Figure
1.
The illustration of the preparation process of PVDF/graphene composite film.
| Citation: |
Yu Zhou, Li Zuo, Azizur Rahman, Bo Hong, Hongwei Chen, Linchao Zhang, Hongbo Ju, Junfeng Yang. Fabrication and Excellent Properties of Polyvinylidene fluoride/Graphene Composite Films as Thermal Interface Materials[J]. Chinese Journal of Chemical Physics , 2024, 37(5): 671-678. DOI: 10.1063/1674-0068/cjcp2312136
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The growing concern about thermal conductivity and electromagnetic shielding in electronic equipment has promoted the development of interfacial film materials. In this work, polyvinylidene fluoride (PVDF)/graphene composite films with different graphene contents were fabricated by high-energy ball milling, cold isostatic pressing, scraping and coating, successively. High-energy ball milling is beneficial to the dispersion of graphene powder, while cold isostatic pressing can greatly enhance thermal conductivity and mechanical strength by reducing the voids in the film and increasing the contact area of graphene sheets. The thermal conductivity, tensile strength and electromagnetic shielding properties of the films were carefully investigated and compared. It was demonstrated that the thermal conductivity increased from 0.19 W·m−1·K−1 for pure PVDF to 103.9 W·m−1·K−1 for the composite film with PVDF:graphene=1:3. Meanwhile the electromagnetic shielding efficiency can reach 36.55 dB. The prepared PVDF/graphene composite films exhibit outstanding overall performance and have the potential for practical applications.
Heat dissipation is more and more crucial for the service life and reliability of the smaller, more powerful and adaptable electronic equipment [1−6]. Normally, a heat sink layer should be used on the heat source to transmit heat. However, due to the surface roughness, there are unavoidable interface voids between the heat source and the heat sink. Heat can only be transmitted slowly through point contacts, as the thermal conductivity of air is mere 0.026 W·m−1·K−1 [7]. Meanwhile, electronics miniaturization further reduces the space for heat sinks, making heat transmission more difficult. Therefore, the high-efficiency radiator is urgently needed for future microelectronics development [8]. Moreover, electronics can produce electromagnetic interference (EMI), which could reduce the efficiency [9]. Therefore, the development of a lightweight and flexible thermal interface material with high thermal conductivity and EMI shielding capabilities has been a top priority [10−12].
Thermal interface materials are classified into three types: inorganic, organic, and composite materials. Inorganic materials possess relatively high thermal conductivity, but their thermal deformation leads to structural instability. Organic polymers benefit from their softness, non-toxicity and low cost. However, the weak thermal conductivity inhibits the application. Composite materials have advantages in both inorganic and organic materials and have become a hot point recently [13].
Polyvinylidene fluoride (PVDF) is a semi-crystalline polymer which is easy to prepare and has the advantages of good thermal stability and flexibility [14]. Meanwhile, inorganic graphene has both exceptionally high thermal and electronic conductivity. Accordingly, the composite of PVDF and graphene would possess both high thermal conductivity and excellent electromagnetic shielding property [15−17]. In this work, the PVDF/graphene composite films were prepared by high-energy ball-milling, scraping and coating processes, successively. The microstructure, thermal conductivity, tensile strength and electromagnetic shielding performance of the composite films were carefully tested and compared.
Multilayer graphene powder (5–50 μm, 95%) was purchased from Hebei Luohong Technology Co. Ltd. PVDF and N-methyl pyrrolidone (NMP) (AR, 99.0%) were obtained from Shanghai Aladdin Biochemical Technology Co., Ltd.
The composite films were prepared as illustrated in FIG. 1, with the following five steps.
(1) Ball milling of graphene powder: the multilayer graphene powder was ground in a high-energy planetary ball milling for 3 h at a rotation speed of 500 r/min.
(2) Preparation of slurry: an appropriate amount of PVDF and graphene powder were added in NMP. The mixture was ultrasonically stirred to create a well-dispersed slurry.
(3) Slurry-coating: copper foil was cleaned ultrasonically in alcohol and deionized water, successively. As-prepared slurry was coated onto the dried Cu foil using a scraper, the thickness of the slurry on the substrate is about 250 μm.
(4) Film-forming: all the films were dried in an oven in air. They were firstly dried at a relatively low temperature of 60 °C for 5 h. Subsequently, they would be further dried at 140 °C for 2 h. Then the PVDF/graphene composite film could be completely peeled off from the substrate.
(5) Cold isostatic pressing: the film was sealed in a polyethylene envelope and pressed under a pressure of 50 MPa for 120 s by cold isostatic pressing.
