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Scientific Reports volume 14, Article number: 29528 (2024 ) Cite this article copper particle image
This study explores the controlled, continuous production of thin carbon rods between graphite electrodes (continued electrode deposits) during an arc discharge of high voltage alternating current with a frequency of 50 Hz in liquid paraffin, along with in situ doping of the resulting material using a suspension of liquid paraffin and iron powder ( <10 μm). The surface morphology of the obtained carbon rod nanomaterials was characterized using scanning electron microscopy (SEM) coupled with energy dispersive X-ray spectroscopy (EDX), scanning transmission electron microscopy (STEM) with EDX chemical composition analysis, X-ray microtomography (micro-CT), and atomic force microscopy (AFM). The AFM technique in scanning thermal microscopy (SThM) and conductive probe (CP) modes was employed to determine the temperature and electrical conductivity of the obtained nanostructures. Qualitative analysis was conducted using Raman spectroscopy, X-ray powder diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). This simple system for producing thin, stable carbon wires (< 1.2 mm thick) enables efficient and low-cost production and doping of these materials. The high-voltage alternating current (HVAC) arc discharge method for growing controlled, metal-doped electrode deposits presents a new approach to producing inexpensive, porous carbon nanomaterials for various scientific and technological applications.
Modern methods of synthesizing carbon materials allow not only the production of graphene1,2,3, carbon nanotubes4,5,6, and fullerenes7,8,9 but also obtaining structures such as AA’-graphite10,11, carbon nanobuds12,13, carbon nanofoams14,15,16, carbide-derived carbon (CDC)17,18,19, linear acetylenic carbon20,21,22, cyclo[C18]carbon23,24,25, and carbon nano-onions26,27,28,29.
Graphite rods for electrodes with a diameter of 10 mm and a length of 60 mm and a declared purity of 99.99% were purchased from Onyxmet (Poland). Paraffin oil (no. 76235) and iron micropowder (no. 12310) were ordered from Sigma Aldrich (USA).
The carbon rods were produced by HVAC arcing between two graphite electrodes immersed in liquid paraffin. The production system consisted of a glass reactor (500 ml beaker) and a manual system for adjusting the distance between electrodes (Fig. 1a), which was based on a drive screw with M6 metric thread with a pitch of 1 mm, ending with a micrometric knob. The electrode holder was designed so that the electrodes are tilted at an angle of 45 degrees. To create a controllable and continuous arc discharge between the electrodes, an electrical system was used (Fig. 1b), which consisted of a MCP lab electronics autotransformer model M10-522-30 (rated supply voltage 230 V, range 0–250 V, power 3 kW, maximum load current 12 A, frequency 50 Hz) and a high voltage (HV) transformer Samsung SHV-EPT08A. The use of an autotransformer allowed for a smooth setting of the desired initial voltage on the secondary winding of the HV transformer.
(a) Diagram of the mechanical system: (1) Adjustable screw, (2) Graphite electrodes, (3) Vessel with a capacity of 500 ml - crystallizer. (4) A thin nanocarbon rods created in an arc between the electrodes. (b) Schematic of the electrical system. (c) Oscillogram of high voltage AC arc discharge. Subsequent stages of the process: (d) nucleation, (e) an image of a cavitation bubble during continuous discharge, (f) produced wires after the completed process.
A medium (liquid paraffin) and a suspension of liquid paraffin with iron powder were prepared with a gradation of less than 10 μm. The liquid volume was 400 ml. In the case of the iron doping process, 10 g of iron was measured and added while stirring for 5 min (100 rpm, Biosan mixer, MM-1000). In the case of the metal powder process, the suspension was prepared immediately before the planned discharge process, which stopped the sedimentation of the added material. The electrodes were then placed at a 0.7 mm distance from each other. Next, the voltage on the autotransformer was set to 125 V, and the measured voltage at the output of the high-voltage transformer was 1.25 kV. The HV transformer increased the output voltage ten times. A discharge was then initiated between the electrodes. The voltage parameters were set using the Tektronix model TDS2024C oscilloscope and an HV differential probe Tektronix 5200 A. The current measurement on the secondary winding of the HV transformer was performed using a Fluke model 323 clamp meter.
