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EMI Shielding Performance and Mechanical Properties of Proton Acid Treated Ti3C2Tx MXene/CNT Composite  PDF

  • Liu Xingmin ✉
  • Yang Jihua
  • Lu Shaowei
  • Yang Dongxu
  • Wang Jijie
  • Liu Chunzhong
  • Wang Sai ✉
College of Materials Science and Engineering, Shenyang Aerospace University, Shenyang 110136, China

Updated：2023-02-09

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  • References
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Abstract

After the colloidal proton acid treatment, the preparation of titanium carbide Ti3C2Tx was achieved. In addition, the single-walled carbon nanotube (SWCNT) was used as reinforcement to improve the mechanical properties of proton acid treated titanium carbide (H-MXene): the tensile property is enhanced by nearly 400% while the electromagnetic shielding performance is retained. This study demonstrates that the H-MXene and carbon nanotube have great potential in electromagnetic interference (EMI) shielding composite materials with excellent mechanical properties.

The proliferation of new generation electronic device leads to the increasing electromagnetic (EM) radiation pollution. Exposure to electromagnetic interference (EMI) can cause negative effects in various fields, including the medicine, military, and navigation[

1‒2]. Therefore, EMI shielding materials are crucial. The primary function of EMI shielding material is to reflect radiation by charge carriers which directly interact with EM fields[3]. Metals (Cu, Ag) are commonly used as EMI shielding material[4], but they are heavy and stiff, which seriously restricts their application in EMI shielding field[5]. New generation EMI material should be light, flexible, and more geometrically malleable.

Recently, a 2D transition metal with carbide and/or nitride, namely MXene (Mn+1Xnene, n=1‒3; M stands for transition metal; X is carbon and/or nitrogen; ene stands for graphene), gradually becomes one of the most applicable EMI composite materials. Besides, MXT (Mn+1XnTx, n=1‒3; T represents a terminating group) material[

6] is further developed based on MXene material.

Ti3C2Tx material possesses extraordinary electrical conduc-tivity[

7] and is commonly used in sensors[8‒9], energy stor-age[10‒11], and EMI shielding[12‒13]. According to the EM wave shielding theory, the magnitude of the induced current directly affects the shielding effect[14], thereby enhancing the electrical properties of materials. However, the surface of 2D Ti3C2Tx material is covered by Ti(II)/Ti(III)-suboxide, -hydroxide, or -fluoride, which can be easily oxidized into Ti(IV)-oxide. In addition, the H2O/O2 diffusion in the bulk material can also accelerate the oxidation degradation of Ti3C2Tx material[15]. With the spread of the intercalant during the exfoliation pro-cess, the interaction of Ti3C2Tx material is weakened, therefore severely restricting the application of Ti3C2Tx material.

Proton acid treatment can remove the intercalant, such as Li+, dimethylsulfoxide, and tetraalkylammonium hydroxide[

16]. Thereby, the reinforcement of hydration stability can be achieved. The proton acid of 6 mol/L H+ was used as the trigger to desorb the intercalant from the nanosheet surface. By gradually adding protic acid into the matrix solution, the suspension of closely aligned Ti3C2Tx stacks was prepared. Then the products were identified as H-Ti3C2Tx film. Compared with that of the specimens without acid treatment, the conductivity of Ti3C2Tx films is greatly increased from 3×105 S/m to 4.5×105 S/m.

Although the proton acid treatment improves the electrical property of Ti3C2Tx material, its mechanical property and flexibility still need enhancement. According to Ref. [

17‒18], the tensile strength and flexibility of MXene films prepared by vacuum filtration are unsatisfied. Therefore, the single-walled carbon nanotubes (SWCNTs) with superb mechanical proper-ties were used as reinforcement in this research because of their seamless defect-free cylindrical graphitic structure. According to Ref.[19‒20], it is confirmed that SWCNT is an effective reinforcement. Through the combination of carbon nanotubes and Ti3C2Tx material, Ti3C2Tx/SWCNT composite materials with different ratios were prepared in this research. The enhancement in mechanical property is achieved, and an EM shielding effectiveness which is comparable to that of the pure H-Ti3C2Tx materials can also be retained, presenting further development of two-dimensional EM shielding material.

