PDOL-Based Solid Electrolyte Toward Practical Application: Opportunities and Challenges

doi:10.1007/s40820-024-01354-z

Abstract

Abstract:

Polymer solid-state lithium batteries (SSLB) are regarded as a promising energy storage technology to meet growing demand due to their high energy density and safety. Ion conductivity, interface stability and battery assembly process are still the main challenges to hurdle the commercialization of SSLB. As the main component of SSLB, poly(1,3-dioxolane) (PDOL)-based solid polymer electrolytes polymerized in-situ are becoming a promising candidate solid electrolyte, for their high ion conductivity at room temperature, good battery electrochemical performances, and simple assembly process. This review analyzes opportunities and challenges of PDOL electrolytes toward practical application for polymer SSLB. The focuses include exploring the polymerization mechanism of DOL, the performance of PDOL composite electrolytes, and the application of PDOL. Furthermore, we provide a perspective on future research directions that need to be emphasized for commercialization of PDOL-based electrolytes in SSLB. The exploration of these schemes facilitates a comprehensive and profound understanding of PDOL-based polymer electrolyte and provides new research ideas to boost them toward practical application in solid-state batteries.

Key words: Poly(1,3-dioxolane), Solid electrolyte, Polymerization mechanism, Composite electrolyte, Practical application

Hua Yang, Maoxiang Jing, Li Wang, Hong Xu, Xiaohong Yan, Xiangming He. PDOL-Based Solid Electrolyte Toward Practical Application: Opportunities and Challenges[J]. Nano-Micro Letters, 2024, 16(1): 127-.

Hua Yang, Maoxiang Jing, Li Wang, Hong Xu, Xiaohong Yan, Xiangming He. [J]. Nano-Micro Letters, 2024, 16(1): 127-.

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URL: https://www.qk.sjtu.edu.cn/nml/EN/10.1007/s40820-024-01354-z

https://www.qk.sjtu.edu.cn/nml/EN/Y2024/V16/I1/127

Figures/Tables 18

Fig. 1 Overview of research progress on PDOL polymer. a Schematic diagram of in-situ polymerization of DOL monomer inside the battery. b Number of publications related to PDOL electrolyte in each year (Keyword: Poly(1,3-dioxolane) electrolyte or PDOL electrolyte; Data from Web of Science). c Development process of PDOL polymer: The polymerization of DOL and the structure of PDOL began to be studied (1968-1972) [60,61,62], Current is used to initiate DOL polymerization (2007) [63], PDOL inhibits the shuttle effect of polysulfides in lithium-sulfur batteries (2017) [56], PDOL/DME gel electrolyte enabled stable cycle with LiFePO₄ cathode (2018) [58], Initiating DOL polymerization with anhydrous participation of trace aluminum salts (2019) [64], PDOL/PLAS thermoresponsive electrolyte prevents thermal runaway (2019) [65], Realizing normal cycling of PDOL initiated with the assistance of AlF₃ and high-voltage NCM cathode (2020) [66], Porous polyimide supported PDOL enhances the mechanical strength of the electrolyte (2022) [67], PDOL added by YSZ enables long life cycling at high voltage (2022) [68], PDOL-based cross-linked electrolyte enhances the stability of lithium metal (2023) [69]

Fig. 2 Polymerization mechanism and Li⁺ conduction mechanism of DOL. a Three polymerization mechanisms of DOL: electrochemical polymerization, electrophilic polymerization, and nucleophilic polymerization [71]. Schematic diagram of b intrachain conduction mechanism and c interchain conduction mechanism for Li.⁺ in PDOL [72]

Fig. 3 Applications of current-initiated DOL polymerization. Schematic diagram of electronic and current movements during a charging and b discharging processes. c Electrochemical polymerization mechanism of DOL. d Battery state after current-initiated DOL polymerization [45]

Fig. 4 Electrophilic polymerization mechanism of DOL [71]

Table 1 Classification of different initiators and performance comparison of the PDOL electrolyte initiated by them