After 240 s discharge, the paraffin became dark and nucleation appeared on both sides of the electrodes (Fig. 1d), preventing further arc discharge. During an arc discharge, a characteristic cavitation bubble also appears (Fig. 1e). The process could be continued after bringing the electrodes closer together by 0.25 mm (manually moving the screw by ¼ turn). As a result, the discharge current parameters (U, I) returned to their initial values. Note that the growing process was very similar to the so-called formation of cathodic deposits during the production of carbon nanomaterials in arc discharge processes46. The voltage-time oscillogram is shown in Fig. 1c, which contains the characteristic waveform for an AC arc discharge (characteristic peaks of ignition and extinction voltage of the electric arc). Before starting the process, the open circuit voltage between the graphite electrodes was 1.25 kV AC. During the process, the maximum amplitude of the voltage between the electrodes decreased to 1.7 kV (2.6 kV peak-to-peak voltage), and the maximum current was set to 3 A. All processes were carried out for 10 min in pure paraffin and paraffin-containing iron powder (initial temperature RT, without temperature stabilization system). Arc processes were repeated many times. Finally, the manufactured products (Fig. 1f) were rinsed with extraction gasoline, dried at room temperature, and then weighed and measured. Table 1 shows the values of the total weight of the obtained rods (nC and nC/Fe), length, and diameter. For example, the measured mass of a nC sample with a length of 70.02 ± 0.27 mm and a diameter of 1.168 ± 0.004 mm was 0.048 ± 0.001 g, while the one of nC/Fe 0.052 ± 0.001 g, with a length of 57.06 ± 0.38 mm and a diameter of 1.199 ± 0.001 mm.
The approximate current density values during the arc discharge process in paraffin were estimated based on the following Eq.
where J is the current density measured in amperes per square meter (A/m²), I is the electric current measured in amperes, S is the cross-sectional area through which the current flows measured in square meters (m²). The diameter value for S in the equation was taken as the diameter of the rod after the formation of nuclei on the surface of the graphite electrode (Fig. 1d), further growth of the rod occurs between the peaks of the formed carbon nuclei. In the case of alternating current, the current (J) is often provided as the root mean square (RMS) value (JRMS), which is related to the peak value (Jmax). Therefore, the peak current (Jmax) was assumed to be 3 A. We calculated the current density for both samples: for nC J= 2.8 × 106 A/m2 and for nC/Fe J= 2.66 × 106 A/m2. These current densities align with the literature data47, which states that maintaining arc discharge requires a current density of at least 106 A/m2. A crucial research issue is the elucidation of the reaction mechanism. A tentative mechanism can be proposed in which the C-H bonds are broken in an electric plasma arc, followed by the recombination of hydrogen atoms into molecular hydrogen. The resulting carbon radicals then recombine and change their hybridization to sp, forming a graphite structure with a high degree of amorphization or disorder. The nucleation of rods and their subsequent growth occurs on the graphite electrodes. However, to establish a consistent mechanism, it will be necessary to identify all discharge products that may be present in the paraffin medium.
Micro-computed tomography (micro-CT) studies were performed using a Rigaku nano3DX scanner (x-ray source: Cu (40 kV, 30 mA), x-ray detector: L1080 (1.1 μm/pixel), field of view (FOV): 3.626 × 2.719 mm, acquisition resolution and binning: 2.2 μm/pixel). Obtained structures were observed using a scanning electron microscope (SEM) Jeol 6010 integrated with a dispersive X-ray spectrometer (EDX) and a scanning transmission electron microscopy (TEM) TALOS F200X X-FEG field emission cathode equipped with 4-inch – column SDD Super X detectors). Raman scattering spectra were recorded in the spectral range of 150 to 3000 cm− 1 at room temperature in the backscattering geometry using the inVia Renishaw micro-Raman system. The near-infrared line of solid-state laser operating at 785 nm was used as the excitation light. The laser beam was tightly focused on the sample surface through a Leica 