GUO Yuxiang, HUANG Liqiang, WANG Gang, WANG Hongzhi. Dual-lithium-salt Gel Complex Electrolyte: Kev Npaj thiab Daim Ntawv Thov hauv Lithium-hlau roj teeb. Phau ntawv Journal of Inorganic Materials, 2023, 38(7): 785-792 DOI:10.15541/jim20220761
Abstract
Metallic Li yog ib qho ntawm cov anodes zoo tshaj plaws rau lub zog siab ceev lithium-ion roj teeb vim nws cov theoretical tshwj xeeb muaj peev xwm, tsis tshua muaj peev xwm txo qis thiab muaj peev xwm ntau. Txawm li cas los xij, daim ntawv thov ntawm Li anodes raug kev txom nyem los ntawm kev tsis sib haum xeeb nrog cov tshuaj organic kua electrolyte. Nyob rau hauv no, ib tug gel complex electrolyte (GCE) nrog txaus siab compatibility nrog metallic Li anode yog tsim los ntawm nyob rau hauv situ polymerization. Ob chav lithium ntsev system nkag mus rau hauv cov electrolyte tuaj yeem koom tes nrog cov khoom siv polymer, uas nthuav dav lub qhov rais hluav taws xob ntawm cov electrolyte mus rau 5.26 V piv rau 3.92 V ntawm cov khoom lag luam electrolyte, thiab tau txais ionic conductivity siab ntawm 1 × 10-3 S· cm-1 ntawm 30 degree thiab. Cov txiaj ntsig ntawm morphology tus cwj pwm thiab kev tsom xam ntawm Li anode nto qhia tias GCE nthuav tawm cov txiaj ntsig tiv thaiv zoo ntawm lithium hlau nyob rau hauv cov xwm txheej ntawm ob lub lithium ntsev system, thiab ntim cov nyhuv thiab dendrite kev loj hlob ntawm Li anode yog pom tseeb inhibited. Nyob rau tib lub sijhawm, cov lithium hlau tag nrho cov roj teeb, sib sau ua ke nrog cov khoom lag luam lithium hlau phosphate (LiFePO4) cathode khoom, nthuav tawm kev ua haujlwm zoo heev thiab kev ua haujlwm zoo. Lub peev xwm tuav tau ntawm lub roj teeb mus txog 92.95 feem pua tom qab 200 cycles ntawm qhov tam sim no ntawm 0.2C (1C=0.67 mA·cm-2) ntawm 25 degree . Txoj kev tshawb no qhia tau hais tias GCE tuaj yeem txhim kho kev nyab xeeb, kev ruaj ntseg thiab kev ua tau zoo ntawm electrochemical kev ua tau zoo ntawm lithium-hlau roj teeb, uas yuav tsum muab lub tswv yim rau universal quasi-solid electrolyte tsim.
Ntsiab lus:hlau Li; nyob rau hauv-situ polymerization; gel complex electrolyte
Txij li thaum lub hom phiaj "Double Carbon" tau muab tso rau hauv 2020, Tuam Tshoj tab tom ntsib txoj kev hloov kho hluav taws xob tsis tau pom dua. Tuam Tshoj yuav tsum ua kom tiav qhov kev txo qis ntawm carbon emissions nyob rau hauv 30 xyoo tom ntej, thiab ntsuab zog yuav maj mam ntxiv dag zog mus txog rau thaum nws hloov lub "monopoly" txoj hauj lwm ntawm ib txwm fossil zog. Raws li ib feem tseem ceeb ntawm lub zog tauj dua tshiab, lithium-ion roj teeb thev naus laus zis tau nyiam cov neeg siv khoom thoob plaws thaum nws tawm los. Tam sim no, ntxiv rau kev ua lub zog tseem ceeb ntawm 3C cov khoom siv hluav taws xob, daim ntawv thov ntawm cov roj teeb lithium hauv kev lag luam tsheb, aerospace thiab cov phiajcim ntse tau maj mam nce, uas ua rau muaj kev xav tau ntau dua rau nws cov kev ua tau zoo. Yuav kom tau txais kev caij nkoj ntev dua, cov roj teeb lithium fais fab yuav tsum tsim kom muaj lub roj teeb uas muaj zog dua. Ntawm lawv, lithium hlau nrog ultra-siab tshwj xeeb muaj peev xwm (3860 mAh g-1) thiab tsis tshua muaj peev xwm txo qis (-3.04 V (vs SHE)) yuav tsum yog cov khoom siv anode rau tiam tom ntej. ntawm high-power density roj teeb. Txawm li cas los xij, thaum lithium hlau nyob rau hauv kev sib cuag nrog cov organic kua electrolytes, cov kev cuam tshuam sab txuas ntxiv tshwm sim ntawm qhov sib cuam tshuam, ua rau kev loj hlob ntawm lithium dendrites tsis tuaj yeem, tho qhov sib cais sab hauv ntawm lub roj teeb, ua rau luv luv thiab txawm tias muaj teeb meem kev nyab xeeb. Hauv kev teb rau qhov tsis xws luag, nws feem ntau xav tias yuav siv cov khoom siv electrolyte es tsis txhob ua kua electrolyte los txhim kho kev nyab xeeb ntawm lub roj teeb. Txawm li cas los xij, nws qhov qis qis hauv chav ionic conductivity thiab tsis zoo interfacial compatibility tiag cuam tshuam nws txoj kev txhim kho ntxiv thiab kev siv.
