Li-ion batteries as a reclaimable power source have been used in a diverseness of electronic devices and energy storage equipment ( Armand and Tarascon, 2008 ), which has aroused a set of interests in the academician community, while the complicate electrochemical process is still mysterious within Li-ion batteries during the cycle ( Qian et al., 2015 ; Ross, 2015 ; Wu et al., 2016 ; Yang et al., 2017 ). In situ characterization techniques are quite suitable to explore the structure-behavior relationship of Li-ion batteries, which can in situ observe the electronic structure, the crystal structure, the development of micro-morphology, etc. ( Yang et al., 2017 ). In recent years, many in situ characterization techniques have been developed, such as in situ x-ray diffraction ( XRD ) ( Hu et al., 2014 ; Liu et al., 2014 ; Sharma et al., 2015 ), in situ Raman spectroscopy ( Gross et al., 2013 ; Lanz et al., 2013 ; Wu et al., 2013a ), in situ Fourier transform infrared spectroscopy ( Cheng et al., 2007 ), and in situ transmission electron microscopy ( Chen et al., 2015 ) .
Li-ion batteries work in a close environment to protect the electrode materials from air air, so it is very unmanageable to be acquired the internal information of these batteries, except for some ex situ characterization techniques after deconstructing the batteries. In order to study the social organization change and surface evolution of electrode materials during the electrochemical reactions, many researchers have made great efforts to develop in situ techniques for Li-ion batteries. Thurston et alabama. ( 1998 ) designed an early on in situ XRD cell to measure electrode materials and intuitively observe lattice expansion and contraction, phase transition, and multi-phase geological formation. In following two decades, in situ XRD cells have been developed sufficiently with a distinctive construction as follows : a fix was created in a protective case or current collector and following sealed by an x-ray crystalline material, such as a Kapton, Be, or Al hydrofoil. They were normally based on the model battery ( Misra et al., 2012 ; He et al., 2013 ; Lin et al., 2013, 2014 ; Roberts et al., 2014 ; Stancovski and Badilescu, 2014 ; Villevieille et al., 2014 ) or the mint cell ( Thorne et al., 2011 ; Fell et al., 2012 ; Zhu et al., 2013 ; Lowe and Gao, 2014 ). The first in situ Raman cell was designed by Inaba et alabama. in 1995, which was used to study the electrochemical Li embolism into Graphite ( Inaba et al., 1995 ). Shu et aluminum. ( 2011 ) besides manufactured an in situ Raman battery to investigate the electrode material of Li4Ti5O12. Most in situ Raman cells were based on the fake battery ( Long et al., 2011 ; Nakagawa et al., 2012 ; Gross et al., 2013 ; Lanz et al., 2013 ; Wu et al., 2013b ; Hy et al., 2014 ). however, these in situ batteries have not been widely spread in the research community, ascribable to their complicated construction, senior high school cost, and inadequate operation fourth dimension .
In this solve, coin-cell-based in situ batteries have been designed and tested for Li-ion batteries. By modifying the normal mint cells, we fabricated in situ XRD and Raman coin cells, with which some excellent measurement results are obtained for Li4Ti5O12 and LiFePO4. Compared with commercial simulate batteries, in situ coin cells have many advantages, such as abject monetary value, simple assembly, and good seal. Thereby, coin-cell-based in situ characterization techniques would arouse wide interests in the electrochemical field.
Reading: Coin-Cell-Based In Situ Characterization Techniques for Li-Ion Batteries
Design of In Situ Coin Cells
As shown in Figure 1 A, a normal coin cellular telephone was composed of a negative battery encase, a battery shrapnel, a lithium anode, a centrifuge, an electrode material, a current collector, and a incontrovertible battery lawsuit from acme to bottom. Based on a convention mint cell, we designed in situ XRD and Raman coin cells ( Figures 1 B, C ). For in situ XRD, a Be sheet as an x-ray windows was hard attached to the bottom casing with a thermoplastic movie. here, the Be sheet was chosen for its high x-ray transmittance and big electrochemical stability window ( 0–4 V vs. Li+/Li ). In the construction, all components were dried in an oven of 80°C for 6 h and then assembled in a glove box filled with Ar gasoline ( H2O, O2 < 1 PPM ). notably, the current collector is a metallic interlock with two conductive tails, and the working electrode was toward the x-ray window, alternatively of the antagonistic electrode in a normal mint cell. The in situ Raman coin cell is alike to the in situ XRD coin cell, except for an ocular window of quartz glass .