50× long working distance (LWD) microscope objective with a numerical aperture (NA) equal to 0.5, forming a laser beam with a diameter of about 2 μm. To prevent damage to the sample, the excitation power was set to 1 mW. The inVia Raman spectrometer allowed for recording the Raman spectra with a spatial resolution of about 1 μm. The spectral resolution was 1 cm− 1. X-ray diffraction (XRD) spectra were obtained using an Aeris instrument (Malvern Panalytical). Parameters of the measurement were as follows: wavelength Kα1 (Å) 1.540598, anode material Cu, voltage (kV) 40.0, current (mA) 7.5, filter: lage beta-filter Nickel, thickness (mm) 0.020, scan range 5°-95° with a step size of 0.0217°, and scan mode continuous. XPS spectra were obtained using a Prevac multichamber UHV analytical system (Photoelectron excitation source: VG Scienta SAX 100 X-ray tube with an aluminum anode, equipped with a VG Scienta XM 780 monochromator, emitting radiation with a characteristic line of Al Kα and an energy of 1486.7 eV). The X-ray tube operating parameters were the accelerating voltage U = 13 kV and the emission current Ie=25 mA. The photoelectron energy analyzer was Scienta R4000. Pressure in the analysis chamber was controlled to be not higher than 10− 8 mbar. Basic analyzer parameters for the survey spectrum were as follows: sweeping operation mode, energy range 0-1315 eV, transition energy Ep = 200 eV, and step 500 meV. For high-resolution spectra, these parameters were adjusted to sweeping operation mode, transition energy Ep = 50 eV, and step 50 mV. Surface topography and imaging in the current conduction mode (CP - AFM) and thermal conduction mode (SThm) were performed using the Park Systems NX10 device. The BudgetSensors All-In-One D microbeam was used with a spring constant of 40 N/m (7–160 N/m). The resonance frequency was 350 kHz (200–500 kHz). The measurement mode used was non-contact (scan resolution: 512 × 512, scanning speed: 0.3–0.5 Hz, measurement temperature: ambient conditions). For CP - AFM mode a NANOSENSORS PPP-CONTSCPt microbeam was used (spring constant 0.2 N/m (0.01–1.87 N/m), resonance frequency 25 kHz (1–57 kHz), scan resolution 512 × 512, scanning speed 0.3–0.5 Hz, measurement temperature RT (approx. 22 °C), microbeam voltage 2 V). SThM mode was used for the preliminary determination of thermal conductivity. A KNT-SThM-2an microbeam with a spring constant of 0.2 N/m (0.01–1.87 N/m) was used (maximum resonance frequency − 205 kHz (1–57 kHz) scan resolution: 512 × 512, scanning speed: 0.3–0.5 Hz, measurement temperature: RT (approx. 22 C), and SThM mode: temperature contrast mode (TCM)).
Figure 2 shows the surface morphology imaged using SEM-EDX and micro-CT. Additionally, we utilized an Amira software (Thermo Fisher Scientific) to visualize the internal structure of the produced rods in 3D, providing a comprehensive representation of their shape and morphology (Fig. 2c and f). The produced carbon wires have a surface morphology of well-packed cauliflower-shaped complex globules, resembling the surface morphology of electrode deposits in the processes of producing carbon nanotubes using the arc discharge technique48,49,50. The nC sample (Fig. 2a) shows much greater porosity than the nC/Fe sample (Fig. 2d). Cross-section of the micro-CT image shows structural differences between nC and nC/Fe samples. The sample produced in pure paraffin has an elongated shape (Fig. 2b), while the nC/Fe sample (Fig. 2e) is more rounded. Around the surface, small structures show x-ray deflection, suggesting the presence of metallic iron or its compounds. Thus, SEM - EDS analysis was performed on the nC/Fe sample to confirm the presence of the Fe element. On the rod side surface (Fig. 2g) and cross-section (Fig. 2h), unevenly distributed nebula-shaped oval iron structures are visible. Based on SEM - EDX chemical maps, it can be concluded that iron is present both on the material’s surface and inside but is distributed unevenly in the volume of the deposited rods. Figure 2c and f show a 3D simulation of the fabricated materials. These images show that the produced carbon material is porous.
SEM image of nC (a) and nC/Fe rods (d). Micro CT cross section image of nC (b) and nC/Fe (e). 3D visualization of nC (c) and nC/Fe (f). Elemental mapping (EDS) of nC/Fe from the side (g) and cross–section of the rod (h).
