carbonate
FEC: fluoroethylene carbonate
PTSI: p-toluenesulfonyl isocyanate
IPDI: isophorone diisocyanate
HDI: hexamethylene diisocyanate
TDI: toluene diisocyanate
MDI: diphenylmethane diisocyanate
HMDI: dicyclohexylmethane diisocyanate
TMSNCS: trimethylsilyl isothiocyanate
HF: hydrofluoric acid
LiFSI: lithium bis (fluorosulfonylimide)
And (3) LiTFSI: bis (trifluoromethanesulfonyl) imide lithium salt
wt%: mass percent of
SOC: state of charge of battery
ICP: inductively coupled plasma emission spectroscopy
PVDF: polyvinylidene fluoride
NMP: n-methyl pyrrolidone
CMC: carboxymethyl cellulose
SBR: styrene butadiene rubber
Super P Li: ultra dense high carbon black
The invention provides a functional electrolyte suitable for an aluminized composite film current collector, which comprises a base electrolyte, and/or lithium salt, and/or an additive,
the base electrolyte is prepared by the following method: firstly, mixing ethylene carbonate and methyl ethyl carbonate in a proportion of 3:7, uniformly mixing in a glove box, adding 2wt% of vinylene carbonate and 1wt% of fluoroethylene carbonate, and uniformly mixing to obtain the ethylene carbonate/fluoroethylene carbonate composite material;
the lithium salt is one or two of LiFSI and LiPF 6;
the additive is one of IPDI, PTSI and HDI.
The moisture content in the glove box is less than 0.01ppm, and the oxygen content is less than 0.01ppm.
The proportion of the lithium salt is preferably one of 7wt% or 14 wt%. When the proportion of the lithium salt is 6 to 20% by weight, a similar effect can be obtained, and the higher the proportion is, the lower the AC resistance is, the better the cycle performance is
The additive is preferably 0.2wt%. When the additive is 0.1wt% to 0.5wt%, similar effects can be obtained, and the higher the proportion is, the lower the iron ion elution amount is, and after exceeding 0.2wt%, the higher the proportion is, the higher the ac impedance is, and the worse the cycle performance is.
It will be understood that the additives IPDI, PTSI, HDI can be substituted with other compounds of the same type containing isocyanate functional groups, such as one or several of Toluene Diisocyanate (TDI), diphenylmethane diisocyanate (MDI), dicyclohexylmethane diisocyanate (HMDI), trimethylsilylisothiocyanate (TMSNCS), in the same mass ratio.
Example 1
Preparing the electrolyte of the lithium ion battery in a glove box (the moisture content is less than 0.01ppm, and the oxygen content is less than 0.01 ppm): mixing 86wt% of base electrolyte, 7wt% of LiFSI, 7wt% of LiPF6 uniformly to obtain the desired electrolyte.
The function of the invention is as follows: compared with the comparative example 1, the lithium salt LiFSI which does not react with water to generate HF is used in the lithium salt part to improve the corrosion of the current collector of the aluminum-plated composite film, improve the high-temperature storage capacity retention rate, the capacity recovery rate and the room-temperature cycle performance of the battery, and reduce the alternating-current internal resistance and the positive iron ion elution amount of the battery.
Example 2
Preparing the electrolyte of the lithium ion battery in a glove box (the moisture content is less than 0.01ppm, and the oxygen content is less than 0.01 ppm): the desired electrolyte was obtained by uniformly mixing 86wt% of the base electrolyte, 1wt% of lifsi, and 7wt% of lipff 6.
The function of the invention is as follows: compared with the comparative example 1, the lithium salt LiTFSI which does not react with water to generate HF is used in the lithium salt part, so that the corrosion of a current collector of the aluminum-plated composite membrane can be improved, the high-temperature storage capacity retention rate, the capacity recovery rate and the room-temperature cycle performance of the battery are improved, and the alternating-current internal resistance and the positive iron ion elution quantity of the battery are reduced.
Example 3
Preparing the electrolyte of the lithium ion battery in a glove box (the moisture content is less than 0.01ppm, and the oxygen content is less than 0.01 ppm): the required electrolyte was obtained by uniformly mixing 86wt% of the base electrolyte and 14wt% of LiFSI.
The function of the invention is as follows: compared with the embodiment 1, the lithium salt LiFSI which is completely used and does not react with water to generate HF can further improve the corrosion of the current collector of the aluminum-plated composite membrane, improve the high-temperature storage capacity retention rate, the capacity recovery rate and the room-temperature cycle performance of the battery, and reduce the alternating internal resistance of the battery and the elution amount of the iron ions of the positive electrode.
Example 4
Preparing the electrolyte of the lithium ion battery in a glove box (the moisture content is less than 0.01ppm, and the oxygen content is less than 0.01 ppm): mixing 85.8wt% of base electrolyte, 14wt% of LiFSI, 0.2wt% of IPDI uniformly to obtain the desired electrolyte.
