Terminal Groups Dependent Near-Field Enhancement Effect of Ti3C2Tx Nanosheets

doi:10.21203/rs.3.rs-73130/v1

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Terminal Groups Dependent Near-Field Enhancement Effect of Ti3C2Tx Nanosheets

https://doi.org/10.21203/rs.3.rs-73130/v1

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published 12 Apr, 2021

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Both multilayered (ML) and few-layered (FL) Ti₃C₂T_x nanosheets with different dominant terminal groups have been prepared through a typical etching and delaminating procedure. Various characterizations confirm that the physical and chemical performance of the nanosheets are dependent on the dominant functional groups. It has been demonstrated that ML-Ti₃C₂T_x has been mainly terminated by O-related groups, which result in better oxidation resistance and stronger near-field enhancement effect. As for FL-Ti₃C₂T_x, which is mainly terminated by hydroxyl groups, it can be better dispersed in aqueous solution and could confine stronger near-field after coupling to Ag nanostructures by electron injection.

Nanoscience

Multilayered Ti3C2Tx

Few-layered Ti3C2Tx

Terminal group

Near-field enhancement

Coupling

Ti₃C₂T_x, a typical two-dimensional layered transition metal carbide with a graphene-like structure, has attracted great attention due to its wide potential applications in fields of catalysis, energy, and medicine thanks to its unique properties, especially large specific surface area and so on [1–6]. It has been demonstrated that the physical and chemical performance of Ti₃C₂T_x will be determined by its terminal groups, referred as T_x in the formula (usually are -F, -O and/or -OH), which can be adjusted by choosing different preparation procedures [7, 8]. For example, some experimental results indicate that the hydrophilic hydrophobic equilibrium of Ti₃C₂T_x can be modulated by interacting some agent groups with -O terminal groups on Ti₃C₂T_x [9], and the Pb adsorption capacity can be improved by connecting with hydroxyl groups on Ti₃C₂T_x [10]. In the meantime, some theoretical works have determined that the attached methoxy groups could improve the stability of Ti₂C and Ti₃C₂ [11], and O-related terminal groups could enhance the lithium ion storage capacity of various nanosheets [12]. Apart from the multifarious applications by taking advantage of the unique layered structure with certain terminal groups, it is found that Ti₃C₂T_x can support near-field confinement as well [13–15]. Therefore, it is interesting to systematically study the relationship between the terminal groups of Ti₃C₂T_x and its near-field enhancement effect, since such effect has been widely employed in many optical related fields due to the strong confined electromagnetic field [16–18].

In this work, instead of HF, mixed etching agent of LiF and HCl has been used to minimize the fluorine terminals not only in the etching process, but also in the delamination procedure by sonication in water, where the multilayered Ti₃C₂T_x (ML-Ti₃C₂T_x) will be delaminated into few-layered Ti₃C₂T_x (FL-Ti₃C₂T_x) without introducing any other reagents [19]. As a result, the obtained Ti₃C₂T_x in this work will be mainly terminated by either OH- or O-related groups, which make ML-Ti₃C₂T_x and FL-Ti₃C₂T_x nanosheets reveal different physical and chemical properties and eventually present different near-filed enhancement performance. In addition, the hybrid structures composed of Ti₃C₂T_x and Ag nanoparticles have been prepared and the corresponding coupling effects have been explored as well.

Preparation of Ti3C2Tx nanosheets

ML-Ti₃C₂T_x was prepared followed a modified previously reported method [21]. The typical etching process started with the preparation of LiF solution by dissolving 1 g of LiF in 20 mL of dilute HCl solution (6 M) with stirring. Subsequently, 1 g of Ti₃AlC₂ powder was slowly added into the above solution, and the etching process was kept at 70 °C for 45 h under stirring. The wet sediment was then washed several times with deionized water until the pH of the suspension liquid was bigger than 6. Afterwards, the suspension was collected and named as ML-Ti₃C₂T_x. To obtain FL-Ti₃C₂T_x, ML-Ti₃C₂T_x was further delaminated by sonication for 2 h in Ar atmosphere and followed by centrifugation at 3500 rpm for 1 h.