Figure 3 (a-f) shows TEM images of the obtained samples. The electric arc in the discharge zone can have a temperature exceeding 2500 K, which is the temperature that allows the ablation process of the aliphatic material to begin. Analyzing TEM images makes it possible to distinguish emerging structures in the amorphous carbon graphene sheet matrix for nC and nC/Fe wires, characterized by a width of several nanometers (Fig. 3c and f). In the nC sample, carbon structures resemble carbon nanotubes with a conical, sharp end. These structures are very similar to carbon nanohorns51 and have pretty large diameters, in the range of 65–85 nm, distributed unevenly in the material. It can be assumed that the paraffin undergoes decomposition (carbonization) in the arc process, and then, partial, uncontrolled graphitization occurs. In the nC/Fe sample, the graphene sheets appearing in the carbon matrix are narrower and wider. Figure 3e shows oval particles with sizes ranging from 72 to 132 nm. Photos in Fig. 3h taken using the STEM - EDX chemical mapping technique confirm the presence of iron and oxygen in the nC/Fe sample. In the nC wire , an uneven distribution of oxygen in the obtained carbon material can be observed (Fig. 3g).
TEM images of the nC (a-c) and nC/Fe (d-f) samples. STEM -EDX image of elemental mapping for nC (g) and nC/Fe (h).
The formation of graphene sheets, initially observed through TEM analysis, is further confirmed by Raman spectroscopy. Figure 4 (a-c) presents the results of Raman spectroscopy, a powerful technique for analyzing and identifying carbon materials. The Raman spectra of both nC and nC/Fe samples exhibit distinctive features that provide valuable insights into their structural characteristics. These spectra were analyzed compared to that of a graphite electrode, which serves as a reference for highly ordered carbon structures in Fig. 4a. A prominent feature in both spectra is the intense D (disordered graphitic) band, which is typically of low intensity in pristine graphite Fig. 4a. The D-band position is observed at 1308 cm− 1 for the nC sample and at 1321 cm− 1 for the nC/Fe sample. This band is indicative of structural defects or disorder in the graphitic lattice. The G (graphitic) band, characteristic of sp2 carbon networks, is also present in both spectra, albeit with lower intensity than the D band52. The G band appears at 1597 cm− 1 for the nC sample and at 1601 cm− 1 for the nC/Fe sample. This band is attributed to the in-plane stretching mode of C-C bonds in graphitic structures.
Characterization of the nC and nC/Fe wires: (a-c) Raman spectra, (d) XRD patterns, (inset in plot (d) shows XRD diffractogram of Fe powder) and (e-f) high– resolution XPS spectra of nC and nC/Fe sample.
Notably, the nC/Fe sample spectrum displays a well-defined peak around 2625 cm− 1, corresponding to the 2D mode. Deconvolution of this 2D mode (Fig. 4b) reveals two components: a more intense and uniform 2D2 mode and a less intense 2D1 mode. This feature is often associated with the number of graphene layers and the stacking order in graphitic materials. The intensity ratio of the D and G bands (ID/IG) provides crucial information about the degree of structural disorder. The calculated ID/IG ratios are 1.21 for nC and 1.36 for nC/Fe material, significantly higher than the 0.33 observed for the graphite electrode material. These elevated ratios suggest a high degree of structural defects and disorder in the synthesized materials compared to highly ordered graphite.
Interestingly, the nC/Fe sample spectrum shows a low-intensity peak around 248 cm− 1, which may be attributed to the radial breathing mode (RBM) of single-walled carbon nanotubes (SWCNTs). The presence of RBM peaks in CVD-synthesized multi-walled carbon nanotubes (MWCNTs) has been previously reported53, suggesting the possibility of SWCNT formation within the complex structure of our material. It’s worth noting that the Raman spectrum of nC/Fe does not exhibit peaks characteristic of iron oxides. This absence may indicate limited oxygen access during the synthesis of carbon wires, resulting in minimal oxidation of the added iron54. The Raman spectroscopy results offer valuable insights into the structural characteristics of our synthesized materials. They reveal a complex carbon nanostructure with a high degree of disorder and potential presence of various carbon allotropes. This finding suggests that the materials are amorphous, with a high degree of disorder and a lack of long-range order.
