CN115656140A - Plasmon enhanced Raman spectroscopy method for representing SEI (solid interphase) formation and evolution process - Google Patents

Plasmon enhanced Raman spectroscopy method for representing SEI (solid interphase) formation and evolution process Download PDF

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CN115656140A
CN115656140A CN202211421483.3A CN202211421483A CN115656140A CN 115656140 A CN115656140 A CN 115656140A CN 202211421483 A CN202211421483 A CN 202211421483A CN 115656140 A CN115656140 A CN 115656140A
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substrate
sei
plasmon
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raman spectroscopy
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谷宇
毛秉伟
田中群
王君豪
周如玉
李剑锋
颜佳伟
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Xiamen University
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Abstract

A plasmon-enhanced raman spectroscopy method of characterizing SEI formation and evolution processes, comprising the steps of: (1) Preparing a nano-structure metal substrate with SERS activity and shell isolated core-shell nanoparticles; (2) Compounding the nanostructured metal substrate with SERS activity prepared in the step (1) with shell isolated core-shell nanoparticles to form a coupling substrate with plasmon enhancement activity, referred to as PERS substrate for short; (3) Assembling the PERS substrate obtained in the step (2) into an airtight Raman electrolytic cell, injecting electrolyte into the airtight Raman electrolytic cell, taking the PERS substrate as a working electrode, carrying out electrochemical control on the working electrode, enabling the electrolyte to react on the PERS substrate to form SEI, and simultaneously carrying out tracking detection by using in-situ electrochemical Raman so as to represent the SEI forming and evolution process.

Description

Plasmon enhanced Raman spectroscopy method for representing SEI (solid interphase) formation and evolution process
Technical Field
The invention relates to the field of surface interface characterization and spectrum characterization of a lithium battery system, in particular to a plasmon enhanced Raman spectrum method for characterizing the SEI forming and evolution process.
Background
In lithium battery systems, the negative electrode/electrolyte interface reactions have a significant impact on the electrochemical performance of the battery. In particular, the formation of Solid Electrolyte Interphase (SEI) at the interface directly affects the electrochemical behavior of lithium metal, such as deposition-dissolution, and further determines the cycling efficiency and stability of the battery (d.lin, y.liu and y.cui, nat Energy,2017,12,194-206, h.wu, h.jia, c.wang, j.g.zhang and w.xu, adv Energy mater,2020,11, 2003092). Therefore, research on the formation of SEI and the evolution process of chemical composition and structure thereof during charge and discharge has been a core problem and a hot direction of lithium battery system research. The composition and structure of SEIs have been extensively studied and have formed a preliminary understanding by various interfacial characterization methods, combined with theoretical simulations for decades (E.Peled and S.Menkin, J Electrochem Soc,2017,164, A1703-A1719). But SEI has various components, complex composition structure and dynamic change, and the overall accurate cognition of SEI is still very poor. Therefore, there is a need to develop a lossless in-situ characterization method with high spatial and temporal resolution to perform in-depth analysis on the SEI formation and dynamic evolution mechanism.
Compared with other characterization techniques, the electrochemical raman spectroscopy has very powerful and unique advantages in-situ analysis of the conventional electrode/electrolyte interface process. However, SEI thicknesses are typically only a few nanometers to a few hundred nanometers, whereas conventional raman signals are weak and relatively difficult to detect, requiring analysis by Surface Enhanced Raman Spectroscopy (SERS) techniques. There are a few reports on SERS technology for studying SEI composition and structure (M.J. Piernas-
Figure BDA0003941953110000011
Tornheim, S.Transk, Z.Zhang and I.bloom, chem Commun,2021,57, 2253-2256). However, according to the electromagnetic effect mechanism, the electromagnetic field in the SERS technology is limited to a few nanometers of the hot spot region, so that the technology can only provide limited SEI composition and structure information in the vicinity of the corresponding hot spot, and cannot comprehensively followThe formation and evolution process of the SEI are detected. In 2010, the applicant's group invented a shell-isolated nanoparticle enhanced raman spectrum, abbreviated as SHINERS (j.f.li, y.f.huang, y.ding, z.l.yang, s.b.li, x.s.zhou, f.r.fan, w.zhang, z.y.zhou, d.y.wu, b.ren, z.l.wang, z.q.tian, nature 2010,464, 392-395). The principle of SHINERS is that a layer of inert ultrathin shell is coated on the surface of a metal nanoparticle with SERS activity to form a core-shell structure, so that the SERS activity of core particles is retained, direct contact between the core particles and a species to be detected is avoided, the core-shell structure particles can be spread on the surface of any substrate to perform interface process tracking, and collected Raman signals are ensured to be completely from the reaction of the substrate. However, due to the complexity of operating in nonaqueous electrolytes, there have been few reports of studies on negative SEI for lithium battery systems using SHINERS. In a word, the research on the process of the cathode/electrolyte interface by using SERS and SHINERS has a great development space, and is worthy of deep excavation and improvement.