The function of the invention is as follows: compared with the embodiment 1, the application of the water/HF additive IPDI can further reduce the HF content in a battery system, improve the corrosion of a current collector of the aluminized composite film, improve the high-temperature storage capacity retention rate, the capacity recovery rate and the room-temperature cycle performance of the battery, and reduce the dissolved quantity of the iron ions of the positive electrode, but the application of the additive slightly increases the SEI film impedance of the battery, thereby slightly increasing the alternating-current internal resistance of the battery.
Example 5
Preparing the electrolyte of the lithium ion battery in a glove box (the moisture content is less than 0.01ppm, and the oxygen content is less than 0.01 ppm): 85.8wt% of the base electrolyte, 14wt% of LiFSI, 0.2wt% of PTSI were uniformly mixed to obtain the desired electrolyte.
The function of the invention is as follows: compared with the embodiment 1, the use of the water/HF additive PTSI is shown to further reduce the HF content in a battery system, improve the corrosion of a current collector of an aluminized composite film, improve the high-temperature storage capacity retention rate, the capacity recovery rate and the room-temperature cycle performance of the battery, and reduce the dissolved quantity of the iron ions of the positive electrode, but the use of the additive slightly increases the SEI film impedance of the battery, thereby slightly increasing the alternating-current internal resistance of the battery.
Example 6
Preparing the electrolyte of the lithium ion battery in a glove box (the moisture content is less than 0.01ppm, and the oxygen content is less than 0.01 ppm): the desired electrolyte was obtained by uniformly mixing 85.8wt% of the base electrolyte, 14wt% of LiFSI, 0.2wt% of HDI.
The function of the invention is as follows: compared with the embodiment 1, the application of the water removal/HF additive HDI is shown to further reduce the HF content in a battery system, improve the corrosion of a current collector of the aluminum-plated composite film, improve the high-temperature storage capacity retention rate, the capacity recovery rate and the room-temperature cycle performance of the battery, and reduce the dissolved quantity of iron ions in the positive electrode, but the application of the additive slightly increases the SEI film impedance of the battery, so that the alternating-current internal resistance of the battery is slightly increased.
The invention also provides a lithium ion battery containing the functional electrolyte suitable for the aluminum-plated composite film current collector.
The preparation method comprises the following steps:
210g of PVDF powder is dissolved in 2791g of NMP, and the solution is uniformly stirred to prepare PVDF glue with 7wt% of solid content for later use. Mixing 10kg of lithium iron phosphate and 0.3kg of Super P Li as a conductive agent by using dry materials, uniformly stirring, adding the prepared PVDF glue solution into the mixed dry materials, uniformly stirring, adjusting the viscosity and solid content of the slurry to be suitable for coating, and coating the slurry on a current collector of an aluminum-plated composite membrane with the thickness of 9 mu m to obtain a positive pole piece;
preparation of a negative electrode: a dope with a solids content of 1.8wt% was prepared by dissolving 72g of CMC powder in 3928g of deionized water. 5kg of artificial graphite and 0.17kg of conductive agent are mixed and stirred uniformly, then proper amount of CMC glue solution and SBR are added, after stirring uniformly, the slurry is adjusted to the proper coating viscosity and solid content, and then the slurry is coated on a copper foil current collector with the thickness of 6 mu m to obtain a negative pole piece.
And sequentially carrying out rolling, die cutting, drying, winding, assembling and injecting the functional electrolyte suitable for the aluminized composite film current collector, sealing, forming and secondary sealing on the positive pole piece and the negative pole piece to obtain the lithium ion battery.
The positive and negative pole pieces are sequentially subjected to rolling, die cutting, drying, winding, assembling and injecting the electrolyte prepared in each embodiment, sealing, forming and secondary sealing to prepare the 4060D0-2.0Ah square soft package lithium ion battery.
The manufactured 4060D0-2.0Ah square soft package lithium ion battery is subjected to performance test in the following way:
(1) And (3) battery cycle test:
1) Charging the lithium ion battery to 3.65V (constant voltage cut-off current 0.02C) at a constant current and a constant voltage of 1C at 25 ℃, standing for 10min, then discharging to 2.0V at a constant current of 1C, standing for 10min, repeating the charging and discharging, and calculating the capacity retention rate of the lithium ion battery after 500 weeks of circulation.
2) The capacity retention rate after n cycles of the lithium ion battery = (discharge capacity after n cycles/discharge capacity of the first cycle) × 100%, and the average value of the capacity retention rates after n cycles of each group of 3 lithium ion batteries is taken as the capacity retention rate after n cycles of the lithium ion battery.