Various PVDF/graphene films with different graphene contents have been prepared. The mass ratio of PVDF to graphene varied from 3:1, 2:1, 1:1, 1:2, 1:3, 1:4 to 1:5. And the corresponding sample numbers were simplified to be PG31, PG21, PG11, PG12, PG13, PG14, and PG15 hereinafter.
The surface and cross-section morphology of the films were characterized by a field emission scanning electron microscope (SEM, HITACHI, SU8020). The film was immersed in liquid nitrogen and then broken by a tweezer for the cross-section observation.
Electromagnetic interference (EMI) shielding measurement was conducted by a coaxial transmission line method in the 8–12 GHz (X-band) frequency range. The electromagnetic signals were emitted and received by a network analyzer (Agilent N524). The parameter S11 symbolizes the reflection coefficient data and S21 stands for the transmission data. The S11 and S21 of each sample were recorded and used to calculate the EMI SE (shielding effectiveness). The power coefficients of reflection (R) transmission (T) and absorption (A) were evaluated based on the following equations:
|
R=|S11|2 |
(1) |
|
T=|S21|2 |
(2) |
|
A=1−R−T |
(3) |
The total EMI shielding efficiency (SET), reflection (SER) and absorption (SEA) can be described as follows [18−20]:
|
SET=SER+SEA+SEM≈SER+SEA |
(4) |
|
SER=−log10(1−R)=−log10(1−S112) |
(5) |
|
SEA=−log10(T1−R)=−log10(S2121−S112) |
(6) |
Tensile testing was carried out by a universal material testing machine (Type 5566, Instron). Rectangular tensile specimens with the length of 80 mm and width of 20 mm were prepared from the as-prepared composite films. Each composition was tested for 5 times in parallel and the mean result was taken as the final result. All tensile tests were performed at a speed of 2 mm/min.
The thermal conductivity (K) was performed by the flash method, and it can be calculated as follows [21]:
|
K=λ⋅Cp⋅ρ |
(7) |
Where λ indicates the thermal diffusivity, Cp represents the specific heat capacity, and ρ is the density of the sample.
The thermal diffusivity was tested by the light flash apparatus (NETZSCH LFA 467). The specific heat capacity was measured by differential scanning calorimetry (DSC 240, Netzsch). The density of samples can be obtained directly by calculating the ratio of mass to volume. Each sample was measured at room temperature, and the final test results of each sample were the average of five measurements.
A four-point probe method was used to test the conductivity of films at room temperature. Samples were also examined by an attenuated total reflection Fourier transform infrared spectrometer (ATR-FTIR, Spectrum 3 Optica), X-ray diffraction (XRD, X'Pert, Netherlands) and Raman spectroscopy (NEXUS, Thermo Nicolet Corporation).
The morphology of graphene sheets is depicted in FIG. 2 (a) and (b). Various wrinkles appeare on the surface and a close interfacial contact between the graphene sheets can be observed, which could be helpful for the thermal conductivity. FIG. 2(c) shows the surface morphologies of PG31 film. It is obvious that some graphene sheets are isolated in the PVDF matrix, which is detrimental to the thermal conductivity. The thickness of PG31 before pressing is about 100 μm as shown in FIG. 2(d). The enlarged image (FIG. 2(e)) shows that the graphene sheets in the film cross with each other. Such a structure would prevent the graphene sheets from forming internal thermal conduction paths [16]. Meanwhile, as the graphene proportion in the film increases, no visible PVDF zone could be found in PG31 (FIG. 2(f)). With the help of cold isostatic pressing, graphene sheets contact well with each other, and the thickness of PG31 could be reduced to about 30 μm (FIG. 2(g)). A larger version proves that the graphene sheets tightly stack together (FIG. 2(h)), and the surface changes to be smoother (FIG. 2(i)), which would be helpful for the interfacial adhesion [22].
During the drying process, the solvent diffuses from the inside of the film to the surface and evaporates in the air. Voids may be formed in the film. When the evaporation rate of the solvent is less than the diffusion rate of the solvent in the film, the gas will wander around in the film, resulting in a lack of tight binding and an increase in the gap of the film. Therefore, drying the film at a low temperature of 60 °C firstly can result in a more uniform internal structure with fewer defects. Subsequently, the drying temperature was increased to 120 °C to ensure that the solvent is completely evaporated.
FIG. 3(a) shows the XRD patterns of PG13 and graphene. PG13 exhibits strong and narrow diffraction peaks at 2θ=20.2°, 26.6° and 54.8°. The peaks at 26.6° and 54.8° meet well with those of graphene. And the peak at 20.2° corresponds to the β-form crystal of PVDF [23]. It proves that the composite film is composed of graphene and PVDF with polar β phase.
