Promoting sodium ion conduction: bridging strategy for sodium ion transport between NASICON ceramic granules

doi:10.21203/rs.3.rs-4639245/v1

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Promoting sodium ion conduction: bridging strategy for sodium ion transport between NASICON ceramic granules

https://doi.org/10.21203/rs.3.rs-4639245/v1

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Aiming to the key issue, the interruption of ion transport across the NASICON ceramic granules caused by ZrO₂, glass and pores, in the Na₃Zr₂Si₂PO₁₂ (NZSP) solid-state electrolytes (SSEs). We propose the bridging strategy, basing on which Zn-NZSP/zeolitic imidazolate frameworks-8 (ZIF-8)/poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-HFP) SSEs with improved ionic conductivity is successfully prepared utilizing Zn-NZSP, ZIF-8 and PVDF-HFP. The impurity phases of ZrO₂ and glass are inhibited via suppressing the volatilization of Na source and P source to avoid impurity hindrance of sodium ion transport. Then, the good interface contact between Zn-NZSP and ZIF-8 is realized via the heterogeneous nucleation and in-situ growth of ZIF-8 along the surface of Zn-NZSP granules, as well as the good interface contact between ZIF-8 and PVDF-HFP is realized through the organic compatibility, constructing a bridging structure without pores. As a result, the optimized Zn-NZSP/ZIF-8/PVDF-HFP SSE delivers a high ionic conductivity of 2.2 mS cm^–1 owing to the dense bridging structure without ZrO₂, glass and pores (0.048 mS cm^− 1 of NZSP). The symmetrical battery of NaǀSSEǀNa displays the charge-discharge voltages of ± 0.15 V and a long cycle life of more than 1500 h. This work pioneers the interface bridging strategy to connect the adjacent NASICON ceramic granules by impurity suppression and good interface contact, which is a powerful strategy to construct high sodium ion transport performance of SSEs for solid-state sodium ion batteries.

Physical sciences/Materials science/Materials for energy and catalysis/Metal–organic frameworks

Physical sciences/Engineering/Chemical engineering

Solid-state electrolyte

NASICON

Bridging strategy

Sodium ionic conductivity

Solid-state electrolytes are of great significance for developing solid-state batteries with enhanced safety and high energy density. In the past years, sodium (Na) superionic conductors (NASICON) have been explored as a promising class of solid-state electrolytes for Na-based solid-state batteries, owing to their high ionic conductivity (> 0.1 mS cm^− 1 at room temperature) and excellent (electro-)chemical stability ^[1–6]. For example, Na₃Zr₂Si₂PO₁₂ (NZSP) is one of the representatives of NASICON-type solid-state electrolytes and has attracted considerable interest ^[7–10]. In the crystal structure of NASICON, the corner-shared oxygen ions link (Si/P)O₄ tetrahedra with ZrO₆ octahedra to create a three-dimensional ionic conduction pathway for the rapid transport of the active Na-ions ^[11–13]. However, the ionic conductivity of NASICON-type solid-state electrolytes remains much lower than that of conventional liquid electrolytes used in batteries (Table S1). Based on the understanding of the crystal structure of NASICON and the ion transport mechanism in NASICON crystal, many approaches have been extensively explored to further enhance the ionic conductivity of NASICON-type solid-state electrolytes ^[14–17].