Disclosure of Invention
The present invention is directed to solve the above problems in the prior art, and provides a plasmon enhanced raman spectroscopy method with high spatial and temporal resolution and in-situ non-loss for characterizing the SEI formation and evolution process, which can reveal the SEI formation and evolution mechanism at a molecular level.
In order to achieve the purpose, the invention adopts the following technical scheme:
a plasmon-enhanced raman spectroscopy method of characterizing SEI formation and evolution processes, comprising the steps of:
(1) Preparing a nano-structure metal substrate with SERS activity and shell isolated core-shell nanoparticles;
(2) Assembling the shell isolated core-shell nanoparticles prepared in the step (1) on a nanostructure metal substrate with SERS activity to form a coupling substrate with plasmon enhancement activity, referred to as PERS substrate for short;
(3) Assembling the PERS substrate obtained in the step (2) into an airtight Raman electrolytic cell, injecting electrolyte into the airtight Raman electrolytic cell, taking the PERS substrate as a working electrode, performing electrochemical control on the working electrode to enable the electrolyte to react on the PERS substrate to form SEI, and simultaneously performing tracking detection by using in-situ electrochemical Raman, namely realizing a PERS substrate-based plasmon enhanced Raman spectroscopy method for representing SEI forming and evolution processes.
Preferably, the material of the nanostructured metal substrate having SERS activity in step (1) is copper, lithium, gold, silver, or nickel.
Preferably, the configuration of the nanostructured metal substrate having SERS activity in step (1) is a planar foil, a three-dimensional mesh, a three-dimensional foam, or a three-dimensional cylinder.
Preferably, in the step (1), the shell layer isolated core-shell nano-particles are Au @ SiO 2 、Au@Al 2 O 3 、Ag@SiO 2 、Ag@Al 2 O 3 At least one of (a).
Preferably, the particle size of the shell layer insulation core-shell nanoparticle in the step (1) is 50-200 nm.
Preferably, the gas-tight raman electrolytic cell configuration in step (3) may be a two-electrode system, i.e. comprising a working electrode and a counter electrode; it can also be a three-electrode system, i.e. containing a working electrode, a counter electrode and a reference electrode.
Preferably, the electrolyte in step (3) may be an aqueous electrolyte, and any suitable electrolyte such as an aqueous lithium ion battery, an aqueous zinc-air battery, or the like may be used; the electrolyte solution may be a nonaqueous electrolyte solution, and any suitable electrolyte solution such as a nonaqueous lithium ion battery, a lithium-sulfur battery, a lithium-air battery, a lithium-mediated nitrogen reduction reaction, and the like can be used.