Figure 4d shows the XRD patterns of nC and nC/Fe samples. In both cases, the pattern is displayed as an intense, sharp diffraction peak around 2θ = 26° and low-intensity diffraction peaks around 42°, 53° and 78°, which are assigned to (002), (100), (004), and (110) diffraction patterns of typical graphite, respectively. The nC/Fe spectrum shows a significant decrease in the intensity of the peak corresponding to the (100) plane and the disappearance of the peaks corresponding to the (004) and (110) planes. Based on the Bragg Eq. (2dsinθ = λ) and the position of (002) peak, the interlayer distance of graphitic carbons is calculated to be 0.342 nm for nC rods and 0.341 nm for nC/Fe rods, which corresponds to the HRTEM results. Iron peaks appear around 2θ = 44°, 65° and 82° in the spectrum of the doped carbon rod. XRD test was also performed on Fe powder, which was a component of the suspension in paraffin, and the results were compared with the diffraction peaks included in the JCPDS file 65-4899. The diffraction angles at 2θ = 44.66°, 65.01, and 82.31° are related to (110), (200), and (211) planes of pure iron (α-Fe), respectively. This pattern shows that a strong diffraction peak corresponds to the (110) plane.
The crystallite size (Lc) of the (002) plane was calculated using the Scherrer equation55:
where b is the peak width at half maximum height (HWHM), θ is the Bragg angle, λ is the X-ray wavelength, k is the Scherrer constant and for the (002) peak is 0.9, while La is the crystalline width in the (100) planes and for the (100) peak is 1.84. In the XRD patterns of this study, the (100) peak is clear only for nC/Fe sample. Therefore, the La crystallite size was determined based on the integrated area ratio between the D and G peak intensities, termed ID and IG, respectively, using the following equation56:
where λ is the laser wavelength in nm. The degree of graphitization (ḡ) for samples nC and nC/Fe was also estimated from the interplanar spacing under the assumption that d(002) = 0.356 nm for ḡ = 0 and d(002) = 0.3354 nm for ḡ =157.
A summary of measured microstructural characteristics of the nC and nC/Fe samples is presented in Table 2. The degree of graphitization was 67.86% for the nC sample and 68% for the nC/Fe sample.
Figure 4 shows the high-resolution C 1s XPS spectra (Fig. 4e for the nC sample and Fig. 4f for nC/Fe), which are decomposed into several Gaussian peaks. In both spectra, peaks at 248.5, 285.1 eV and a very low noise characteristic peak at 286.7 eV can be distinguished. In the literature, peaks at 284.5 ± 0.2 and 285.1 ± 0.2 eV are assigned to the sp2 and sp3 hybridization of the C-C or C-H bonds, respectively. The peak around 286.7 eV corresponds to the associated C-O. It can thus be concluded that the produced carbon structures are additionally oxidized. Combined with Raman spectra, the XPS results show that sp2 bonds dominate in both samples.
Figure 5 shows the AFM images of the prepared nC and nC/Fe carbon wires. The nC sample has an average height of 312.2 nm. The roughness coefficient Rq is 81.32 ± 5.61 nm, and the Ra parameter is 66.29 ± 7.41 nm. (Ra is the arithmetic average of the absolute values of the profile heights over the evaluation length, and Rq is the root mean square average of the profile heights over the evaluation length). The nC/Fe sample has an average height of 325.6 nm. The roughness coefficients are 94.24 ± 7.98 nm for the Rq parameter and 73.86 ± 12.17 nm for the Ra parameter. Figure 6 (a-b) shows CP–AFM imaging, which is commonly used to characterize the current distribution (e.g., local conductivity) of various types of samples such as insulators, semiconductors, and conductors. In this technique, a bias voltage is applied to the sample during scanning, and the tip measures the current flow. The average current conductivity for the nC sample (Fig. 6a) is 44.5 pA. The median current conductivity is 37.2 pA. The conductive area covers 24.5% of the surface. The average current conductivity for the nC/Fe sample (Fig. 6b) is 33.1 pA, while the median current conductivity is 27.1 pA. The surface coverage with a conductive area is 60.35%. The SThm mode of AFM allows measuring the thermal conductivity of the surface of the tested material. The lever, made of two types of metals with different thermal conductivities, reacts with different deflections to changes in the thermal conductivity of the sample. The measurement results in an image of the topography of the sample. The temperature conductivity study showed no changes in conductivity for either of the two samples tested (Fig. 6c and d), and the maps obtained are homogeneous. Therefore, it can be concluded that the temperature conductivity of the samples is the same over the entire surface.