Type of initiator	Initiator	Initiation factor	Initiator content	DOL conversion rate (%)	PDOL molecular weight	Electrolyte state	Ionic conductivity (mS cm⁻¹)	Oxidation potential (V)	Refs
Lithium salt	LiPF₆	Protonic acid	2.0 M	91	~ 53 000 (Mn)	Gel	3.8	4.6	[58]
	LiPF₆	Protonic acid	1.0 wt%	98.5	23 588 (Mw)	Solid	0.28	5.2	[68]
	LiDFOB	Protonic acid	0.3 M	90	/	Gel	0.39	5.1	[75]
	LiBF₄	Protonic acid	0.2 M	81.2	-	Solid	0.3	4.9	[76]
	LiFSI	Protonic acid	3.5 M	75	-	Gel	7.9	4.7	[77]
Aluminum salt	Al(OTf)₃	Lewis acid	0.5 mM	86	15 000 (Mn)	Solid	1.1	5.0	[64]
	Al(OTf)₃ + AlF₃	Lewis acid	0.5 mM + 0.3 M	12	18 000 (Mw)	Solid	1.8	4.7	[66]
	AlI₃	Lewis acid	600 ppm	84	-	Gel	-	-	[57]
Tin salt	Sn(OTf)₂	Lewis acid	2.0 mM	90	12 417 (Mw)	Gel	6.2 × 10^-2	4.9	[78]
Tin salt	SnF₂	Lewis acid	1.5 wt%	92	29 552 (Mw)	Solid	1.7 × 10^-2	5.0	[79]
Other salts	ZnCl₂	Lewis acid	25 wt%	-	51 798 (Mn)	-	-	-	[50]
	Sc(OTf)₃	Lewis acid	1.0 mM	84	48 963 (Mn)	Solid	8.7 × 10^-2	~ 5.0	[80]
	Mg(OTf)₂	Lewis acid	1.0 wt%	79.9	~ 57 000 (Mn)	Solid	0.5	4.3	[81]
Acidized materials	Acidized Al₂O₃	Protonic acid	4.0 wt%	89.6	32 000 (Mn)	Gel	3.37	4.5	[82]
Acidized materials	Acidized CNT paper	Protonic acid	-	-	-	Gel	-	-	[56]
Organic materials	TB	Protonic acid	3.0 wt%	89	-	Solid	1.16	4.8	[83]
	S(C₂H₄O₄)	Lewis acid	0.3 M	88.2	5 391 (Mn)	Solid	0.38	4.7	[84]
	HFiP	Nucleophilic	0.5 wt%	67	-	Gel	1.6	4.7	[85]

Fig. 5 Schematic diagram of LiPF₆-initiated DOL polymerization process. a Structure of DOL-PF₅ obtained from the 3ps QM-MD simulation of PF₅-DOL system. b Four possible paths of DOL ring-opening polymerization under the action of PF₅ and c reaction Gibbs free energy [86]

Fig. 6 LiDFOB (LiBF₄) or LiFSI initiated DOL polymerization. a Schematic illustration of the LiDFOB initiated DOL ring-opening polymerization process. b Interphase evolution of ordinary non-in situ polymer electrolytes leads to incomplete interface contact, resulting in uneven ion transport and rapid growth of lithium dendrites [87]. c LiDFOB in-situ initiated polymerization of PDOL electrolyte generates SEI rich in boron oxide compounds at the electrolyte/lithium anode interface, which guides ion uniform deposition, resulting in a more stable interphase and longer cycle life. d LiFSI initiates DOL ring-opening polymerization process. e DOL polymerization conversion rate at different LiFSI content and standing time. f Comparison of ionic conductivity of PDOL gel electrolyte initiated by LiFSI with other PDOL electrolytes. g TOF-SIMS of C + , F + , S + , N + and Li + species on the lithium surface after cycling in the gel electrolyte: species concentration at initial sputtering [77]

Fig. 7 Aluminum salt initiates DOL polymerization. a Mechanism of DOL polymerization initiated by Al(OTf)₃. b DOL polymerization conversion rate and c molecular weight of PDOL initiated by different aluminum salt initiators content [64]. After adding different contents of AlF₃, d the molecular weight and dispersity of PDOL, and e cycle life of PDOL [66]