1 Experiment

Ti3AlC2 (0.038 μm, AR, 99%, Ningbo Jinlei Nano Material Technology Co., Ltd), high-purity SWCNT powder (95%, Chengdu Organic Chemicals Co., Ltd), lithium fluoride (LiF, AR, 99%, Shanghai Macklin Biochemical Co., Ltd), hydrochloric acid (9 mol/L, Tianjin Fengchuan Chemical Reagent Co., Ltd) were used in this research.

Vacuum-assisted filtration (180 W, water-circulation multifunction vacuum pump, Shanghai Jinfu Experimental Equipment Co., Ltd), cellulose separator membrane (pore size of 0.22 μm, Shanghai Xinya Purification Equipment Co., Ltd), scanning electron microscope (SEM, Zeiss Gemini SEM500/300), and X-ray diffractometer (XRD, DX-2700BH, Haoyuan Instrument Co., Ltd) were used in this research. Tensile tests were conducted with the Instron material testing system (XM-DZSC001).

MXene of Ti3C2Tx material was prepared by selective etch-ing of the Ti3AlC2 precursor, as shown in Fig.1 (Step I). The etching solution was prepared by slowly adding 1.6 g lithium fluoride into 20 mL hydrochloric acid solution (9 mol/L) with stirring for about 5 min. Then, 1 g Ti3AlC2 powder was added into the solution intermittently. Via ice bath, the reaction temperature was strictly controlled below 10 °C to avoid oxidation. After the powder addition, the mixture was stirred at room temperature for 24 h. The deionized water was used to wash the acid mixture via centrifugation at 3500 r/min for several times (5 min for each cycle) until pH≈6. Then the solution was ultrasonically cleaned for 20 min for the delamination of multi-layer MXene. High-purity argon gas circulation treatment was used to prevent oxidation. Finally, the solution was freeze-dried to calibrate the content of delaminated MXene (Step II in Fig.1).

Fig.1  Schematic diagrams of preparation process of SWCNT/MXene and SWCNT/H-MXene materials

During vigorous stirring, 6 mol/L HCl was added dropwise into the delaminated MXene suspension until pH=1 for the proton acid treatment. Then obvious coagulation in the solution could be observed. The solution was placed in centrifuge at 5000 r/min, and the upper liquid was abandoned (Step III and Step IV). Repeat this process for several times until pH=6 and the proton acid-treated MXene, namely H-MXene material, was prepared. The degree of solute coagulation in the solution was gradually decreased with increasing the pH value.

SWCNT powder (0.5 g) was put into a grinder. Extract 2 mL triton solution, inject it into the SWCNT powder uniformly, and then grind them clockwise for 40 min. The deionized water was used to wash the grinder and the grinding rod, and the used water was separately collected in the large beakers. The used water was stirred for 2.5 h with stirring head in the middle position of the used water. Then the solution was ultrasonically cleaned with the ultrasonic probe inserted into the solution. The ultrasonic wave was released every 1 s and last for 1 s. The whole process lasted for 60 min.

SWCNT of different contents was added into MXene and H-MXene materials to prepare SWCNT/MXene and SWCNT/H+-introduced MXene mixtures, respectively. After SWCNT addition, the mixture was subjected to magnetic stirring at 300 r/min for 1 h for uniform mixture. Then, the specimen films were prepared by vacuum-assisted filtration (Step V and Step VI). The mass ratio of SWCNT to MXene was 3:1, 5:1, 10:1, 15:1, and 20:1, and the corresponding specimen was named as SCM3, SCM5, SCM10, SCM15, amd SCM20, respectively. Similarly, the ratio of SWCNT to H-MXene was 3:1, 5:1, 10:1, 15:1, and 20:1, and the corresponding specimen was named as SCHM3, SCHM5, SCHM10, SCHM15, amd SCHM20, respectively.