AFM 3D image of nC (a) and nC/Fe (d) wires. AFM image of nC (b) and nC/Fe (e) and corresponding surface roughness profiles extracted from AFM images for nC (c) and nC/Fe (f).
CP-AFM current conductivity map and topography of nC (a) and nC/Fe (b) rods. SThm-AFM thermal conductivity map and topography of the same nC (c) and nC/Fe (d) rods.
Until now, electrode deposits (usually cathodic ones, which accompany DC arc discharge processes) have not been of much interest to researchers. They were rather treated as process waste. This situation may now change due to the ability to control the growth and composition of these structures. Here, we have shown that it is possible to create and control the growth of carbon rods with a diameter of approximately 1.2 mm. It has also been demonstrated that this method can produce a composite carbon/graphite material by simply adding metal microparticles to the precursor medium during the discharge process. Introducing iron directly into the carbon structure during synthesis enables the creation of materials with unique morphological and chemical properties. Deposited carbon structures contain graphene sheets randomly arranged in an amorphous carbon matrix of size Lc= 9.35 nm for nC, and Lc=7.56 nm for nC/Fe, characterized by significant shape degradation (folded, scrolled, bundled). During an arc discharge oval nanometric metal particles are formed from a suspension of Fe micropowder and embedded in the carbon material.
Interestingly, XPS tests did not reveal peaks in the 705–730 eV region associated with iron oxides, and both Raman spectra and XRD analysis confirmed the absence of oxygen-iron bonds. The presence of iron was verified through SEM-EDX and STEM-EDX chemical mapping, with XRD analysis showing consistency. Notably, the Fe-doped sample (nC/Fe) demonstrated a significant increase in current conductivity, as evidenced by CP-AFM measurements.
Future research should focus on understanding the impact of temperature stabilization on the medium and developing methods to achieve a higher degree of doping and graphitization, which currently stands at around 70%. A significant challenge is ensuring the uniform distribution of metal powders within the suspension as they enter the arc discharge zone, potentially requiring more advanced mixing techniques. One potential approach to improving doping control is the use of organometallic compounds instead of metal powders. Since in the light of current research, the alkane-immersed discharge arc produces graphitized wires, it would be interesting to investigate its discharge in aromatic precursor solvents. Additionally, an important aspect of future research will be to elucidate the mechanism of rod formation by identifying all the arc discharge products. Addressing these challenges, including refining synthesis parameters and enhancing process stability, could lead to the production of higher-quality carbon materials with superior electrical and mechanical properties.
The datasets used and/or analyzed during the current study available from the corresponding author on reasonable request.
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Institute of Nanotechnology and Nanobiology, Jacob of Paradies University, Chopina 52, Gorzow Wielkopolski, 66-400, Poland
Krzysztof Jankowski, Agnes Ostafin, Mikołaj Tomasik & Szymon Całuch
Department of Mechanical Science and Engineering, University of Illinois at Urbana, 1206 West Green Street, Champaign, Urbana, IL, 61801, USA
Iwona Jasiuk & Christian Bonney
Centre of Molecular and Macromolecular Studies, Polish Academy of Sciences, Sienkiewicza 112, Lodz, 90 -363, Poland
Paweł Uznański & Romuald Brzozowski
Faculty of Materials Engineering and Technical Physics, Poznan Universityof Technology, Piotrowo 3A, Poznan, 61-138, Poland
Department of Civil and Environmental Engineering, University of Illinois at Urbana, 205 North Mathews Avenue, Champaign, Urbana, IL, 61801, USA
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KJ, IJ, PU, AO, RB - wrote the main text of the article, MS, CB, MT, MM - prepared and processed data from Raman study, AFM and micro-CT, SC - performed the synthesis of thin rods.All authors reviewed the manuscript.
The authors declare no competing interests.
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Jankowski, K., Jasiuk, I., Uznański, P. et al. In situ Fe-doped thin carbon wires via AC high voltage arc discharge. Sci Rep 14, 29528 (2024). https://doi.org/10.1038/s41598-024-81096-5
DOI: https://doi.org/10.1038/s41598-024-81096-5
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