Tawm tsam keeb kwm yav dhau los no, gel-state electrolytes muaj peev xwm ntsuas kev sib cuag ntawm lub ntsej muag thiab ionic conductivity tau txais kev saib xyuas ntxiv. Tan Shuangjie et al tau tsim ib qho uas tsis yog-flammable gel-state electrolyte los ntawm immobilizing nplaim-retardant organophosphates nyob rau hauv ib tug polymer matrix ntawm polyvinylene carbonate nrog siab mechanical zog. Cov electrolyte muaj qhov zoo ntawm kev ua haujlwm siab ionic thiab lithium-ion hloov pauv tus lej, tsis muaj nplaim taws, siab txhua yam muaj zog, thiab zoo electrochemical compatibility. Tsis tas li ntawd, cov gel electrolyte tsim nyob rau hauv lub roj teeb los ntawm in-situ polymerization muaj cov yam ntxwv ntawm tsawg viscosity, yooj yim tuav, thiab muaj zog wetting muaj peev xwm, uas muaj peev xwm nkag mus rau tag nrho cov active cov ntaub ntawv thiab tsim zoo tagnrho interfacial kev sib cuag, yog li tau txais ib tug zoo ion tsiv teb tsaws txoj kev. . Piv txwv li, Guo Yuguo pawg tshawb fawb tau sib xyaw cov tshuaj ether-based monomer 1,3-dioxolane (1,3-Dioxolane, DOL) nrog 1,2-dimethoxyethane (1,{{15}) }Dimethoxyethane, DME), kev lag luam Lithium Hexafluorophosphate (LiPF6) raws li cov ntsev lithium tuaj yeem ua rau lub nplhaib-qhib polymerization ntawm DOL tib lub sijhawm, thiab cov gel-xeev electrolyte tshiab uas tuaj yeem ua haujlwm ruaj khov hauv lithium-sulfur roj teeb thiab cov roj teeb coj mus muag cathode. ua tau. Txawm hais tias polyether-raws li polymer yog ib qho ntawm cov electrolytes ruaj khov tshaj plaws rau lithium hlau anodes, nws cov qhov rai electrochemical nqaim thiab qis ionic conductivity ntawm chav tsev kub txwv nws daim ntawv thov nyob rau hauv high-power density roj teeb. Txawm hais tias LiPF6 muaj qhov zoo tshaj plaws ionic conductivity thiab zoo heev electrode compatibility, nws muaj qhov teeb meem ntawm tsis zoo electrochemical stability. Yog li ntawd, txhawm rau txhim kho gel-state electrolyte nrog kev ua haujlwm zoo, nws yog ib qho tsim nyog los xaiv cov khoom tsim nyog polymer, lithium ntsev thiab lwm yam khoom.
Txhawm rau sib npaug kev sib raug zoo ntawm cov conductivity, high-voltage stability, thiab electrode compatibility, ib tug khoom-kua composite high-performance GCE tau tsim nyob rau hauv txoj kev tshawb no. Cov txheej txheem thermally pib hauv-situ polymerization tau saws, PEGDA tau siv los ua cov monomer, cov kuab tshuaj sib xyaw ntawm Ethylene Carbonate thiab Diethyl Carbonate tau ntxiv, thiab LiTFSI thiab LiDFOB tau qhia ua ob chav lithium ntsev ua haujlwm ua ke nrog cov khoom siv polymer. Thaum txhim kho cov electrochemical kev ua tau zoo, lub interface stability ntawm lub electrolyte thiab lithium hlau anode yog ntxiv txhim khu kev qha.
1 Kev sim txoj kev
1.1 Kev Npaj GCE
LiTFSI, LiDFOB, EC thiab DEC (Suzhou Duoduo Chemical Technology Co., Ltd.) yog tag nrho cov khoom siv roj teeb uas tsis muaj dej. Cov EC thiab DEC reagents tau sib xyaw, thiab LiTFSI thiab LiDFOB tau hnyav thiab yaj hauv cov kuab tshuaj. Qhov npaj ob-ntsev ntsev electrolyte (Liquid Electrolyte, LE) yog ib qho EC/DEC (ntim piv 1: 1) tov ntawm 1 mol/L LiTFSI thiab 0.2 mol/L LiDFOB. PEGDA ( Ntau dua lossis sib npaug li 99 feem pua , Mn=400) thiab azobisisobutyronitrile (Azodiisobutyronitrile, AIBN, 98 feem pua) tau yuav los ntawm Shanghai Aladdin Reagent Co., Ltd. Cov tshuaj ua ntej ntawm GCE tau npaj los ntawm kev sib xyaw PEGDA thiab LE , thiab feem ntau ntawm PEGDA yog 10 feem pua, 20 feem pua, thiab 30 feem pua. Ntxiv 1 feem pua ntawm cov khoom siv thermal pib AIBN thiab do zoo. PEGDA precursor tov yog rhuab ntawm 70 degree rau 2 h kom tau cov polymerized PEGDA-raws li gel composite electrolytes, uas yog hu ua GCE-x (x=10, 20, 30). Cov kev sim saum toj no tau ua tiav nyob rau hauv ib lub thawv uas tsis muaj dej thiab tsis muaj oxygen.
1.2 Sib dhos ntawm roj teeb
Roj teeb sib dhos ntawm CR2025 khawm cell (316 stainless hlau, SS), lithium hlau ntawv (14 hli × 0.45 hli, Li), txhuas ntawv ci (roj teeb qib). Raws li kev xeem sib txawv, SS|| SS roj teeb, Li||SS roj teeb, Li||Li roj teeb, thiab Li||LiFePO4 roj teeb tau sib sau ua ke hauv lub hnab looj tes. Qhov loj piv ntawm LiFePO4, Ketjen Dub, thiab Polyvinylidene Difluoride (PVDF) nyob rau hauv cov khoom siv cathode yog 90 : 5 : 5, thiab lub peev xwm ntawm thaj chaw yog 0.67 mAh·cm-2. Saib Cov Khoom Siv Ntxiv S1 kom paub meej txog cov txheej txheem kev npaj ntawm daim ntawv zoo electrode thiab cov txheej txheem sib dhos roj teeb.