(2) And (3) testing the iron ion elution amount:
and disassembling the battery after circulation, taking out the negative pole piece, scraping the powder, and testing the iron ion content in the negative pole powder digestion solution by using ICP (inductively coupled plasma).
(3) 60-degree high-temperature storage 30D test:
1) Charging the battery to 3.65V (constant voltage cut-off current 0.02C) at constant current of 0.5C at normal temperature, standing for 10 minutes, discharging to 3.0V at constant current of 1C, standing for 10 minutes, and recording the capacity as original capacity C 0 ，
2) 100% SOC cell was placed in a 60 ℃ incubator and stored for 30 days.
3) Taking out the battery after high-temperature storage, standing at room temperature for 8h, discharging to 2.0V at constant current of 1C, and recording the capacity as C 1 Then, the mixture was charged to 3.65V (constant voltage cut-off current 0.02C) at a constant current of 0.5C, left to stand for 10 minutes, and discharged at a constant current of 1CTo 2.0V, left to stand for 10 minutes, and charged and discharged 3 times in this manner, and the maximum discharge capacity was recorded as C 2 。
4) Capacity retention ratio = C 1 /C 0 X is 100%; capacity recovery ratio = C 2 /C 0 ×100％。
The battery properties prepared according to the electrolytes of embodiment examples 1 to 6 and comparative examples 1 to 2 are shown in table 1:
TABLE 1
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A functional electrolyte suitable for an aluminized composite film current collector is characterized by comprising a base electrolyte and/or a lithium salt and/or an additive,
the basic electrolyte is prepared by the following method: firstly, mixing ethylene carbonate and methyl ethyl carbonate in a ratio of (3-5): (5-7) uniformly mixing in a glove box, adding 2-4wt% of vinylene carbonate and 1-3wt% of fluoroethylene carbonate, and uniformly mixing to obtain the ethylene carbonate/fluoroethylene carbonate composite material;
the lithium salt is one or two of LiFSI and LiPF 6;
the additive is one of IPDI, PTSI and HDI.
2. The functional electrolyte suitable for the aluminized composite film current collector according to claim 1, wherein: the moisture content in the glove box is less than 0.01ppm, and the oxygen content is less than 0.01ppm.
3. The functional electrolyte suitable for the aluminized composite film current collector according to claim 1, wherein: the mass ratio of the ethylene carbonate to the ethyl methyl carbonate is 3:7.
4. the functional electrolyte suitable for the aluminized composite film current collector according to claim 3, wherein: the proportion of the lithium salt is one of 7wt% or 14 wt%.
5. The functional electrolyte suitable for the aluminized composite film current collector according to claim 1, wherein: the vinylene carbonate content is 2wt%, and the fluoroethylene carbonate content is 1wt%.
6. The functional electrolyte suitable for the aluminized composite film current collector according to claim 5, wherein: the additive was 0.2wt%.
7. A lithium electronic battery comprising the functional electrolyte suitable for an aluminum-plated composite film current collector according to any one of claims 1 to 7.
8. A lithium ion battery according to claim 7, characterized in that it comprises the following preparation process:
preparing a positive electrode, dissolving PVDF powder in NMP, uniformly stirring to prepare a PVDF glue solution for later use, mixing and uniformly stirring dry materials of lithium iron phosphate and conductive carbon black, adding the PVDF glue solution into the mixed dry materials, uniformly stirring, adjusting the slurry to a proper coating viscosity and a proper solid content, and coating the slurry on a current collector of an aluminum-plated thick composite film to obtain a positive electrode piece;
preparing a negative electrode, dissolving CMC powder in deionized water to prepare a glue solution for later use, mixing and stirring the artificial graphite and a conductive agent uniformly, adding the CMC glue solution and SBR, stirring uniformly, adjusting the slurry to a proper coating viscosity and solid content, and coating the slurry on a thick copper foil current collector to obtain a negative electrode plate;
and sequentially carrying out rolling, die cutting, drying, winding, assembling and injecting the functional electrolyte suitable for the aluminized composite membrane current collector, sealing, forming and secondary sealing on the positive pole piece and the negative pole piece to obtain the lithium ion battery.
9. A lithium ion battery according to claim 8, characterized in that: the conductive agent is Super P Li.
10. A lithium ion battery according to claim 8, characterized in that: the lithium ion battery is a 4060D0-2.0Ah square soft package lithium ion battery.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116730880A (en) * | 2023-08-14 | 2023-09-12 | 江苏天合储能有限公司 | Electrolyte water removal additive, electrolyte and lithium ion battery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116730880A (en) * | 2023-08-14 | 2023-09-12 | 江苏天合储能有限公司 | Electrolyte water removal additive, electrolyte and lithium ion battery |
| CN116730880B (en) * | 2023-08-14 | 2023-10-27 | 江苏天合储能有限公司 | Electrolyte water removal additive, electrolyte and lithium ion battery |
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