Figure 1. Structure diagram and real photos of normal coin cell and in situ coin cell. (A) Normal mint cell. (B) In situ roentgenogram diffraction coin cellular telephone. (C) In situ Raman coin cell .
Preparation of Working Electrode
For in situ XRD, one working electrode was prepared as a mix spread containing 42.5 wt. % Li4Ti5O12 ( Ishihara Sangyo Kaisha, Ltd. ), 42.5 wt. % acetylene black, and 15 wt. % teflon ( PTFE ), which was pressed on a stainless steel net. Another was prepared as a mix paste containing 80 wt. % LiFePO4 ( Sumitomo Osaka Cement Co. Ltd., Japan ), 10 wt. % acetylene blacken, and 10 wt. % PTFE, which was pressed on an Al net ( 100 mesh topology ) with a batch load of approximately 5 mg cm−2. The counter electrode of lithium alloy was separated from the working electrode by a Celgard film 2400 porous polypropylene movie, and the electrolyte was 1 M LiClO4 in a mix of ethylene carbonate ( EC ) /diethyl carbonate ( DEC ) ( 1:1 in book ) or 1 M LiPF6 in a assortment of EC and dimethyl carbonate ( DMC ) ( 1:1 in book ) .
For in situ Raman, the working electrode was composed of 90 wt. % Li4Ti5O12 and 10 wt. % PTFE which was pressed onto a stainless steel mesh. For comparison, the carbon subject was tailored as 10 and 42.5 wt. % in the shape electrode. The counter electrode of lithium metallic was separated from the working electrode by a Celgard film 2400 holey polypropylene film, and the electrolyte was 1 M LiClO4 in a assortment of EC/DEC ( 1:1 in book ) .
In Situ Measurements
electrochemical measurements were conducted on a Battery Testing System ( BioLogic VSP-300 ) at the room temperature, with a electric potential range of 1.2–2.0 V for Li4Ti5O12 and 2.8–4.0 V for LiFePO4. simultaneously, XRD patterns were acquired by using a Bruker D2 PHASER diffractometer with Cu kα radiation, or Raman spectra were collected on Thermo Scientific DXR Micro-Raman Spectrometer .
Results and Discussion
Our in situ XRD/Raman mint cells were tested with the working electrode materials of Li4Ti5O12 and LiFePO4, and their constructions were optimized according to the experimental results. For in situ XRD coin cell, we selected two Be sheets of 0.2 and 0.5 mm blockheaded to in situ standard the LiFePO4 electrode. During the charge from 2.8 to 4.0 V with a rate of 0.1 C, in situ XRD measurements were conducted simultaneously. As shown in Figure 2 A, the diffraction peaks of LiFePO4 can be observed for the Be tabloid of 0.2 mm thick, but it is unmanageable for the Be sheet of 0.5 mm slurred, as shown in Figure 2 B, because the blockheaded Be sail would absorb the x-ray strongly. In the in situ XRD practice of LiFePO4, an XRD bill of LiFePO4 ( 211 ) ( labeled “ T ” ) decreases during the charge process and two XRD peaks of FePO4 ( 020 ) and ( 211 ) ( labeled “ H ” ) emerges and increases, which was same as the literature reported in the by ( Gibot et al., 2008 ; Meethong et al., 2012 ). Thereby, the top out intensity is dependent on the thickness of Be sheet, and the thickness of 0.2 millimeter is desirable for in situ XRD measurements .
Figure 2. In situ x ray diffraction ( XRD ) measurement with different Be sheets. The in situ XRD results of LiFePO4 with a Be sheet of (A) 0.2 millimeter and (B) 0.5 millimeter thick, respectively. “ H ” represents heterosite ( lithium-poor phase, FePO4 ), “ T ” represents triphylite ( lithium-rich phase, LiFePO4 ) .