1.3 Cov yam ntxwv ntawm cov khoom siv
Cov pab pawg ua haujlwm thiab cov qauv tshuaj lom neeg ntawm PEGDA monomers thiab lawv cov polymers tau txheeb xyuas siv lub Thermo NiColet iS50 Fourier Transform Infrared Spectrometer (Fourier Transform Infrared Spectrometer, FT-IR) los ntawm Thermo Fisher Scientific Corporation ntawm Tebchaws Meskas, nrog lub wavelength ntau ntawm {{ 2}} cm -1 . Lub crystallinity ntawm gel-state electrolytes nrog cov khoom sib txawv ntawm cov polymer yog tus cwj pwm los ntawm D2 Phaser X-ray diffractometer (X-Ray Diffractometer, XRD) los ntawm Bruker AXS Company, Lub teb chaws Yelemees, thiab cov scanning ntau yog 2θ=5 degree ~ 80 degree. Lub OCA40Micro lub kaum sab xis ntsuas ntsuas ntawm Beijing Dongfang Defei Instrument Co., Ltd. tau siv los kuaj lub kaum sab xis ntawm cov kev daws teeb meem ua ntej nrog PEGDA cov ntsiab lus sib txawv ntawm daim ntawv LiFePO4 electrode. Lub microscopic morphology ntawm ntu ntu thiab saum npoo ntawm cov ntawv hlau lithium tau pom los ntawm JElectronics JSM-7500F field emission scanning electron microscope (Field Emission Scanning Electron Microscope, FESEM). Cov ntaub ntawv tseem ceeb nyob rau saum npoo ntawm cov ntawv hlau lithium tau txheeb xyuas siv Escalab 250Xi X-ray photoelectron spectrometer (X-ray Photoelectron Spectroscopy, XPS) los ntawm Thermo Fisher Scientific Corporation ntawm Tebchaws Meskas.
1.4 Electrochemical xeem
Lub qhov rais electrochemical stability ntawm cov electrolyte tau kuaj los ntawm linear sweep voltammetry (LSV), qhov voltage ntau yog los ntawm qhib Circuit Court voltage (OCV) mus rau 6 V, thiab cheb tus nqi yog 1 mV·s -1. Qhov ntau zaus ntawm Electrochemical Impedance Spectroscopy (EIS) yog 10-2 ~ 106 Hz, thiab qhov hluav taws xob perturbation yog 10 mV. Chronoamperometry tau siv los ntsuas qhov kev tsiv teb tsaws ntawm lithium ions hauv electrolyte, qhov sib txawv muaj peev xwm tau teeb tsa rau 10 mV, thiab lub sijhawm yog 800 s, thiab cov neeg tsiv teb tsaws ntawm lithium ions tau txais raws li cov qauv (1):
Ntawm lawv, tLi ntxiv yog tus lej hloov pauv ntawm lithium ions, ΔV yog qhov sib txawv, R{{{0}}} thiab RS yog qhov cuam tshuam cuam tshuam ntawm cov electrode thiab electrolyte ua ntej thiab tom qab kuaj, feem, thiab I0 thiab IS yog thawj lub xeev tam sim no thiab lub xeev khov kho tam sim no, feem. Cov kev ntsuam xyuas saum toj no tau ua tiav ntawm PARSTAT MC multi-channel electrochemical workstation ntawm AMETEK, Tebchaws Asmeskas. Kev ntsuas hluav taws xob ua haujlwm ntawm lub roj teeb tau sim siv LAND CT3001A-1U roj teeb sim platform ntawm Wuhan Landian Electronics Co., Ltd.
2 Cov txiaj ntsig thiab kev sib tham
2.1 Kev npaj thiab kev txheeb xyuas cov qauv ntawm GCE
Hauv txoj kev tshawb no, PEGDA tau siv los ua monomer, AIBN tau siv los ua polymerization pib, thiab EC thiab DEC tau qhia ua plasticizers. Ib qho gel-state electrolyte nrog cross-linked polymeric polyethylene glycol dimethacrylate (p(PEGDA)) tau ua ke ntawm 70 degree. Cov tshuaj tiv thaiv polymerization yog qhia hauv daim duab 1(a). Tom qab ntxiv cov thermal pib AIBN, PEGDA nrog ob lub davhlau ya nyob twg C=C pab pawg tau nrawm nrawm rau kev sib xyaw ua ke ntawm homopolymerization thaum cua sov rau 70 degree. Cov chains nquag ntawm AIBN ua rau cov saw hlau molecular txuas nrog ib leeg lossis sab hauv, thiab thaum kawg tau txais p (PEGDA) network skeleton qauv, thiab ua tiav siv txoj hauv kev polymerization kom tau txais gel lub xeev electrolyte hauv lub roj teeb. Raws li pom hauv daim duab S1, peb qhov kev daws teeb meem ua ntej nrog PEGDA cov ntsiab lus sib txawv txhua qhov pom tias muaj kev ntub dej zoo ntawm LiFePO4 zoo electrode daim ntawv, uas yog tus yuam sij kom tau txais kev sib cuag zoo ntawm cov electrolyte thiab electrode.