Preferably, the electrochemical control in step (3) is at least one of constant potential polarization, constant current polarization, variable potential polarization, and variable current polarization.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) Raman enhancement factor of PERS substrate of the invention is up to 10 10 The spatial resolution is sub-nanometer, so that the Raman signal of the SEI can be effectively enhanced;
(2) The PERS substrate has the characteristic of depth sensitivity, and can accurately detect components and structures at different depths of SEIs and SEIs, namely the nanostructured metal substrate with SERS activity can detect the composition and structure information of the inner side of the initial period of SEI formation, the nanostructured metal substrate with SERS activity and shell isolated core-shell nanoparticles are coupled to detect the change of the outer composition of the SEI and the composition and structure of the SEI at the later period, in a word, the PERS substrate can be combined inside and outside and tracks the film forming process of the SEI from bottom to top, and the SEI formation and evolution mechanism is comprehensively understood;
(3) The plasmon enhanced Raman spectroscopy method based on the PERS substrate can implement accurate real-time and nondestructive detection on the SEI;
(4) The plasmon enhanced Raman spectroscopy method based on the PERS substrate can meet the in-situ characterization of SEI film forming processes of different electrolyte systems, and is wide in universality.
Drawings
Fig. 1 is a flow chart of SEI characterization by a plasmon enhanced raman spectroscopy method based on a PERS substrate.
FIG. 2 is a scanning electron microscope image of a nano copper foil substrate.
FIG. 3 is a Raman spectrum of pyridine adsorbed on a nano-copper foil substrate and a planar copper foil substrate.
FIG. 4 is a core-shell isolated Au @ SiO 2 Transmission electron microscopy images of nanoparticles.
FIG. 5 is a scanning electron micrograph of a PERS substrate.
FIG. 6 is a Raman spectrum diagram for characterizing the formation and evolution process of SEI in LiTFSI/DME-DOL electrolyte by a PERS substrate-based plasmon enhanced Raman spectroscopy method.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects of the present invention clearer and clearer, the present invention is described in further detail below with reference to embodiments and accompanying drawings. The following embodiments are only preferred embodiments of the present invention, and therefore, the scope of the present invention should not be limited by the following embodiments, and all equivalent changes and modifications made according to the claims and the contents of the specification should be included in the scope of the present invention.
Example 1
The invention provides a plasmon enhanced Raman spectroscopy method for characterizing SEI (solid state imaging) formation and evolution processes, which is shown in a flow chart in figure 1 and comprises the following steps of:
(1) Preparing a nano-structure metal substrate with SERS activity and shell isolated core-shell nanoparticles;
this example takes the preparation of a nanocopper foil with SERS activity as an example:
immersing a copper foil with the diameter of 2mm in a 0.1MKCl aqueous solution, treating the copper foil working electrode by adopting an electrochemical oxidation-reduction cycle method by taking the copper foil as a working electrode, a foil as a counter electrode and a saturated calomel electrode as a reference electrode: the oxidation potential is controlled to be 0.4V, and the duration is 10-30 s; the reduction potential is controlled to be minus 0.4V, and the duration is 10 to 30s; the cycle times are 2-20 times; washing the copper foil working electrode with deionized water after electrochemical oxidation-reduction circulation to remove residual solution, drying the copper foil working electrode in a vacuum drying oven after drying the copper foil working electrode with high-purity nitrogen, and obtaining the nano copper foil substrate with SERS activity; FIG. 2 is a scanning electron micrograph of the surface of the copper foil after treatment with the electrochemical oxidation-reduction cycling method, showing that the surface of the copper foil forms spherical nanostructures after treatment; in order to investigate the SERS activity of the nano copper foil substrate, pyridine is used as a probe molecule for SERS detection, and the result is shown in FIG. 3, it can be seen that compared with a planar copper foil which is not treated by an electrochemical oxidation-reduction cycle method, a strong pyridine analysis signal is detected on the copper foil substrate with a spherical nano structure on the surface, and the nano copper foil substrate has strong SERS activity on the surface.
