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Cellulose nanofibers (CNF) can be obtained from natural sources such as plant and wood fibers. CNF-reinforced thermoplastic resin composites have a number of properties, including excellent mechanical strength. Since the mechanical properties of CNF-reinforced composites are affected by the amount of fiber added, it is important to determine the concentration of CNF filler in the matrix after injection molding or extrusion molding. We confirmed a good linear relationship between CNF concentration and terahertz absorption. We could discern differences in CNF concentrations at 1% points using terahertz time domain spectroscopy. In addition, we evaluated the mechanical properties of CNF nanocomposites using terahertz information.
Cellulose nanofibers (CNFs) are typically less than 100 nm in diameter and are derived from natural sources such as plant and wood fibers1,2. CNFs have high mechanical strength3, high optical transparency4,5,6, large surface area, and low thermal expansion coefficient7,8. Therefore, they are expected to be used as sustainable and high performance materials in a variety of applications, including electronic materials9, medical materials10 and building materials11. Composites reinforced with UNV are light and strong. Therefore, CNF-reinforced composites can help improve the fuel efficiency of vehicles due to their light weight.
To achieve high performance, uniform distribution of CNFs in hydrophobic polymer matrices such as polypropylene (PP) is important. Therefore, there is a need for non-destructive testing of composites reinforced with CNF. Non-destructive testing of polymer composites has been reported12,13,14,15,16. In addition, non-destructive testing of CNF-reinforced composites based on X-ray computed tomography (CT) has been reported 17 . However, it is difficult to distinguish CNFs from matrices due to the low image contrast. Fluorescent labeling analysis18 and infrared analysis19 provide clear visualization of CNFs and templates. However, we can only get superficial information. Therefore, these methods require cutting (destructive testing) to obtain internal information. Therefore, we offer non-destructive testing based on terahertz (THz) technology. Terahertz waves are electromagnetic waves with frequencies ranging from 0.1 to 10 terahertz. Terahertz waves are transparent to materials. In particular, polymer and wood materials are transparent to terahertz waves. The evaluation of the orientation of liquid crystal polymers21 and the measurement of the deformation of elastomers22,23 using the terahertz method have been reported. In addition, terahertz detection of wood damage caused by insects and fungal infections in wood has been demonstrated24,25.
We propose to use the non-destructive testing method to obtain the mechanical properties of CNF-reinforced composites using terahertz technology. In this study, we investigate the terahertz spectra of CNF-reinforced composites (CNF/PP) and demonstrate the use of terahertz information to estimate the concentration of CNF.
Since the samples were prepared by injection molding, they may be affected by polarization. On fig. 1 shows the relationship between the polarization of the terahertz wave and the orientation of the sample. To confirm the polarization dependence of CNFs, their optical properties were measured depending on the vertical (Fig. 1a) and horizontal polarization (Fig. 1b). Typically, compatibilizers are used to uniformly disperse CNFs in a matrix. However, the effect of compatibilizers on THz measurements has not been studied. Transport measurements are difficult if the terahertz absorption of the compatibilizer is high. In addition, the THz optical properties (refractive index and absorption coefficient) can be affected by the concentration of the compatibilizer. In addition, there are homopolymerized polypropylene and block polypropylene matrices for CNF composites. Homo-PP is just a polypropylene homopolymer with excellent stiffness and heat resistance. Block polypropylene, also known as impact copolymer, has better impact resistance than homopolymer polypropylene. In addition to homopolymerized PP, block PP also contains components of an ethylene-propylene copolymer, and the amorphous phase obtained from the copolymer plays a similar role to rubber in shock absorption. The terahertz spectra were not compared. Therefore, we first estimated the THz spectrum of the OP, including the compatibilizer. In addition, we compared the terahertz spectra of homopolypropylene and block polypropylene.
Schematic diagram of transmission measurement of CNF-reinforced composites. (a) vertical polarization, (b) horizontal polarization.
Samples of block PP were prepared using maleic anhydride polypropylene (MAPP) as a compatibilizer (Umex, Sanyo Chemical Industries, Ltd.). On fig. 2a,b shows the THz refractive index obtained for vertical and horizontal polarizations, respectively. On fig. 2c,d show the THz absorption coefficients obtained for vertical and horizontal polarizations, respectively. As shown in fig. 2a–2d, no significant difference was observed between the terahertz optical properties (refractive index and absorption coefficient) for vertical and horizontal polarizations. In addition, compatibilizers have little effect on the results of THz absorption.
Optical properties of several PPs with different compatibilizer concentrations: (a) refractive index obtained in the vertical direction, (b) refractive index obtained in the horizontal direction, (c) absorption coefficient obtained in the vertical direction, and (d) absorption coefficient obtained in the horizontal direction.