It is well known that the sample for XRD measurement must be placed in a specify plane, and the measured point would shift with the acme of the flat. In our in situ XRD mint cell, the thin Be sheet would be bent under a adult press, which is expected to influence the measure bill more of less. As shown in Figure 3 A, we prepared two in situ XRD mint cells ( A-battery and B-battery ) with the battery shim of 0.8 and 1.0 millimeter, respectively. The Be sheet is very bland in A-battery while it is obviously curved in B-battery, owing to the different pressures from the peak to the bottom. figure 3 B shows XRD patterns of Li4Ti5O12 measured with these two in situ coin cells. The XRD acme of B-battery is obviously broader than that of A-battery, with a quite boastfully acme shoulder in the minor slant. actually, the deflect Be plane made different parts of the working electrode located at unlike heights, so the broad and asymmetrical acme of B-battery was the principle of superposition of partial derivative XRD peaks at different angles. thereby, we chose the battery shim of 0.8 mm blockheaded to obtain a apartment x-ray window under a proper atmospheric pressure .
Figure 3. influence of the electrode bending on x ray diffraction ( XRD ) results. (A) Schematics of the flat and bent electrode films pressed on the Be sheets. (B) XRD patterns of Li4Ti5O12 measured with two different in situ coin cells in (A) .
To check the in situ XRD mint cell with unlike electrolytes, the cathode substantial of LiFePO4 was measured in a potential range of 2.8–4.0 V with two common electrolytes as 1 M LiClO4 in EC/DEC ( 1:1 in volume ) and 1 M LiPF6 in EC/DMC ( 1:1 in book ). As shown in Figure 4, the cathexis and discharge curves are quite estimable for LiPF6, while the charge wind for LiClO4 shows an abnormal tableland at the electric potential of 3.8 V. Actually, the abnormal tableland should be attributed to a english reaction, as the LiClO4 with a firm oxidizability might react with the Be sail at a high electric potential. thus, the electrolyte of LiPF6 ( EC/DMC = 1:1 in volume ) is proved to be a thoroughly option for the cathode material in the in situ XRD coin cell. On the other bridge player, the anode material of Li4Ti5O12 can be in situ measured excellently for both the electrolytes with a electric potential image of 1.2–2.0 V .
Figure 4. The charge and discharge wind of in situ roentgenogram diffraction coin cells with unlike electrolytes as 1 M LiClO4 in a assortment of ethylene carbonate ( EC ) and diethyl carbonate ( 1:1 in volume, green ) or 1 M LiPF6 in a mix of EC and dimethyl carbonate ( 1:1 in volume, crimson ). here, the charge–discharge measurements were conducted at a current rate of C/10 within a electric potential image of 2.8−4.0 V .
Using this in situ XRD mint cell, we successfully obtained the in situ XRD patterns during the electrochemical reaction, as shown in Figure 5, which can be deeply analyzed to reveal the structural development of electrode materials. For Li4Ti5O12, the electrochemical measurement was performed as : charge at C/10 to 2.0 V and then potentiostatic within 10 henry ; discharge at C/10 to 1.2 V and then potentiostatic within 10 h. Simultaneously, in situ XRD patterns were acquired every 1 h ( including the measurement time of 42 min and the time interval time of 18 minute ). As shown in Figure 5 B, the loss and amobarbital sodium curves were measured during the cathexis and free processes, respectively. The XRD peaks can be excellently fitted with the Lorentzian function to retrieve the acme position, flower volume, peak area, and full width at half maximal. For Peak ( 111 ) of Li4Ti5O12, the extremum side shifted to the little slant during the charge serve and then the bill position gradually recovered during the exhaust process, as shown in Figure 5 C. meanwhile, the vertex volume decreased and recovered during the agitate and fire processes, respectively, as shown in Figure 5 D. however, the fit results of vertex placement and saturation are not indeed fluent, which should be attributed to the modest signal-noise ratio. furthermore, the top out put and intensity can be used to evaluate the phase fraction and wicket constants, which is significant to study the geomorphologic evolution in Li-ion batteries .
Figure 5. In situ word picture of Li4Ti5O12 electrode. (A) A charge/discharge curve of an in situ coin cell with Li4Ti5O12 electrode : bang at C/10 to 2.0 V and then potentiostatic within 10 henry ; free at C/10 to 1.2 V and then potentiostatic within 10 h. (B) In situ x-ray diffraction ( XRD ) patterns of this in situ mint cellular telephone during the charge and acquit processes. The version of (C) position and (D) saturation of peak ( 111 ) retrieved from in situ XRD patterns in (B) .