Fig. 1 Kev npaj thiab kev txheeb xyuas cov qauv ntawm GCE
(a) Polymerization cov tshuaj tiv thaiv ntawm PEGDA; (b) Cov duab kho qhov muag ntawm GCE-x; (c, d) FT-IR spectra of GCE-20, PEGDA and LE; (e) XRD qauv ntawm GCE-x; Cov duab muaj yeeb yuj muaj nyob rau ntawm lub vev xaib
Txhawm rau kom tau txais GCE nrog cov ionic conductivity siab, LiTFSI, uas muaj kev sib cais siab hauv cov polymer, tau siv los ua cov lithium ntsev, thiab 0.2 mol / L LiDFOB tau qhia los tsim cov gel network ntawm ob chav ntsev system. LiDFOB muaj zoo solubility thiab thermal stability, tshwj xeeb tshaj yog nyob rau hauv film-forming zog. Thaum cov kuab tshuaj carbonate nyob rau hauv kev sib cuag nrog lithium hlau anodes, ib tug loj tus naj npawb ntawm xoob ntxeem tau los yog dendritic lithium deposition txheej yuav tsim nyob rau saum npoo ntawm lithium hlau. Kev taw qhia ntawm LiDFOB tuaj yeem pab tsim HF-dawb khoom electrolyte interphase (Solid Electrolyte Interphase, SEI) txheej thiab txhim kho kev sib raug zoo nrog lithium hlau anodes. Nyob rau tib lub sijhawm, LiTFSI muaj cov nyhuv corrosive rau cov hlau tam sim no, thaum LiDFOB tuaj yeem cuam tshuam cov hlau txhuas thiab txo cov nyhuv corrosion ntawm LiTFSI ntawm cov khoom tam sim no. Txawm li cas los xij, ib leeg- ntsev electrolyte ntawm LiDFOB nthuav tawm ntau dua impedance dua li LiTFSI-LiDFOB dual-ntsev electrolyte ntawm tib qhov concentration. Raws li pom nyob rau hauv daim duab S2, lub Li||LiFePO4 roj teeb tau sib sau ua ke siv 1.2 mol/L LiDFOB thiab LiTFSI-LiDFOB gel electrolytes, feem, thiab impedance ntawm LiTFSI-LiDFOB roj teeb yog ho me me.
Cov txiaj ntsig kev tshawb fawb tam sim no qhia tau tias LiTFSI thiab LiDFOB tuaj yeem muaj kev sib koom ua ke, txhim kho kev sib raug zoo ntawm electrolyte nrog lithium hlau anode. Jiao Shung et al. siv XPS thiab FT-IR kom pom tias ob lub ntsev electrolyte ntawm LiTFSI thiab LiDFOB tuaj yeem hla cov txhuas tam sim no cov khoom siv hluav taws xob zoo thiab tsim cov txheej txheem SEI ruaj khov rau saum npoo ntawm lithium hlau tsis zoo electrode kom ua tiav lub caij nyoog ruaj khov. ntawm lithium hlau roj teeb. Ntawm no, Liu Yue et al. [26] siv hybrid molecular dynamics simulation los kawm txog kev sib koom ua haujlwm ntawm LiTFSI thiab LiDFOB hauv lithium hlau roj teeb, thiab piav qhia txog kev tiv thaiv ntawm LiTFSI ntawm LiDFOB. Cov kev tshawb fawb tau pom tias BO daim ntawv cog lus ntawm LiDFOB yog qhov tsis muaj zog tshaj plaws thiab muaj feem cuam tshuam. LiDFOB yuav sai sai decompose nyob rau hauv qhov kev txiav txim ntawm dawb radicals thiab react nrog lithium hlau los tsim dawb Li0 thiab boron atoms. Lub boron atom insertion cov tshuaj tiv thaiv ua rau cov kuab tshuaj molecules nyob rau hauv cov electrolyte decompose, thiab qhov tshwm sim molecular fragments yuav txuas ntxiv mus nrog lithium ntsev molecular fragments thiab boron atoms. Hauv cov txheej txheem ntsev dilithium, txawm li cas los xij, LiTFSI decomposes nyiam, tso siab rau "kev txi mechanism" los tiv thaiv LiDFOB, tus nqi decomposition ntawm LiDFOB txo qis heev. Li no txo tus naj npawb ntawm cov dawb Li0 thiab boron atoms, uas tuaj yeem txhim kho SEI txheej thiab tiv thaiv lithium hlau anode.
Raws li pom nyob rau hauv daim duab 1(b), GCE-x yog ib yam nkaus thiab pob tshab jelly-zoo li, tsis muaj dej ntxiv lawm. Txhawm rau txheeb xyuas monomer polymerization ntxiv, FT-IR tau siv los ua tus yam ntxwv ntawm cov qauv tshuaj ntawm LE, PEGDA monomer thiab GCE-20. Raws li pom nyob rau hauv daim duab 1(c), tag nrho peb cov qauv qhia tau hais tias lub ncov haum ntawm C=O stretching vibration (~1726 cm-1). Lub ncov siab ntawm 1280 cm-1 ntawm GCE sib raug rau cov antisymmetric thiab symmetric stretching peaks ntawm ether daim ntawv cog lus, qhia tias -(CH2CH2)n- nyob rau hauv lub monomer tsis puas thaum lub sij hawm lub polymerization. Lub ncov ntawm 1095 thiab 2867 cm-1 yog -COOR thiab -CH2, feem. Raws li pom hauv daim duab 1(d), tus yam ntxwv ncov ntawm C=C daim ntawv cog lus ntawm PEGDA nyob ntawm 1616-1636 cm-1, tab sis nws ploj mus hauv GCE, qhia tias PEGDA tau raug polymerized kiag li.
Txij li thaum lithium ions tsiv teb tsaws tsuas yog hauv thaj av amorphous ntawm GCE, txo cov crystallinity ntawm electrolyte yog qhov zoo los txhim kho cov ionic conductivity. Daim duab 1(e) yog XRD qauv ntawm GCE-x. Peb hom kev kuaj tag nrho muaj qhov tshwj xeeb diffraction absorption ncov ntawm 2θ=21 degree, qhia tias cov electrolyte npaj tau muaj thaj tsam amorphous nrog rau me me ntawm crystallites. Raws li cov ntsiab lus ntawm PEGDA nce, lub ncov cheeb tsam ntawm lub spectrum nce loj, qhov feem ntawm amorphous cheeb tsam ntawm cov gel electrolyte txo, thiab cov ntsiab lus ntawm amorphous Cheebtsam nyob rau hauv lub electrolyte txo, uas yog tsis conducive rau ion migration.