Compared to homogeneous liquid electrolytes, NASICON-type solid-state electrolytes are generally a continuous network composed of NASICON ceramic granules ^[18–20]. Therefore, the Na-ions transport process in NASICON-type solid-state electrolytes contains two steps: the bulk diffusion of Na-ions in crystalline NASICON ceramic granules and the interfacial conduction of Na-ions between adjacent NASICON ceramic granules ^[21–23]. As known, NASICON-type solid-state electrolytes are usually accompanied by the ZrO₂ phase due to the evaporation loss of Na and P during the sintering process ^{[24, 25]}. The presence of the ZrO₂ phase causes Si and Na elements to be enriched on the surface of NASICON ceramic granules, eventually forming a glassy phase. The ionic conductivity of the glass phase is much lower than that of NASICON ceramics and thus creates additional interfacial ion transport resistance between NASICON ceramic granules ^{[26, 27]}. Accordingly, besides enhancing the native ionic conductivity of NASICON-type solid-state electrolytes, reducing the interfacial resistance for ionic transport across the NASICON ceramic granules is also critical for improving the overall ionic conductivity of NASICON-type solid-state electrolytes. So far, several strategies have been proposed to improve both inner- and inter-granular sodium ion conduction in NASICON-type solid-state electrolytes. For example, replacing Zr in ZrO₆ octahedra with other transition metals can optimize the transport channel for sodium ion conduction in ZrO₆ octahedra, but it cannot inhibit the formation of the glass phase ^[28]; adding excess Na and P resources can compensate for the evaporation loss of Na and P, partially suppressing the formation of the ZrO₂ phase ^{[29, 30]}; a combination of the two above strategies has also proved to be an efficient way ^[21]. Although these strategies have led to a notable improvement in the inner-granular ionic conductivity of NASICON-type solid-state electrolytes, the ZrO₂ phase still cannot be eliminated in NASICON-type solid-state electrolytes, and thus there is still a high interfacial resistance for sodium ion conduction between NASICON ceramic granules. It is important to explore new strategies and develop related theories to reduce such interfacial resistance.

An ideal strategy is urgent to promote the sodium ion transport through reducing interfacial resistance. As shown in Fig. 1, the bridging idea for increasing sodium ion conductivity is proposed. Before surface functionalization, it is necessary to eliminate the barrier caused by ZrO₂ and glass impurities for sodium ion transport. Reasonable doping of transition metal ions has obvious potential for eliminating impurities. Moreover, it is necessary to explore the suitable interfacial bridging agent. Zeolitic imidazolate framework − 8 (ZIF − 8) is a class of metal–organic frameworks constructed from tetrahedrally coordinated Zn ions linked by anionic imidazolate ligands, displaying both organic property and inorganic property ^{[31, 32]}. It is also a porous materials with ultra − high surface areas and abundance of mesopores for high sodium ion transport properties ^{[33, 34]}. Moreover, our previous work proved that ZIF − 8 possesses the excellent film forming properties and builds good contact interfaces along the surface of inorganic material ^[35]. Poly(vinylidenefluoride − co − hexafluoropropylene) (PVDF − HFP) has been widely studied as a polymer matrix owing to the relatively higher ionic conductivity ^{[36, 37]}. Remarkably, the organic properties of PVDF-HFP and ZIF-8 are easy to form a good contact interface.

In this work, ZnO, a typical flux for the high-temperature melting method, was utilized as additives to prepare NASICON-type solid-state electrolytes, Zn-NZSP. Through precisely tuning the contents of ZnO additives, the ZrO₂ phase was successfully eliminated in the as-prepared NZSP, and at the same time, Zr⁴⁺ in ZrO₆ octahedra was partially replaced by Zn²⁺. Furthermore, the surface of NZSP granules was functionalized with a thin layer of ZIF-8 to facilitate the sodium ion transport between NZSP granules. Attributed to the increase of ionic conductivity in NZSP granules and the decrease of interfacial ionic transport resistance between NZSP granules, the overall sodium ion conductivity of NZSP was significantly improved, reaching 2.2 mS cm^–1. Finally, a symmetrical battery of NaǀSSEǀNa was assembled with the as-prepared NZSP as the solid-state electrolyte and exhibited high energy storage performance with charge-discharge voltages of ± 0.15 V and a long cycle life of more than 1500 h. The interface bridging strategy may be used to reduce the sodium ion transfer resistance between ceramic granules, riching the approaches to enhance SSE conductivity for high performance energy storage devices.