There besides exist some limitations in our invention. Although the Be tabloid is very popular for in situ XRD, Be is identical toxic in the form of powder and it can be oxidized easily at a high potential, therefore, it was sometimes substituted by Al film or Al-plastic film. In the in situ XRD mint cell, the small detective windows limited the multitude load of the working electrode, the edge of coin cell blocked the small-angle diffraction, and the Be sheet absorbed the x-ray specially for the small diffraction slant, which result in a moo signal-noise proportion. This problem can be resolved by lengthening the measurement clock or enhancing the x-ray intensity. In our lab-based XRD instrumental role, the low roentgenogram saturation requires a long solicitation fourth dimension to achieve a high signal-noise proportion. In comparison, the synchrotron XRD legal document has a potent roentgenogram glow with a short wavelength, which can penetrate through in situ XRD batteries easily, so the XRD bespeak is strong adequate for the real-time monitor of electrode materials. however, ascribable to the senior high school intensity, the x ray of synchrotron might decompose the electrolyte of Li-ion batteries .
On the other hand, the in situ Raman mint cell was optimized by tailoring the carbon paper content in working electrode. We prepared three sour electrodes of Li4Ti5O12 with different carbon paper contents as 0 % C, 5 % C, and 42.5 % C. As shown in Figure 6 A, the Raman spectrum of the Li4Ti5O12 is very conclusion to those previously reported, in which three bands at 238, 433, and 680 cm−1 are attributed to O–Li–O deflect in the octahedral whole LiO6, Li–O stretching in the tetrahedral whole LiO4, and Ti–O stretching in the octahedral whole TiO6, respectively ( Liu et al., 1994 ; Leonidov et al., 2003 ; Julien and Zaghib, 2004 ). obviously, the signal for 0 % C is much stronger than those for 5 % C and 42.5 % C, and the Raman peaks of PTFE for 0 % C were observed as three Raman bands at 1,200–1,400 cm−1 region, as shown in Figure 6 B. however, the conduction of Li4Ti5O12 is identical poor, and no carbon additive will lead to a big polarization. Contrastively, the Raman D-band and G-band of carbon paper were observed for 5 % C and 42.5 % C, and the weak signal should be attributed to the strong ocular preoccupation of carbon .
Figure 6. Raman spectrum of Li4Ti5O12 electrodes with unlike carbon contents. (A) Raman spectrum of three Li4Ti5O12 electrodes and (B) enlarged view of (A) .
If the electrode fabric exhibits a thoroughly electrical conduction, the in situ Raman measurement can be directly conducted without the carbon additive. Nevertheless, considering the poor people electric conduction of some electrode materials, we suggest a electric potential solution that adopts Surface Enhanced Raman Scattering ( SERS ), which can be conducted by dropping gold-dielectric nanocomposites on a normal electrode with carbon. tied if the electrode material contains the carbon additive, the Raman signal can be enhanced significantly by the gold-dielectric nanoparticles. To achieve a non-destructive and ultrasensitive SERS, respective nanoparticles have been synthesized. Li et aluminum. first reported shell-isolated nanoparticle-enhanced Raman spectroscopy ( SHINERS ) ( Li et al., 2010 ), and then Yu et aluminum. used the SHINERS to investigate that the by-products and overpotential were reduced in Li–O batteries by water accession ( Yu et al., 2017 ). similarly, Huang et alabama. ( 2013 ) synthesized a novel Au−Pd bimetallistic nanostructure as a platform for highly sensitive monitoring of catalytic reactions by SERS .
Through the quartz window of in situ Raman coin cellular telephone, the Raman laser is directly illuminated on the working electrode with electrolyte for a long prison term, so the laser source might influence the measurement. therefore, two identical in situ Raman mint cells are assembled with the working electrode of Li4Ti5O12 and the electrolyte of 1 M LiClO4 in EC/DEC ( 1:1 in volume ), and we adopted two different Raman laser sources for comparison. As a solution, the Raman spectrum of Li4Ti5O12 was very stable for the wavelength of 780 nm, while the Raman D-band and G-band of carbon emerged after 10 min for the wavelength of 532 nm, as shown in Figure 7. By promote increasing the measure meter, only carbon signal can be observed in the spectrum for the wavelength of 532 nm. obviously, the electrolyte was decomposed and carbonized badly under the light of short-wavelength laser. Thereby, in situ measurement can be conducted for a long prison term by using the long-wavelength laser with a humble photon department of energy .