Preparation of Ag/Ti3C2Tx nanocomposites

The synthesis of the hybrid materials was started with the preparation of the mixed solution of AgNO₃ (12.5 mL, 2 mmol/L) and NaC₆H₅O₇ (12.5 mL, 4 mmol/L) at room temperature. After rapidly adding PVP solution (25 mL, 0.1 g/mL), Ti₃C₂T_x solution (5 mL, 0.05 mg/mL) was then slowly added into the mixed solution with stirring for 10 min at room temperature. Subsequently, the above mixed solution was heated up to 70 °C to react for 45 h. After centrifuging, the products were kept in water and named as Ag/ML-Ti₃C₂T_x and Ag/FL- Ti₃C₂T_x, respectively, according to the type of Ti₃C₂T_x used in the procedure.

Characterization

A field emission scanning electron microscope (Carl ZEISS Sigma) and two transmission electron microscopes (JEM-2100F and JEM-1400Flash) have been employed to determine the morphologies of the samples. The X-ray diffraction (XRD) patterns in the range of 2θ = 5–80° with a step of 0.02° were recorded on a powder diffractometer (X'Pert PRO MPD). Zeta potentials and surface states of ML-Ti₃C₂T_x and FL-Ti₃C₂T_x were measured by a Malvern Zetasizer (Nano-ZS90) and an X-ray photoelectron spectroscopy (XPS, ESCALAB 250Xi), respectively. The absorption and Raman performance of samples were recorded by a UV-Vis spectrophotometer (CARY 5000) and a Raman spectroscopy (LabRAM HR Evolution), respectively. The excitation wavelength of Raman detection was 532 nm, and the laser powers for usual Raman measurements and surface enhanced Raman scattering (SERS) characterizations were 12.5 mW and 0.05 mW, respectively.

Both morphologies of ML-Ti₃C₂T_x and FL-Ti₃C₂T_x have been shown in Fig. 1a, 1b and 1c, 1d, respectively. It can be seen that FL-Ti₃C₂T_x looks more transparent, indicating that its layer number is much less than ML-Ti₃C₂T_x. Figure 1e shows the XRD patterns of all samples. Ti₃AlC₂ and ML-Ti₃C₂T_x show their typical phase features, which agree well with some previous reports [20–22]. It can be readily observed that the intense (002) peak of ML-Ti₃C₂T_x shifts to the lower angle comparing with that of Ti₃AlC₂, implying the removal of Al atoms from the MAX phase and the expanding along the c axis. Compared with the diffraction peaks of ML-Ti₃C₂T_x, both broadened (002) peak and disappeared (004) and (008) peaks of FL-Ti₃C₂T_x determined the successful preparation of the few-layered sample [23]. Moreover, the (002) peak of FL-Ti₃C₂T_x locates at a little higher angle than that of ML-Ti₃C₂T_x, indicating that ML-Ti₃C₂T_x and FL-Ti₃C₂T_x might are mainly terminated with -O and -OH groups, respectively [19, 24].

Figure 2a shows Raman spectra of ML-Ti₃C₂T_x and FL-Ti₃C₂T_x. As it can be seen that the Raman signals in the range of 200–800 cm^− 1 for both samples are quite similar. Among them, the peak at 717 cm^− 1 is due to the A_1g symmetrical out-of-plane vibration of Ti and C atoms, while the peaks at 244, 366 and 570 cm^− 1 are arising from the in-plane (shear) modes of Ti, C and surface terminal groups, respectively [25, 26]. As for the Raman signals ranging from 800 to 1800 cm^− 1, comparing with ML-Ti₃C₂T_x, FL-Ti₃C₂T_x not only shows stronger Raman signal at 1580 cm^− 1 (G band), but also presents two emerging Raman bands at 1000–1200 cm^− 1 and 1300 cm^− 1 (D band). Herein, the appearance of D band indicates that some Ti atoms have been peeled away and more C atoms are exposed to the surroundings [27]. Therefore, the integrated Raman intensity of FL-Ti₃C₂T_x in this range is slightly larger than that of ML-Ti₃C₂T_x, implying that FL-Ti₃C₂T_x adsorbs more terminal groups. Zeta potentials of ML-Ti₃C₂T_x and FL-Ti₃C₂T_x are − 4.38 and − 26.9 mV, respectively as shown in Fig. S1, which further confirm that FL-Ti₃C₂T_x are terminated by more groups with negative charges.