2 Results and Discussion

2.1 Characterization

Significant MXene coagulation can be observed in the solution during the proton acid treatment with low pH values. This phenomenon is attributed to the charge screening effect of cations[

21]: the proton acid shifts the zeta potential of Ti3C2Tx nanosheets to a relatively positive one, destabilizing Ti3C2Tx colloids. Chen et al[22] analyzed the reduced activity of protons in titration experiments and concluded that the coagulation of MXene layers in the early stages of proton acid treatment is mainly caused by the formation of hydrogen bonds between layers and the hydrophobic action of reaction layer surface.

According to Ref.[

23], the intercalated Li+ ions lead to the stabilization of intercalated H2O in multi-layered Ti3C2Tx material. XRD patterns of MXene and H-MXene materials are shown in Fig.2. It is revealed that H-MXene material has a clearly smaller interlayer distance than MXene material does. The strong and sharp peak of (002) plane can be detected in both two materials, proving the good alignment of MXene nanosheets. With the proton acid treatment proceeding, the d-spacing is decreased from 1.592 43 nm (MXene) to 1.400 04 nm (H-MXene). These phenomena all result from the decrease in intercalated H2O between Ti3C2Tx layers.

Fig.2  XRD patterns of MXene and H-MXene materials

The surface of proton acid-treated Ti3C2Tx material, i.e., H-MXene material, shows more undulation and folds than the MXene material does, implying that the self-assembly of Ti3C2Tx nanosheets during proton acid process results in the formation of larger aggregates. According to Fig.3, the dominant laminar structure can be clearly observed in all specimens. In addition, the layer spacing reduction is obvious in H-MXene material, compared with that of the MXene material. The film thickness of H-MXene material is also thinner than that of MXene material after vacuum-assisted filtration. The H+ introduction declines the disorder in stacking and reunion process of MXene flakes (Fig.3a and 3b). According to Fig.3c and 3d, SWCNT is densely distributed between the MXene layers in the SCM20 and SCHM20 specimens, indicating the formation of 1D/2D hybrid network.

Fig.3  SEM cross-sectional morphologies of MXene (a), H-MXene (b), SCM20 (c), and SCHM20 (d) materials

2.2 Performance

All SWCNT/MXene and SWCNT/H-MXene specimens were prepared via vacuum-assisted filtration and vacuum-dried at 60 °C for 2 h. The initial concentration of MXene material in suspension is 2.24 mg/mL and it changes to 1.05 mg/mL after introduction of 0.1 mol/L H+. The coagulation of MXene layers exists the whole time during the washing stage. The average thickness of the SWCNT/H-MXene film is 10 μm. With increasing the SWCNT content in the composite, the color of specimen is changed from gray black to dark black, as shown in Fig.4. Besides, the surface of specimen after proton acid treatment is flawless and flat (Fig.4b).

Fig.4  Appearances of MXene (a) and SCHM5 (b) materials

EMI shielding performance tests of X-band (8.20‒12.4 GHz) were conducted for SWCNT/MXene and SWCNT/ H-MXene materials with different ratios via vector network analyzer (PAN-L N5230C Agilent Technologies, waveguide). The specimens were sliced into a rectangular form of 22.9 mm×10.2 mm. The scattering parameters (S11, S12, and S21) of all specimens were recorded. The reflection (R), transmission (T), absorption (A), reflection shielding effectiveness (SER), absorption shielding effectiveness (SEA), and total EMI shielding effectiveness (SET) can be calculated by Eq.(1‒6), respectively:

R=|S11|2=|S12|2 (1)
T=|S12|2=|S21|2 (2)
R+A+T=1 (3)
SER=10lg11-R=10lg11-|S11|2 (4)
SEA=10lg1-RT10lg1-|S11|2|S21|2 (5)
SET=SEA+SER+SEM (6)

where SEM represents the multiple internal reflection of material (usually negligible when SET≥15 dB[

24]). The total EMI shielding effectiveness (SET) of different materials is shown in Fig.5.

