Stability and improvement of two-dimensional transition metal carbides and/or carbonitrides (MXene)
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摘要: 二維（2D）過渡金屬碳化物/碳氮化物(Mxene)材料，因其良好的親水性、導電性、柔韌性以及高贗電容等特性，在儲能、海水淡化、催化、電磁干擾屏蔽、透明導電薄膜等領域有著巨大的應用潛力。然而，由于MXene材料中活性過渡金屬、表面官能團以及結構缺陷的存在，使其在無保護的環境中（含有水、氧等）很容易被氧化，導致穩定性較差。MXene材料的氧化破壞了其片狀結構，降低了其電導率，限制了其更廣泛的應用。本文簡要介紹了MXene的結構和合成方法；綜述了MXene在不同條件下不穩定的機理，即表面官能團和周圍介質發生氧化反應；并從儲存條件、合成方法、氣氛熱處理、表面電性修飾、摻雜等方面討論了提高MXene穩定性的方法。Abstract: In recent years, a new family of two-dimensional (2D) transition metal carbides and/or carbonitrides, labeled MXenes, has attracted immense attention from researchers. Due to unusual hydrophilicity, electrical conductivity, flexibility, and pseudocapacitance, MXenes have great potential application in energy storage, water desalination, catalysis, electromagnetic interference shielding, transparent conductive films, and so on. However, MXenes exhibit poor stability because of their structural defects, active transition metals, and termination groups. These greatly destroy the sheet structure and decrease their conductivity, thereby restricting their application fields. In this review, the structure and synthesis methods of MXenes are briefly introduced. Then, we focus on current research studies regarding the stability of MXenes. The mechanism of oxidation is also discussed. Ti vacancies and the edges are the preferential oxidation sites in MXene sheets. Based on this, the methods to improve the MXene stability, including controlling the storage environment, improving the synthesis method, annealing in an atmosphere, modification based on the surface electric state, and doping impurities, are further discussed. First, the optimal requirements for MXenes storage are low temperature, desiccation, and oxygen isolation. Second, soft etching methods must be applied to synthesize MXenes to reduce the defect density of their sheet surface. Then, annealing MXenes in an atmosphere can enable the tailoring of the surface structure and functional groups for enhanced MXene stability. Lastly, more methods have been applied to improve the stability of MXenes based on their surface electric state. Since the MXene sheet surface is electronegative, their oxidation can be impeded by loading cations into the sheets. Similarly, since the edge of these sheets is electropositive, polyanions can be absorbed onto the edge to protect the MXene sheets. Moreover, compositing metal oxides, organic macromolecules, and nanocarbon on their surface can also improve the stability of MXenes. Finally, doping with impurities can also improve the band energy of MXenes. Meanwhile, our idea to improve the stability of MXenes is also briefly introduced.
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Key words:
- MXene /
- stability /
- mechanism /
- oxidation /
- improvement
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圖 1 MXene合成從2011年到2019年發展的時間線
Figure 1. Timeline of MXene: a journey from 2011 to 2019
圖 2 (a)Ti3C2Tx氧化過程，其中碳在內部電場的正電側被氧化，而Ti離子在負電側被氧化，電子向凸面位置的快速傳遞和Ti離子的緩慢擴散促進了內部電場的形成[30]；(b)氧化機制示意圖，其中頂部和底部的Ti層首先被氧化形成非常薄的銳鈦礦納米顆粒，然后Ti從中間層擴散到表層，促進完整的3D納米顆粒生長[31]