The UV-Vis spectra shown in Fig. 2b reveal that both FL-Ti₃C₂T_x and ML-Ti₃C₂T_x present two dominant absorption bands. In the UV region (225–325 nm), FL-Ti₃C₂T_x displays relatively stronger absorption band which corresponds to the band gap transition [28], implying that there are more functional groups have been terminated on FL-Ti₃C₂T_x [29]. On the other hand, the comparison between the long wavelength absorption bands (600–1000 nm) of both samples shows that the relative intensity of FL-Ti₃C₂T_x is obviously lower than that of ML-Ti₃C₂T_x. Such weakened absorbance in the visible and near-infrared range implies that FL-Ti₃C₂T_x and ML-Ti₃C₂T_x have been terminated by -OH and -O, respectively [29]. FL-Ti₃C₂T_x with more -OH terminal groups shows hydrophilicity and electrostatic repulsion between sheets [25, 30]. As a result, FL-Ti₃C₂T_x can be well dispersed in the aqueous solution. As for ML-Ti₃C₂T_x with more -O terminals, it can only form a suspension in the beginning and will deposit subsequently as shown in Fig. S2a.

In order to shed more light on the surface groups terminated on ML-Ti₃C₂T_x and FL-Ti₃C₂T_x, XPS spectra of both samples were collected and have been shown in Fig. 3. All corresponding detailed information regarding the surface states have been summarized in Table S1. The fraction of Ti-C in FL-Ti₃C₂T_x (9.80%) is lower than that in ML-Ti₃C₂T_x (17.31%), while the ratio of C-C in FL-Ti₃C₂T_x (44.62%) is higher. Such surface states changing evidences the loss of Ti atoms and the more exposed C atoms on the surface of FL-Ti₃C₂T_x, which agrees with the emerging D band in its Raman spectrum shown in Fig. 2a. The increased C-Ti-T_x ratio in FL-Ti₃C₂T_x (21.27%) indicates that there should be more active terminal groups adsorbed on its surface than ML-Ti₃C₂T_x, which agrees with the Zeta potential results shown in Fig. S1. Apart from the quantity of the terminal groups, the analysis of XPS results also reveal that FL-Ti₃C₂T_x and ML-Ti₃C₂T_x have been terminated by different dominant functional groups, which also has been suggested by the (002) diffraction peaks shown in Fig. 1e. Regarding O 1 s spectra of these two samples, it can be clearly seen that there are more O-related states have been found on the surface of ML-Ti₃C₂T_x, and some of them are adsorbed oxygen molecules, which can dissociate to form Ti₃C₂O_x and therefore will repel O₂ in air to prevent further oxidation of ML-Ti₃C₂T_x [31]. As a result, ML-Ti₃C₂T_x presents a better oxidation resistance with a lower TiO₂ ratio (13.98%) than FL-Ti₃C₂T_x (19.60%).

Based on the observations and analyses of Figs. 1, 2 and 3, it can be concluded that although both ML-Ti₃C₂T_x and FL-Ti₃C₂T_x are terminated by some functional groups with negative charge, the amount and dominant type of the groups are quite different. On one hand, the quantity of terminal groups on FL-Ti₃C₂T_x is larger than that of ML-Ti₃C₂T_x. On the other hand, the dominant terminal structure on ML-Ti₃C₂T_x is Ti₃C₂O₂, which makes ML-Ti₃C₂T_x to be more stable in the air [32], while for FL-Ti₃C₂T_x, it is mainly terminated by Ti₃C₂(OH)₂, which helps FL-Ti₃C₂T_x to be well-dispersed in aqueous solutions [30].

Ti₃C₂T_x with functional terminal groups could reveal good adsorption performance and therefore could act as a surface-enhanced Raman scattering (SERS) substrate to improve the Raman activity of positively charged probe molecules [3, 33, 34]. Comparing with ML-Ti₃C₂T_x, FL-Ti₃C₂T_x should present better adsorption ability since it has been determined that it is terminated with more negative charges. Such better adsorption performance has been demonstrated by the optical photographs of the mixed solution with R6G and FL-Ti₃C₂T_x as shown in Fig. S2b. However, Fig. 4a reveals that ML-Ti₃C₂T_x substrate obviously performs better SERS activities than FL-Ti₃C₂T_x substrate. Considering ML-Ti₃C₂T_x with -O terminal presents stronger absorption band centered at around 800 nm, which can be assigned to the surface plasmon resonant absorption [3, 14, 33, 35], it therefore can be concluded that ML-Ti₃C₂T_x with stronger SERS activity may result from the stronger near-field effect induced by the relatively stronger surface plasmon resonance as shown in Fig. 2b.