This example to prepare Au @ SiO 2 Nanoparticles are exemplified:
stirring and heating 200mL of chloroauric acid aqueous solution with the mass fraction of 0.01% to boil, quickly adding 1.4mL of sodium citrate aqueous solution with the mass fraction of 1%, heating and refluxing for 0.5-1 h, then stopping heating, and cooling in the air to obtain Au nano particle sol with the average particle size of about 60 nm; taking 30mL of the Au nanoparticle sol, adding 0.4mL of 1mM 3-aminopropyltrimethoxysilane aqueous solution into a round-bottom flask, stirring for 10-15 min, adding 3.2mL of 0.54% sodium silicate aqueous solution, and continuing to addStirring for 5-10 min, transferring the round-bottom flask into a boiling water bath, heating and stirring for 15-60 min, and cooling to obtain SiO 2 Au @ SiO with shell thickness of about 2nm 2 Nanoparticles; prepared shell isolated core-shell Au @ SiO 2 The transmission electron micrograph of the nanoparticles is shown in FIG. 4;
(2) Assembling the shell isolated core-shell nanoparticles prepared in the step (1) on a nano-structure metal substrate with SERS activity to form a coupling substrate with plasmon enhancement activity, namely a PERS substrate for short;
taking the shell layer to isolate the core shell Au @ SiO 2 Dripping 0.05-0.2 mL of nano particles on a nano copper foil substrate with SERS activity, and fully dehydrating and drying in a vacuum drying oven to obtain a coupling substrate with plasmon enhancement activity, namely a PERS substrate; the scanning electron micrograph of the PERS substrate is shown in FIG. 5; the enhancement capability of the PERS substrate is calculated by adopting a finite element method, and the result shows that the Raman enhancement factor of the PERS substrate is up to 10 10 And the spatial resolution is sub-nanometer, so that the Raman signal of the SEI can be effectively enhanced.
(3) Assembling the PERS substrate obtained in the step (2) into an airtight Raman electrolytic cell, injecting electrolyte into the airtight Raman electrolytic cell, taking the PERS substrate as a working electrode, performing electrochemical control on the working electrode to enable the electrolyte to react on the PERS substrate to form SEI, and simultaneously performing tracking detection by using in-situ electrochemical Raman, namely realizing a PERS substrate-based plasmon enhanced Raman spectroscopy method for representing SEI forming and evolution processes.
Specifically, in the embodiment, a plasmon enhanced raman spectroscopy method based on a PERS substrate is used for representing the formation and evolution process of SEI in the LiTFSI/DME-DOL electrolyte:
assembling the PERS substrate into an airtight Raman electrolytic cell in an argon atmosphere glove box, wherein the PERS substrate is used as a working electrode, a lithium sheet is used as a counter electrode, and a lithium wire is used as a reference electrode; injecting an ether electrolyte LiTFSI/DME-DOL into the Raman electrolytic cell; applying variable potential polarization control to the PERS working electrode to reduce the electrolyte on the PERS working electrode, and simultaneously performing tracking detection by using an in-situ Raman spectrum: the laser wavelength is 785nm, the laser power is 0.3mW, and the acquisition time is 60s; the foregoing processes are used to characterize the formation and evolution process of the SEI.
Fig. 6 is a raman spectrogram representing the formation and evolution processes of SEI in LiTFSI/DME-DOL electrolyte by using a PERS-based plasmon enhanced raman spectroscopy method, wherein the thickness of SEI in the system is about 10-15 nm, and it can be seen that characteristic peaks (marked with asterisks in fig. 6) of SEI components appear in the spectrogram successively along with the continuous change of potential, which illustrates that the PERS-based plasmon enhanced raman spectroscopy method can monitor the formation of SEI and the components and structural features at different depths in real time and without damage.
Example 2
PERS substrates were prepared in the same manner as in steps (1) to (2) of example 1; assembling the PERS substrate into an airtight Raman electrolytic cell in an argon atmosphere glove box, wherein the PERS substrate is used as a working electrode, a lithium sheet is used as a counter electrode, and a lithium wire is used as a reference electrode; injecting carbonate electrolyte LiDFOB-LiBF into the Raman electrolytic cell 4 DEC-FEC; applying constant current polarization control to the PERS working electrode to reduce the electrolyte on the PERS working electrode, and simultaneously performing tracking detection by using an in-situ Raman spectrum: the laser wavelength is 785nm, the laser power is 0.3mW, and the acquisition time is 60s; the foregoing processes are used to characterize the formation and evolution process of the SEI. Carbonic acid ester electrolyte LiDFOB-LiBF 4 The thickness of SEI formed by a DEC-FEC system is about 30-40 nm, and the formation and evolution processes of SEIs with different thicknesses and different electrolyte systems can be monitored in real time and in a lossless manner by a PERS substrate-based plasmon enhanced Raman spectroscopy method.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.