Figure 2. (a) Illustration of Ti3C2Tx oxidation with carbon and Ti-ions being oxidized at the positive and negative sides of the internal electric field, respectively. Fast electron transport toward a convex location and slow diffusion of Ti-ions enable the internal electric field formation[30]; (b) oxidation mechanisms, wherein the top and bottom Ti layers are first oxidized to form very thin anatase nanoparticles, followed by Ti diffusion from the middle layer to the complete growth of 3D nanoparticles[31]
圖 3 (a)新制Ti3C2Tx溶液和在室溫空氣環境中保存(b)7 d和(c)30 d的TEM圖像; (d～f)分別為(a～c)的高分辨率TEM圖像; (d)中插入的是其對應的SAED圖形，(e)和(f)中插入的是對應的FFT圖像[35]
Figure 3. TEM images of (a) MXene sheets from fresh Ti3C2Tx solution and aged solutions in Air-RT for (b) 7 days and (c) 30 days, respectively; (d–f) high-resolution TEM images in panels (a–c), respectively; the inset in panel (d) is the corresponding SAED pattern, and those in panels (e) and (f) are the corresponding FFT patterns[35]
圖 6 MXene水溶液分散體（0.5 mg·mL?1）在(a)室溫下(～25 oC), (b) ?20 °C儲存的照片; (c)新制Mxene, (d)在–20 oC下保存650 d的Mxene, 以及(e)在室溫下保存2 d的MXene的TEM圖像[43]
Figure 6. Photos of the aqueous MXene dispersion (0.5 mg·mL?1) stored at (a) room temperature (RT, ～25 oC) and (b) –20°C; TEM images of (c) fresh MXene, (d) MXene stored at ?20 oC for 650 days, and (e) MXene stored at room temperature for two days[43]
圖 7 (a)Ti3C2Tx薄膜經真空抽濾后，在不同溫度和濕度下儲存8周后的歸一化電阻; (b)MXene溶液經真空過濾后在D@?80, D@?18, D@5和E@5條件下存儲5周后獲得的Ti3C2Tx薄膜光學圖像[38]
Figure 7. (a) Normalized resistances of various Ti3C2Tx MXene films obtained with vacuum filtration after storage for up to eight weeks under various temperatures and humidities; (b) optical images of Ti3C2Tx films obtained from MXene solutions with vacuum filtration after five weeks of storage in D@?80, D@?18, D@5, and E@5[38]
圖 8 (a)d-Ti2CTx在Ar-LT中儲存12 h后的TEM圖像; (b)Ti3C2Tx膠體在不同環境下的穩定性曲線(實線是根據經驗方程A = Aunre + Aree?t/τ擬合的結果)[43]
Figure 8. (a) TEM image of d-Ti2CTx stored in Ar-LT for 12 h; (b) stability of colloidal Ti3C2Tx in different environments(the dotted lines are the fitting results according to the empirical equation A = Aunre + Aree?t/τ) [43]
圖 10 (a)由不同儲存時間溶液制成的Al?Ti3C2Tx薄膜的導電性; (b)由不同儲存時間溶液制成的薄膜的拉曼光譜; (c)新制的Al?Ti3C2Tx薄片和(d)儲存10個月后溶液中的Al?Ti3C2Tx薄片的TEM圖像(紅色圓圈表示薄片中所有可觀測到的孔洞)[45]
Figure 10. (a) Electronic conductivity of freestanding Al?Ti3C2Tx films made from solutions stored for different periods; (b) Raman spectra of films made from solutions stored for different periods; TEM images of a fresh Al?Ti3C2Tx flake (c) and an Al?Ti3C2Tx flake from a 10-month-old solution (d) (the red circles mark all the observable pinholes in the flake)[45]
圖 11 (a)Ti3C2薄膜在氫氣退火前后，在100%相對濕度和70 °C下進行氧化穩定性試驗時，薄片電阻的隨時間變化的曲線; (b)氧化前和氧化1 d后氫退火樣品（900 °C）的XRD譜圖; (c)氫退火后的樣品和(d)普通樣品在70 °C和100% RH下保存1 d后的SEM圖像[46]
Figure 11. (a) Time evolution of the sheet resistances of Ti3C2 MXene thin films subjected to oxidation stability tests in 100% relative humidity and at 70 °C, before and after the films were annealed under hydrogen; (b) XRD patterns of an as-prepared sample and a hydrogen-annealed sample (900 °C) before and after oxidation for 1 day; SEM images of (c) a hydrogen-annealed and (d) an as-prepared sample after maintaining at 70 °C and 100% RH for 1 day[46]