In order to further explore the relationship between the terminal groups and the near-filed effect of Ti₃C₂T_x nanosheets, the hybrid structures composed of Ti₃C₂T_x nanosheets, including few layered and multilayered, and Ag nanoparticles (NPs) have been synthesized, which are accordingly labeled as Ag/FL-Ti₃C₂T_x and Ag/ML-Ti₃C₂T_x, respectively. The morphologies of both hybrid samples have been shown in Fig. S3. The insets indicate the corresponding size distributions of Ag NPs loading on ML-Ti₃C₂T_x (5–40 nm) is larger than that on FL-Ti₃C₂T_x (2–20 nm). Intuitively, it might be concluded that Ag/ML-Ti₃C₂T_x could perform better SERS activity than Ag/FL-Ti₃C₂T_x since both larger Ag NPs and relative stronger surface plasmon resonance of ML-Ti₃C₂T_x are beneficial to confine stronger near-field. However, the SERS spectra shown in Fig. 4b reveal a counterintuitive result. It is clear that the enhancement effect offered by Ag/FL-Ti₃C₂T_x is nearly 3 times of that by Ag/ML-Ti₃C₂T_x, implying that the coupling between Ag NPs and FL-Ti₃C₂T_x should play an important role during the detection process. As confirmed above that FL-Ti₃C₂T_x has been mainly terminated by -OH groups with lots of surface electrons, which will result in the formation of Ti₃C₂(OH)₂ structure with a work function of 1.6–2.8 eV [36, 37]. As shown in Fig. 4c, the abundant surface electrons will therefore transfer from FL-Ti₃C₂T_x to Ag NPs with a work function of 4.7 eV [38]. With the extra injection of hot electrons from FL-Ti₃C₂T_x, Ag NPs with smaller size could present stronger resonance under the excitation and eventually perform better SERS activity due to the coupling induced stronger electromagnetic effect. It is worth noting that the work function of Ti₃C₂O₂ structure formed on the surface of ML-Ti₃C₂T_x is around 6.0 eV [37], which will result in electron transfer from Ag NPs surface to ML-Ti₃C₂T_x nanosheets and therefore will weaken the near-field enhanced effect supported by the Ag NPs.

In summary, ML-Ti₃C₂T_x and FL-Ti₃C₂T_x terminated with different dominant functional groups have been successfully prepared. It has been demonstrated that ML-Ti₃C₂T_x is more stable in the air due to the surface structure of Ti₃C₂O₂ and show stronger SERS activity than FL-Ti₃C₂T_x because it can reveal stronger near-field effect. However, FL-Ti₃C₂T_x terminated by Ti₃C₂(OH)₂ can be well dispersed in aqueous solution and will show better SERS performance after coupling to the Ag NPs. Such research regarding the terminal groups-dependent near-field enhancement performance will help people to expand the potential applications of Ti₃C₂T_x in the optical related fields.

ML-Ti₃C₂T_x: Multilayered Ti₃C₂T_x, FL-Ti₃C₂T_x: Few layered Ti₃C₂T_x, SERS: surface enhanced Raman scattering, NPs: Nanoparticles

Acknowledgments

This work was financially supported by the National Natural Science Foundation of China (61675061 and 11774077), the Fundamental Research Funds for the Central Universities (PA2019GDQT0013), and the Provincial Innovation and Entrepreneurship Training Program for College Students (S201910359033).

Authors’ contributions

YYY planned and conducted the experiment and wrote the manuscript. WTZ, WLS, QQZ, HJX and JZ performed the background study and helped synthesis of nanosheets and hybrid samples. SC and PFL offered guidance on characterizations. YWL managed the checking and revising of the manuscript. The authors read and approved the final manuscript.

Funding

This work is supported by the National Natural Science Foundation of China (61675061 and 11774077), the Fundamental Research Funds for the Central Universities (PA2019GDQT0013), and the Provincial Innovation and Entrepreneurship Training Program for College Students (S201910359033).

Availability of data and materials

The rwa dataset obtained analyzed during the experimental work is avaiable from the corresponding author on reasonable request.

Competing interests

The authors declare that they have no competing interests.

Author details

¹School of Materials Science and Engineering, Hefei University of Technology, Hefei 230009, P. R. China. ²Instrumental Analysis Center, Hefei University of Technology, Hefei 230009, P. R. China. ³Engineering Research Center of High Performance Copper Alloy Materials and Processing, Ministry of Education, Hefei University of Technology, Hefei 230009, P. R. China

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You are reading this latest preprint version

Terminal Groups Dependent Near-Field Enhancement Effect of Ti3C2Tx Nanosheets

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Introduction

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Preparation of Ti3C2Tx nanosheets

Preparation of Ag/Ti3C2Tx nanocomposites

Characterization

Results And Discussion

Conclusions

Abbreviations

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