The phase compositions of NZSP and Zn-NZSP samples prepared according to Table S2 were analyzed by X-ray diffraction (XRD) (Fig. 2a). The results show that the peaks of all samples are indexed to the NZSP phase (PDF No. 84-1200). However, the extra peaks marked by ★ and ▲ of NZSP sample are indexed to the ZrO₂ phase (PDF No. 86-1451) and Na₂ZrSi₂O₇ phase (PDF No. 73-2309), while the pattern of 0.15Zn-NZSP sample displays the peak marked by ⚪ of Na₂ZnSiO₄ phase (PDF No. 87-1572). These results indicate that the doping of Zn element can reduce the unexpected ZrO₂ and Na₂ZrSi₂O₇ phases, however, the amount of dopant needs to be limited. As shown in Fig. 2b and Fig. 2c, the high resolution transmission electron microscope (HRTEM) images the crystalline phases of NZSP and 0.1Zn-NZSP samples, respectively. In addition to the NASICON phase, the HRTEM results also indicate the co-existence of ZrO₂, Na₂ZrSi₂O₇ and glass phases in NZSP samples. Because ZnO, as a typical flux, helps to NASICON crystal growth and inhibit the volatilization of Na and P sources, 0.1Zn-NZSP sample only displays the NZSP phase ^{[38, 39]}. The scanning electron microscope (SEM) images of NZSP and 0.1Zn-NZSP samples are shown in Fig. S1 and Fig. S2, respectively. The granule size of NZSP is a range of 0.1 − 1.5 µm, while the size of 0.1Zn-NZSP is a range of 0.5 − 3.0 µm, and it suggests that ZnO can be used to increase the granule size. The thermogravimetry (TG)-differential scanning calorimeter (DSC) analysis is shown in Fig. 2d. The red lines are the DSC curves and the blue lines are the TG curves. The pronounced peaks at 109°C, 293°C and 572°C can be assigned to the volatilization of free water, the decomposition of ammonium dihydrogen phosphate and the decomposition of sodium carbonate, respectively. While the peaks at 1080°C corresponding to the crystallization of NZSP. These results indicate that appropriate Zn-doping can reduce the unexpected ZrO₂ and Na₂ZrSi₂O₇ phases. Electrochemical impedance spectroscopy (EIS) analyses were used to examine the ion transport performance. The EIS spectra are in the form of a semi-circle with the real axis intercepts occurring at the lower frequency end, this corresponds to the total resistance, including the grain and interfacial resistances. The EIS curves of NZSP, 0.05Zn-NZSP, 0.1Zn-NZSP, 0.15Zn-NZSP samples are shown in Fig. S3. The total conductivities were calculated for the sample optimization (Fig. 2e). The divalent metal Zn can replace Zr into ZrO₆ octahedron to modify the sodium transport channel ^{[40, 41]}, thus 0.1Zn-NZSP sample displays the highest ion conductivity of 0.32 mS cm^− 1, while that of NZSP sample is 0.048 mS cm^− 1. These results prove that ZnO is a good dopant to suppress the ZrO₂ and Na₂ZrSi₂O₇ phases, thus improving the ion conductivity.

A schematic illustration of the synthesis route for the Zn-NZSP/ZIF-8/PVDF-HFP SSEs is shown in Fig. 3a. Firstly, the raw materials with strictly stoichiometry were mixed to obtain the precursor, the precursor was transformed into Zn-NZSP after annealed in an air atmosphere. Secondly, the ZIF-8 film grow up along with the ZnO₆ octahedron on the surface of Zn-NZSP granules via heterogeneous nucleation and growth of ZIF-8, forming the Zn-NZSP/ZIF-8 intermediate. Finally, the Zn-NZSP/ZIF-8 intermediates were evenly dispersed in PVDF-HFP solution, the Zn-NZSP/ZIF-8/PVDF-HFP samples were obtained after consolidation and drying. The ratios of Zn-NZSP and ZIF-8 were used to optimize ZIF-8 film (Table S3). As-obtained samples were probed by XRD and SEM. The thin ZIF-8 film on the surface of Zn-NZSP can’t be probed by XRD, so only the pure NASICON phase is displayed (Fig. S4). Notably, the SEM image in Fig. S5 exhibits the rough surface compared with the image in Fig. S2, suggesting the ZIF-8 surface coating on the Zn-NZSP granules. The XRD (Fig. S4) and SEM (Fig. S6) results indicate the formation of SSEs with good interface contact. The EIS curves of all samples were obtained at different temperatures (Fig. S7). As-obtained total sodium ionic conductivities in Fig. 3b indicate that C sample possesses the highest conductivity of 2.2 mS cm^–1 at 25 ^oC, and the sodium ion conductivities of C sample at 30 to 80 ^oC are the highest among all of samples (Fig. 3c). Remarkably, the SSE films of NZSP/PVDF-HFP, NZSP/ZIF-8 and ZIF-8/PVDF-HFP can’t be formed through such technology.