We subsequently measured pure block-PP and pure homo-PP. On fig. Figures 3a and 3b show the THz refractive indices of pure bulk PP and pure homogeneous PP, obtained for vertical and horizontal polarizations, respectively. The refractive index of block PP and homo PP is slightly different. On fig. Figures 3c and 3d show the THz absorption coefficients of pure block PP and pure homo-PP obtained for vertical and horizontal polarizations, respectively. No difference was observed between the absorption coefficients of block PP and homo-PP.
(a) block PP refractive index, (b) homo PP refractive index, (c) block PP absorption coefficient, (d) homo PP absorption coefficient.
In addition, we evaluated composites reinforced with CNF. In THz measurements of CNF-reinforced composites, it is necessary to confirm the CNF dispersion in the composites. Therefore, we first evaluated the CNF dispersion in composites using infrared imaging before measuring the mechanical and terahertz optical properties. Prepare cross sections of samples using a microtome. Infrared images were acquired using an Attenuated Total Reflection (ATR) imaging system (Frontier-Spotlight400, resolution 8 cm-1, pixel size 1.56 µm, accumulation 2 times/pixel, measurement area 200 × 200 µm, PerkinElmer). Based on the method proposed by Wang et al.17,26, each pixel displays a value obtained by dividing the area of ​​the 1050 cm-1 peak from cellulose by the area of ​​the 1380 cm-1 peak from polypropylene. Figure 4 shows images for visualizing the distribution of CNF in PP calculated from the combined absorption coefficient of CNF and PP. We noticed that there were several places where CNFs were highly aggregated. In addition, the coefficient of variation (CV) was calculated by applying averaging filters with different window sizes. On fig. 6 shows the relationship between the average filter window size and CV.
Two-dimensional distribution of CNF in PP, calculated using the integral absorption coefficient of CNF to PP: (a) Block-PP/1 wt.% CNF, (b) block-PP/5 wt.% CNF, (c) block-PP/10 wt% CNF, (d) block-PP/20 wt% CNF, (e) homo-PP/1 wt% CNF, (f) homo-PP/5 wt% CNF, (g) homo -PP/10 wt. %% CNF, (h) HomoPP/20 wt% CNF (see Supplementary Information).
Although comparison between different concentrations is inappropriate, as shown in Fig. 5, we observed that CNFs in block PP and homo-PP exhibited close dispersion. For all concentrations, except for 1 wt% CNF, CV values ​​were less than 1.0 with a gentle gradient slope. Therefore, they are considered highly dispersed. In general, CV values ​​tend to be higher for small window sizes at low concentrations.
The relationship between the average filter window size and the dispersion coefficient of the integral absorption coefficient: (a) Block-PP/CNF, (b) Homo-PP/CNF.
The terahertz optical properties of composites reinforced with CNFs have been obtained. On fig. 6 shows the optical properties of several PP/CNF composites with various CNF concentrations. As shown in fig. 6a and 6b, in general, the terahertz refractive index of block PP and homo-PP increases with increasing CNF concentration. However, it was difficult to distinguish between samples with 0 and 1 wt.% due to overlap. In addition to the refractive index, we also confirmed that the terahertz absorption coefficient of bulk PP and homo-PP increases with increasing CNF concentration. In addition, we can distinguish between samples with 0 and 1 wt.% on the results of the absorption coefficient, regardless of the direction of polarization.
Optical properties of several PP/CNF composites with different CNF concentrations: (a) refractive index of block-PP/CNF, (b) refractive index of homo-PP/CNF, (c) absorption coefficient of block-PP/CNF, (d) absorption coefficient homo-PP/UNV.
We confirmed a linear relationship between THz absorption and CNF concentration. The relationship between the CNF concentration and the THz absorption coefficient is shown in Fig.7. The block-PP and homo-PP results showed a good linear relationship between THz absorption and CNF concentration. The reason for this good linearity can be explained as follows. The diameter of the UNV fiber is much smaller than that of the terahertz wavelength range. Therefore, there is practically no scattering of terahertz waves in the sample. For samples that do not scatter, absorption and concentration have the following relationship (Beer-Lambert law)27.
where A, ε, l, and c are absorbance, molar absorptivity, effective path length of light through the sample matrix, and concentration, respectively. If ε and l are constant, absorption is proportional to concentration.
Relationship between absorption in THz and CNF concentration and linear fit obtained by the least squares method: (a) Block-PP (1 THz), (b) Block-PP (2 THz), (c) Homo-PP (1 THz), (d) Homo-PP (2 THz). Solid line: linear least squares fit.