圖 12 (a)Ti3C2Tx薄膜制備原理圖； (b)Ti3AlC2、退火前的薄膜，退火后的薄膜在水中儲存10個月后的XRD譜圖; (c)在水中貯存10個月的退火MXene膜的光學圖像[47]
Figure 12. (a) Schematic of the Ti3C2Tx film preparation; (b) X-ray diffraction (XRD) spectra of Ti3AlC2 MAX phase particles, the as-prepared film made by nanosheets prior to annealing, and annealed MXene films subject to 10-month storage in water; (c) optical images of annealed MXene films subject to 10-month storage in water[47]
圖 13 (a) 微流控裝置示意圖; (b)MXene膜72 h后在去離子水中保持穩定，而GO膜則不穩定; (c) MXene膜在浸泡前(dry)、浸泡后(wet)和再干燥后的XRD圖譜，表明MXene膜在浸泡過程中很大程度上保留了層狀結構[48]
Figure 13. (a) Schematic illustration of the nanofluidic device; (b) neat MXene membrane remained stable in deionized (DI) water after 72 h. Conversely, the neat graphene oxide (GO) membrane was not stable; (c) XRD pattern of the MXene membrane before immersion (dry), after immersion (wet), and after redrying, suggesting that its laminar structure is largely retained during these processes[48]
圖 14 (a)加載聚陰離子封裝MXene薄片邊界的原理示意圖; (b)用于EELS分析的薄片的環形暗場-掃描透射電子顯微鏡(STEM-ADF)圖像; (c, d) P、Ti和C的EELS信號沿著圖(b)中c和d處標記箭頭從真空走向MXene薄片邊緣的歸一化強度(箭頭有一個從藍色到紅色的漸變，其中藍色代表真空區域，紅色代表MXene薄片區域，箭頭標記對應著從那里獲得信號的位置)[49]
Figure 14. (a) The schematic of edge capping of MXene sheets by polyanions; (b) STEM-ADF image of the flake used for EELS analysis; (c, d) normalized intensities of P, Ti, and C EELS signals transitioning from vacuum toward the edge of the MXene flake along the marked arrows c and d (The arrow has a gradient from blue to red, where the blue color represents the area over vacuum and red, the area over the MXene flake. The arrow marks correspond to the positions from where the signal was obtained. Similar arrows are marked on the STEM-ADF image shown in (b) for easy comparison)[49]
圖 16 (a)鍍納米碳穩定Ti3C2Tx的合成示意圖,它包括葡萄糖分子通過氫鍵在MXene表面的優先吸附，葡萄糖與水熱碳（R =烷基、乙烯基、環烷基或芳基）的原位聚合，以及隨后的高溫熱碳化; 鍍納米碳Ti3C2Tx MXene的(b)SEM圖像和(c)TEM圖像[52]
Figure 16. (a) Schematic illustration of the strategy for stabilizing Ti3C2Tx MXene by carbon nanoplating, it involves the preferential adsorption of glucose molecules on the MXene surface via hydrogen bonding, the in-situ polymerization of glucose to hydrothermal carbon (R = alkyl, vinyl, cycloalkyl, or aryl groups), and subsequent thermal carbonization at high temperature; (b) SEM image and (c) TEM image of carbon-nanoplated Ti3C2Tx MXene [52]
圖 17 (a)不同方法合成SnO2/MXene的合成示意圖; SnO2/MXene的(b)低分辨TEM圖像和(c)傅里葉濾波高分辨率RGB圖像((b)中插圖為其對應的SAED圖像)[53]
Figure 17. (a) Schematic illustration of the various methods used for SnO2 deposition on Ti3C2 MXene sheets; (b) TEM image and (c) Fourier-filtered high-resolution RGB image of SnO2/MXene (the inset of (b) is the corresponding SAED pattern of SnO2/Mxene)[53]
久色视频
圖 18 (a)褶皺N?Ti3C2Tx的合成示意圖; 褶皺N?Ti3C2Tx的(b)低倍和(c) 高倍SEM圖像; (d)摻雜N元素和未摻雜的Ti3C2Tx 1000次循環的循環性能[56]
Figure 18. (a) Schematic illustration of the synthesis of crumpled N?Ti3C2Tx; (b) low magnifications and (c) high magnifications SEM images of N?Ti3C2Tx; (d) cycling performances of crumpled N?Ti3C2Tx/S electrodes and mixed-Ti3C2Tx/S electrodes for 1000 cycles[56]
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