2.2 Electrochemical kev ua tau zoo ntawm GCE thiab Li hlau compatibility tsom xam
Txhawm rau kawm txog kev sib raug zoo ntawm electrolytes nrog cov ntsiab lus sib txawv ntawm cov polymer nrog lithium hlau anodes hauv cov roj teeb, cov impedance spectra ntawm Li||Li symmetric batteries nrog GCE-x electrolytes hauv thawj lub xeev tau txheeb xyuas (raws li qhia hauv daim duab S3). Hauv daim duab, qhov cuam tshuam impedance qhov tseem ceeb ntawm GCE-10 thiab GCE-20 roj teeb yog ob qho tib si me, 93 thiab 152 Ω, raws li, thiab GCE -30 roj teeb nce mus txog 409 Ω. Nws qhia tau hais tias kev tsiv teb tsaws ntawm lithium ions hauv GCE nrog cov ntsiab lus polymer siab dua yuav tsum tau kov yeej qhov cuam tshuam loj ntawm kev tsiv teb tsaws, uas tsis tsim nyog rau kev ua haujlwm sai ntawm lithium ions ntawm lub interface.
Kev soj ntsuam qhov muaj peev xwm dhau ntawm Li || Li symmetric roj teeb nyob rau hauv qhov kev ntsuas hluav taws xob hluav taws xob, peb tuaj yeem paub qhov txawv ntawm qhov sib txawv tsim los ntawm ion khub tsiv teb tsaws thaum lub sijhawm txheej txheem no, thiab tom qab ntawd ntsuas cov lithium deposition / stripping tus cwj pwm. Daim duab S4 qhia qhov voltage-time curves ntawm Li ||Li symmetric cell ntawm GCE-x. Qhov ntsuas kub yog 25 degree, thiab lub roj teeb tau them thiab tso tawm raws li qhov tam sim no tsis tu ncua nrog lub peev xwm tshwj xeeb ntawm 0.5 mAh cm-2 thiab qhov ceev tam sim no ntawm 0.5 mA cm -2. Thawj qhov muaj peev xwm dhau ntawm Li|GCE-10|Li hlwb yog 22 mV, thiab qhov hluav taws xob tau nce mus rau 137 mV tom qab 250 h. Lub overpotential ntawm GCE -30 symmetric roj teeb yog 104 mV nyob rau hauv thawj theem, thiab lub overpotential tau nce sai heev nyob rau hauv lub tom ntej cycles, mus txog ib tug ncov nqi ntawm 509 mV nyob rau hauv 227 h thiab ces poob sharply, qhia tias lub roj teeb muaj ib qho luv luv Circuit Court. Hauv qhov sib piv, GCE{19}} roj teeb tuaj yeem ua haujlwm ntawm qhov tsis muaj peev xwm dhau ze li 30 mV, thiab muaj qhov ua tau zoo tshaj plaws ntawm electrochemical. Cov hauv qab no yuav tsom mus rau GCE-20 electrolyte.
Lub ionic conductivity ntawm electrolyte ncaj qha qhia txog lub peev xwm ntawm ions mus rau hauv ib qho hluav taws xob teb. Cov ionic conductivity ntawm LE thiab GCE {{0}} tau sim ntawm 60, 50, 40, 30, 20, 10 thiab 0 degree, raws li. Raws li pom hauv daim duab 2(a), ionic conductivity ntawm GCE-20 ntawm 30 degree yog 1.00 mS cm-1, thiab thaum ntsuas kub nce mus txog 60 degree, cov conductivity nce mus txog 1.39 mS cm-1. Qhov no yog vim hais tias lub zog ua kom txo qis nrog qhov nce ntawm qhov ntsuas kub, thiab kev txav mus los ntawm cov saw hlau polymer thiab lithium ions nce. Txawm li cas los xij, qhov kev txav ceev ntawm cov saw hlau polymer yog pom tseeb cuam tshuam los ntawm qhov kub thiab txias, yog li cov conductivity ntawm GCE -20 gel electrolyte hloov ntau dua li cov tshuaj electrolyte.
Daim duab 2 Electrochemical kev ua tau zoo ntawm GCE-20
(a) Ionic conductivities ntawm LE thiab GCE-20; (b) LSV curves of LE and GCE-20; (c) Tam sim no-lub sij hawm profile ntawm Li|GCE-20|Li cell nrog inset uas qhia txog Nyquist plots; (d) Voltage-time curves of symmetric Li||Li cells assembled with LE and GCE-20; (e) Nyquist plots of Li|GCE-20|Li cell tom qab caij tsheb kauj vab; (f) Voltage-time thiab tam sim no ceev-lub sij hawm nkhaus ntawm Li|GCE-20|Li cell; Cov duab muaj yeeb yuj muaj nyob rau ntawm lub vev xaib
Kev txhim kho lub zog ceev ntawm cov roj teeb yuav tsum ua kom muaj kev ruaj ntseg ntawm cov electrolyte ntawm kev ua haujlwm siab. Cov kev tshawb fawb tau pom tias carbonyl-coordinated polymer-raws li electrolytes feem ntau muaj lub qhov rais electrochemical dav thiab zoo stability ntawm kev khiav hauj lwm voltages. Daim duab 2(b) qhia tau tias LSV nkhaus ntawm GCE-20 roj teeb pib hloov pauv ntawm 5.26 V, thiab nws tuaj yeem txiav txim siab tias lub qhov rais electrochemical ntawm GCE-20 gel electrolyte ncav cuag 5.26 V. Nyob rau hauv sib piv, lub qhov rais electrochemical ntawm lub lag luam electrolyte tsuas yog 3.92 V. Yog li ntawd, gel-lub xeev electrolyte muaj zoo heev electrochemical stability ntawm high voltage.