FIG. 3(b) displays the Raman spectra of composite films. The D peak appeares at about 1358 cm−1 and G peak appears at about 1585 cm−1 [24]. The D peak originates from the disordered vibration of defects in carbon materials, while the G peak is attributed to the in-plane stretching vibration of carbon atoms with sp2, which is the distinctive peak of graphite carbon [25]. In the Raman spectra of PG31, PG21, PG11, and PG12, a small peak is observed at about 1433 cm−1. This peak corresponds to the stretching vibration of the C–H bond in the polymer PVDF molecule, providing evidence of the presence of PVDF. When the PVDF proportion in the film decreases, the peak at 1433 cm−1 gradually disappears, and the 2D peaks at about 2700 cm−1 grow stronger. It proves that the high crystallinity of graphene leads to stronger Raman peaks, which obscures those of PVDF and the graphene has multiple layers [26].
The FTIR curves of PG13 and PVDF are shown in FIG. 3(c). The peak at 1179 cm−1 indicates the symmetric and asymmetric stretching vibrations of the CF2. The peak at 1241 cm−1 is the asymmetric stretching vibration peak of CF2. The absorption peak at 1404 cm−1 represents CF2 and CH2 deformation vibration. The absorption peak at 822 cm−1 is the characteristic absorption peak of amorphous phase [27]. The infrared spectra of the film show that no new chemical bond is formed between the graphene and PVDF.
The heat conduction of carbon materials is dominated by phonons. Due to the strong covalent bond sp2 and small carbon atomic mass, effective heat transfer can be achieved through lattice vibration [28]. Phonons would scatter at interfaces between different materials. Therefore, the transmission direction would be altered and the thermal conductivity of the materials would be influenced. The tested thermal conductivity of the film is significantly lower than the theoretical value, due to the increased contact thermal resistance between graphene sheets and the interfacial thermal resistance between graphene and PVDF. Therefore, the construction of a continuous graphene conductive network is an effective method to improve the thermal conductivity of polymer/graphene composites.
To investigate the effect of graphene content, the thermal conductivity of composite films with different graphene contents are compared. The thermal conductivity of PVDF is only 0.19 W·m−1·K−1 (FIG. 4(a)). The continuous heat-conducting network between the graphene sheets can hardly form when the graphene proportion is low in samples PG31 and PG21, resulting in a relatively low thermal conductivity. However, it could be increased significantly with more graphene. When the continuous heat-conducting network of graphene is established in PG11, the thermal conductivity is raised to 74.53 W·m−1·K−1, and that of PG13 reaches 103.9 W·m−1·K−1. However, the thermal conductivity of PG31 before cold isostatic pressing is only 73.08 W·m−1·K−1. It proves that mechanical pressing can efficiently increase the connectivity between graphene sheets, reduce phonon scattering, and improve the thermal conductivity. With further higher graphene content, the thermal conductivity shows a downward trend. With higher graphene proportion in the film, the inadequate PVDF results in poor dispersion and agglomeration of the graphene. And the film would be loose with a significant number of voids [29]. It is worth noting that air has a thermal conductivity of only 0.026 W·m−1·K−1. Therefore, the film with more graphene exhibits a lower thermal conductivity as shown in FIG. 4(a) [30].
Compared with the literature reports (shown in Table I), the PG31 sample shows a remarkable higher thermal conductivity, due to the higher graphene content and improved preparation process.
| Materials | Contents | Thermal conductivity /(W·m−1·K−1) |
EMI SE/dB | Reference |
| Graphene/PVDF | 0.27 vol% Graphene | 1.16 ± 0.06 | [31] | |
| AlN/PVDF | 60 vol% AlN | 11.5 | [32] | |
| BN/PVDF | 30 wt% BN | 7.29 | [33] | |
| MXene/PVDF | 5 wt% MXene | 0.363 | [34] | |
| TPU/MPTU | 15 wt% MPTU | 28.35 | [35] | |
| Graphene/PS | 10 wt% Graphene | 18 | [36] | |
| Graphene/PVDF | 10 wt% Graphene | 18.70 | [37] | |
| PG13 | 75 wt% Graphene | 103.9 | 31.07 | This work |
| Note: AIN is aluminum nitride , BN is Boron nitride, MXene is Ti3C2Tx, TPU is thermoplastic polyurethane, MPTU is polyester hot-melt adhesive, PS is polystyrene. | ||||
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FIG. 4(b) shows the tensile strength of PVDF and all the composite films. It proves that the tensile strength of the films decreases with the increasing graphene content. The tensile strength of PVDF, PG31, PG21, PG11, PG12, PG13, PG14, and PG15 are 38.97, 30.01, 22.19, 15.59, 12.92, 11.09, 10.93, and 8.32 MPa, respectively. It is included that the intermolecular force between PVDF chains is weakened by graphene [38]. And the aggregation and uneven distribution of graphene in the film further exacerbate the mechanical properties.