Claims (10)

1. A plasmon-enhanced raman spectroscopy method of characterizing SEI formation and evolution processes, comprising the steps of:
(1) Preparing a nano-structure metal substrate with SERS activity and shell layer isolated core-shell nanoparticles;
(2) Assembling the shell isolated core-shell nanoparticles prepared in the step (1) on a nano-structure metal substrate with SERS activity to form a coupling substrate with plasmon enhancement activity, namely a PERS substrate for short;
(3) Assembling the PERS substrate obtained in the step (2) into an airtight Raman electrolytic cell, injecting electrolyte into the airtight Raman electrolytic cell, taking the PERS substrate as a working electrode, performing electrochemical control on the PERS substrate to enable the electrolyte to react on the PERS substrate to form SEI, and simultaneously performing tracking detection by using in-situ electrochemical Raman, namely realizing a plasma enhanced Raman spectroscopy method based on the PERS substrate to characterize the SEI forming and evolution process.
2. The plasmon-enhanced raman spectroscopy method of characterizing SEI formation and evolution processes of claim 1, wherein: the nanostructured metal substrate with SERS activity in the step (1) is made of copper, lithium, gold, silver or nickel.
3. The plasmon-enhanced raman spectroscopy method of characterizing SEI formation and evolution processes of claim 1, wherein: the nano-structure metal substrate with SERS activity in the step (1) is in a planar foil, three-dimensional net, three-dimensional foam or three-dimensional cylinder configuration.
4. The plasmon-enhanced raman spectroscopy method of claim 1 for characterizing SEI formation and evolution processes, wherein: in the step (1), the shell layer isolated core-shell nano particles are Au @ SiO 2 、Au@Al 2 O 3 、Ag@SiO 2 、Ag@Al 2 O 3 At least one of (1).
5. The plasmon-enhanced raman spectroscopy method of claim 1 for characterizing SEI formation and evolution processes, wherein in step (1) the shell-insulating core-shell nanoparticles have a particle size of 50-200 nm.
6. The plasmon-enhanced raman spectroscopy method of characterizing SEI formation and evolution processes of claim 1, wherein: the configuration of the airtight Raman electrolytic cell in the step (3) can be a two-electrode system, namely the airtight Raman electrolytic cell comprises a working electrode and a counter electrode; a three-electrode system, i.e., comprising a working electrode, a counter electrode, and a reference electrode, is also possible.
7. The plasmon-enhanced raman spectroscopy method of claim 1 for characterizing SEI formation and evolution processes, wherein: the electrolyte in step (3) may be an aqueous electrolyte or a non-aqueous electrolyte.
8. The plasmon-enhanced raman spectroscopy method of characterizing SEI formation and evolution processes of claim 7, wherein: the aqueous electrolyte is suitable for aqueous lithium ion batteries, aqueous zinc ion batteries and aqueous zinc-air batteries.
9. The plasmon-enhanced raman spectroscopy method of characterizing SEI formation and evolution processes of claim 7, wherein: the non-aqueous electrolyte is suitable for non-aqueous lithium ion batteries, lithium-sulfur batteries, lithium-air batteries and lithium-mediated nitrogen reduction reactions.
10. The plasmon-enhanced raman spectroscopy method of claim 1 for characterizing SEI formation and evolution processes, wherein: and (3) controlling the electrochemistry to be at least one of constant potential polarization, constant current polarization, variable potential polarization and variable current polarization.
CN202211421483.3A 2022-11-14 2022-11-14 Plasmon enhanced Raman spectroscopy method for representing SEI (solid interphase) formation and evolution process Pending CN115656140A (en)

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