The ZIF-8 structure on the NZSP surface was probed by the TEM and EDS mapping. In Fig. 4a, the low magnification image displays some granules with the size range of 0.5 − 2 µm, it is consistent with the SEM result (Fig. S2). The enlarged image shown in Fig. 4b displays that the d-spacing of 0.452 nm corresponds to the (020) plane of NZSP around by the amorphous structure. The clear and orderly diffraction pattern in the inset of Fig. 4b indicates the single crystal feature. Note that the position marked by the red dashed line reveals the good connected interface between NZSP and ZIF-8. In Fig. 4c, the elemental mappings of Na, Zr, Si, P and O exhibit the phase interface between NZSP and ZIF-8, while the mappings of Zn and N are uniformly distributed, indicating the uniformity of ZIF-8 coating layer. Therefore, above TEM and EDS mapping results prove that the good interface was constructed between the NZSP and the ZIF-8 layer. Furthermore, XPS was employed to identify the interface contact between the NZSP, ZIF-8 and PVDF-HFP. The peak located at 285.0 eV was used for the spectrum calibration. The survey spectra of the Zn-NZSP/ZIF-8 and Zn-NZSP/ZIF-8/PVDF-HFP samples evidence the presence of Na, Zr, Zn, Si, P, N (Fig. S8) and Na, Zr, Zn, Si, P, N, C, F (Fig. S9), respectively. In addition, the peak locations of Na, Zr, Zn, Si, P in the high − resolution XPS spectra indicate the bonding consistency. As shown in Fig. 4d, compared to the N 1s peak at 399.2 eV of ZIF-8 sample, the N 1s peak at 399.1 eV of 0.1Zn-NZSP/ZIF-8 confirm the formation of good interface. While, the N 1s peak at 400.0 eV of Zn-NZSP/ZIF-8/PVDF-HFP sample indicate the bonding combination of N in ZIF-8 layer was increased. Similarly, the F 1s peak (686.6 eV) of PVDF-HFP moved in the direction of large bonding energy (688.3 eV) in Fig. 4e, indicating the bonding combination of F in PVDF-HFP layer was increased. Therefore, the XPS results confirm that the formation of compatibility interface in Zn-NZSP/ZIF-8/PVDF-HFP bridging structure^{[42, 43]}, which are attributed to both rigid (inorganic) and flexible (organic) properties of ZIF-8 ^{[44, 45]}.

In order to highlight the bridging effect of ZIF-8/PVDF-HFP, we compare the structure and performance of the NZSP, 0.1Zn-NZSP and 0.1Zn-NZSP/ZIF-8/PVDF-HFP samples. The schematic illustration of such sample structures is shown in Fig. 5a. The pores, cracks and ZrO₂ impurity in the NZSP sample (Fig. 5b) hindered the sodium ion transport. After Zn-doping, the cracks and ZrO₂ impurity were avoided due to the assistive melting effect of ZnO, but the size range of pores increased (Fig. 5c) due to the foaming caused by oxygen production. The performance enhancement (Fig. 2e) after Zn-doping indicates the avoiding of cracks and ZrO₂ impurity is significant. Furthermore, the formation of Zn-NZSP/ZIF-8/PVDF-HFP avoided the pore structure (Fig. 5c) evidenced by the SEM results in Fig. 5d, delivering the improved sodium ion transport performance (Fig. 3).