Tsis tas li ntawd, tus lej ntawm lithium ion tsiv teb tsaws ntawm cov electrolyte kuj yog ib qho ntawm cov ntsuas ntsuas lithium ion conductivity. Nws txhais tau tias yog qhov piv ntawm cov lithium ions dhau los ntawm ib ntu ntawm cov electrolyte perpendicular mus rau cov kev taw qhia ntawm lithium ion tsiv teb tsaws nyob rau ib chav tsev lub sij hawm rau cov sum ntawm anions thiab cations dhau los ntawm seem. Qhov siab dua tus nqi, qhov loj dua qhov kev faib ua feem ntawm lithium ions nyob rau hauv cov txheej txheem kev tsiv teb tsaws ion, thiab ntau dua qhov kev tsiv teb tsaws chaw. Daim duab 2(c) yog chronoamperometry nkhaus ntawm Li|GCE-20|Li roj teeb, qhov inset yog qhov sib piv ntawm electrochemical impedance ntawm lub roj teeb ua ntej thiab tom qab kuaj. Raws li formula (1), lithium ion migration tooj ntawm GCE-20 yog 0.21. Kev taw qhia txog cov khoom siv ntxiv lossis doping nrog cov khoom siv hauv cov khoom siv tuaj yeem tau txais ntau dua lithium ion tsiv teb tsaws tus nqi, uas tsis yog tsuas yog muaj txiaj ntsig zoo los txhim kho tus nqi thiab tawm ntawm lub roj teeb, tab sis kuj txhim kho nws lub voj voog ruaj khov.
Thaum lub sij hawm them thiab tso tawm ntawm Li || Li symmetric roj teeb, cov anions thiab cations nyob rau hauv cov electrolyte undergo counter-migration. Thaum them nyiaj, lithium ions tsiv mus rau qhov tsis zoo electrode, thiab cov anions tsiv mus rau qhov zoo electrode, thiab qhov ntxeev yog qhov tseeb thaum tso tawm. Yog li ntawd, thaum lub sij hawm them thiab tso tawm cov txheej txheem, cov ion concentration gradient ntawm qhov zoo thiab tsis zoo electrodes thiab cov hluav taws xob ua hluav taws xob maj mam nce, cuam tshuam qhov kev txav ntawm cov anions thiab cations, uas ua rau cov concentration polarization hauv lub roj teeb, ua rau muaj kev hloov pauv. nyob rau hauv overpotential. Raws li pom hauv daim duab 2(d), Li|GCE-20|Li roj teeb muaj peev xwm dhau ntawm 46 mV tom qab kev caij tsheb kauj vab ruaj khov rau 300 teev. Txawm li cas los xij, lub peev xwm dhau los ntawm Li|LE|Li roj teeb thaum lub sij hawm sim yog qhov siab dua li ntawm Li|GCE-20|Li roj teeb (65 ~ 118 mV). Qhov no yog vim qhov loj hlob lithium dendrites ua rau cov luv luv luv ntawm qee qhov chaw sab hauv. Cov txiaj ntsig tau pom tias tus cwj pwm electrochemical hauv GCE-20 roj teeb yog qhov zoo tshaj plaws. Daim duab 2(e) yog qhov kev ntsuam xyuas EIS ntawm cov roj teeb symmetrical tom qab 10, 20, 50 thiab 100 cycles. Raws li tus naj npawb ntawm cov nqi them tawm mus nce, lub roj teeb impedance yuav txo qis. Thaum lub sij hawm tus txheej txheem no, ib tug ruaj khov SEI txheej tau tsim los ntawm cov electrolyte thiab lithium hlau interface, thiab kev sib cuag interface tau optimized, thiaj li hais tias lub interface impedance poob ho.
Ntawm 25 degree, Li|GCE-20|Li roj teeb tau raug rau 10 them-tso tawm mus rau qhov ceev tam sim no ntawm 0.2, {{10} }.5, 1, 2, 0.2 thiab 0.5 mA cm{14}}, ntsig txog. Daim duab 2(f) qhia txog qhov sib txawv ntawm qhov overpotential ntawm symmetric cell nyob rau lub sij hawm thaum tus txheej txheem no. Lub overpotential ntawm qhov tsawg tam sim no yog me me thiab tuaj yeem nyob ruaj khov. Tom qab qhov ceev tam sim no nce, qhov overpotential nce raws li, thiab tsis muaj qhov nce / txo qis hauv qhov hluav taws xob thaum lub sijhawm ua haujlwm.
Lub morphology ntawm lithium daim ntawv txheej tom qab kev caij tsheb kauj vab tuaj yeem pom tus yam ntxwv ntawm kev tso nyiaj / stripping tus cwj pwm ntawm lithium hauv lub roj teeb. Lub Li||Li symmetric roj teeb tau disassembled tom qab them thiab tso tawm rau 100 h ntawm lub peev xwm ntawm 0.5 mAh cm-2 thiab tam sim no ceev ntawm 0.5 mA cm{{6} }, thiab lub microscopic morphology ntawm ntu ntu thiab saum npoo ntawm lithium hlau ntawv tau pom los ntawm FESEM. Raws li pom nyob rau hauv daim duab 3(a, b), lub thickness ntawm cov tsis kho pristine lithium ntawv yog 353 µm, thiab cov nto yog tiaj thiab du. Kev sib cuam tshuam ntawm cov kua electrolyte thiab lithium hlau ua rau cov deposition ntawm ib tug ntau ntawm xoob thiab ntxeem tau lithium deposition txheej nyob rau saum npoo ntawm lithium daim ntawv ntawm Li|LE|Li roj teeb, feem ntau nyob rau hauv cov duab zoo thiab tsis sib xws moss. Thaum lub thickness ntawm lithium hlau ntawv nce mus rau 446 µm, muaj ib tug pom tseeb ntim expansion nyhuv, thiab ib tug loj tus naj npawb ntawm dendrites yog generated. Nyob rau hauv sib piv, lub thickness ntawm cov lithium ntawv nyob rau hauv lub Li|GCE{11}}|Li roj teeb yog 391 μm, thiab cov deg deposition txheej yog ntom thiab uniform, thiab tsis muaj finely faib lithium txheej (Fig. 3(c. )). Nws qhia tau hais tias gel-state electrolyte tuaj yeem ua rau lub ntim nthuav dav ntawm lithium hlau anode. LiDFOB hauv GCE-20 tuaj yeem pab tsim cov txheej txheem SEI ruaj khov kom sib npaug ntawm lub peev xwm sab hauv ntawm lub roj teeb, thiab ncua kev loj hlob ntawm lithium dendrites los ntawm inducing uniform deposition ntawm lithium. Yog li ntawd, rau qee qhov, nws tuaj yeem ua kom zoo dua lithium deposition / stripping tus cwj pwm thiab tiv thaiv lithium hlau anode.