Fig.5  Total EMI shielding effectiveness of different materials

According to EM theory, with increasing the frequency, the EM radiation capacity is increased, and EM harassment tends to the far field area, resulting in the non-negligible negative effects on electric and magnetic fields[

24]. Because the electric and magnetic fields of high-frequency EM waves characterized by radiation are interdependent, shielding one of them is enough to achieve superb effects in practice. Based on Schelkunoff formula[24] and Simon principle[25], shielding effectiveness (SE) is proportional to the relative conductivity of shielding materials, which is consistent with the high conductivity of H-MXene material (4000-5000 S/cm). The specific shielding effectiveness (SSE) can be used to evaluate the EM shielding performance of materials. However, it only considers the material density (d), which is not sufficient. Therefore, the absolute shielding effectiveness (dB·cm2·g-1), which simultaneously considers the density d and thickness t of material, is introduced, as follows:

SSE/t=SE/tb (7)

The absolute shielding effectiveness can directly reflect the material performance, which is calculated based on the normalization of SET with respect to density and thickness. High SSE/t values are crucial for the lightweight shielding materials. Fig.6 and Fig.7 show the SE performance, absolute shielding effectiveness, and EC of different materials. It can be seen that the absolute shielding effectiveness of H-MXene material is several times higher than that of the MXene material. The proton acid treatment reduces the spacing between MXene layers, leading to a better conductivity of H-MXene material. Besides, the introduction of SWCNTs barely causes a negative effect on EMI shielding performance of MXene material. Table 1 shows the comparison of EMI shielding performance of different materials. Due to the abundant free electrons on the surface of MXene and SWCNT/H-MXene materials[

35], the MXene flake can directly reflect some EM waves when they come into connect. Because of the well-aligned layered structure of MXene materials (Fig.3a and 3b) and the ohm loss caused by the high electron density, the energy of the remaining EM waves declines when they pass through the flakes. As EM waves are transmitted to a new MXene layer, the process is repeated (Fig.8). The multiple internal reflection loss inside the shield material is negligible once the total shielding effectiveness is more than 15 dB. However, this conclusion does not apply to the MXene material with the multi-layered structure. According to Fig.6, SEA accounts for more than 50% of the total shielding effectiveness of all materials. Actually, SEM is included in SEA because the EM waves are absorbed or dissipated in the form of heat within the material[36]. In addition, the dipoles can be produced on the surface of MXene flakes between the termination group and titanium, which improves the overall shielding performance by interacting with EM waves. The EMI absolute shielding effectiveness of SWCNT is 127.9 dB·cm2·g-1, which is much lower than that of the prepared MXene material. Because SWCNT is at nanoscale, it is suitable to enhance the mechanical properties and environ-mental adaptability of the matrix without influence on the base EM shielding performance. The introduction of SWCNT results in smoother surface and greater flexibility of H-MXene materials: SCHM3 film can bend of nearly 180° and the film surface only has minor folding scratches after recovery. According to Ref.[37‒39], the tensile strength of carbon nanotubes is nearly three times higher than that of the MXene material. Thus, the introduction of SWCNT can greatly improve the tensile strength of MXene material.

Fig.6  EMI shielding effectiveness (X-band) of different materials

Fig.7  Absolute shielding effectiveness (SSE/t) and electrical conductivity (EC) of different materials

Table 1  EMI shielding performance of different materials
TypeMaterialAbsolute shielding effectiveness/dB·cm2·g-1Ref.
Metal-based Copper 32.3 [26]
Al foil 30 555 [27]
CuNi-carbon nanotubes 1 580 [28]
Cu foil 7 812 [27]
Ag nanowire 2 416 [29]
Carbon-based Carbon foam 1 250 [30]
Reduced graphene oxide (rGO) 692 [31]
rGO/Fe3O4 1 033 [32]
SWCNT/epoxy 72 [33]
MXene-based Ti3C2Tx/carbon nanofibers 2 647 [34]
Ti3C2Tx-sodium alginate 30 830 [27]
Ti3C2Tx-SWCNT 49 336‒55 204 -

Fig.8  EMI shielding mechanism of MXene layer structure

The film specimens for stretch performance tests were prepared by vacuum-assisted filtration with the thickness of 8‒10 μm, gauge length of 5 mm, and width of 3 mm. Stress and strain were recorded at extension rate of 1 mm·min-1. More than three strips of each type of specimens were tested via XM-DZSC001 equipment (Yitong Testing Equipment Technology Co., Ltd) with load cell of 10 N. The fracture surface is perpendicular to the loading direction. According to Ref.[