To explore the reasons for performance improvement, the EIS curves of NZSP, 0.1Zn-NZSP and C samples at 30 − 80 ^oC (Fig. S10) were obtained to calculate the sodium ion conductivities of these samples for the inner-granular, intergranular and total. Please see the sodium ion conductivities of NZSP and 0.1Zn-NZSP samples at different temperatures in Fig. 6a and Fig. 6b. The crossover phenomenon is very obvious, especially before the granule bridging, the total conductivity is significantly affected by temperature. Differently, the sodium ion conductivities of C sample are smoothly enhanced with the temperature increasing (Fig. 6c). This pattern indicates that the regular consistency of inner-granular, intergranular and total conductivities with the temperature variation is conducive to obtaining high performance. In Fig. S11, the curves of 1000/T − lnɑ were used to obtain the activation energies, the results are compared in Fig. 6d. The minimum difference in activation energy between grains and boundaries determines the minimum value of total activation energy (0.25 eV). It is the result of bridging effect of ZIF-8/PVDF-HFP among the NASICON granules, resulting in a homogeneous ion transport.

For proof-of-application, the battery performances of the Zn-NZSP/ZIF-8/PVDF-HFP SSEs were evaluated via the symmetrical Na|SSEs|Na cells, the charge-discharge were tested at 1 mA cm^− 2. As shown in Fig. 7a, the charge-discharge performances of all samples are compared, the cell with C sample displays the smooth charge-discharge voltages of ± 0.15 V, such optimize result is consistent with the optimized ionic conductivity. Furthermore, the optimal sample was used to compare with the commercial glass fiber SSE and polypropylene SSE (Fig. 7b), exhibiting sufficient stability due to the excellent interface connectivity via the bridging structure ^{[46, 47]}. In Fig. 7c, the long cycle test displays good stability for more than 1500 h, reflecting the good structural stability. Moreover, the voltage window of the best sample is 6.5 V (Fig. S12), indicating its stability.

In summary, we designed a novel bridging structure, Zn-NZSP/ZIF-8/PVDF-HFP, to connect the adjacent NASICON ceramic granules and reduce the interfacial resistance for ionic transport across the NASICON ceramic granules. Remarkably, the impurity phase such as ZrO₂ was eliminated by the ZnO dopant inhibiting the volatilization of sodium and phosphorus sources, and the transport path of sodium ion was modified by replacing Zr with Zn. Then, the excellent interface connectivity via the bridging structure between Zn-NZSP, ZIF-8 and PVDF-HFP was realized via the heterogeneous nucleation and in-situ growth of ZIF-8 along the surface of Zn-NZSP granules, as well as solidification of PVDF-HFP. The optimized Zn-NZSP/ZIF-8/PVDF-HFP sample delivered an ionic conductivity of 2.2 mS cm^–1 and an unprecedented low activation energy of 0.25 eV based on above bridging structure. Moreover, in a symmetrical battery of NaǀSSEsǀNa, the charge-discharge voltages were ± 0.15 V and a long cycle life was more than 1500 h. This work provides a convenient and effective bridging strategy, an enlightening insights into material interface treatment and a new opportunities for advancing high-performance energy storage technologies and beyond.

Sample preparation

Zn-NZSP powder

Firstly, according to the stoichiometric ratio in Table S2, each chemical reagent was placed in the ball mill tank. The chemical reagent powder was ground with a planetary ball mill at a speed of 290 rpm/min for 24 h. Subsequently, the mixture precursors were dried at 85 ^oC for 12 h. Then, calcined in a muffle furnace at a high temperature of 1150 ^oC for 5 h with a heating rate of 5 ^oC/min. In order to obtain powder with a more uniform granule size, the calcined powder needs to be ball milled and dried again under the process conditions of 290 rpm/min for 24 h.