Fig. 3 SEM cov duab ntawm hlau Li
Hla-sectional (nce) thiab sab saum toj-saib (down) SEM cov duab ntawm (a) cov xim hlau tshiab Li thiab lithium deposition morphology hauv symmetric Li||Li hlwb nrog (b) LE thiab (c) GCE-20
Tom qab ntawd, XPS qhov chaw tsom xam tau siv los tshawb xyuas qhov muaj pes tsawg leeg ntawm SEI txheej ntawm cov lithium hlau anode nyob rau hauv qhov kev txiav txim ntawm LiTFSI-LiDFOB ob chav ntsev system GCE. Daim duab S5 yog XPS spectrum ntawm lithium hlau anode nto siv LE thiab GCE-20. Lub spectrum ntawm C1s (Fig. S5(a, d)) feem ntau muaj 4 lub teeb liab peaks, sib xws rau CC / CH ntawm 284.8 eV. Ob lub ncov ntawm 286.4 thiab 289.4 eV sib raug rau CO thiab C=O, raws li, thiab lawv yog cov khoom lag luam decomposition ntawm cov kuab tshuaj carbonate (xws li ROCO2-, ROC-, thiab lwm yam) . Lub ncov ntawm 292.7 eV sib raug rau CF3, uas feem ntau yog los ntawm cov khoom decomposition ntawm lithium ntsev. Hauv O1s spectrum (Daim duab S5(b, e)), lub ncov ntawm 531.1 thiab 532.3 eV sib raug rau C=O thiab CO, raws li, thiab cov ntsiab lus txheeb ze ntawm CO yog txo qis, uas feem ntau cuam tshuam nrog txo cov ntsiab lus ntawm cov khoom decomposition. Raws li kev sib koom tes ntawm LiTFSI thiab LiDFOB, kev tsim ntawm LiOCH3, Li2O2C2H4 thiab lwm yam khoom lag luam raug txwv. Tsis tas li ntawd, tsis zoo li LE (Fig. S5(e)), nyob rau hauv F1s spectrum ntawm GCE-20 (Fig. S5(f)), lub teeb liab siab ntawm LiF yog 684.5 eV, thiab LiF tuaj yeem pab hauv tsim ntawm ib tug ntom thiab ruaj khov SEI txheej.
2.3 Electrochemical kev ua tau zoo ntawm Li||LiFePO4 roj teeb
LiFePO4 muaj qhov zoo ntawm lub peev xwm siab, lub neej voj voog ntev, thiab kev nyab xeeb zoo, thiab yog cov khoom siv hluav taws xob zoo electrode. Nws lub peev xwm theoretical tshwj xeeb yog 170 mAh·g-1. Ntawm 25 degree, Li|GCE-20|LiFePO4 roj teeb tau them thiab tso tawm 200 zaug ntawm qhov tam sim no ntawm 0.2C (1C=0.67 mA·cm{12 }}). Raws li pom hauv daim duab 4(a, b), qhov tso tawm tshwj xeeb ntawm thawj lub voj voog yog 141.4 mAh·g-1. Lub peev xwm tso tawm ntawm 200th lap yog 131.4 mAh·g-1, lub peev xwm tuav tau nce mus txog 92.95 feem pua, thiab ib leeg-tig muaj peev xwm lwj yog tsawg dua 0.04 feem pua. Lub platform voltage yog ruaj khov, nyob rau hauv txoj kab nrog cov yam ntxwv ntawm LiFePO4 roj teeb. Coulombic efficiency, raws li ib qho tseem ceeb qhia rau kev ntsuam xyuas lub roj teeb lub voj voog stability, hais txog qhov piv ntawm lub roj teeb tso peev xwm kom them peev xwm nyob rau hauv tib lub voj voog. Thawj lub voj voog coulombic efficiency ntawm Li|GCE-20|LiFePO4 roj teeb yog 97.8 feem pua. Vim yog tsim ntawm SEI txheej thaum lub sij hawm thawj lub voj voog tawm txheej txheem, ib feem ntawm lub peev xwm irreversible yog generated, uas ua rau ib tug tsawg thawj lub voj voog coulombic efficiency.
Daim duab 4 Electrochemical kev ua tau zoo ntawm Li|GCE-20|LiFePO4 hlwb
(a) Cycling kev ua tau zoo thiab (b) sib thooj voltage-capacity curves ntawm 0.2C; (c) Rate kev ua tau zoo thiab (d) sib thooj voltage-capacity curves; Cov duab muaj yeeb yuj muaj nyob rau ntawm lub vev xaib
Tsis tas li ntawd, kev ntsuas kev them nqi thiab tso tawm tau ua tiav ntawm Li|GCE{{0}}|LiFePO4 ntawm 0.3C, 0.5C, 1C, 1.5C, thiab {{12 }}.5C tus nqi tam sim no los tshawb txog nws qhov kev ua tau zoo. Raws li pom hauv daim duab 4(c), thaum tus nqi tam sim no yog 0.5C, thawj lub voj voog tso tawm lub peev xwm ntawm lub roj teeb yog 160.2 mAh·g-1. Raws li tus nqi tam sim no nce, qhov tso tawm tshwj xeeb ntawm lub roj teeb txo qis hauv qhov kev tswj tau ntau. Tus nqi nce mus rau 2C, thiab lub peev xwm tshwj xeeb ntawm thawj lub voj voog tawm yog 130 mAh·g-1. Tom qab ntawd, tus nqi tam sim no rov qab mus rau 0.5C dua, thiab lub peev xwm tshwj xeeb ntawm thawj lub voj voog tawm yog 156.1 mAh·g-1. Qhov cuam tshuam voltage-capacity curves yog qhia hauv daim duab 4(d). Lub toj siab voltage ntawm cov nqi sib txawv yog ruaj khov yam tsis ua rau muaj kev nce hauv overpotential, thiab lub roj teeb qhia tau hais tias qhov kev ua tau zoo thiab kev thim rov qab.