Fig. 8 Scandium salt and TB initiate DOL polymerization. a Mechanism of DOL polymerization initiated by Sc(SO₃CF₃)₃. b DOL polymerization conversion and c ionic conductivity of PDOL electrolyte initiated with different initiator concentrations [92]. d TB initiates the DOL polymerization process. e DOL polymerization conversion rate and f room temperature ionic conductivity initiated by different TB contents [83]

Fig. 9 Nucleophilic polymerization mechanism of DOL. a Some free radicals generated from the decomposition of HFiP and their free energy for ring-opening reactions with DOL. b Schematic diagram of HFiP initiated nucleophilic polymerization of DOL [85]

Fig. 10 Contact mode and interface optimization between PDOL electrolyte and solid-state electrode. a Differences in interface contact modes between electrolytes and solid-state electrodes in ex-situ polymerization and in-situ polymerization [64]. b The uneven deposition of lithium ions on common lithium metal anodes leads to rapid growth of lithium dendrites: in areas where lithium ions are concentrated and deposited, it will further guide the aggregation of ions and currents, leading to the growth of dendrites. c In the SnF₂-initiated PDOL electrolyte, the initiator undergoes a reaction with lithium to generate Li-Sn alloy, and it then forms a robust LiF/Li₅Sn₂-rich SEI incorporating LiF. The SEI facilitates the homogeneous deposition of lithium ions and the even distribution of current, providing protection to the lithium metal anode [79]. d Mechanism diagram of proton corrosion of aluminum current collector caused by Lewis acid interface reaction. e Mechanism diagram of aluminum current collector corrosion inhibition after adding AlF₃ [66]

Fig. 11 Improvement of PDOL electrolyte performance by plasticizers. a PDOL polymers without plasticizers possess a significant amount of crystalline domains in their structure, which hinders the mobility of polymer chains. b The addition of plasticizers to PDOL increases the amorphous domains, facilitating chain segment mobility and resulting in enhanced ion conductivity. c The reported types of plasticizers and their enhancements on the performance of PDOL polymers. d The internal rotational motion of N₁₂₂₂FSI leads to orientation disorder and the generation of lattice vacancies in PDOL, thereby enhancing ion conductivity [87]. e The effect of different SN contents on the ion conductivity of PDOL GPE. f The CEI and SEI gradually formed during the cycling process of GPE protect the cathode and anode, respectively [75]

Fig. 12 Function and classification of support skeleton. a In the absence of a support skeleton, the electrode may come into contact and experience short circuits under external pressure during the in-situ polymerization process of DOL. b The presence of support skeletons effectively serves as a mechanical barrier, preventing electrode contact and mitigating the risk of short circuits during the in-situ polymerization process. c The types of support skeletons and their corresponding advantages, they can be broadly categorized into two main groups: polymer-based and inorganic-based materials. d Schematic diagram of the battery structure after DOL gradient polymerization initiated by modified PE, the densely polymerized PDOL solid electrolyte adjacent to the anode serves as a protective barrier for the lithium metal, while the partially polymerized PDOL gel electrolyte in close proximity to the porous cathode effectively permeates and infiltrates the electrode [131]. e Schematic diagram of bidirectional gradient polymerization of DOL on modified cellulose paper [132]. f Schematic diagram of the interphase layer between electrolyte and LP to enhance ion conductivity [76]

Fig. 13 Inorganic fiber materials as PDOL support skeleton. a The precursor of inorganic materials is electrospun to prepare a fiber network at high voltage. b Inorganic material precursors are sintered to form inorganic fiber support skeletons. c Structural diagram of a battery supported by an inorganic fiber skeleton through in-situ polymerization. d The interface between Al₂O₃ nanowires and PDOL polymer segments constructs a high-speed ion transport channel, accelerating Li⁺ transport [92]. e The oxygen atoms of PDOL and the Si-O bonds of SiO₂ collectively create a highly efficient pathway for Li⁺ migration [139]. f LLTO NFs possess Li⁺ transport capability, while the interface between LLTO NFs and PDOL also exhibits high-speed Li⁺ transport capability, the synergistic conduction of both components enhances the overall ionic conductivity of the electrolyte [80]