The mechanical properties of PP/CNF composites were obtained at various CNF concentrations. For tensile strength, bending strength, and bending modulus, the number of samples was 5 (N = 5). For Charpy impact strength, the sample size is 10 (N = 10). These values ​​are in accordance with the destructive test standards (JIS: Japanese Industrial Standards) for measuring mechanical strength. On fig. Figure 8 shows the relationship between mechanical properties and CNF concentration, including estimated values, where plots were derived from the 1 THz calibration curve shown in Figure 8. 7a, p. The curves were plotted based on the relationship between concentrations (0% wt., 1% wt., 5% wt., 10% wt. and 20% wt.) and mechanical properties. The scatter points are plotted on the graph of calculated concentrations versus mechanical properties at 0% wt., 1% wt., 5% wt., 10% wt. and 20% wt.
Mechanical properties of block-PP (solid line) and homo-PP (dashed line) as a function of CNF concentration, CNF concentration in block-PP estimated from the THz absorption coefficient obtained from vertical polarization (triangles), CNF concentration in block-PP PP The CNF concentration is estimated from the THz absorption coefficient obtained from the horizontal polarization (circles), the CNF concentration in the related PP is estimated from the THz absorption coefficient obtained from the vertical polarization (diamonds), the CNF concentration in the related PP is estimated from the THz obtained from the horizontal polarization Estimates absorption coefficient (squares): (a) tensile strength, (b) flexural strength, (c) flexural modulus, (d) Charpy impact strength.
In general, as shown in Fig. 8, the mechanical properties of block polypropylene composites are better than homopolymer polypropylene composites. The impact strength of a PP block according to Charpy decreases with an increase in the concentration of CNF. In the case of block PP, when PP and a CNF-containing masterbatch (MB) were mixed to form a composite, the CNF formed entanglements with the PP chains, however, some PP chains entangled with the copolymer. In addition, dispersion is suppressed. As a result, the impact-absorbing copolymer is inhibited by insufficiently dispersed CNFs, resulting in reduced impact resistance. In the case of homopolymer PP, the CNF and PP are well dispersed and the network structure of the CNF is thought to be responsible for cushioning.
In addition, calculated CNF concentration values ​​are plotted on curves showing the relationship between mechanical properties and actual CNF concentration. These results were found to be independent of terahertz polarization. Thus, we can non-destructively investigate the mechanical properties of CNF-reinforced composites, regardless of terahertz polarization, using terahertz measurements.
CNF-reinforced thermoplastic resin composites have a number of properties, including excellent mechanical strength. The mechanical properties of CNF-reinforced composites are affected by the amount of added fiber. We propose to apply the method of non-destructive testing using terahertz information to obtain the mechanical properties of composites reinforced with CNF. We have observed that compatibilizers commonly added to CNF composites do not affect THz measurements. We can use the absorption coefficient in the terahertz range for non-destructive evaluation of the mechanical properties of CNF-reinforced composites, regardless of polarization in the terahertz range. In addition, this method is applicable to UNV block-PP (UNV/block-PP) and UNV homo-PP (UNV/homo-PP) composites. In this study, composite CNF samples with good dispersion were prepared. However, depending on the manufacturing conditions, CNFs can be less well dispersed in composites. As a result, the mechanical properties of CNF composites deteriorated due to poor dispersion. Terahertz imaging28 can be used to non-destructively obtain the CNF distribution. However, the information in the depth direction is summarized and averaged. THz tomography24 for 3D reconstruction of internal structures can confirm the depth distribution. Thus, terahertz imaging and terahertz tomography provide detailed information with which we can investigate the degradation of mechanical properties caused by CNF inhomogeneity. In the future, we plan to use terahertz imaging and terahertz tomography for CNF-reinforced composites.
The THz-TDS measurement system is based on a femtosecond laser (room temperature 25 °C, humidity 20%). The femtosecond laser beam is split into a pump beam and a probe beam using a beam splitter (BR) to generate and detect terahertz waves, respectively. The pump beam is focused on the emitter (photoresistive antenna). The generated terahertz beam is focused on the sample site. The waist of a focused terahertz beam is approximately 1.5 mm (FWHM). The terahertz beam then passes through the sample and is collimated. The collimated beam reaches the receiver (photoconductive antenna). In the THz-TDS measurement analysis method, the received terahertz electric field of the reference signal and signal sample in the time domain is converted into the electric field of the complex frequency domain (respectively Eref(ω) and Esam(ω)), through a fast Fourier transform (FFT). Complex transfer function T(ω) can be expressed using the following equation 29
where A is the ratio of the amplitudes of the reference and reference signals, and φ is the phase difference between the reference and reference signals. Then the refractive index n(ω) and the absorption coefficient α(ω) can be calculated using the following equations:
Datasets generated and/or analyzed during the current study are available from the respective authors upon reasonable request.
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