3 Kev xaus
PEGDA-based GCE yog tsim los ntawm thermally pib hauv-situ polymerization. FT-IR thiab XRD tus yam ntxwv tsom xam ntawm GCE, ua ke nrog cov kev ntsuam xyuas electrochemical, tau tshuaj xyuas qhov zoo tshaj plaws GCE formulation. Txuas ntxiv txuas lub roj teeb los kawm txog kev ua haujlwm ntawm electrochemical ntawm cov electrolyte, thiab txheeb xyuas qhov kev tiv thaiv ntawm cov electrolyte ntawm lithium hlau tsis zoo electrode los ntawm kev soj ntsuam cov microscopic morphology thiab nto keeb yam ntxwv ntawm lithium hlau, piav qhia:
1) GCE-x (x=10, 20, 30) npaj los ntawm in-situ polymerization tuaj yeem ntub cov electrode daim ntawv zoo, thiab cov electrolyte muaj qhov zoo tshaj plaws electrochemical stability thaum lub loj feem ntawm PEGDA yog 20 feem pua.
2) Lub dilithium ntsev system ntawm LiTFSI thiab LiDFOB tau qhia, uas tuaj yeem tsim kev sib cuam tshuam zoo nrog cov khoom siv polymer. Cov electrolyte muaj lub qhov rais dav electrochemical (5.26 V) thiab siab ionic conductivity (30 degree , 1 × 10-3 S·cm-1). Tib lub sijhawm, dilithium ntsev system tuaj yeem siv los tsim cov txheej txheem SEI ruaj khov thiab tiv thaiv cov lithium hlau anode zoo.
3) Siv GCE-20 kom phim cov khoom lag luam LiFePO4 cathode, cov roj teeb sib sau ua ke tuaj yeem ruaj khov thiab tso tawm rau 200 cycles ntawm tam sim no ntawm 0.2C, nrog lub peev xwm tuav tau ntawm 92.95 feem pua , thiab nthuav qhia tus nqi zoo.
Hauv cov ntsiab lus, txoj haujlwm no tau txais kev nyab xeeb thiab zoo heev electrochemical kev ua tau zoo ntawm GCE, uas muab cov kev daws teeb meem zoo rau kev txhim kho kev nyab xeeb thiab ruaj khov siab zog lithium hlau roj teeb.
Cov khoom siv ntxiv:
S1 roj teeb txheej txheem npaj
Sib tov thiab zom LiFePO4, Ketjen Dub thiab PVDF raws li lub hom phiaj piv, ntxiv cov kuab tshuaj N-Methylpyrrolidone (N-Methylpyrrolidone, NMP), tag nrho do thiab disperse, thiab tau txais ib tug uniform thiab viscous active khoom slurry. Lub slurry yog scraped-coated rau ntawm aluminium ntawv ci nrog lub tiaj coater, ces xa mus rau lub tshuab nqus tsev qhov cub, thiab qhuav ntawm 80 degree rau 12 teev. Tom qab txiav cov ntawv electrode, qhuav nws dua thiab hloov mus rau lub hnab looj tes tsis muaj dej thiab tsis muaj oxygen.
Lub gasket, shrapnel, thiab lithium hlau ntawv tau muab tso rau hauv nruab nrab ntawm cov ntaub ntawv tsis zoo electrode nyob rau hauv ib ntus, thiab lub thickness ntawm lithium hlau ntawv yog 0.35 hli. Tom qab ntawd, cov tshuaj precursor ntawm GCE tau ntxiv dropwise rau ntawm qhov chaw ntawm qhov chaw ntawm qhov tsis zoo electrode (50 µL) siv rab phom pipette, thiab tom qab ntawd Celgard 2500 roj teeb cais thiab daim ntawv zoo electrode (Celgard 2500 roj teeb cais) tau muab tso rau hauv ib ntus. Ua ntej sib sau ua ke Li||LiFePO4 roj teeb, cov ncej zoo tau hnyav thiab cov khoom siv thauj khoom tau kaw. Lub active khoom nto loading ntawm LiFePO4 zoo electrode yog 3.94 mg cm -2. Thaum kawg, nias thiab kaw lub roj teeb ntawm lub roj teeb sealing tshuab, hloov mus rau 70 degree ib puag ncig thiab ua kom sov rau 2 teev los pib polymerization kom tau txais gel lub xeev electrolyte. Txhawm rau kom ntseeg tau tias cov electrolyte tau nkag mus rau hauv LiFePO4 ncej, lub roj teeb yuav tsum tau tso tseg kom sawv ntsug li 1 teev tom qab sib dhos.
Fig. S1 Sib cuag cov ces kaum ntawm polymer precursor tov thiab cathodes
(a) LE; (b) GCE-10; (c) GCE-20; (d) GCE-30
Daim duab S2 Nyquist thaj av ntawm GCE sib sau Li ||LiFePO4 hlwb nrog cov lithium ntsev sib txawv
Daim duab S3 Nyquist thaj av ntawm symmetric Li||Li hlwb sib sau ua ke nrog GCE-x electrolytes
Daim duab S4 Voltage-time profiles ntawm symmetric Li||Li hlwb sib sau ua ke nrog GCE-x electrolytes
Fig. S5 XPS spectra of metallic Li anode in symmetric Li||Li cells
(a, d) C1s, (b, e) O1s, (c, f) F1s XPS spectra of metallic Li anode with (ac) LE and (df) GCE-20
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