38], the ultrasonic pretreatment for 30 min can compact the layered MXene materials, i.e., the Ti3C2Tx flakes are stacked more tightly. According to Fig.3a and 3b, the spacing between Ti3C2Tx flakes reduces, which leads to the increase in tensile strength of MXene material (Fig.9). With the introduction of SWCNT, the tensile strength of MXene material is further enhanced. The tensile strength of SCHM3 specimen is 128.8 MPa, which is almost 6 and 4 times higher than that of the MXene and H-MXene materials. The cross-sectional morphologies of the failed strips (Fig.3) indicate that Ti3C2Tx material has a flat, straight, and brittle-like fracture surface, which is a common fracture morphology of 2D film materials[40‒41]. Because the Ti3C2Tx film is stacked as lamellar structure, the applied tensile stress is maintained by the shear stress transfer between overlapping Ti3C2Tx flakes and by the straining of the flakes. The overlapping causes the relative slipping between the flakes, and then a critical transverse crack at the junction of adjacent flakes is formed and propagated rapidly, resulting in strip failure.

Fig.9  Tensile strength of different materials (a); schematic diagrams of tensile strength curve of MXene (b), H-MXene (c) and

SCHM3 (d) materials

The tensile-fracture process of MXene material can be divided into three stages: straightening, linear elasticity, and plastic deformation[

38]. After proton acid treatment, MXene material exhibits a state of nearly complete linear elastic-plastic deformation tension. This phenomenon reveals that the introduction of H+ greatly shortens the straightening process. Since the proton acid treatment also decreases the sheet spacing in MXene material, the straightening process is basically completed during the extraction process. With the SWCNT introduction of different contents, the stretching patterns gradually recover. It can be observed that SWCNT distributed between layers reduces the fracture formation and increases the tensile strength and toughness of materials. The EMI shielding ability and tensile strength of SCHM3 specimen are comparable to those of other EMI shielding materials, as shown in Table 2. SCHM3 specimen has the absolute shielding effectiveness of 49 336 dB·cm2·g-1, which is comparable to that of the MXene material. A great increase in tensile strength (128.8 MPa) is also achieved for SCHM3 specimen. Therefore, compared with those of MXene materials, the absolute shielding effectiveness and the tensile strength are increased by 200% and 400% for the SCHM3 specimen, respectively.

Table 2  Absolute shielding effectiveness and tensile strength of different materials
MaterialAbsolute shielding effectiveness/dB·cm2·g-1Tensile strength/MPaRef.
Copper 32.26 366.00 [27]
PEI/graphene 166.54 5.50 [42]
Carbon fiber/PC film 1 201.74 115.10 [43]
FSPF film 1 2607.4 0.94 [44]
CEF-NF 6 294.02 20.74 [45]
NCF 30 039.42 11.21 [46]
MWCNT-NCF composite 23 223.86 68.28 [46]
Stainless steel 27.46 515.00 [27]
PI-rGO foam 937.46 11.40 [47]
SCHM3 49 336 128.80 -

Note:   PEI-poly(ethylene imine); PC-polycarbonate; FSPF-Fe3O4@SiO2@polypyrrole; CEF-carbon fiber or polypropylene/polyethylene core/sheath bicomponent fiber; NF-nonwoven fabric; MWCNT-multiwalled carbon nanotube; NCF-neat carbon fabric; PI-polyimide

3 Conclusions

1) Singe-walled carbon nanotube (SWCNT) as the reinforcement can effectively improve the tensile properties of transition metal with carbide and/or nitride (MXene) materials with slight influence on the absolute electromagnetic shielding performance.

2) MXene material after proton acid treatment (H-MXene) with the SWCNT addition (mass ratio of H-MXene to SWCNT is 3:1) has the absolute shielding effectiveness of

49 336 dB·cm2·g-1 and the tensile strength of 128.8 MPa, which are increased by 200% and 400%, respectively, compared with those of MXene materials.

3) The MXene materials show great potential in electromagnetic shielding composites, which should be further developed.

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