As it turns out in thermal conductivity, mechanical pressing can also improve tensile strength. The tensile strength of PG13 is only 8.50 MPa before cold isostatic pressing, which increase to 11.09 MPa after compression. The reason may be the improved density and better integration between graphene and PVDF.
In addition, the composite films could be arbitrarily bent and repeatedly folded, showing great flexibility. Even after being bent 180° for 100 cycles, the films show no signs of breakage or creasing. Meanwhile, the density of the films ranges from 1.5 g/cm3 to 2.0 g/cm3, which is significantly lower than that of copper (8.96 g/cm³).
The EMI shielding performance of composite materials is closely associated with the electrical properties [39]. When electromagnetic waves act on graphene, free electrons will absorb the energy of the electromagnetic waves and re-radiate it, leading to the reflection of electromagnetic waves. FIG. 5(a) indicates the effect of graphene content on electrical conductivity. With the increase of graphene content, more effective charge transport pathways are formed between graphene sheets, which is conducive to charge transport. Higher conductivity can lead to more electromagnetic wave loss. The higher the electrical conductivity, the better the EMI shielding performance. Therefore, the reflection coefficient R is closely related to conductivity. FIG. 5(b) shows that the trend of the R curve is highly consistent with that of the conductivity curve [40, 41].
When the graphene content is low, the conductivity of PG31 and PG21 are only 4.52 S/m and 9.06 S/m, respectively. Meanwhile, the value of R is lower than that of A. The film exhibits poor conductivity and its electromagnetic shielding performance is low. In this case, the shielding mechanism for electromagnetic waves is mainly absorption loss. When the graphene content is sufficient, the value of R is significantly higher than that of A, which proves that the reflection effectiveness is more essential to the electromagnetic shielding performance than absorption loss.
FIG. 5(c) depicts the EMI SE of films. As the graphene content increases, the SEA and SER of all the samples exhibit the same growing tendency. The PVDF film has a very low EMI SE of only 1.08 dB. The value is changed to be about 3 times larger with only 25% addition of graphene in PG31. And the more graphene in the film, the higher the EMI SE. The microstructure is vital in advancing EMI shielding [42−44], of which the densified laminate is primarily responsible. The lamellar structure causes multiple reflections of incident microwaves, resulting in extra propagation routes and incident microwave polarization loss.
Table I also shows EMI SE for several composite films reported in the literatures. The PG31 outperforms the others in EMI shielding performance with an EMI SE value of 31.07 dB.
To improve the thermal conductivity and electromagnetic shielding performance of PVDF, a practical thermal interface material is prepared by mixing PVDF and graphene in this study. By adjusting the graphene content and optimizing the preparation process, the prepared film shows excellent thermal conductivity, high tensile strength, and excellent EMI shielding performance. It proves that the high-energy ball milling, specific drying process and the cold isostatic pressing help the uniformity of graphene and the close integration between PVDF and graphene. The addition of graphene could dramatically improve the thermal conductivity to 103.9 W·m−1·K−1 and increase the EMI SE to over 30 dB.
This work was supported by the National Natural Science Foundation of China (No.U22B2066, No.12064044), the Major Science and Technology Projects of Anhui Province (No.202103a05020016), and the open competition project to select the best candidates to undertake major science and key research projects of Tongling city, Anhui Province (No.202101JB002). A proportion of this work was supported by the High Magnetic Field Laboratory of Anhui Province and Academician workstation of Hangzhou Xingyu Carbon Environmental Tech Co., Ltd., and the Hefei Institutes of Physical Science Director’s Fund (No. YZJJ-GGZX-2022-01).
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| Materials | Contents | Thermal conductivity /(W·m−1·K−1) |
EMI SE/dB | Reference |
| Graphene/PVDF | 0.27 vol% Graphene | 1.16 ± 0.06 | [31] | |
| AlN/PVDF | 60 vol% AlN | 11.5 | [32] | |
| BN/PVDF | 30 wt% BN | 7.29 | [33] | |
| MXene/PVDF | 5 wt% MXene | 0.363 | [34] | |
| TPU/MPTU | 15 wt% MPTU | 28.35 | [35] | |
| Graphene/PS | 10 wt% Graphene | 18 | [36] | |
| Graphene/PVDF | 10 wt% Graphene | 18.70 | [37] | |
| PG13 | 75 wt% Graphene | 103.9 | 31.07 | This work |
| Note: AIN is aluminum nitride , BN is Boron nitride, MXene is Ti3C2Tx, TPU is thermoplastic polyurethane, MPTU is polyester hot-melt adhesive, PS is polystyrene. | ||||
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