Figure 7. Raman spectrum of Li4Ti5O12 electrodes measured by using different laser sources, with the laser wavelength of 532 and 780 nanometer for the blasphemous and red curves, respectively .
By using our in situ Raman coin cell, the in situ Raman spectrum were collected for the ferment electrode of Li4Ti5O12, as shown in Figure 8. At the charge country, we observed the typical Raman bands of Li4Ti5O12. After dismissal, these Raman bands disappeared clearly, while they recovered after recharge. These phenomena are excellently coherent with early literatures ( Schneider et al., 2011 ; Shu et al., 2011 ). presently, it is silent not clear about the disappearance of Raman bespeak in this subject. normally, it might be owing to structure change during phase passage ( Schneider et al., 2011 ). In addition, Li4Ti5O12 substantial becomes electrically conductive after dispatch, and then the ocular clamber astuteness of the laser will be reduced, which in turning will lead to the disappearance of Raman signals. consequently, the in situ Raman signals can be used to study the local structures and variations, which is quite useful to reveal the structure abasement in Li-ion batteries .
Figure 8. In situ Raman spectrum of Li4Ti5O12 electrode. The Raman spectrum evolved as the charged electrode ( bottom crimson bend ) was discharged to 1.2 V ( middle aristocratic curvature ) and then charged to 2.0 V ( top green curl ) .
however, in situ Raman was rarely adopted in Li-ion batteries for some problems. In the in situ Raman mint cell, the conductive agent of carbon paper would seriously suppress the Raman signals in the cultivate electrode, which can be overcome by using the SERS technique as dropping gold-dielectric nanocomposites on a normal electrode with carbon. To prevent the decomposition of electrolyte, we can replace the short-wavelength laser with the long-wavelength laser, while some vibrational modes might be lost in the new Raman spectrum. During continuous charging and empty, the fluorescent background would be increased with the electrolyte decay, resulting in a weak Raman signal well .
In this solve, we designed the in situ XRD/Raman mint cells and optimized their configurations by testing the working electrodes of Li4Ti5O12 and LiFePO4. In the in situ XRD coin cell, the Be plane of 0.2 mm thickly was chosen to reduce the x-ray concentration, and the internal pressure was tailored to prevent bending the thin Be sheet. The electrolyte of LiPF6 was proved to be a well choice for both cathode and anode materials, while the electrolyte of LiClO4 could not be adopted for the cathode materials. From the in situ XRD results, the flower put and intensity can be used to evaluate the phase fraction and lattice constants, which is significant to study the structural development in Li-ion batteries. On the other hand, in the in situ Raman coin cell, the conductive agent of carbon would suppress the Raman signals in the work electrode, which can be resolved by reducing the carbon message for conductive electrode materials or adopting SERS for normal electrodes. The long-wavelength laser was better for in situ Raman measurements, for the electrolyte of Li-ion batteries would be decomposed and carbonized seriously under the illuminance of short-wavelength laser. According to the in situ Raman results, the local anesthetic structures and variations can be investigated to reveal the structure abasement in Li-ion batteries. therefore, in situ coin cells could be improved to investigate a assortment of electrode materials, and this proficiency would arouse wide-eyed interests in the electrochemical playing field .
YC directed the project, DL took charge of this investigation, LZ optimized in situ cells, analyzed the datum, and authored the manuscript, XG designed the original in situ cells, and all authors contributed to the discussion .
Conflict of Interest Statement
The authors declare that the research was conducted in the absence of any commercial or fiscal relationships that could be construed as a likely battle of concern .
This bring was financially supported by the NSFC ( No. 21603048 and No. 51362009 ), Natural Science Foundation of Hainan ( Grant No. 20165186 ), the Science and Technology Development Special Fund Project ( ZY2016HN07 ), the International Science & Technology Cooperation Program of Hainan ( KJHZ2015-02 ), and the Hainan University ’ s Scientific Research Foundation ( kyqd1545 ) .
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