Zn-NZSP/ZIF-8

According to the stoichiometric ratio in Table S3, the NZSP powder was dispersed into methanol to form a uniform slurry by ultrasonic. Then, Zn(NO₃)₂·6H₂O and 2-methylimidazole were dissolved into the above slurry by magnetic stirring for 1 h. The mixture was aged at room temperature for 24 h, then the white powders were precipitated. After washing with methanol and drying at 85 ^oC for 12 h, the samples of Zn-NZSP/ZIF-8 were obtained.

Zn-NZSP/ZIF-8/PVDF-HFP SSEs: 10 g PVDF-HFP was added into 2.5 ml NMP and stirred in 50°C water bath for 6 h to obtain uniform and transparent sol. As-obtained A − E samples of Zn-NZSP/ZIF-8 were dispersed into above sol by magnetic stirring for 10 h, respectively, the Zn-NZSP/ZIF-8:sol = 1 g:2 ml. Such uniform slurry was uniformly coated on a clean glass plate and solidified at 50°C for 10 h to obtain Zn-NZSP/ZIF-8/PVDF-HFP SSEs. Corresponding to the Zn-NZSP/ZIF-8 samples of 1 − 5, the Zn-NZSP/ZIF-8/PVDF-HFP SSE samples were named as Zn-NZSP/ZIF-8/PVDF-HFP-1 (A), Zn-NZSP/ZIF-8/PVDF-HFP-2 (B), Zn-NZSP/ZIF-8/PVDF-HFP-3 (C), Zn-NZSP/ZIF-8/PVDF-HFP-4 (D) and Zn-NZSP/ZIF-8/PVDF-HFP-5 (E), respectively.

Characterization

The structures, compositions, and morphologies of all samples were analyzed using X-ray diffraction (XRD, Rigaku Smartlab with Cu Kα radiation of λ = 0.154 nm), scanning electron microscopy (SEM, Zeiss Zigma), transmission electron microscopy (TEM, FEI Talos F200s) with EDS mapping, X-ray photoelectron spectroscopy (XPS, VG Scientific ESCALAB250), and simultaneous thermal analyzer (STA 449F3, Netzsch, Selb, Germany) combined with differential scanning calorimetry with thermogravimetry (TG).

Electrochemical evaluation

The electrochemical impedance spectroscopy (EIS) measurements were performed on a CHI 760E electrochemical workstation to measure the ionic conductivities of solid state electrolytes. EIS was also recorded with frequencies ranging from 1000 kHz to 10 mHz and an AC signal of 5 mV in amplitude as the perturbation. The high-temperature ionic conductivity was used to evaluate the activation energy (Ea) of the SSE samples, the test temperature range was 30°C − 80°C. The charge-discharge performances were determined with CR 2032 coin cells consisted of Na electrodes and as-prepared SSEs.

Acknowledgements

This research was supported by Universities Twenty Foundational Items of Jinan City (2021GXRC039), Major innovation project for integrating science, education & industry of Qilu University of Technology (Shandong Academy of Sciences) (grant No. 2022JBZ01-07), Shandong SMES promotion project (2023TSGC0572), Taishan Scholar Program of Shandong Province (tstp20230631), the Qilu University of Technology (Shandong Academy of Sciences) Peixin Fund (grant no. 2023PX003) and 2023TSGC0572.

Conflict of Interest

The authors declare no conflict of interest.

Author Contributions

Xiaolong Xu and Xiaopeng Hao conceived the idea, wrote the manuscript. Zizheng Ai and Yongzhong Wu are overall logical thinking and revising the manuscript. Zhiliang Xiu, Yongliang Shao, Huaping Zhao, Yong Lei and Yucheng Sun, helped with the preparation of NZSP powders, battery assembly, electrochemical tests, and data analyses. All authors participated in discussing and writing the manuscript, read and approved the final manuscript.

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Promoting sodium ion conduction: bridging strategy for sodium ion transport between NASICON ceramic granules

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