Fig. 14 Inorganic materials enhance the performance of PDOL. a Schematic diagram of PEG grafting on the surface of SiO₂ and co-crystallization with PDOL. b Average coulombic efficiency for 200 cycles of Li//Cu battery assembled with PDOL-SiO₂ composite electrolyte [151]. c DFT calculated ring-opening binding energy of DOL monomer with initiator, ZrO₂, zirconium atom on YSZ and oxygen vacancy on YSZ. d The auxiliary activation of YSZ substantially enhances the monomer conversion rate of DOL, resulting in a significant improvement in the high voltage capability of the electrolyte, this enhancement enables the attainment of a long service life that aligns with high voltage cathode materials [68]

Table 2 Cyclic performance of PDOL polymer electrolyte matched with different cathodes

Battery type	Cathode materials	Initiator	Additive	Voltage range (V)	Initial specific capacity (mAh g⁻¹)	Rate (C)	Cycle number	Capacity retention (%)	Refs
Lithium-sulfur batteries	Sulfur	ACNTP	-	1.7-3.0	683	1.0	400	66.5	[56]
	Sulfur	LiPF₆	DME	1.8-3.0	1005	0.5	500	73.7	[58]
	Sulfur	LiPF₆	DME/Al₂O₃	1.8-3.0	1102	0.1	200	73.0	[59]
	Sulfur	LiFSI	DME	1.7-2.8	910	0.2	300	75.5	[77]
	Sulfur	HFiP	DME	1.8-2.8	1025	0.5	500	68.1	[85]
	Sulfur	LiPF₆	DME	1.7-2.8	870	0.1	500	45.0	[163]
Lithium-ion batteries	LFP	LiPF₆	DME	2.5-4.0	137	0.5	700	95.6	[58]
	LFP	LiDFOB	SN	2.5-4.0	127	1.0	1 000	83.55	[75]
	LFP	LiFSI	DME	2.5-3.8	147	1.0	500	69.3	[77]
	LFP	Sc(OTf)₃	-	2.5-4.0	155	0.5	200	83.5	[91]
	LFP	Al(OTf)₃	PDA	3-3.75	145	1.0	200	87.1	[137]
	LFP	Y(OTf)₃	LLZTO	2.8-3.8	135	0.2	200	~ 70.0	[142]
	LFP	LiPF₆	PI/DME	2.5-3.7	152	0.5	200	91.8	[67]
	LFP	Mg(OTf)₂	FEC	2.8-4.2	127	1.0	2 000	94.0	[81]
	LFP	LiDFOB	FEC/SN	2.8-4.3	142	2.0	1 000	95.0	[123]
	NCM622	LiPF₆	DME	2.8-4.3	165	0.1	100	90.9	[58]
	NCM622	Al(OTf)₃	AlF₃	2.8-4.2	160	0.5	30	80	[66]
	NCM622	LiPF₆	-	2.8-4.3	138	0.5	300	85	[129]
	NCM622	LiPF₆	YSZ	2.8-4.3	165	0.5	800	74	[68]
	NCM523	LiFSI	-	3.0-4.3	136	0.1	100	94	[89]
	NCM811	LiDFOB	FEC/SN	2.8-4.3	145	0.2	100	70.6	[123]
	NCM83	S(C₂H₄O₄)	-	2.8-4.5	205	0.5	100	89.5	[84]
	LCO	LiDFOB	SN	2.8-4.3	140	0.1	60	57.1	[75]
	LMFP	LiBF₄	TTE	3.0-4.3	130	0.2	100	~ 90	[76]
Sodium-ion batteries	NVP	Al(OTf)₃	FEC	2.0-3.8	99	5.0	2 000	93.6	[125]

Fig. 15 Low temperature performance of PDOL. a Li-O integrated RDF of PDOL and PEO (r_mono-Li = 8:1). b Local coordination number of Li⁺ and O atoms of PDOL and PEO at −30 °C (r_mono-Li = 8:1) [166]. c The first Li⁺ solvation sheath and snapshot of QSPE from MD simulation for QSPE at -20 °C. d The coordination numbers of Li⁺ in the first solvation shell (3 Å) in QSPE at − 20 °C [128]

Fig. 16 Advantages of PDOL polymer electrolytes and existing challenges in practical applications

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